A method for synthesizing sucralose by enzymatic catalysis, relating to the technical field of sucralose production. The method comprises the following steps: S1, mixing sucrose with DMF, heating to dissolve, maintaining the heat, and then adding water and mixing uniformly to obtain a dissolved sugar solution; S2, cooling and concentrating the dissolved sugar solution to obtain a sugar solution; S3, sequentially adding trichloroethane and thionyl chloride into the sugar solution for a chlorination reaction to obtain a chlorinated solution; and S4, adding dehalogenase into the chlorinated solution for an orienting reaction for selective dehalogenation to obtain sucralose, wherein the dehalogenase is haloalkane dehalogenase EC 3.8.1.5. By means of the high regioselective and high stereoselective catalytic properties of dehalogenase, selective dehalogenation is carried out to directly obtain sucralose; the synthesis conditions are mild; the synthesis steps of sucralose are simplified; the production efficiency is greatly improved compared with that of a monoester method; the utilization rate of raw materials is increased; and the overall generation of waste gas, waste water, and waste residue is reduced.
Provided is a method for purifying sucralose-6-acetate, including: preparation: providing a saturated solution of crude sucralose-6-acetate in ethyl acetate that is heated to a predetermined temperature; gradient crystallization: subjecting the saturated solution to multiple cooling crystallization and filtration, and collecting crude sucralose-6-acetate obtained after the multiple cooling crystallization and filtration, where during each cooling crystallization process, a low-polarity solvent is added dropwise to the saturated solution to reduce a polarity of the saturated solution during crystallization step by step; and purification: subjecting a collected crude sucralose-6-acetate to recrystallization for purification by using a mixed solution of ethyl acetate and the low-polarity solvent to obtain fine sucralose-6-acetate of high purity.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
The present invention provides a method for treating crude sugar in a chlorination neutralization solution of sucralose-6-ester, and relates to the technical field of sucralose production. The present invention recovers trichloromethane firstly and then recovers DMF, thereby significantly reducing the content of impurities in an obtained concentrated drying liquid, and improving the yield and purity of the obtained crude sugar. The present invention regulates the pH value of the system to 6 to 9 by using weak-base ammonia water, thereby avoiding the generation of sucralose by alkaline hydrolysis of sucralose-6-ester due to too strong alkalinity, and improving the yield and purity of the crude sugar. Moreover, the method provided by the present invention does not need to consume a large amount of acid, hydrogen peroxide, an organic solvent (an oxidation reaction stage) and heat energy (thermal extraction for multiple times), and the treatment costs of the chlorination neutralization solution are low. In addition, the treatment method provided by the present invention can improve the conversion rate and daily capacity of sucralose-6-ester in the chlorination neutralization solution, and reduce the generation amount of wastewater and waste activated carbon, the three wastes are few, the energy consumption is low, and the production costs are low.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
4.
TREATMENT METHOD FOR CHLORINATION NEUTRALIZATION LIQUID OF SUCRALOSE-6-ESTER
The present invention comprises: first recovering trichloroethane and then recovering DMF, so as to remarkably reduce the impurity content of an obtained concentrated dry liquid, such that the yield and purity of an obtained sucralose-6-ester crude product are improved. The present invention uses a weak alkali, ammonium hydroxide, to adjust the pH value of the system to 6-9, thereby preventing excessively strong alkalinity causing sucralose-6-ester alkaline hydrolysis to generate sucralose, and thus improving the yield and purity of the sucralose-6-ester crude product. Besides, the method provided by the present invention does not need consuming a large amount of acid, hydrogen peroxide, organic solvent (for an oxidation reaction step) and heat energy (for multiple times of hot extraction), thereby achieving a low treatment cost for chlorination neutralization liquid. In addition, the treatment method provided by the present invention can improve the conversion rate and daily production capacity of sucralose-6-ester in the chlorination neutralization liquid and reduce the generation amount of wastewater and waste activated charcoal, thereby producing less waste water, waste gas and solid waste and achieving low energy consumption and low production cost.
C07C 233/03 - Amides d'acides carboxyliques ayant des atomes de carbone de groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone acycliques ayant les atomes d'azote des groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone de radicaux hydrocarbonés non substitués avec des atomes de carbone de groupes carboxamides liés à des atomes d'hydrogène
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07C 273/18 - Préparation d'urée ou de ses dérivés, c.-à-d. de composés contenant l'un des groupes les atomes d'azote ne faisant pas partie de groupes nitro ou nitroso d'urées substituées
C07C 275/06 - Dérivés d'urée, c.-à-d. composés contenant l'un des groupes les atomes d'azote ne faisant pas partie de groupes nitro ou nitroso ayant des atomes d'azote de groupes urée liés à des atomes de carbone acycliques d'un squelette carboné acyclique et saturé
5.
TREATMENT METHOD FOR DICHLOROMETHANE IN ACESULFAME PRODUCTION
The present invention relates to the technical field of acesulfame production, and provides a treatment method for dichloromethane in acesulfame production. In the present invention, firstly, the dichloromethane crude product is layered to remove most of water, and then rectification is carried out through a dividing-wall column by using the characteristic that different components in a dichloromethane phase have different boiling points, thereby achieving the purposes of removing impurities at the bottom of the column, dehydrating at the top of the column, and extracting a finished product in the column; a liquid dichloromethane finished product can be obtained by directly carrying out rectification using the dividing-wall column and then carrying out condensation by means of a plate heat exchanger, so that two processes of pre-evaporation impurity removal and dehydration are omitted, the process is simple, steam energy consumption and chilled brine load are reduced, and energy consumption is significantly reduced. Moreover, according to the treatment method of the present invention, the whole process can be continuously and automatically carried out, a lot of labor and equipment input are saved, and costs are reduced while improving a field operation environment. In addition, the treatment method provided by the present invention does not require the additional use of potassium hydroxide and hydrogen peroxide reagents, thereby greatly reducing the recovery treatment cost of dichloromethane.
A preparation method for a psicose crystal, comprising the following steps: performing one-effect evaporation and concentration on a psicose solution to obtain a one-effect concentrated sugar solution; performing two-effect evaporation and concentration on the one-effect concentrated sugar solution by using the heat released by the one-effect evaporation and concentration to obtain a two-effect concentrated sugar solution; and cooling the two-effect concentrated sugar solution to 40-50°C, mixing same with a psicose seed crystal and the lower alcohol, and performing cooling crystallization to obtain the psicose crystal, the cooling crystallization time being less than or equal to 30 h. The psicose seed crystal and the lower alcohol are added, and the cooling crystallization manner is used, so that the crystallization time is greatly shortened, the crystallization speed is high, the crystallization period is short, the yield is high, the particles and the crystal forms of the crystal are smoother and flatter, the granularity is small, the uniformity is good, and the operation is simple; and a double-effect evaporation system is used for concentration, thereby achieving low energy consumption.
A preparation method for sucralose, pertaining to the technical field of fine chemical engineering. The preparation method comprises the following steps: mixing sucrose, N,N-dimethylformamide, trichloroethane, and thionyl chloride, and carrying out a chlorination reaction to obtain a chlorination product liquid; making the chlorination product liquid alkaline, and carrying out a decomposition reaction to obtain tetrachlorosucrose; and mixing the tetrachlorosucrose with water and an alkaline hydrolysis agent, and carrying out an alkaline hydrolysis reaction to obtain sucralose. The method does not involve a traditional method that requires hydroxyl protection at locant 6 of sucrose, but directly uses sucrose as a starting material for chlorination to prepare tetrachlorosucrose. Since the chlorine atom group at locant 6 of tetrachlorosucrose is more active than the other groups, dechlorination can be carried out at locant 6 under the action of the alkaline hydrolysis agent to finally obtain sucralose. The method has a short process and a high sucralose yield.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
The present invention relates to the technical field of fermentation, and provides a method for producing psicose by fermentation and isomerization of bacillus subtilis. According to the method of the present invention, fermentation parameters are strictly controlled, and catalytic reaction is performed by using recombinant bacillus subtilis obtained by fermentation as enzyme liquid, so that the conversion rate of psicose in a system is improved, the problems of low enzyme catalytic reaction efficiency and low yield are solved, and the method is simple to operate and environment-friendly.
C12N 15/75 - Vecteurs ou systèmes d'expression spécialement adaptés aux hôtes procaryotes autres que E. coli, p. ex. Lactobacillus, Micromonospora pour Bacillus
C12N 1/21 - BactériesLeurs milieux de culture modifiés par l'introduction de matériel génétique étranger
Provided in the present invention is a method for preparing a sucralose crude product by using a sucralose-6-acetate crystallization mother liquor. In the present invention, by using an alkali metal hydroxide for alkaline hydrolysis, sucralose-6-acetate can be subjected to alkaline hydrolysis, thereby converting sucralose-6-acetate, sucralose diester and tetrachlorosaccharose-6-acetate, which remain in the crystallization mother liquor, into sucralose, such that the yield of sucralose is significantly improved; water-soluble impurities and fat-soluble impurities in a system can be effectively separated by means of a method of mutual extraction-back extraction-recycling of an ethyl-acetate-water double-solvent system, such that sufficient crystallization of sucralose in ethyl acetate is achieved, thereby improving the yield of scattered sucralose, and a step of removing impurities by oxidizing with an oxidizing agent can also be avoided, thereby simplifying a preparation step of sucralose; and by recycling a sixth water phase and a seventh water phase, sucralose is efficiently and stably prepared from the sucralose-6-acetate crystallization mother liquor, and the yield of sucralose is high.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
The present invention provides a preparation method for a sucralose refined product, and relates to the technical field of fine chemical engineering. In the present invention, by means of subjecting a sucralose crude product to ethyl acetate pulping treatment, two instances of activated carbon decolorization and impurity removal at different stages and three instances of crystallization, impurities in the sucralose crude product and impurities generated by oxidation during a crystallization mother liquor use process can be effectively removed, and the problem of impurity enrichment during the recycling process of a crystallization mother liquor is solved, such that crystallization mother liquor generated during the refining process can be recycled, the loss of sucralose during the purification process is reduced, and the yield of sucralose is significantly improved. Furthermore, the preparation method for a sucralose refined product provided in the present invention can be effectively combined with a preparation method for a sucralose crude product, such that the mother liquor formed during the preparation process of the sucralose refined product can be recycled, the yield of sucralose is significantly increased, the production cost is significantly reduced, and the preparation method has relatively good industrial prospects.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
The present invention provides a method for preparing a sucralose crude product by using an alcohol-water alkaline hydrolysis system, and relates to the technical field of fine chemical engineering. In the present invention, an aqueous solution comprising sucralose-6-acetate, sucralose diester and tetrachlorosucrose-6-acetate is used as a raw material solution, and is subjected to alkaline hydrolysis in an alkali metal hydroxide and water system, such that sucralose-6-acetate and chlorosucrose ester impurities (sucralose diester and tetrachlorosucrose-6-acetate) in the raw material solution can both be converted into sucralose, thereby significantly improving the yield of sucralose. In the present invention, separation is carried out by using multiple instances of concentration and multiple instances of extraction-back extraction of an ethyl acetate/water double-solvent system, such that fat-soluble impurities and water-soluble impurities are balanced in the system, and the phenomenon of saccharide coking during a concentration process can be avoided, thereby fully crystallizing sucralose in ethyl acetate, and improving the yield of sucralose.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
12.
METHOD FOR PREPARING SUCRALOSE CRUDE PRODUCT BY USING IMPROVED HYDROLYSIS SYSTEM
The present invention provides a method for preparing a sucralose crude product by using an alcohol-water alkaline hydrolysis system, and relates to the technical field of fine chemical engineering. In the present invention, an aqueous solution comprising sucralose-6-acetate, sucralose diester and tetrachlorosucrose-6-acetate is taken as a first aqueous solution, and is subjected to alkaline hydrolysis in an alkali metal hydroxide and water system, such that sucralose-6-acetate and chlorosucrose ester impurities (sucralose diester and tetrachlorosucrose-6-acetate) in the first aqueous solution can both be converted into sucralose, thereby significantly improving the yield of sucralose. In the present invention, separation is realized by carrying out multiple instances of concentration and multiple instances of extraction-back extraction in an ethyl acetate/water double-solvent system, such that fat-soluble impurities and water-soluble impurities are balanced in the system, and the phenomenon of saccharide coking during the concentration process can be avoided, thereby fully crystallizing sucralose in ethyl acetate, and improving the yield of sucralose.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
The present invention provides a method for preparing a sucralose crude product by using an alcohol-water alkaline hydrolysis system, and relates to the technical field of fine chemical engineering. In the present invention, an aqueous solution of sucralose-6-acetate crude product is taken as a raw material, and is subjected to alkaline hydrolysis in an alkali metal hydroxide and methanol-water system, such that sucralose-6-acetate and chlorosucrose ester impurities (sucralose diester and tetrachlorosucrose-6-acetate) in the aqueous solution of sucralose-6-acetate crude product are both converted into sucralose, thereby significantly improving the yield of sucralose. In the present invention, separation is realized by carrying out multiple instances of concentration and multiple instances of extraction-back extraction in an ethyl acetate/water double-solvent system, such that fat-soluble impurities and water-soluble impurities are balanced in the system, and the phenomenon of saccharide coking during the concentration process can be avoided, thereby fully crystallizing sucralose in ethyl acetate, improving the yield of sucralose, efficiently separating inorganic salts from sucralose, and reducing the treatment cost of subsequent high-salinity wastewater.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
14.
METHOD FOR PREPARING CRUDE SUCRALOSE USING IMPROVED ALCOHOL-WATER ALKALINE HYDROLYSIS SYSTEM
The present invention relates to the technical field of fine chemical engineering, and provides a method for preparing a crude sucralose by using an alcohol-water alkaline hydrolysis system. According to the present invention, a sucralose-6-acetate crude aqueous solution is used as a raw material, and alkaline hydrolysis is performed in an alkali metal hydroxide and methanol water system, so that sucralose-6-acetate in the sucralose-6-acetate crude aqueous solution and chlorosucrose ester impurities (sucralose diester and tetrachlorosucrose-6-acetate) can be converted into sucralose, thereby remarkably increasing the yield of sucralose. According to the present invention, multiple times of concentration and multiple times of extraction-back extraction between ethyl acetate/water double-solvent system are used for separation, so that fat-soluble impurities and water-soluble impurities are balanced in a system, the phenomenon of saccharides coking in the concentration process can be avoided, sucralose is fully crystallized in ethyl acetate, the yield of sucralose is increased, the inorganic salt is effectively separated from sucralose, and the treatment cost of subsequent high-salinity wastewater is reduced.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
15.
SUPPORTED ORGANOTIN CATALYST AND PREPARATION METHOD FOR SUCROSE-6-CARBOXYLATE
Described herein is a supported organotin catalyst and a preparation method for a sucrose-6-carboxylate. The supported organotin catalyst is prepared by coupling an organotin functional group to an inorganic carrier. The supported organotin catalyst of the present application can be used for catalyzing the generation of a sucrose-6-carboxylate, and after reaction, the supported organotin catalyst can be directly filtered and recovered only by adding a small amount of water to quench an acylating agent, so that the subsequent dehydration process is simpler and easier, and the supported organotin catalyst is thus very economical in terms of manpower, equipment and energy.
B01J 31/02 - Catalyseurs contenant des hydrures, des complexes de coordination ou des composés organiques contenant des composés organiques ou des hydrures métalliques
C07H 13/08 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés directement à des carbocycles
Described herein is a method for preparing acesulfame potassium, comprising: pressing an acetoacetamide-N-sulfonic acid triethylamine salt solution and a cyclizing agent solution into a Venturireactor via different inlets, mixing same at a mixing section and a diffusion section of the Venturireactor, and then injecting the obtained mixture into a flow reactor, wherein the cyclizing agent solution is formed by dissolving sulfur trioxide in a first organic solvent; subjecting the mixture passing through the flow reactor to a sulfonation cyclization reaction under the action of a supported solid base heterogeneous catalyst preset in the flow reactor, and entering the obtained sulfonated cyclized product into a hydrolysis reactor; subjecting the sulfonated cyclized product and a hydrolysis agent preset in the hydrolysis reactor to a hydrolysis reaction to obtain a hydrolysis product solution; and adding potassium hydroxide into an organic phase of the hydrolysate solution for a salt-forming reaction to obtain the acesulfame potassium.
Disclosed in the present disclosure is a purification method for sucralose-6-ethyl ester, and the method comprises: a secondary water boiling step: taking a sucralose-6-ethyl ester mother liquor, which has been subjected to boiling with water and a negative pressure treatment, adding a predetermined proportion of water to the sucralose-6-ethyl ester mother liquor, fully stirring and heating for boiling with water, and after stirring and boiling with water for a predetermined time, carrying out solid-liquid separation to obtain a secondary water-boiled mother liquor in which sucralose-6-ethyl ester is dissolved; a phase separating extraction step: leaving the secondary water-boiled mother liquor to stand for phase separation, taking the separated upper phase, extracting with an alkane extractant at a predetermined temperature, and removing residual white oil in the upper phase; a recrystallizing purification step: evaporating a lower-layer effluent obtained from extraction, so as to obtain a solid, and purifying the solid by means of recrystallization to obtain sucralose-6-ethyl ester; and a recycling step: separating the extracted upper-layer effluent, recovering the alkane extractant, and circulating the alkane extractant for use in the phase separation and extraction step. The method is simple, efficient and of low cost, and can effectively remove trace white oil and improve the purity of sucralose-6-ethyl ester.
Provided are a supported catalyst and a method for synthesizing a sucrose-6-ester. The supported catalyst includes an active functional component and an inorganic carrier, wherein the active functional component is a compound shown in formula (1), wherein n is a natural number greater than or equal to 2; R is an atom linked to a surface of the inorganic carrier; and one or two of R1, R2, and R3 is/are hydrocarbyl, and the rest are independently any one selected from the group consisting of oxygen, hydroxyl, hydrocarbyloxy, and acetoxy.
B01J 23/14 - Catalyseurs contenant des métaux, oxydes ou hydroxydes métalliques non prévus dans le groupe du germanium, de l'étain ou du plomb
C07D 407/12 - Composés hétérocycliques contenant plusieurs hétérocycles, au moins un cycle comportant des atomes d'oxygène comme uniques hétéro-atomes du cycle, non prévus par le groupe contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
B01J 31/12 - Catalyseurs contenant des hydrures, des complexes de coordination ou des composés organiques contenant des composés organiques ou des hydrures métalliques contenant des composés organométalliques ou des hydrures métalliques
19.
MONO-TIN ORGANIC COMPOUND AND PREPARATION METHOD AND USE THEREOF
Provided is a mono-tin organic compound for the synthesis of sucrose-6-carboxylate. The compound has a structure shown in formula (1), wherein R1, R2, and R3 each are independently selected from the group consisting of C1 to C8 linear or branched saturated alkyl, C2 to C8 linear or branched unsaturated alkyl, C3 to C8 substituted or unsubstituted saturated cycloalkyl, C3 to C8 substituted or unsubstituted unsaturated cycloalkyl, and C6 to C12 aryl or substituted aryl; and R4 is selected from the group consisting of C1 to C6 linear or branched saturated alkyl and C6 to C12 aryl or substituted aryl.
C07H 1/00 - Procédés de préparation des dérivés du sucre
C07H 13/10 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés directement à des hétérocycles
The present invention provides a process for producing chloroethane, comprising the following steps: (1) separating sucralose tail gas to prepare concentrated hydrochloric acid; (2) desorption and concentration of the concentrated hydrochloric acid; and (3) synthesis and purification of chloroethane. The present invention utilizes the hydrogen chloride waste gas produced as a by-product in the production of sucralose and realizes the reuse of the by-product hydrogen chloride waste gas and the continuous production of chloroethane. This technique is characterized by high yield, low cost, little wastewater, low energy consumption, high chloroethane purity, and the like.
A production apparatus and a production method of sucrose-6-ester are provided. The production apparatus includes a tank, a rotary distillation device, and a condensation device, the tank includes a separation chamber and a reaction chamber; the condensation device is sheathed inside the rotary distillation device, and the rotary distillation device is slidably connected in the separation chamber; a turntable of the rotary distillation device is fixed on a top surface of a drum, and a first heating device is provided on an outer wall of the turntable; the condensation device includes a condenser pipe, a water receiving plate, and a condensate water box that are connected sequentially from top to bottom; the condensation device is sheathed inside the drum of the rotary distillation device in a non-contact manner, and the condenser pipe is arranged to penetrate through the turntable and contacts a top surface of the tank.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
B01D 3/08 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction dans des récipients en rotationAtomisation sur disques tournants
B01D 5/00 - Condensation de vapeursRécupération de solvants volatils par condensation
B01D 3/00 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction
B01D 3/34 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction avec une ou plusieurs substances auxiliaires
Disclosed is a method for purifying sucralose, including: removing a solvent from a sucralose reaction solution to obtain a concentrated crude sucralose solution; under stirring, adding ethyl acetate into the concentrated crude sucralose solution, heating to a preset temperature, and holding at the preset temperature for a first preset time to obtain a crude product slurry with a certain amount of a sucralose crystal; and subjecting the crude product slurry to gradient cooling to an endpoint temperature, holding at the endpoint temperature for a second preset time, and filtering to obtain a sucralose crystal.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
Provided is a method for refining acesulfame potassium (Ace K), including: adding hydrogen peroxide and activated carbon to an Ace K crude product-containing solution to obtain a mixture, maintaining the mixture at a first preset temperature for a first preset time, and filtering the mixture to obtain an Ace K mother liquor; conducting concentration on the Ace K mother liquor to a preset concentration to obtain a concentrated solution, allowing the concentrated solution to stand at a second preset temperature for a second preset time to form an Ace K crystal nucleus, and obtaining a crystal nucleus-containing solution; conducting programmed freezing on the crystal nucleus-containing solution to obtain a solution with a large number of Ace K crystals; and conducting centrifugation, water washing, and drying on the solution with a large number of Ace K crystals to obtain an Ace K crystal product.
Disclosed is a method for purifying sucralose, sequentially including: adding sucralose to ultrapure water, heating the resulting mixture for dissolution to obtain a dissolved solution, filtering the dissolved solution to obtain a filtrate, and then extracting the filtrate with an extraction solvent to remove non-polar impurities; subjecting the extracted recrystallization solution to concentration by evaporation to obtain a concentrated recrystallization solution with a preset concentration, and leaving the concentrated recrystallization solution to stand at a preset temperature for a preset time to produce a sucralose crystal nucleus in the concentrated recrystallization solution; subjecting the concentrated recrystallization solution containing the sucralose crystal nucleus to programmed cooling to obtain a recrystallization solution with a large amount of a sucralose crystal; and centrifuging the recrystallization solution with a large amount of a sucralose crystal to obtain a solid, and subjecting the solid to water-washing and drying to obtain a sucralose crystal.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
Disclosed are a device and a method for preparing a sucrose-6-ester. The device includes a tank body, a heating pipe, an annular cooling apparatus, and a motor, wherein the annular cooling device and the heating pipe are arranged in the tank body in nested manner; the annular cooling apparatus includes a condensation inner wall, a condenser pipe, and a condensation outer wall that are arranged in nested manner; a distillation chamber is formed between the heating pipe and the tank body, a condensation chamber is formed between the heating pipe and the condensation outer wall, and a hollow portion of the condensation inner wall forms a reaction chamber; the heating pipe and the condensation inner wall are drove by the motor to rotate; the heating pipe is provided with a vapor outlet; an evaporation residue channel is formed at an end of the heating pipe away from the feed inlet.
B01D 3/00 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
B01D 5/00 - Condensation de vapeursRécupération de solvants volatils par condensation
26.
COOLING DEVICE AND COOLING METHOD FOR MALTOL SUBLIMATION SECTION
The invention provides a cooling device and a cooling method for a sublimation section. The cooling device comprises a reaction kettle (1) provided with a smooth inner wall, wherein the top of the reaction kettle (1) is provided with a gas phase port (11), the bottom of the reaction kettle (1) is provided with a discharge port (12), the middle of the reaction kettle (1) is provided with a sublimation gas phase inlet (13), and a wall of the reaction kettle (1) is further provided with a jacket (2).
Disclosed is a device for distillation decolorization and purification of alcohol in maltol production. The device comprises a rectification column, an alkali hydrolysis kettle and an alkali hydrolysis rectification column. An upper outlet of the rectification column is connected to an inlet of the alkali hydrolysis kettle, an outlet of the alkali hydrolysis kettle is connected to an inlet of the alkali hydrolysis rectification column, and an upper outlet of the alkali hydrolysis rectification column is connected to an inlet of a finished product tank. Further disclosed is a method for distillation decolorization and purification of alcohol in maltol production. A product processed by the solution of the present application has a high purity.
Provided is a method for preparing a sucrose-6-ester, including: preparing a reaction solution of sucrose and an organo-tin compound; atomizing the reaction solution to form droplets; thoroughly mixing and contacting the droplets with a gasified dehydration medium such that the droplets undergo a dehydration reaction to obtain an intermediate mixture containing sucrose organic tin ester droplets; separating the intermediate mixture to obtain a sucrose organic tin ester solution and a dehydrated gas-liquid mixture; recovering the sucrose organic tin ester solution obtained in the separation step and cycling to the atomization and dehydration steps several times; and subjecting an organic acid anhydride to an acylation reaction with the sucrose organic tin ester solution to obtain the sucrose-6-ester.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 1/00 - Procédés de préparation des dérivés du sucre
29.
PRODUCTION APPARATUS AND PRODUCTION METHOD OF SUCROSE-6-ESTER
A production apparatus of sucrose-6-ester is disclosed and includes a distillation separation tank, a reaction tank, and a condensated water collection tank, where the distillation separation tank is arranged above the reaction tank and the condensated water collection tank, and includes a shell and a heating-roller distillation device including a plurality of heating rollers arranged from top to bottom between front and rear side walls of the shell; two ends of the U-shaped plate are respectively fixed to bottoms of the front and rear side walls; a feed pipe is provided at a top of the shell, the condensated water outlet pipe is arranged at a bottom surface of the shell and is connected to the condensated water collection tank, and the liquid evaporation residue discharge pipe penetrates through the bottom surface of the shell, is connected to the U-shaped plate, and is connected to the reaction tank.
B01D 1/22 - Évaporation par amenée d'une pellicule liquide au contact d'une surface chauffée
B01D 5/00 - Condensation de vapeursRécupération de solvants volatils par condensation
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
B01J 19/24 - Réacteurs fixes sans élément interne mobile
The invention provides a DMF recycling method, the method comprises: neutralization step, extraction and crystallization step, layering step, evaporation step; a condensate obtained by evaporation of the upper layer liquid phase is recycled into the anti-solvent, a concentrated solution obtained by evaporation of the upper layer liquid phase and a condensate obtained by evaporation of the lower layer liquid phase are mixed to obtain a crude DMF solution for recycling of DMF. The recycling method overcomes the problem that acetic acid in the stock solution corrodes the equipment and produces impurities, so as to improve the recycling purity and reduce the equipment cost.
Provided is a post-treatment method for a sucrose-6-carboxylate chlorination reaction solution, including: adding ammonia water or water to the sucrose-6-carboxylate chlorination reaction solution to obtain a mixture, and subjecting the mixture to preliminary neutralization reaction; introducing an ammonia gas into a resulting reaction solution at a predetermined temperature, adjusting a pH of the resulting reaction solution to a predetermined alkalinity range, and conducting a reaction at a reaction temperature for a period of time; and adjusting a pH of a reaction solution obtained after the ammonia gas neutralization using an acid to a predetermined acidity range.
C07H 13/08 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés directement à des carbocycles
Provided are a device and a method for producing a sucrose-6-ester. The device includes a shell, a film scraping apparatus, and a base, wherein the film scraping apparatus is arranged on the base, and the shell covers the film scraping apparatus and the base; the shell is provided with a reaction solution inlet and a condensated water outlet; the base is provided with a carboxylate feed pipe, a reaction product discharge pipe, and a reaction channel connected to the carboxylate feed pipe; the film scraping apparatus includes a temperature control unit, a rotary tube, and a plurality of scrapers arranged on an inner wall of the rotary tube, and an outer edge of each of the scrapers abuts against an outer wall of the temperature control unit; and the rotary tube is able to rotate around the temperature control unit.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
B01J 19/18 - Réacteurs fixes avec éléments internes mobiles
33.
METHOD FOR HYDROLYTIC PREPARATION OF ACESULFAME, AND METHOD FOR PRODUCING ACESULFAME POTASSIUM
The present application discloses a method for hydrolytic preparation of acesulfame, which comprises the following steps: step 1: mixing and reacting sulfamic acid and triethylamine to obtain sulfamic acid triethylamine salt; step 2: reacting the sulfamic acid triethylamine salt with diketene to obtain acetyl acesulfame triethylamine salt; step 3: reacting the acetyl acesulfame triethylamine salt with sulfur trioxide to obtain a first material; and step 4, reacting the first material with a hydrolysis agent to obtain a second material, wherein the hydrolysis agent is a sulfuric acid aqueous solution. A hydrolysis product of a method of the present application has a consistent quality, and the speed of hydrolysis is fast.
The present application discloses an industrial preparation method for acetoacetyl-N-sulfamate, the acetyl-N-sulfamate being used as an intermediate for synthesizing Acesulfame-K. The method comprises the following steps: step 1, dissolving sulfamic acid in an inert organic solvent; step 2, dropwise adding an amine to the product obtained in step 1; step 3: dropwise adding glacial acetic acid into the product obtained in step 2; step 4, dropwise adding diketene to the product obtained in step 3, and then carrying out a reaction. In the product obtained in step 4, the acetoacetyl-N-sulfamate product content is greater than 35%. The product obtained by the present preparation method has a high yield.
C07C 307/02 - Monoamides d'acides sulfuriques ou de leurs esters, p. ex. acides sulfamiques
C07C 303/34 - Préparation d'esters ou d'amides d'acides sulfuriquesPréparation d'acides sulfoniques ou de leurs esters, halogénures, anhydrides ou amides d'amides d'acides sulfuriques
The present application discloses a method for the continuous preparation of an acesulfame intermediate. Step 1: mixing and reacting sulfamic acid and an amine to obtain a sulfamic acid amine salt; step 2: reacting the sulfamic acid amine salt with diketene to obtain a first material; and step 3: reacting the first material with a sulfur trioxide solution to obtain a second material, where in step 3, a mist formed by the first material and a mist formed by the sulfur trioxide solution mix and undergo a reaction. The present application implements efficient and continuous preparation of an acesulfame intermediate.
The present application discloses a method for processing a hydrolysis reaction product containing acesulfame, comprising the following steps: step 1, letting the hydrolysis reaction product containing acesulfame stand and separate into layers, to obtain a separated water phase and organic phase; step 2, extracting the water phase using an organic extraction agent, and rinsing the organic phase with a rinsing agent. The method of the present application can improve hydrolysis conditions, and effectively reduce pollution caused by hydrolysis.
Disclosed in the present application is a method for preparing acesulfame potassium. The method comprises the following steps: step 1, mixing sulfamic acid and an amine for reaction to prepare amino sulfamate; step 2, reacting the amino sulfamate with diketene to obtain a first material; step 3, reacting the first material with a sulfur trioxide solution to obtain a second material; step 4, reacting the second material with a hydrolysate to obtain a third material; and step 5, reacting an organic phase separated from the third material with a potassium-containing compound to prepare acesulfame potassium, wherein amino acetyl acetyl-N-sulfamate in the first material in step 3 continuously reacts with sulfur trioxide in a constant molar ratio. The present application has the advantage of continuous reaction.
Provided is a method for preparing sucralose. The method comprises the steps of: feeding a chlorination reaction solution for preparing sucralose-6 ester, a first liquid alkali and first reuse water into a neutralization reaction rectifying column in sections, subjecting same to a neutralization reaction under evaporation conditions, and then extracting a solvent mixture from the top of the neutralization reaction rectifying column; extracting a chlorination reaction neutralization solution from the bottom of the neutralization reaction rectifying column; feeding the chlorination reaction neutralization solution, a second liquid alkali and second reuse water into a hydrolysis reaction rectifying column in sections, subjecting same to an alkaline hydrolysis reaction under evaporation conditions, extracting a waste aqueous solution from the top of the hydrolysis reaction rectifying column, and extracting a sucralose aqueous solution from the bottom of the hydrolysis reaction rectifying column; adjusting the sucralose aqueous solution to be neutral, then successively subjecting same to extraction, oxidation and back extraction for purification; and crystallization.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
B01D 53/00 - Séparation de gaz ou de vapeursRécupération de vapeurs de solvants volatils dans les gazÉpuration chimique ou biologique des gaz résiduaires, p. ex. gaz d'échappement des moteurs à combustion, fumées, vapeurs, gaz de combustion ou aérosols
B01D 53/02 - Séparation de gaz ou de vapeursRécupération de vapeurs de solvants volatils dans les gazÉpuration chimique ou biologique des gaz résiduaires, p. ex. gaz d'échappement des moteurs à combustion, fumées, vapeurs, gaz de combustion ou aérosols par adsorption, p. ex. chromatographie préparatoire en phase gazeuse
B01D 53/18 - Unités d'absorptionDistributeurs de liquides
The present application provides a method for purifying sucralose-6-ester. The method comprises: adding an oxidizing agent to a mother solution to be purified, carrying out an oxidation reaction under a first preset condition, then adding an alkaline hydrolysis agent thereto, and carrying out an alkaline hydrolysis reaction under a second preset condition to convert a target impurity into sucralose-6-ester so as to obtain an oxidized alkaline hydrolysis reaction solution; adjusting the pH value of the oxidized alkaline hydrolysis reaction solution to be neutral, keeping same for a period of time, then heating and filtering same to remove insoluble impurities, and then carrying out liquid separation to obtain a first aqueous phase and a first organic phase; extracting the first aqueous phase by using an extracting agent, and combining a second organic phase, which is obtained by means of the extraction, with the first organic phase to obtain a mother solution to be crystallized; and a step of crystallization, involving: concentrating the mother solution to be crystallized, and carrying out crystallization under a third preset condition to obtain a crude product of sucralose-6-ester and a first filtrate. By means of the present application, the yield of a target product is greatly improved while the impurity content is effectively removed.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
The present application provides a method for preparing an organotin-sucrose complex, comprising: acylating a DMF solution of sucrose with an organotin ester catalyst under predetermined conditions to generate an organotin-sucrose complex and a DMF vapor; condensing and adsorbing the DMF vapor using a condensing and adsorption apparatus provided with a solid adsorbent, removing the moisture therein to obtain regenerated DMF; collecting the regenerated DMF and recycling same into a DMF solution of sucrose entering the acylation step; and purging the solid adsorbent using hot dry air to regenerate the solid adsorbent. The present application greatly reduces DMF consumption, decreasing the burden of DMF post-treatment, and can effectively remove water from the reaction system, promoting the generation of an organotin-sucrose complex, and improving yield of the organotin-sucrose complex. The whole process is simple, equipment costs are low, and the application value and the economic value are extremely high.
The present application provides a method for purifying sucralose-6-ester, comprising: a concentration step: concentrating a mother liquor to be purified so as to remove an organic solvent, and adding water after concentration is complete, forming an aqueous solution to be purified; an oxidation step: sequentially adding an oxidant and a decolorant to the aqueous solution to be purified, performing an oxidation decolorization reaction, and then adding an alkaline hydrolysis agent so as to oxidize target impurities into sucralose-6-ester and remove colored impurities; after a period of reaction, performing solid-liquid separation, and obtaining solid waste and a first filtrate; and a crystallization step: after the first filtrate is adjusted to neutral, adding an extractant, simultaneously performing extraction and crystallization, and obtaining a sucralose-6-ester crude product and a second filtrate. According to the present application, the yield of a target product can be greatly improved while impurity content is effectively removed; moreover, the overall treatment process is simple, the economic costs are low, and the practicability is high; in addition, the COD content in wastewater can be significantly reduced.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
C07H 1/00 - Procédés de préparation des dérivés du sucre
43.
SUPPORTED ORGANOTIN CATALYST AND PREPARATION METHOD FOR SUCROSE-6-CARBOXYLATE
Disclosed are a supported organotin catalyst and a preparation method for a sucrose-6-carboxylate. The supported organotin catalyst is prepared by coupling an organotin functional group to an inorganic carrier. The supported organotin catalyst of the present application can be used for catalyzing the generation of a sucrose-6-carboxylate, and after reaction, the supported organotin catalyst can be directly filtered and recovered only by adding a small amount of water to quench an acylating agent, so that the subsequent dehydration process is simpler and easier, and the supported organotin catalyst is thus very economical in terms of manpower, equipment and energy. Moreover, according to the present application, the organotin functional group is supported on the inorganic carrier by means of a covalent bond of a coupling atom, so that the organotin functional group is hardly lost after filtration and is basically completed recovered, and therefore, there is not only no need to add a new supported organotin catalyst after each production, but also no bad influence on the subsequent chlorination reaction due to the product being entrained with the supported organotin catalyst.
B01J 31/12 - Catalyseurs contenant des hydrures, des complexes de coordination ou des composés organiques contenant des composés organiques ou des hydrures métalliques contenant des composés organométalliques ou des hydrures métalliques
C07H 1/00 - Procédés de préparation des dérivés du sucre
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
44.
TREATMENT METHOD FOR ACESULFAME POTASSIUM WASTE LIQUID
A treatment method for an acesulfame potassium waste liquid. The acesulfame potassium waste liquid is a waste liquid generated in preparation of acesulfame potassium by adopting a diketene-sulfur trioxide method. The treatment method comprises: a pH adjustment step: adding a first material flow into the acesulfame potassium waste liquid until the pH value of the acesulfame potassium waste liquid is not less than 13, so as to obtain a second material flow, wherein the first material flow is a residual liquid generated in the following crystallization step or a saturated sodium hydroxide or potassium hydroxide solution; a neutralization and separation step: adding a sodium hydroxide or potassium hydroxide solid into the first material flow, stirring until the sodium hydroxide or potassium hydroxide solid is completely dissolved, standing for a period of time to obtain an organic phase and an aqueous phase, and recycling the organic phase as a triethylamine crude product; and a crystallization step: crystallizing the aqueous phase, and filtering same to obtain sodium sulfate or potassium sulfate and the residual liquid.
Provided is a preparation method for acesulfame potassium, comprising: a salt-forming step: separating a sulfonation cyclization product solution into an organic phase and an inorganic phase, and adding an ethanolic solution of potassium ethoxide to the organic phase to carry out a salt-forming reaction, wherein the sulfonation cyclization product solution is obtained by hydrolysis of the product of cycloaddition of acetoacetamide-N-sulfonic acid triethylamine salt and sulfur trioxide; and a washing step: after the salt-forming reaction is completed, filtering to obtain a solid product, and washing the solid product with ethanol to obtain a crude product of acesulfame potassium. The method greatly reduces the content of inorganic impurities in the crude product of acesulfame potassium, thereby significantly improving the purity of a final product, i.e., acesulfame potassium, simplifies the subsequent process for the crude product of acesulfame potassium, reduces the costs of purification of the crude product of acesulfame potassium, and can improve the yield of acesulfame potassium.
A method for preparing acesulfame potassium, the method comprising: pressing an acetoacetamide-N-sulfonic acid triethylamine salt solution and a cyclizing agent solution into a Venturi reactor via different inlets, mixing same at a mixing section and a diffusion section of the Venturi reactor, and then spraying the obtained mixture into a flow reactor, wherein the cyclizing agent solution is formed by dissolving sulfur trioxide in a first organic solvent; subjecting the mixture passing through the flow reactor to a sulfonation cyclization reaction under the action of a loaded solid alkali heterogeneous catalyst preset in the flow reactor, and the obtained sulfonation cyclization product entering a hydrolysis reactor; subjecting the sulfonation cyclization product and a hydrolysis agent preset in the hydrolysis reactor to a hydrolysis reaction to obtain a hydrolysis product solution; and adding potassium hydroxide into an organic phase of the hydrolysate solution for a salt-forming reaction to obtain the acesulfame potassium. According to the preparation method, the purity and yield of the acesulfame potassium are improved, and a post-treatment process for the acesulfame potassium is simplified.
B01J 31/26 - Catalyseurs contenant des hydrures, des complexes de coordination ou des composés organiques contenant en outre des composés métalliques inorganiques non prévus dans les groupes
A preparation method for acesulfame potassium, comprising: adding triethylamine to a sulfamic acid solution, and carrying out an amination reaction to generate a sulfamic acid ammonium salt solution; adding diketene to the obtained sulfamic acid ammonium salt solution, and under the action of a solid superacid catalyst, carrying out an acylation reaction to obtain an intermediate solution; dissolving sulfur trioxide in a solvent to form a cyclizing agent solution; adding the cyclizing agent solution to the intermediate solution, and carrying out a sulfonation cyclization reaction to obtain a cyclization product solution; adding a hydrolysis agent to the cyclization product solution, and carrying out a hydrolysis reaction to obtain a hydrolysis product solution; and adding a potassium hydroxide solution to the organic phase of the hydrolysis product solution to obtain acesulfame potassium. The method can reduce the impurity content in acesulfame K, thereby making the quality of acesulfame K better, and improve the conversion rate of a raw material, thereby greatly improving the yield of a cyclization product, further improving the yield of a final product, i.e., acesulfame K, and reducing the production costs of acesulfame K.
Provided is a potassium acetylsulfonate composition, comprising potassium acetylsulfonate and a chloride thereof, wherein the content of the chloride is less than 300 ppm. The composition is prepared by the following method: adding triethylamine into a sulfamic acid solution for an amination reaction to generate an ammonium sulfamate solution; adding diketene into same for an acylation reaction under the action of a solid acidic catalyst to obtain an intermediate solution; subjecting the intermediate solution and a cyclizing agent solution to a sulfonation cyclization reaction under the action of a supported solid alkali heterogeneous catalyst to obtain a sulfonation cyclization product; and carrying out hydrolysis and salt formation. The potassium acetylsulfonate composition, which has an extremely low impurity content, can be prepared by using two catalysts in combination, such that a post-treatment process of the potassium acetylsulfonate is reduced, and the production cost is reduced.
Provided is an method for treating an acesulfame potassium waste liquid, the method comprising: adding first liquid ammonia into an acesulfame potassium waste liquid, and subjecting same to a neutralization reaction in a closed reactor under a preset condition to obtain a first material; separating the first material into a first organic phase and a first water phase, and evaporating the first water phase until the water content reaches a preset water content so as to obtain a second material; adding second liquid ammonia into the second material, and subjecting same to a neutralization reaction in the closed reactor under a preset condition to obtain a third material; separating the third material into a second organic phase and a second water phase; recovering the first organic phase and the second organic phase as crude triethylamine products; and subjecting the second water phase to solid-liquid separation to obtain a crude ammonium sulfate product and a residual liquid. According to the method provided by the present application, the reaction is rapid, the conversion rate of triethylamine sulfate is high, and the reaction is carried out more thoroughly; and the process for treating an acesulfame potassium waste liquid is simplified, the treatment time is shortened, and the recovery efficiency of amine is improved.
C02F 103/36 - Nature de l'eau, des eaux résiduaires ou des eaux ou boues d'égout à traiter provenant de l'industrie chimique non prévue dans les groupes provenant de la fabrication de composés organiques
50.
TREATMENT METHOD FOR ACESULFAME POTASSIUM WASTE LIQUID
Provided is a treatment method for an acesulfame potassium waste liquid, that is, a waste liquid produced in the preparation of acesulfame potassium by a diketene-sulfur trioxide method, and the method comprises the following steps: a moisture evaporation step: at a first preset temperature, evaporating the acesulfame potassium waste liquid until the water content reaches a preset water content, so as to obtain a first material; a neutralization reaction step: adding liquid ammonia to the first material, and then subjecting same to a neutralization reaction in a closed reactor, so as to obtain a second material; a product separation step: separating the second material into an organic phase and a water phase, and subjecting the water phase to solid-liquid separation, so as to obtain an ammonium sulfate crude product and a residual liquid; and recycling the organic phase as a triethylamine crude product.
C07C 1/24 - Préparation d'hydrocarbures à partir d'un ou plusieurs composés, aucun d'eux n'étant un hydrocarbure à partir de composés organiques ne renfermant que des atomes d'oxygène en tant qu'hétéro-atomes par élimination d'eau
Provided is a preparation method for acesulfame potassium, which comprises: a pretreatment step, involving: treating an acetoacetamide-N-sulfonic acid triethylamine salt solution with a weakly alkaline inorganic substance to obtain an intermediate solution; a sulfonation cyclization step, involving: dissolving sulfur trioxide in a solvent to form a cyclizing agent solution, and subjecting the intermediate solution and the cyclizing agent solution to a sulfonation cyclization reaction so as to obtain a sulfonation cyclization product; a hydrolysis step, involving: adding a hydrolysis agent to a solution of the sulfonation cyclization product, and carrying out a hydrolysis reaction to obtain a hydrolysate solution; and a salt-forming step, involving: adding a salt-forming agent to an organic phase of the hydrolysate solution, and carrying out a salt-forming reaction to obtain acesulfame potassium. According to the method, on the one hand, an acid catalyst remaining in the final product acesulfame potassium is removed; on the other hand, the reaction environment provided by the weakly alkaline inorganic substance inhibits the generation of by-products and increases the purity of the acesulfame potassium product; and the yield of the acesulfame potassium can be significantly increased, and the production cost of the acesulfame potassium is lowered.
Provided is an acesulfame potassium preparation method, comprising: using an acetoacetamide-N-sulfonic acid triethylamine salt solution as a working fluid, and dissolving sulfur trioxide in a solvent to form a cyclizing agent solution as a driving fluid; introducing the working fluid from a nozzle of a Venturi reactor, introducing the driving fluid from an air suction chamber of the Venturi reactor, and controlling the pressure of the working fluid to be higher than that of the driving fluid; mixing the working fluid and the driving fluid in a mixing section and a diffusion section of the Venturi reactor, performing sulfonation cyclization reaction, and spraying a sulfonation cyclization product into a flow reactor; performing hydrolysis reaction on the sulfonation cyclization product and a hydrolysis agent preset in the flow reactor to obtain a hydrolysis product solution; and adding potassium hydroxide into the organic phase of the hydrolysis product solution to obtain acesulfame potassium. The preparation method reduces the probability that organic impurities remaining in the final product acesulfame potassium, improves the purity of acesulfame potassium, and is suitable for large-scale industrial production.
A method for preparing an acetoacetamide-N-sulfonic acid triethylamine salt, the method comprising: an amination reaction step, involving: dissolving sulfamic acid in first dichloromethane to obtain a first reaction solution; dissolving triethylamine in second dichloromethane to obtain a second reaction solution, and adding the second reaction solution into the first reaction solution for an amination reaction to form an ammonium sulfamate solution; and an acylation reaction step, involving: dissolving diketene in third dichloromethane to prepare a third reaction solution; filling a fixed bed reactor with a solid heteropolyacid catalyst, sequentially introducing the ammonium sulfamate solution and the third reaction solution into the fixed bed reactor and reacting same under preset conditions to form the acetoacetamide-N-sulfonic acid triethylamine salt. According to the method, a post-treatment process for the product is simplified, such that the final acesulfame potassium product has a better appearance; and the large-scale continuous production of an acetoacetamide-N-sulfonic acid triethylamine salt is achieved, the reaction time is shortened, the reaction yield is increased, and the production cost of acesulfame potassium is lowered.
C07C 303/34 - Préparation d'esters ou d'amides d'acides sulfuriquesPréparation d'acides sulfoniques ou de leurs esters, halogénures, anhydrides ou amides d'amides d'acides sulfuriques
C07C 307/02 - Monoamides d'acides sulfuriques ou de leurs esters, p. ex. acides sulfamiques
C07C 209/68 - Préparation de composés contenant des groupes amino liés à un squelette carboné à partir d'amines, par des réactions n'impliquant pas de groupes amino, p. ex. réduction d'amines non saturées, aromatisation ou substitution du squelette carboné
A method for preparing an acetoacetamide-N-sulfonic acid triethylamine salt, the method comprising: dissolving sulfamic acid in first dichloromethane to prepare a first reaction solution; dissolving triethylamine in second dichloromethane to prepare a second reaction solution, and adding the second reaction solution into the first reaction solution for an amination reaction to form an ammonium sulfamate solution; filling a fixed bed reactor with a zeolite catalyst, sequentially introducing the ammonium sulfamate solution and diketene into the fixed bed reactor and reacting same under preset conditions to form an acetoacetamide-N-triethylamine sulfonate solution. According to the method, a post-treatment process for the product is simplified, such that the final acesulfame potassium product has a better appearance, and the usage experience is significantly improved; in addition, the large-scale continuous production of an acetoacetamide-N-sulfonic acid triethylamine salt is achieved, the reaction time is greatly shortened, the reaction yield is increased, and the production cost of acesulfame potassium is further lowered.
C07C 303/34 - Préparation d'esters ou d'amides d'acides sulfuriquesPréparation d'acides sulfoniques ou de leurs esters, halogénures, anhydrides ou amides d'amides d'acides sulfuriques
C07C 307/02 - Monoamides d'acides sulfuriques ou de leurs esters, p. ex. acides sulfamiques
C07C 209/00 - Préparation de composés contenant des groupes amino liés à un squelette carboné
Disclosed in the present invention is a method for purifying sucralose-6-ethyl ester, the method comprising: a second instance of boiling with water step, involving: taking a sucralose-6-ethyl ester mother solution, which has been subjected to boiling with water and a negative pressure treatment, adding a predetermined proportion of water to the sucralose-6-ethyl ester mother solution, thoroughly stirring and heating same for boiling same with water, and after stirring and boiling same with water for a preset time, carrying out solid-liquid separation to obtain a twice-water-boiled mother solution in which sucralose-6-ethyl ester is dissolved; a phase separation and extraction step, involving: leaving the twice-water-boiled mother solution to stand for phase separation, taking the separated upper phase, extracting same by using an alkane extraction agent at a preset temperature, and removing residual white oil in the upper phase; a recrystallization purification step, involving: evaporating a lower-layer effluent obtained from extraction, so as to obtain a solid, and purifying the solid by means of recrystallization to obtain sucralose-6-ethyl ester; and a recovering and recycling step: separating the extracted upper-layer effluent, recovering the alkane extraction agent, and recycling the alkane extraction agent for use in the phase separation and extraction step. The method is simple, efficient and low cost, and can effectively remove trace white oil and improve the purity of sucralose-6-ethyl ester.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
Provided are a supported catalyst and a synthesis method for sucrose-6-ester. The supported catalyst is used for catalyzing a transesterification reaction of sucrose and a carboxylic ester. The catalyst comprises an active functional component and an inorganic carrier, wherein the active functional component is a compound represented by formula (1), wherein n is a natural number greater than or equal to 2; R is an atom connected to the surface of the inorganic carrier; one or two of R1, R2 and R3 are a hydrocarbyl, and the rest are respectively and independently selected from any one of an oxygen atom, hydroxyl, hydrocarbyloxy and acetoxy. The catalyst of the present application can catalyze a transesterification reaction of sucrose and an ester of a carboxylic acid and a lower alcohol with a high selectivity to obtain sucrose-6-ester. The catalyst can be recovered by means of filtration after the reaction and has little loss, and the use of a restricted article, i.e. a carboxylic acid anhydride, is avoided.
B01J 31/12 - Catalyseurs contenant des hydrures, des complexes de coordination ou des composés organiques contenant des composés organiques ou des hydrures métalliques contenant des composés organométalliques ou des hydrures métalliques
A production apparatus for sucrose-6-ester, comprising a distillation separation tank, a reaction tank, and a condensed water collection tank. The distillation separation tank is arranged above the reaction tank and the condensed water collection tank; the distillation separation tank comprises a housing and a hot roller distillation device; the hot roller distillation device comprises a plurality of heating rollers, and the plurality of heating rollers are closely arranged vertically and horizontally between a front side wall and a rear side wall of the housing; two ends of a U-shaped plate are fixed on the bottom of the front side wall and the rear side wall of the housing; a plurality of heat exchange tubes are provided in an inner cavity formed by the U-shaped plate, and penetrate through the front side wall and the rear side wall of the housing; a feeding tube is provided at the top of the housing, a condensed water outlet tube is provided on a bottom surface of the housing, and a distillation residual liquid outlet tube penetrates through the bottom surface of the housing and is connected to the U-shaped plate; the condensed water collection tank is connected to the condensed water outlet tube; and the reaction tank is connected to the distillation residual liquid outlet tube. With the production apparatus, continuous production of sucrose-6-ester is realized, the volume of the production apparatus is reduced, the floor space is saved, and the yield of sucrose-6-ester is improved.
A production apparatus and production method for sucrose-6-ester; said apparatus comprises a tank body, a heating pipe, an annular cooling device, and a motor; the annular cooling device and the heating pipe are sequentially nested in the tank body from inside to outside; the annular cooling device comprises a condensation inner wall, condensation pipes and a condensation outer wall which are sequentially nested from inside to outside; the heating pipe and the tank body form a distillation cavity, the heating pipe and the condensation outer wall form a condensation cavity, and the hollow portion of the condensation inner wall is a reaction cavity; the motor is electrically connected to the heating pipe and the condensation inner wall and can drive the heating pipe and the condensation inner wall to rotate, so that a reaction liquid is separated into water vapour and distillation residue; and a vapour outlet is provided on the heating pipe, so that the water vapour can enter the condensation cavity from the distillation cavity; a distillation residue channel is provided at the end of the heating pipe away from a feeding port; and the distillation residue channel is arranged not in contact with the annular cooling device and is in communication with the reaction cavity. Said apparatus allows for the continuous production of sucrose-6-ester, greatly shortening a production period.
B01D 3/00 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 1/00 - Procédés de préparation des dérivés du sucre
59.
PRODUCTION APPARATUS AND PRODUCTION METHOD FOR SUCROSE-6-ESTER
A production apparatus and a production method for sucrose-6-ester, the apparatus comprising a tank, a rotary distillation device, and a condensing device, wherein the tank comprises a separation cavity and a reaction cavity, the condensing device is sleeved in the rotary distillation device, and the rotary distillation device is slidably connected in the separation cavity; a turntable for rotary distillation is fixed on a top surface of a rotating drum by a plurality of connecting plates, and a first heating device is provided on an outer wall of the turntable; the condensing device comprises a condensing pipe, a water-receiving plate and a water-condensing water tank, which are vertically connected in sequence; the condensing device is sleeved in the rotating drum of the rotary distillation device in a non-contact manner, and the condensing pipe runs through the turntable to be in contact with a top surface of the tank; and the rotary distillation device can rotate about a central axis of the turntable, so as to separate a reaction liquid entering from a reaction liquid feed pipe into steam and residual liquid after distillation. The apparatus realizes continuous production of sucrose-6-ester, greatly shortens the production cycle and improves the production efficiency.
B01D 3/00 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction
B01D 3/08 - Distillation ou procédés d'échange apparentés dans lesquels des liquides sont en contact avec des milieux gazeux, p. ex. extraction dans des récipients en rotationAtomisation sur disques tournants
C07H 1/00 - Procédés de préparation des dérivés du sucre
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 13/08 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés directement à des carbocycles
60.
PRODUCTION DEVICE AND PRODUCTION METHOD FOR SUCROSE-6-ESTER
Provided are a production device and production method for sucrose-6-ester. The device comprises separators and a reactor; each separator comprises an accommodation cavity and a condensation cavity which are provided closely and in communication with each other; a feeding port is provided at the top end of the accommodation cavity, a residual evaporation liquid outlet portion is provided at the bottom end of the accommodation cavity, and the residual evaporation liquid outlet portion is connected to the reactor by means of a conveying pipe; a condensed water outlet is provided in the condensation cavity; a film scraping apparatus is provided in the accommodation cavity, and the film scraping apparatus comprises a guide disk and several scraping plates which are arranged in the radial direction of the center axis of the guide disk and intersect with the guide disk in a penetrating manner; and the film scraping apparatus can rotate in the center axis of the guide disk, so that the scraping plates can scrape reaction liquid flowing down from the guide disk into a liquid film on the inner wall of the condensation cavity and separate the reaction liquid into residual evaporation liquid and water vapor. By mean of this, the reaction raw materials can be continuously added into the production device, and the reaction liquid separation step and the esterification reaction step are continuously performed, achieving the continuous production of sucrose-6-ester, greatly shortening the production cycle, and increasing the yield of sucrose-6-ester.
B01D 1/22 - Évaporation par amenée d'une pellicule liquide au contact d'une surface chauffée
C07H 13/02 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 13/08 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés directement à des carbocycles
C07H 1/00 - Procédés de préparation des dérivés du sucre
61.
PRODUCTION EQUIPMENT AND PRODUCTION METHOD FOR SUCROSE-6-ESTER
Production equipment and a production method for sucrose-6-ester, wherein the equipment comprises a housing, a film scraping device, and a base. The film scraping device is disposed on the base, and the housing covers the outer sides of the film scraping device and the base. The housing is provided with a reaction liquid feeding port and a condensed water outlet. The base is provided with a carboxylic ester feeding pipe, a reaction product discharging pipe, and a reaction channel connected to the carboxylic ester feeding pipe. The film scraping device comprises a temperature control device, a rotating pipe, and a plurality of scraping blades disposed on the inner wall of the rotating pipe. The outer edges of the scraping blades abut against the outer wall of the temperature control device. The rotating pipe can rotate around the temperature control device, so that the scraping blades can scrape a reaction liquid that enters from the reaction liquid feeding port and flows down along the outer wall of the temperature control device into a liquid film on the outer wall of the temperature control device, and separate the liquid film into an evaporation residue and water vapor. According to the equipment, the integrated design of a separation device and a reaction device is realized, the volume of the production equipment is reduced, floor space is saved, the yield of sucrose-6-ester is improved, and the production cost is greatly reduced.
An immobilization method of a liquid lipase. The immobilization method comprises the following steps performed in sequence: a dissolving step: adding alginate into deionized water to completely dissolve, and adding a liquid lipase at a preset temperature to obtain a mixed solution; an immobilization step: mixing the mixed solution with a metal cross-linking agent solution, and maintaining for a preset time period to obtain a spherical gel, so that the liquid lipase is immobilized; and a chelating step: after the spherical gel is washed, adding a buffer solution and an organic complexing agent solution to perform a chelating reaction, and then washing with a buffer solution to obtain the immobilized liquid lipase. The obtained gel has extremely high physical strength, can be more stable in the reaction system, is basically not broken and decomposed, can be repeatedly used for multiple times, is more suitable for producing sucrose-6-acetate by using industrial large-scale continuous esterification. The manufacturing method is simple, and the cost is low.
C12N 11/10 - Enzymes ou cellules microbiennes immobilisées sur ou dans un support organique le support étant un hydrate de carbone
C12N 11/04 - Enzymes ou cellules microbiennes immobilisées sur ou dans un support organique piégées à l’intérieur du support, p. ex. dans un gel ou dans des fibres creuses
The present application provides a preparation method for sucralose and a crude product solution thereof. The preparation method comprises: dissolving sucralose-6-ethyl ester in methanol to form a sucralose-6-ethyl ester reaction solution; adding tert-butylamine to the sucralose-6-ethyl ester reaction solution as a catalyst for reaction under a preset condition, so that the sucralose-6-ethyl ester undergoes a deacylation reaction to form a sucralose mixed solution; and distilling the sucralose mixed solution to obtain a sucralose crude product solution. The present application has the following beneficial effects: by using volatile tert-butylamine as a catalyst, the catalyst can be removed and recycled only by means of a simple distillation process while efficiently and reliably catalyzing the deacylation reaction of the sucralose-6-ethyl ester, thereby simplifying the process step of catalyst separation, reducing material consumption and wastewater generation, and greatly reducing the production cost of sucralose; and clean production is facilitated.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
64.
SUCRALOSE PREPARATION METHOD, CRUDE PRODUCT SOLUTION, AND SUCRALOSE
A sucralose preparation method, a crude product solution, and sucralose, the method comprising: dissolving sucralose-6-ethyl ester in ethanol to form a sucralose-6-ethyl ester reaction solution; distilling the sucralose-6-ethyl ester reaction solution to remove the moisture therein; adding an alkaline catalyst such as sodium hydroxide or potassium hydroxide to the sucralose-6-ethyl ester reaction solution to form a sucralose mixed solution; and filtering the sucralose mixed solution to obtain a sucralose crude product solution.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
1233 each independently represent C1-C8 linear or branched saturated alkyl, C2-C8 linear or branched unsaturated alkyl, C3-C8 substituted or unsubstituted saturated cycloalkyl, C3-C8 substituted or unsubstituted unsaturated cycloalkyl or C6-C12 aryl or substituted aryl, and R4 represents C1-C6 linear or branched saturated alkyl or C6-C12 aryl or substituted aryl. The mono-tin organic compound of the present application enables accurate metering and feeding in the process of synthesizing sucrose-6-carboxylate, improves the catalyst recovery rate and reduces the occurrence of a subsequent chlorination side reaction at the same time, and has faster reaction, lower energy consumption and a higher yield per unit volume.
The present application provides a chlorination method for a sucrose-6-carboxylate, comprising: dissolving a solid phosgene into a first solvent to obtain a solid phosgene solution, and dissolving a sucrose-6-carboxylate into a second solvent to obtain a carboxylate solution, adding a catalyst to the carboxylate solution, and then slowly dropwise adding the solid phosgene solution into the carboxylate solution containing the catalyst at a first preset temperature, followed by operating the reactant mixing step a plurality of times to obtain a reaction mixture solution, maintaining the reaction mixture solution at the first preset temperature for a first preset time, and then heating same to a second preset temperature and maintaining the reaction for a second preset time for a chlorination reaction. The present application avoids the current situation of caking of the Vilsmeier reagent and DMF, improves the safety, reliability and environmental friendliness of the reaction, and reduces the reaction cost. In addition, the reaction conditions are mild, and the process is convenient to operate, the selectivity of the trichloride substance is high, the side reactions are few, and the yield of the product is high, and the discharge amount of waste gas and waste liquid is small.
A preparation method for sucralose, a crude product solution, and sucralose, the method comprising: dissolving a sucralose-6-acetate into methanol, adding calcium oxide into the reaction solution of the sucralose-6-acetate for a deacylation reaction, and filtering same and recovering calcium oxide from the reaction mixture to obtain a sucralose crude product solution.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
Disclosed is a device for continuous liquid alkane introduction in a Grignard reaction. The device comprises a liquid alkane storage tank and a Grignard reaction kettle, which are characterized in that: an outlet of the liquid alkane storage tank is connected to the interior of the Grignard reaction kettle by means of a pipeline and a metering pump on the pipeline, and an atomizer at the tail end of the pipeline. Also disclosed is a method for continuous liquid alkane introduction in a Grignard reaction. The reaction process in the present application is stable, the material is fully reacted, and the Grignard production efficiency can be effectively improved.
Disclosed is a device for alcohol distillation decoloring and purification in maltol production. The device is characterized in comprising a rectifying column, an alkaline hydrolysis kettle and an alkaline hydrolysis rectifying column. An outlet on the upper side of the rectification column is in communication with an inlet of the alkaline hydrolysis kettle, an outlet end of the alkaline hydrolysis kettle column is in communication with an inlet end of the alkaline hydrolysis rectifying column, and an outlet on the upper side of the alkaline hydrolysis rectification column is in communication with an inlet end of a finished product trough. Further disclosed is a method for alcohol distillation decoloring and purification in maltol production. A product processed by the solution of the present application has a high purity.
Disclosed in the present application is a method for back-extraction purification of a crude product obtained by sublimation of maltol or ethyl maltol, comprising the following steps: step 1: heating the crude product obtained by sublimation of maltol or ethyl maltol, and water to 80±5℃ for material dissolution; step 2: allowing the material obtained in step 1 to stand to separate into layers, separating an upper aqueous solution layer, and then lowering the temperature of the upper aqueous solution layer to 10-15 ℃; and step 3: centrifuging to obtain a maltol or ethyl maltol crystal subjected to impurity removal. Also disclosed is a purification device. The technical solution for purification of the present application is high in yield and high in product purity.
A cooling device and cooling method for a sublimation section. The cooling device comprises a reaction kettle (1) provided with a smooth inner wall, wherein the top of the reaction kettle (1) is provided with a gas phase port (11), the bottom of the reaction kettle (1) is provided with a discharge port (12), the middle of the reaction kettle (1) is provided with a sublimation gas phase inlet (13), and a wall of the reaction kettle (1) is further provided with a jacket (2).
Disclosed is a method for purifying a maltol Grignard procedure intermediate characterized by comprising the following steps: step 1: an intermediate enters a distillation tower for coarse separation of furfuryl alcohol and a solvent, the temperature at the bottom of the distillation tower is higher than the temperature at the top of the tower; step 2: a fluid from the bottom of the distillation tower enters a first-stage flash distillation kettle, the temperature of the first-stage flash distillation kettle is higher than the temperature at the bottom of the distillation tower, and a gas phase of the first-stage flash distillation kettle is condensed and then enters a second-stage flash distillation kettle; step 3: the temperature of the second-stage flash distillation kettle is lower than the temperature of the first-stage flash distillation kettle, and a gas phase of the second-stage flash distillation kettle is condensed and then enters the third-stage flash distillation kettle; step 4: the temperature of the third-stage flash distillation kettle is lower than the temperature of the second-stage flash distillation kettle, and a gas phase of the third-stage flash distillation kettle is condensed and then collected. Also disclosed is a device for purifying a maltol Grignard procedure intermediate. The present method and device may increase the content and yield of furfuryl alcohol.
A method for purifying sucralose-6-ethyl ester, comprising: a preparation step: obtaining an ethyl acetate saturated solution of crude sucralose-6-ethyl ester heated to a predetermined temperature; a gradient crystallization step: performing cooling crystallization and filtration on the saturated solution for multiple times, dropwise adding a low-polarity solvent into the solution in each cooling crystallization process to gradually reduce the polarity of a solution system during crystallization, and collecting a sucralose-6-ethyl ester crude product obtained by means of multiple times of crystallization and filtration; and a purification step: recrystallizing and purifying the collected sucralose-6-ethyl ester crude product by using a mixed solution of ethyl acetate and the low-polarity solvent, so as to obtain a sucralose-6-ethyl ester refined product having higher purity. On the basis of cooling crystallization of sucralose-6-ethyl ester by using ethyl acetate as an initial solvent, the polarity of the mixed solvent is reduced by gradually adding the low-polarity solvent, such that the effectiveness of impurity separation in each gradient stage is improved, the product yield is high, and the product quality is good.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
A method for purifying sucralose, comprising: removing a solvent from a sucralose reaction liquid to obtain a concentrated solution of a sucralose crude product; under stirring, adding ethyl acetate to the concentrated solution of the sucralose crude product, heating same to a preset temperature and maintaining the temperature for first preset time to obtain a crude product slurry containing some sucralose crystals; and reducing the temperature of the crude product slurry in a gradient manner to a temperature end point, maintaining the temperature for second preset time, and performing filtering to obtain sucralose crystals. The present invention has the advantages of simple and convenient operation, small treatment capacity, a less required solvent amount, etc.; in addition, no additional species is added to the process flow by using ethyl acetate, and the boiling point of ethyl acetate is much lower than that of butyl acetate, such that the energy consumption in the distillation removal and recovery process is greatly reduced, and thus, the production efficiency is improved, and the production cost is reduced.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
A DMF recycling method. The method comprises: a neutralization step: adding an alkaline neutralizer into a DMF stock solution, controlling the pH value of the mixed solution to be within a preset range, and carrying out a neutralization reaction to convert acetic acid in the DMF stock solution into acetate; an extraction and crystallization step: adding an anti-solvent insoluble with the acetate into the neutralized solution, mixing and stirring to extract DMF by means of the anti-solvent, crystallizing and separating out acetate hydrate, and filtering to obtain mother liquor containing DMF; a layering step: standing and layering the mother liquor to obtain an upper liquid phase and a lower liquid phase; and an evaporation step: respectively evaporating and concentrating the upper liquid phase and the lower liquid phase, condensate obtained by means of upper liquid phase evaporation being recycled into the anti-solvent, and concentrated liquid obtained by means of upper liquid phase evaporation and condensate obtained by means of lower liquid phase evaporation being mixed to be used for recycling DMF. The recycling method solves the problem that acetic acid exists in a stock solution and corrodes a device to produce impurities, improves the recycling purity, and reduces the device cost.
C07C 233/03 - Amides d'acides carboxyliques ayant des atomes de carbone de groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone acycliques ayant les atomes d'azote des groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone de radicaux hydrocarbonés non substitués avec des atomes de carbone de groupes carboxamides liés à des atomes d'hydrogène
C07C 233/05 - Amides d'acides carboxyliques ayant des atomes de carbone de groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone acycliques ayant les atomes d'azote des groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone de radicaux hydrocarbonés non substitués avec des atomes de carbone de groupes carboxamide liés à des atomes de carbone d'un squelette carboné saturé acyclique ayant les atomes d'azote des groupes carboxamide liés à des atomes d'hydrogène ou à des atomes de carbone acycliques
C02F 103/36 - Nature de l'eau, des eaux résiduaires ou des eaux ou boues d'égout à traiter provenant de l'industrie chimique non prévue dans les groupes provenant de la fabrication de composés organiques
C02F 1/26 - Traitement de l'eau, des eaux résiduaires ou des eaux d'égout par extraction
A sucralose purification method, sequentially comprising: putting sucralose in ultrapure water, heating for dissolving and then filtering, and extracting with an extraction solvent to remove non-polar impurities; evaporating an extracted recrystallization solution to concentrate same to a preset concentration; leaving the solution to stand at a preset temperature for a preset time to form sucralose crystal nuclei; carrying out programmed cooling on the recrystallization solution containing crystal nuclei to obtain a recrystallization solution containing a large amount of sucralose crystals; and centrifuging the recrystallization solution containing a large amount of sucralose crystals, washing with water, and drying to obtain sucralose crystals. Extraction and impurity removal are carried out at first, next, the formation of crystal nuclei is promoted, and then, the growth of crystals is accelerated by means of a secondary nucleation process to ensure full crystallization, such that the obtained sucralose crystals have a single crystal form, are completely crystallized, have a regular shape, extremely high purity, nice color, high accumulation density, and long storage time, and can meet the requirements of high-end products for sugar substitutes.
C07H 5/02 - Composés contenant des radicaux saccharide dans lesquels les liaisons carbone-oxygène ont été remplacées par le même nombre de liaisons carbone-hétéro-atomes à des atomes d'halogènes, d'azote, de soufre, de sélénium ou de tellure à des halogènes
Provided is a preparation method for sucrose-6-carboxylate. The method of the present application comprises: passing a mixed solution containing sucrose, a mixed solvent and an organotin compound through a gas-liquid exchange reactor, and using an anhydrous dehydration medium to quickly remove moisture generated in a reaction system, so as to efficiently prepare a sucrose organotin ester intermediate. The method can rapidly realize an esterification dehydration reaction in an extremely short time; has good sucrose-6-carboxylate selectivity and a high yield of same; has few side reactions; has a simple reaction process and is simple to operate; is especially suitable for large-scale industrial production; and overcomes the defects of a long reaction time, high energy consumption, many side reactions, operation complexity, a low yield, etc. in the traditional preparation of sucrose-6-carboxylate.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 1/00 - Procédés de préparation des dérivés du sucre
B01J 10/00 - Procédés chimiques généraux faisant réagir un liquide avec des milieux gazeux autrement qu'en présence de particules solidesAppareillage spécialement adapté à cet effet
Provided is a refining method for acesulfame. The method comprises: adding hydrogen peroxide and activated carbon into an acesulfame-containing crude product solution, keeping same at a first preset temperature for a first preset time, and filtering same to obtain an acesulfame mother solution; concentrating the acesulfame mother solution to a preset concentration so as to obtain a concentrated solution, and leaving the concentrated solution to stand at a second preset temperature for a second preset time to form acesulfame crystal nucleuses, so as to obtain a crystal-nucleus-containing solution; subjecting the crystal-nucleus-containing solution to programmed cooling, so as to acquire a solution containing a large amount of acesulfame crystals; and subjecting the solution containing a large amount of acesulfame crystals to centrifugation, washing and drying, so as to acquire an acesulfame crystal product. The present invention has the beneficial effects of obtaining a high-quality and high-purity crystal product with low impurity content by means of controlling the crystallization procedure and process, thus significantly improving the purity and quality of the acesulfame crystals; and the process is simple, has mild and controllable conditions, has low technical requirements in terms of equipment and personnel, and is very suitable for large-scale industrial production.
The present application provides a post-treatment method of a sucrose-6-carboxylic ester chlorination reaction liquid. The method comprises: adding ammonia water or water into the sucrose-6-carboxylic ester chlorination reaction liquid to perform a primary neutralization reaction; introducing ammonia gas into the obtained reaction liquid at a preset temperature, adjusting the pH value to a preset alkaline range, and continuously keeping the reaction for a period of time at a reaction temperature; and adding acid into the reaction liquid obtained in the ammonia gas neutralization step, and adjusting the pH value to a preset acidity range. In the present invention, a small amount of ammonia water or water is added, so that the subsequent ammonia gas absorption efficiency can be effectively improved, and an ammonia gas utilization rate is increased; generation of a hydrolysis side reaction of sucrose-6-carboxylic ester is avoided, and the conversion rate and selectivity of the reaction are improved; an organic solvent recovered by subsequent distillation can be directly recycled only by means of simple treatment, so that tedious procedures such as dehydration and rectification treatment on the organic solvent are reduced. The problems such as generation of a large amount of wastewater and treatment of the wastewater are avoided, and the production cost is greatly reduced.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
The present application provides a method for preparing sucrose-6-ester, comprising: preparing a reaction solution of sucrose and an organotin compound; atomizing the reaction solution to form small droplets; fully mixing and contacting the small droplets with a gasified dehydration medium to cause the small droplets to undergo a dehydration reaction, so as to produce an intermediate mixture containing sucrose-organotin ester small droplets; separating the intermediate mixture to obtain a sucrose-organotin ester solution and a dehydrated gas-liquid mixture; recovering the sucrose-organotin ester solution obtained in the separation step and recycling same to the atomization step and the dehydration step several times; subjecting the sucrose-organotin ester solution to an acylation reaction with an organic acid anhydride to produce sucrose-6-ester. The present application can enable rapid and efficient dehydration in an esterification reaction within a short period of time, to efficiently prepare a sucrose-organotin ester intermediate, thereby reducing decomposition of saccharide substances and occurrence of side reactions in the system to a great extent; moreover, the energy consumption is low, the product yield is high, the selectivity is strong, and the sucrose reaction is more thorough.
C07H 13/04 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques comportant les radicaux carboxyle estérifiants liés à des atomes de carbone acycliques
C07H 13/02 - Composés contenant des radicaux saccharide estérifiés soit par l'acide carbonique ou ses dérivés, soit par des acides organiques, p. ex. acides phosphoniques par des acides carboxyliques
C07H 1/00 - Procédés de préparation des dérivés du sucre
30 - Aliments de base, thé, café, pâtisseries et confiseries
Produits et services
Aromatic preparations for food; essences for foodstuffs,
except etheric essences and essential oils; flavorings,
other than essential oils, for cakes; flavorings, other than
essential oils, for beverages.
30 - Aliments de base, thé, café, pâtisseries et confiseries
Produits et services
Aromatic preparations for food in nature of scented water for flavoring beverages, and Flavourings, other than essential oils, for foods; essences for foodstuffs, except etheric essences and essential oils, namely, coffee essences; flavorings, other than essential oils, for cakes; flavorings, other than essential oils, for beverages
30 - Aliments de base, thé, café, pâtisseries et confiseries
Produits et services
(1) Additives for use as food flavouring; beverage flavourings; bread flavoured with spices; cake flavouring extracts; flavourings for butter; flavourings for cheeses; flavourings for soups; food flavourings; food seasonings; fruit flavourings; vanilla flavorings
01 - Produits chimiques destinés à l'industrie, aux sciences ainsi qu'à l'agriculture
Produits et services
Methyl alcohol (methanol) for industrial purposes; Formaldehyde; artificial sweeteners; Acesulfame Potassium being artificial sweetener; adhesives for industrial purposes; chemicals for use in industry, namely, firming agents; melamine
30 - Aliments de base, thé, café, pâtisseries et confiseries
Produits et services
Flavorings for beverages; Flavorings for beverages, other than essential oils; Flavourings and seasonings; Flavourings, other than essential oils, for cakes; Food additives for non-nutritional purposes for use as a flavoring; Food flavourings
