A gas chromatography system for high-purity chlorine trifluoride, comprising a sample pretreatment unit (1), a negative pressure sampling unit (3), a carrier gas unit (4), and a test unit (5). The negative pressure sampling unit (3) can effectively implement a sampling operation of a chlorine trifluoride sample by means of a negative pressure sampling/sample introduction mode, so as to ensure that when leaking, a chlorine trifluoride pipeline will not leak a chlorine trifluoride gas to ensure the safety of analysts and the environment, and can effectively keep the purity of the chlorine trifluoride sample under test, so as to ensure the precision of a subsequent test result. The whole test process of the test unit (5) can be continuously carried out and, during the test process, tested samples can all enter a second adsorption tank (7) to be decontaminated and then discharged, thereby obviously reducing mutual effects among three tests so as to improve test precision and greatly improve the test efficiency of the samples.
A packing layer bed in a chlorine trifluoride distillation column, a preparation method therefor and a use method thereof, comprising the following steps: S1, leveling nickel chloride, placing same in a tray, placing into an oven for initial baking, to remove moisture, and drying at a high temperature until brownish yellow, and crushing the baked nickel chloride powder; S2, mixing the nickel chloride with sodium chloride powder and sintering to obtain particles, to obtain a packing layer bed. By means of optimizing the distribution ratio of a packing section of a reaction chamber, the proportion of nickel used to adhere to the hydrogen fluoride in chlorine trifluoride is increased, thereby improving distillation yield.
Provided in the present invention are a one-step synthesis method for chlorine trifluoride and a device. The method comprises: S1, providing stable fluorine gas and chlorine gas, and fully mixing the fluorine gas and the chlorine gas at a stoichiometric ratio to form mixed gas; and S2, introducing the gas mixture into a microchannel reactor, and controlling the reaction temperature to prepare chlorine trifluoride gas, wherein the material of the microchannel reactor is selected from a corrosion-resistant nickel-based alloy, the nickel-based alloy undergoes a passivation reaction with the chlorine gas and the fluorine gas, and by means of control over the parameters of the reaction process, a graded fluorinated film with a porous structure is generated. The graded fluorinated film can effectively disperse hydrogen fluoride-fluorine gas molecular groups, thereby forming effective active groups of fluorine and chlorine, so that the synthesis conversion rate of chlorine trifluoride is improved, the corrosiveness of chlorine trifluoride on metal materials is greatly reduced, and the conversion efficiency is greatly improved.
22222-NaF framework. The special modified sodium fluoride adsorbent can effectively disperse chlorine trifluoride and hydrogen fluoride molecules; the optimal adsorption efficiency thereof for hydrogen fluoride is improved to 98% or more; and the optimal adsorption efficiency thereof for chlorine trifluoride is reduced to about 3%. Furthermore, the special modified sodium fluoride adsorbent has a simple manufacturing process, a low production cost, and good economic benefits, and can be subjected to industrial production.
B01J 20/04 - Solid sorbent compositions or filter aid compositionsSorbents for chromatographyProcesses for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
B01J 20/30 - Processes for preparing, regenerating or reactivating
B01D 53/02 - Separation of gases or vapoursRecovering vapours of volatile solvents from gasesChemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases or aerosols by adsorption, e.g. preparative gas chromatography
Provided is a production method for recovering and purifying electronic-grade hexafluoroethane from industrial waste gas resulting from the production of carbon tetrafluoride. The production method comprises: conveying hexafluoroethane-containing carbon tetrafluoride waste gas to a vaporizer and a gas buffer device which are connected in sequence; pressurizing the gas by means of a diaphragm compressor, and then introducing same into an adsorption device, wherein the adsorption device comprises a first high-pressure adsorption tower, a second high-pressure adsorption tower, and a third high-pressure adsorption tower, which is filled with a fluoride adsorbent having a high cohesive energy density; then introducing same into a precision filter for filtering, returning the carbon tetrafluoride gas introduced into the top of a low-boiling-point rectifying tower to a carbon tetrafluoride production system, and introducing a tower-bottom liquid to a first high-boiling-point tower via a valve group; and bringing hexafluoroethane gas containing high-boiling-point impurities into the first high-boiling-point tower, then removing the high-boiling-point impurities at the bottom of the tower, bringing hexafluoroethane, which contains a small amount of high-boiling-point impurities and is discharged from the top of the tower, into a second high-boiling-point tower via a valve group, and bringing product gas at the top of the second high-boiling-point tower, namely electronic-grade hexafluoroethane, into a product tank.
222O additive to SiCO ceramic powder, and sintering at 310-330°C for 18-22 hours; S2, after grinding the sintered material to 2-3 mm, mixing same with polyacrylonitrile to form a composite polymer; and S3, shaping the composite polymer by vacuum baking at 75-85°C, and then ball milling and sieving to form the high-cohesive-energy fluoride adsorbent. Also provided are an adsorbent prepared by the method and an application thereof.
B01J 20/30 - Processes for preparing, regenerating or reactivating
B01D 53/02 - Separation of gases or vapoursRecovering vapours of volatile solvents from gasesChemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases or aerosols by adsorption, e.g. preparative gas chromatography
7.
ELECTRONIC GRADE CHLORINE TRIFLUORIDE SEPARATION DEVICE, AND SEPARATION METHOD
An electronic grade chlorine trifluoride separation device, and a separation method therefor. The separation method comprises: S1, heating an alkali metal adsorbent in a three-stage layered metal adsorbent bed, so that the alkali metal adsorbent is associated with hydrogen fluoride molecules to form firmer hydrogen bonds for separation, to achieve primary purification; and S2, further dissociating hydrogen fluoride and chlorine trifluoride association molecules by means of a two-stage cryogenic distillation device, to achieve secondary purification.
B01D 53/02 - Separation of gases or vapoursRecovering vapours of volatile solvents from gasesChemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases or aerosols by adsorption, e.g. preparative gas chromatography
Provided is a rectification device for electronic grade chlorine trifluoride. The device comprises two stages of low-temperature rectification devices, wherein an extraction agent for dispersing associated molecules of hydrogen fluoride and chlorine trifluoride is arranged in each stage of low-temperature rectification device. Further provided are a rectification method using the rectification device, a purification system comprising the device, and a control method for the purification system. By means of the device, the stability of reflux ratio parameters of a gas-liquid (chlorine trifluoride-hydrogen fluoride) phase equilibrium system can be effectively improved by means of tower plate temperature control, wide dynamic equilibrium operation under various working conditions is achieved, and therefore, effective separation of chlorine trifluoride from various impurity components is achieved by means of deep rectification, resulting in purified electronic grade chlorine trifluoride.
patents