CN117482864A - Preparation system and method of electronic grade chlorine trifluoride - Google Patents
Preparation system and method of electronic grade chlorine trifluoride Download PDFInfo
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- CN117482864A CN117482864A CN202311411118.9A CN202311411118A CN117482864A CN 117482864 A CN117482864 A CN 117482864A CN 202311411118 A CN202311411118 A CN 202311411118A CN 117482864 A CN117482864 A CN 117482864A
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- chlorine
- chlorine trifluoride
- gas
- fluorine gas
- trifluoride
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- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims description 20
- 239000007789 gas Substances 0.000 claims abstract description 141
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 114
- 239000011737 fluorine Substances 0.000 claims abstract description 114
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 114
- 238000000746 purification Methods 0.000 claims abstract description 61
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000460 chlorine Substances 0.000 claims abstract description 49
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 49
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 37
- 238000011049 filling Methods 0.000 claims abstract description 31
- 238000009833 condensation Methods 0.000 claims abstract description 28
- 230000005494 condensation Effects 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 56
- 239000012535 impurity Substances 0.000 claims description 42
- 238000007872 degassing Methods 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 18
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 0.000 claims description 15
- 239000002808 molecular sieve Substances 0.000 claims description 14
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 14
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 12
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000005868 electrolysis reaction Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000005796 dehydrofluorination reaction Methods 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000000066 reactive distillation Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 18
- 239000012530 fluid Substances 0.000 description 16
- 230000015572 biosynthetic process Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 239000003507 refrigerant Substances 0.000 description 11
- 230000006872 improvement Effects 0.000 description 9
- 239000012528 membrane Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000001308 synthesis method Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/24—Inter-halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/005—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation system and a preparation method of electronic grade chlorine trifluoride, wherein the preparation system comprises the following steps: the raw material purifying unit comprises a chlorine purifying device and a fluorine purifying device which are arranged in parallel; the micro-channel reactor comprises a lower layer mixing section for mixing chlorine and fluorine gas and a catalyst section for catalyzing the chlorine and the fluorine gas to generate chlorine trifluoride; a primary purification unit comprising a condensation separation structure; the purification unit comprises a metal adsorption structure and a rectification structure, and the metal adsorption structure and the rectification structure remove hydrogen fluoride gas in the chlorine trifluoride separated by the condensation separation structure; the filling unit comprises a gaseous maintaining structure and an automatic filling structure connected with the gaseous maintaining structure, and adopts three steps of raw material purification and preliminary purification, metal-based fluoride adsorption and reactive distillation to purify the chlorine trifluoride to 99.995 percent so as to reach the standard of electronic grade use.
Description
Technical Field
The invention relates to a preparation device of chlorine trifluoride, in particular to a preparation system of electronic grade chlorine trifluoride and a method thereof.
Background
Chlorine trifluoride is a new generation of green environment-friendly semiconductor new dry in-situ etching cleaning agent, has extremely high etching rate and cleaning efficiency, and is mainly applied to chip manufacturing; meanwhile, the chlorine trifluoride has extremely strong oxidizing property and is applied to the fields of special advanced materials and special major equipment manufacturing.
The existing internationally-based chlorine trifluoride production process mainly adopts a three-step synthesis and traditional purification technology represented by central nitrate in Japan, and has the problems of low product purity, high production cost, poor safety, high energy consumption and the like, and the existing domestic patent technology also has some chlorine trifluoride synthesis and purification methods, such as: the patent with publication number (CN 113562699A) discloses a purification system and a preparation system of high-purity grade chlorine trifluoride, wherein the system only uses two steps of adsorption and rectification for purification, and has the defect of low purification efficiency; further, as disclosed in the patent with publication number (CN 104477849 a), a synthesis method and a purification method of chlorine trifluoride are disclosed, in which fluorine gas and inert gas are mixed to synthesize chlorine trifluoride, and the synthesis method has the disadvantages of low synthesis efficiency and increased purification difficulty, and the like.
The scheme aims to provide a preparation system and a preparation method of electronic grade chlorine trifluoride, which adopt three steps of raw material purification and preliminary purification, metal-based fluoride adsorption and reactive distillation to purify the chlorine trifluoride to 99.995%, reach the standard of electronic grade use, and reduce the most important impurity HF in the chlorine trifluoride to below 50ppmv, which is at least 1 order of magnitude higher than the existing electronic grade product.
Disclosure of Invention
The invention provides a system and a method for preparing electronic grade chlorine trifluoride, which can effectively solve the problems.
The invention is realized in the following way:
a system for preparing electronic grade chlorine trifluoride comprising:
the raw material purifying unit comprises a chlorine purifying device and a fluorine purifying device which are arranged in parallel, wherein the chlorine purifying device is connected with a chlorine inlet end and is used for physically drying the introduced chlorine, and the fluorine purifying device is connected with an outlet end of an electrolytic tank and is used for carrying out dehydrofluorination treatment on fluorine;
the micro-channel reactor comprises an air inlet section connected with the chlorine purification device and the fluorine gas purification device, a lower layer mixing section for mixing the chlorine gas and the fluorine gas, and a catalyst section for catalyzing the chlorine gas and the fluorine gas to generate chlorine trifluoride;
a primary purification unit comprising a condensation separation structure for receiving chlorine trifluoride, the condensation separation structure for separating chlorine trifluoride gas from liquid impurities;
the purification unit comprises a metal adsorption structure and a rectification structure, and the metal adsorption structure and the rectification structure remove hydrogen fluoride gas in the chlorine trifluoride separated by the condensation separation structure;
and the filling unit comprises a gaseous maintaining structure and an automatic filling structure connected with the gaseous maintaining structure.
As a further improvement, the chlorine purification device comprises a plurality of molecular sieves, wherein the molecular sieves are 3A molecular sieves or 13X molecular sieves.
As a further improvement, the fluorine gas purification device comprises a precooling tank body connected with the gas outlet end of the electrolytic tank and a degassing tank body connected with the gas outlet end of the precooling tank body; an adsorber connected with the degassing tank and used for adsorbing hydrogen fluoride in fluorine gas.
As a further improvement, the catalyst section is built up from nickel-based metal.
As a further improvement, the primary purification unit further comprises a tail gas collecting and treating structure connected with the condensation and separation structure, and impurities separated by the condensation and separation structure are introduced into the tail gas collecting and treating structure for preparing carbon tetrafluoride.
The invention also provides a preparation method of the electronic grade chlorine trifluoride, which is applied to the preparation system of the electronic grade chlorine trifluoride and comprises the following steps:
s1, performing S1; purifying raw materials: introducing chlorine into a chlorine purification device, performing multistage physical drying on the chlorine, introducing impurity-containing chlorine generated by electrolysis into a fluorine gas purification device for purification, removing hydrogen fluoride in fluorine gas, and introducing dried chlorine and purified fluorine gas into a microchannel reactor;
s2, performing S2; preparation of chlorine trifluoride: the introduced fluorine gas and chlorine gas enter a lower mixing section in the microchannel reactor, the chlorine gas and the fluorine gas are fully mixed through a plurality of channels in the lower mixing section, and chlorine trifluoride and impurities are generated under the catalysis of a catalyst section;
s3, performing S3; impurity primary purification: condensing generated chlorine trifluoride and impurities through a condensation separation structure, separating fluorine gas and chlorine monofluoride impurities in the chlorine trifluoride, and realizing primary purification and collection of the chlorine trifluoride;
s4, performing S4; impurity is refined: introducing the separated chlorine trifluoride into a purification unit for purification, and removing hydrogen fluoride gas in the chlorine trifluoride to realize that the purity of the chlorine trifluoride reaches 99.995%;
s5, performing S5; chlorine trifluoride is fully automatically filled into the filling tank in a gaseous state.
As a further improvement, the S1 specifically includes:
s11, performing S11; introducing fluorine gas into a precooling tank body for precooling;
s12, performing S12; enabling the pre-cooled fluorine gas to pass through a degassing tank body with lower temperature, condensing and precipitating hydrogen fluoride in the fluorine gas, and reducing the hydrogen fluoride in the fluorine gas;
s13, performing S13; the fluoride in the fluorine gas is physically adsorbed by the metal fluoride in the adsorber, and the hydrogen fluoride in the fluorine gas is reduced again.
As a further improvement, the temperature in the precooling tank body is-80 ℃ to-85 ℃.
As a further improvement, the temperature in the degassing tank is-85 ℃ to-90 ℃.
As a further improvement, the step S3 further includes: the impurities after condensation and separation are collected by a separate tail gas collecting and treating structure and then are used for preparing carbon tetrafluoride.
The beneficial effects of the invention are as follows:
the raw materials of the invention contain chlorine and fluorine gas, the moisture in the chlorine can influence the synthesis process and generate acid substances such as HF, so that the chlorine is subjected to multistage physical drying through a chlorine purification device, the water content of the chlorine is greatly reduced, thereby avoiding the generation of hydrofluoric acid, when the fluorine gas is provided, the fluorine gas is generated by electrolysis of an electrolytic tank special for chlorine trifluoride, the shape and structure of a carbon plate in the electrolytic tank are optimized, the desorption capacity and the bearing current density of the fluorine gas are enhanced, the yield of the fluorine gas is improved, the entrainment quantity of hydrogen fluoride is reduced, and the fluorine gas is subjected to the hydrogen fluoride removal treatment through a fluorine gas purification device, so that the fluorine gas can meet the requirements of synthesizing the chlorine trifluoride.
The existing synthesis method is generally low in synthesis efficiency, excessive impurities such as chlorine fluoride and the like are generated in the reaction process, so that the treatment difficulty of the rear end is increased, the novel reactor in a micro-channel mode is innovatively used for solving the current situation that the synthesis efficiency of chlorine trifluoride is low, purified chlorine and fluorine gas are directly introduced into the micro-channel reactor, the micro-channel reactor is divided into two sections, the lower section is a lower mixing section, each channel is of a structure combining a Y type with an inverted Y type of 0.1-0.5mm, the efficiency of the first-step reaction of fluorine gas and fluorine gas is improved, the upper end is a catalyst section piled up by nickel-based metal, the synthesis efficiency of the chlorine trifluoride is improved, and the outlet concentration of the chlorine trifluoride after the reaction of the micro-channel reactor is more than or equal to 93%.
In the invention, the chlorine trifluoride generated by a microchannel reactor has higher purity, but still has substances such as fluorine gas, chlorine monofluoride and the like, and the purity of the chlorine trifluoride can be directly influenced, so that a primary purification unit is adopted to pretreat the chlorine trifluoride firstly, the pretreatment is to collect the chlorine trifluoride by utilizing the difference of boiling points of the chlorine trifluoride and other impurities and using a condensation mode, and the substances such as fluorine gas, chlorine monofluoride and the like are separated, so that the primary purification and collection of the chlorine trifluoride are realized;
in the process of treating substances such as fluorine gas, chlorine monofluoride and the like, the fluorine gas which is not completely consumed and the byproduct chlorine monofluoride can produce carbon tetrafluoride after being treated by a tail gas collecting and treating structure, and the produced carbon tetrafluoride is used for purifying electronic grade carbon tetrafluoride, so that the comprehensive treatment of waste gas is realized.
After separating fluorine gas, chlorine monofluoride and other substances, hydrogen fluoride exists in chlorine trifluoride, interaction force exists between chlorine trifluoride molecules and hydrogen fluoride molecules, complex and stable planar chain-shaped and annular polymers are easily formed by association, and hydrogen fluoride is difficult to separate from chlorine trifluoride.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a system for preparing electronic grade chlorine trifluoride according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for preparing electronic grade chlorine trifluoride according to a second embodiment of the present invention.
Fig. 3 is a schematic structural view of a degassing tank according to a third embodiment of the present invention.
Fig. 4 is a schematic front view of a driving structure and a cold air circulation structure according to a third embodiment of the present invention.
Fig. 5 is a schematic structural diagram of a cold air circulation structure according to a third embodiment of the present invention.
Detailed Description
For the purpose of making embodiments of the present invention fall within the scope of the present invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as referring to purposes, technical solutions and advantages of the present invention in any way. All other implementations, which can be derived by a person skilled in the art without making any inventive effort, show or imply relative importance or implicitly indicate the number of technical features indicated on the basis of the implementations in the invention. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Example 1
Referring to fig. 1 to 5, a system for preparing electronic grade chlorine trifluoride comprises: the raw material purifying unit 10, wherein the raw material purifying unit 10 comprises a chlorine purifying device 11 and a fluorine gas purifying device 12 which are arranged in parallel, the chlorine purifying device 11 is connected with a chlorine inlet end and is used for physically drying the introduced chlorine, and the fluorine gas purifying device 12 is connected with an outlet end of an electrolytic tank and is used for carrying out dehydrofluorination treatment on fluorine gas; a micro-channel reactor 20, wherein the micro-channel reactor 20 comprises an air inlet section connected with the chlorine purifying device 11 and the fluorine purifying device 12, a lower layer mixing section 21 for mixing chlorine and fluorine, and a catalyst section 22 for catalyzing the chlorine and the fluorine to generate chlorine trifluoride; a primary purification unit 30, the primary purification unit 30 comprising a condensation separation structure for receiving chlorine trifluoride, the condensation separation structure for separating chlorine trifluoride gas from liquid impurities; a purifying unit 40, wherein the purifying unit 40 comprises a metal adsorption structure 41 and a rectification structure 41, and the metal adsorption structure 41 and the rectification structure 41 remove hydrogen fluoride gas in the chlorine trifluoride separated by the condensation separation structure; a filling unit 50, said filling unit 50 comprising a gaseous holding structure and an automatic filling structure connected to said gaseous holding structure.
In this embodiment, the chlorine purifying device 11 includes a plurality of molecular sieves, wherein the molecular sieves may be 3A molecular sieves or 13X molecular sieves.
In this embodiment, the fluorine gas purifying device 12 includes a pre-cooling tank 121 connected to the outlet end of the electrolytic tank, and a degassing tank 122 connected to the outlet end of the pre-cooling tank 121; an adsorber 123 connected to the degassing tank 122 and used for adsorbing hydrogen fluoride in fluorine gas, purifying the fluorine gas by adopting a mode of 1+2+1, wherein the first step is pre-cooling the fluorine gas (the temperature is-80 ℃ to-85 ℃), using a substance with large specific heat capacity as a refrigerant, improving the controllability of the pressure of the fluorine gas in the system, reducing the possibility of liquefying the fluorine gas and improving the safety; the second step is to remove hydrogen fluoride by 2-level deep low-temperature freezing (the temperature is-85 ℃ to-90 ℃), so as to further reduce the hydrogen fluoride in the fluorine gas; and thirdly, carrying out physical deep adsorption on hydrogen fluoride in the fluorine gas by utilizing metal fluoride, so that the fluorine gas can meet the synthesis requirement.
The raw materials of the embodiment contain chlorine and fluorine gas, the moisture in the chlorine can influence the synthesis process and generate acidic substances such as HF, so that the chlorine is subjected to multistage physical drying through a molecular sieve, the water content of the chlorine is greatly reduced, thereby avoiding the generation of hydrofluoric acid, when the fluorine gas is provided, the fluorine gas is generated by electrolysis of an electrolytic tank special for chlorine trifluoride, the shape and structure of a carbon plate in the electrolytic tank are optimized, the desorption capacity and the bearing current density of the fluorine gas are enhanced, the entrainment amount of the hydrogen fluoride is reduced while the yield of the fluorine gas is improved, and the fluorine gas is subjected to the hydrogen fluoride removal treatment through a precooling tank body 121, a gas removal tank body 122 and an absorber 123, so that the fluorine gas can meet the requirement of synthesizing the chlorine trifluoride.
The provided raw materials are purer by treating the two raw materials, so that the impurities are fewer, and the impurities generated during the generation of the chlorine trifluoride are fewer, thereby laying a good foundation for the purity of the chlorine trifluoride.
The existing synthesis method is generally low in synthesis efficiency, excessive impurities such as chlorine fluoride and the like are generated in the reaction process, so that the treatment difficulty of the rear end is increased, the novel reactor in a micro-channel mode is innovatively used for solving the current situation that the synthesis efficiency of chlorine trifluoride is low, purified chlorine and fluorine gas are directly introduced into the micro-channel reactor 20, the micro-channel reactor 20 is divided into two sections, the lower section is a lower mixing section 21, each channel is of a structure combining a Y type with an inverted Y type with 0.1-0.5mm, so that the efficiency of the first-step reaction of fluorine gas and fluorine gas is improved, the upper end is a catalyst section 22 stacked by nickel-based metal, so that the synthesis efficiency of chlorine trifluoride is improved, the outlet concentration of the chlorine trifluoride after the reaction of the micro-channel reactor 20 is more than or equal to 93%, and preferably, the catalyst section 22 is stacked by the nickel-based metal.
The purity of the chlorine trifluoride generated by the microchannel reactor 20 is relatively high, but the chlorine trifluoride is still provided with substances such as fluorine gas, chlorine monofluoride and the like, and the purity of the chlorine trifluoride can be directly influenced, so the primary purification unit 30 is adopted to pretreat the chlorine trifluoride firstly, the chlorine trifluoride is collected by utilizing the difference of boiling points of the chlorine trifluoride and other impurities in the pretreatment, the substances such as fluorine gas, chlorine monofluoride and the like are separated by using a condensation mode, and the primary purification and collection of the chlorine trifluoride are realized;
in the process of treating substances such as fluorine gas, chlorine monofluoride and the like, the primary purification unit 30 further comprises a tail gas collecting and treating structure 31 connected with the condensation and separation structure, impurities separated by the condensation and separation structure are introduced into the tail gas collecting and treating structure 31 to prepare carbon tetrafluoride, so that unconsumed complete fluorine gas and byproduct chlorine monofluoride can be treated by the tail gas collecting and treating structure 31 to produce carbon tetrafluoride, and the produced carbon tetrafluoride is used for purifying electronic grade carbon tetrafluoride to realize comprehensive treatment of waste gas, wherein the tail gas collecting and treating structure 31 can be a rectifying tower or other adsorption structures.
After separating fluorine gas, chlorine monofluoride and other substances, hydrogen fluoride exists in chlorine trifluoride, interaction force exists between chlorine trifluoride molecules and hydrogen fluoride molecules, complex and stable planar chain-shaped and annular polymers are easily formed by association, and hydrogen fluoride is difficult to separate from chlorine trifluoride.
After the purity of the chlorine trifluoride is prepared to 99.995%, the chlorine trifluoride is required to be filled into a filling tank, but the filling of the electronic-grade chlorine trifluoride has a plurality of difficulties, wherein the most difficult is the selection of the filling equipment and the efficient and safe planning of the filling flow by the strong corrosiveness of the chlorine trifluoride, so the gaseous filling mode adopted in the embodiment reduces the corrosion of products to facility equipment, and the innovative filling mode using the variable temperature improves the safety performance, and adds inert protective gas, full-automatic filling devices and the like, thereby comprehensively ensuring the high efficiency and safety of the chlorine trifluoride filling, and the specific filling steps are as follows:
a1; establishing a connection relationship between the filling tank and a filling control system of the temperature difference type isolation filling cabinet;
a2; a pretreatment pipeline is built, and pretreatment is carried out on the interior of the filling tank through the pretreatment pipeline;
a3; after the connection of the filling tank is completed, introducing chlorine trifluoride liquid into the air supply unit, changing the phase state change of the chlorine trifluoride by controlling the temperature difference, and pressurizing the chlorine trifluoride gas in the air supply unit to ensure that the chlorine trifluoride gas is transmitted to the rear end;
a4; conveying chlorine trifluoride gas at constant temperature, and establishing an inert gas layer on the outer side of the pipeline for protection;
a5; the temperature difference type isolation filling cabinet receives constant-temperature chlorine trifluoride gas, and the temperature of the chlorine trifluoride gas is reduced through the temperature difference type isolation filling cabinet, and the chlorine trifluoride gas is liquefied into liquid in the filling tank and is stored in the filling tank.
The step A3 specifically includes:
a31; the temperature is controlled to be between minus 30 ℃ and 0 ℃ by a temperature control unit, and the normal gas-liquid two-phase state of the chlorine trifluoride liquid during storage is maintained;
a32; the temperature is regulated to 0-50 ℃ by a temperature control unit, the phase state of the chlorine trifluoride is changed, and the chlorine trifluoride liquid is gasified into chlorine trifluoride gas;
a33; the pressure in the air supply unit is kept between 0.2MPa and 0.3MPa, and charging power is provided for chlorine trifluoride gas.
Embodiment two:
referring to fig. 2, the present embodiment also provides a method for preparing electronic grade chlorine trifluoride, which is applied to the system for preparing electronic grade chlorine trifluoride in the first embodiment, and includes the following steps:
s1, performing S1; purifying raw materials: introducing chlorine into a chlorine purification device 11, performing multistage physical drying on the chlorine, introducing impurity-containing chlorine generated by electrolysis into a fluorine gas purification device 12 for purification, removing hydrogen fluoride in fluorine gas, and introducing dried chlorine and purified fluorine gas into a microchannel reactor 20;
s2, performing S2; preparation of chlorine trifluoride: the introduced fluorine gas and chlorine gas enter a lower mixing section 21 in the microchannel reactor 20, the chlorine gas and the fluorine gas are fully mixed through a plurality of channels in the lower mixing section 21, and chlorine trifluoride and impurities are generated under the catalysis of a catalyst section 22;
s3, performing S3; impurity primary purification: condensing generated chlorine trifluoride and impurities through a condensation separation structure, separating fluorine gas and chlorine monofluoride impurities in the chlorine trifluoride, and realizing primary purification and collection of the chlorine trifluoride;
s4, performing S4; impurity is refined: introducing the separated chlorine trifluoride into a purification unit 40 for purification, and removing hydrogen fluoride gas in the chlorine trifluoride to achieve the purity of the chlorine trifluoride to 99.995%;
s5, performing S5; chlorine trifluoride is fully automatically filled into the filling tank in a gaseous state.
Further, the S1 specifically includes:
s11, performing S11; fluorine gas is firstly introduced into the precooling tank body 121 for precooling;
s12, performing S12; the pre-cooled fluorine gas passes through the degassing tank 122 with lower temperature, so that the hydrogen fluoride in the fluorine gas is condensed and precipitated, and the hydrogen fluoride in the fluorine gas is reduced;
s13, performing S13; the metal fluoride in the adsorber 123 physically adsorbs fluoride in the fluorine gas, and hydrogen fluoride in the fluorine gas is reduced again.
Preferably, the temperature in the pre-cooling tank 121 is-80 ℃ to-85 ℃, and the temperature in the degassing tank 122 is-85 ℃ to-90 ℃.
Further, the step S3 further includes: the condensed and separated impurities are collected by a separate tail gas collection structure 31 for use in the preparation of carbon tetrafluoride.
Embodiment III:
the present embodiment is different from the first embodiment in that: a specific description will be given of the deaeration tank 122 in the first embodiment, with reference to fig. 1, 3 to 5:
the degassing tank 122 includes a second feeding pipe 1221 connected to the air inlet end of the pre-cooling tank 121, a reaction chamber 1222 disposed in the pre-cooling tank 121 and communicating with the second feeding pipe 1221 at intervals, a unidirectional flow plate 1223 disposed at the top of the reaction chamber 1222, the unidirectional flow plate 1223 having an equal diameter with the inner diameter of the pre-cooling tank 121, a cooling chamber 1224 nested below the reaction chamber 1222, an air guide chamber 1225 formed between the reaction chamber 1222, the cooling chamber 1224 and the inner wall of the pre-cooling tank 121, the cooling chamber 1224 includes a cooling cylinder 12241 filled with a refrigerant, a plurality of waterproof membranes 12242 disposed in the middle of the cooling cylinder 12241, a mounting cylinder 12243 inserted in the bottom of the cooling cylinder 12241 and extending to the bottom of the degassing tank 122, and a driving structure 1224 disposed outside the mounting cylinder 12243, wherein the driving structure 1224 is used for driving the cooling cylinder 12241 to rotate.
The conventional fluorine gas impurity removal process all needs to be condensed and cooled, thereby precipitating high-boiling impurities, improving the purity of the fluorine gas, further guaranteeing the purity of the chlorine trifluoride, and often adopting a condenser tube arrangement mode in the existing condensation structure, but in practice, because the large-area occupation ratio of the purification tank body and the coil-shaped condenser tube have a certain gap, the cooling temperature of the whole purification tank body is difficult to guarantee in the raw material purification process, and the fluorine gas is easy to liquefy when the cooling temperature is not fine enough, thereby leading to the non-accident loss of the fluorine gas, improving the production cost and also affecting the purity of the fluorine gas, and aiming at the problems: in this embodiment, the degassing tank 122 in the purification tank is divided into two parts, one part is a cooling chamber 1224, the other part is an air guide chamber 1225, so that impurities in the fluid introduced into the degassing tank 122 are directly condensed in the cooling chamber 1224, the condensed impurity liquid is directly sunk, the rest gas is directly led out from the waterproof membrane 12242 to the air guide chamber 1225, and is led out from the top of the degassing tank 122 through the air guide chamber 1225, the arrangement area of the condensation structure can be reduced by adopting the cooling cylinder 12241 in the cooling chamber 1224, and the contact area between the cylindrical and full-contact cooling cylinder 12241 and the fluid is increased, so that the impurity removing effect is achieved, meanwhile, the cost is saved, and the gas separation mode of the separated chambers is not easy to lead the fluorine element to be lost.
Compared with the mode of directly setting the condenser pipe in the intermediate layer in prior art, adopt the cooling cylinder 12241 of small tracts of land not only can guarantee the temperature of condensation, improve simultaneously again greatly with fluidic contact surface, can guarantee the same condensation effect with the bulky condenser pipe.
In the process of contacting the fluid with the cooling cylinder 12241, the fluid is in a motion state and can be fully influenced by low temperature, however, if the fluid is directly rotated, the pressure in the cooling cylinder 12241 is easy to change, so that part of impurity liquid seeps out through the waterproof membrane 12242 and the purity of fluorine is easy to influence, so that the position of the cooling cylinder 12241 is changed by adopting a mode of rotating the cooling cylinder 12241, thereby promoting the flow of the fluid in the cooling cylinder 12241 to a certain extent, ensuring that the contact of the fluid with the cooling cylinder 12241 is more complete, and the speed of separating out the hydrogen fluoride is faster, and in the embodiment, the waterproof membrane 12242 is a PTFE membrane and can resist fluorine and the hydrogen fluoride while blocking water.
In the above description, the fluid is directly introduced into the reaction chamber 1222, and at this time, the fluid is not cooled, and is further mixed with more impurities, if the fluid is not limited, the fluid is easy to be overflowed from the top of the degassing tank 122 to the next stage, so as to affect the purity of fluorine gas, so that in the present invention, a unidirectional flow plate 1223 is disposed at the top of the reaction chamber 1222, and the unidirectional flow plate 1223 includes a forward single-side flow plate 12231 and a reverse single-side flow plate 12232 connected to the outer side of the forward single-side flow plate 12231, where the diameter of the forward single-side flow plate 12231 is equal to the diameter of the reaction chamber 1222, and the forward single-side flow plate 12231 is used to seal the path of gas flowing from the reaction chamber 1222 to the degassing tank 122 and make the liquid in the degassing tank 122 flow from the top to the reaction chamber 1222, and the reverse single-side flow plate 12232 is a ring plate structure, and the reverse single-side flow plate 12232 is used to seal the space above the degassing tank 122 and make the liquid flow from the space above the degassing tank 122 to the space below the degassing tank 122;
wherein the forward single-sided flow plate 12231 of the unidirectional flow plate 1223 is capable of avoiding the direct overflow of the fluid entering the reaction chamber 1222, but although the condensation reaction is said to occur in the cooling chamber 1224 in most cases, as the reaction proceeds and the temperature spreads, the top of the degassing tank 122 is actually in a low temperature state, and it is estimated that some of the fluid will not condense when it is about to flow to the outlet of the degassing tank 122, at this time the condensed fluid can flow into the reaction chamber 1222 through the unidirectional forward single-sided flow plate 12231 until the bottom of the degassing tank 122, and in either case the condensation reaction can be discharged without accumulating in the tank;
if the condensed liquid is discharged into the air guiding chamber 1225, the upward fluorine gas is easy to be blocked, so that the outside of the forward single-side flow plate 12231 is also provided with the reverse single-side flow plate 12232, and the reverse single-side flow plate 12232 and the forward single-side flow plate 12231 are opposite in one-way conduction direction, so that the condensed impurity liquid and the fluorine gas simple substance are not interfered with each other, preferably, an anti-corrosion air pump structure is arranged at a position corresponding to the waterproof membrane 12242, the gas which is permeated from the waterproof membrane 12242 is pumped out directly, and if the leaked liquid is not pumped out due to the large dead weight, the leaked liquid can directly fall to the bottom of the air guiding chamber 1225, and if necessary, the air guiding chamber 1225 can be communicated to the position of the mounting cylinder 12243.
In the present invention, the cooling cylinder 12241 is a hollow and hollow cylinder structure, two sides of the bottom of the cooling cylinder 12241 extend outwards to form an outer butt plate 411, a rotating disc 412 is welded at the bottom of the outer butt plate 411, the driving structure 12244 rotates to drive the rotating disc 412 to rotate so as to make the cooling cylinder 12241 contact with gas uniformly, in order to ensure the gaseous state of fluorine gas, hydrogen with the largest specific heat capacity is used as a refrigerant, the cooling cylinder 12241 is emptied, low-temperature hydrogen is injected into the cooling cylinder 12241 from the position of the outer butt plate 411, and the cooling cylinder 12241 and the outer butt plate 411 rotate under the action of the driving structure 12244 through the rotating disc 412, thereby making the fluid contact with the cooling cylinder 12241 uniformly.
The driving structure 12244 needs to consider the problem of tightness between the driving structure 1224 and the outside in the process of driving the rotating disc 412 to rotate, so as to avoid pollution caused by fluid overflowing to the outside, and in this way, the driving structure 12244 includes a sealing clamping seat 441 clamped on the outer butt plate 411 and the outer side of the rotating disc 412, an engaging wheel 442 arranged on the inner side of the sealing clamping seat 441, and a rotating member 443 for driving the engaging wheel 442 to rotate, where the rotating member 443 is arranged in the degassing tank 122, or the rotating member 443 is arranged outside the degassing tank 122, and the whole driving structure 12244 is limited in a fixed area by the uniform sealing clamping seat 441.
Because the refrigerant adopted in the embodiment is hydrogen, the temperature of the refrigerant is updated in a ventilation mode, and the specific updating structure is as follows: the outer side of the outer butt plate 411 is provided with at least an air inlet pipe and an air outlet pipe, the degassing tank 122 further comprises a cold air circulation structure 1226, and the cold air circulation structure 1226 is connected with the air inlet pipe and the air outlet pipe for ventilation after the cooling cylinder 12241 stops rotating.
The conventional condensation structure is very easy to replace the refrigerant, namely, the refrigerant is injected through the liquid injection pipe at the top, and then the warmed-up refrigerant is output from the liquid outlet end at the bottom, thereby forming a virtuous circle, but in the invention, because the cooling cylinder 12241 is in a rotating state, a fixed circulation mode cannot be formed, so that the invention adopts a fixed-point circulation refrigerant mode, a temperature sensor (not shown in the figure) is arranged in the cooling cylinder 12241, an inductor (not shown in the figure) is arranged on the outer butt plate 411, the temperature sensor is electrically connected with the power end of the driving structure 12244, the inductor is electrically connected with the power end of the driving structure 1224 and the power end of the cold air circulation structure 1226, the cold air circulation structure 1226 comprises a sliding part which is inversely arranged at the inner side of the sealing clamping seat 441, the air inlet guide head 262 and the air outlet guide head 263 are respectively and movably connected with the air inlet pipe and the air outlet guide head 263, the air guide head 262 is firstly rotatably arranged at the cooling cylinder 1224 and the cooling cylinder 1224, when the temperature of the air guide head 262 is in the cooling cylinder 1224 is in a normal state, the cooling cylinder 1221 is gradually cooled down, and the refrigerant is cooled down to the cooling cylinder 1221 in the cooling cylinder 1221, and the cooling structure is gradually cooled down in the cooling state when the cooling cylinder 1221 is cooled down, the cooling cylinder 1221 is cooled down in the cooling state, and the cooling cylinder 1224 is gradually, meanwhile, the low-temperature refrigerant is quickly introduced into the cooling cylinder 12241 to form quick fixed-point replacement, wherein the sliding part 261 can be a push rod motor or a hydraulic motor, and only a sealing design is needed.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A system for preparing electronic grade chlorine trifluoride, comprising:
the raw material purifying unit (10), the raw material purifying unit (10) comprises a chlorine purifying device (11) and a fluorine gas purifying device (12) which are arranged in parallel, the chlorine purifying device (11) is connected with a chlorine gas inlet end and is used for physically drying the introduced chlorine gas, and the fluorine gas purifying device (12) is connected with a gas outlet end of an electrolytic tank and is used for carrying out dehydrofluorination treatment on fluorine gas;
a microchannel reactor (20), wherein the microchannel reactor (20) comprises an air inlet section connected with a chlorine purifying device (11) and a fluorine purifying device (12), a lower layer mixing section (21) for mixing chlorine and fluorine, and a catalyst section (22) for catalyzing the chlorine and the fluorine to generate chlorine trifluoride;
a primary purification unit (30), the primary purification unit (30) comprising a condensation separation structure for receiving chlorine trifluoride, the condensation separation structure for separating chlorine trifluoride gas from liquid impurities;
the purification unit (40), the purification unit (40) comprises a metal adsorption structure (41) and a rectification structure (41), and the metal adsorption structure (41) and the rectification structure (41) remove hydrogen fluoride gas in the chlorine trifluoride separated by the condensation separation structure;
-a filling unit (50), said filling unit (50) comprising a gaseous holding structure, and an automatic filling structure connected to said gaseous holding structure.
2. The system for preparing electronic grade chlorine trifluoride according to claim 1, characterized in that said chlorine purification installation (11) comprises a plurality of molecular sieves, said molecular sieves being 3A molecular sieves or, alternatively, said molecular sieves being 13X molecular sieves.
3. The system for preparing electronic grade chlorine trifluoride according to claim 1, characterized in that said fluorine gas purification device (12) comprises a pre-cooling tank (121) connected to the outlet end of said electrolyzer, a degassing tank (122) connected to the outlet end of said pre-cooling tank (121); and an adsorber (123) connected to the degassing tank (122) and used for adsorbing hydrogen fluoride in fluorine gas.
4. The system for preparing electronic grade chlorine trifluoride of claim 1, wherein the catalyst section (22) is formed by stacking nickel-based metals.
5. The system for preparing electronic grade chlorine trifluoride according to claim 1, characterized in that said primary purification unit (30) further comprises a tail gas collection and treatment structure (31) connected to said condensation and separation structure, and the impurities separated by said condensation and separation structure are introduced into the tail gas collection and treatment structure (31) for preparing carbon tetrafluoride.
6. A method for preparing electronic grade chlorine trifluoride, which uses the system for preparing electronic grade chlorine trifluoride as claimed in any one of claims 1-5, and is characterized by comprising the following steps:
s1, performing S1; purifying raw materials: introducing chlorine into a chlorine purification device (11), performing multistage physical drying on the chlorine, introducing impurity-containing chlorine generated by electrolysis into a fluorine gas purification device (12) for purification, removing hydrogen fluoride in fluorine gas, and introducing the dried chlorine and the purified fluorine gas into a microchannel reactor (20);
s2, performing S2; preparation of chlorine trifluoride: the introduced fluorine gas and chlorine gas enter a lower mixing section (21) in the microchannel reactor (20), the chlorine gas and the fluorine gas are fully mixed through a plurality of channels in the lower mixing section (21), and chlorine trifluoride and impurities are generated under the catalysis of a catalyst section (22);
s3, performing S3; impurity primary purification: condensing generated chlorine trifluoride and impurities through a condensation separation structure, separating fluorine gas and chlorine monofluoride impurities in the chlorine trifluoride, and realizing primary purification and collection of the chlorine trifluoride;
s4, performing S4; impurity is refined: introducing the separated chlorine trifluoride into a purification unit (40) for purification, and removing hydrogen fluoride gas in the chlorine trifluoride to realize that the purity of the chlorine trifluoride reaches 99.995%;
s5, performing S5; chlorine trifluoride is fully automatically filled into the filling tank in a gaseous state.
7. The method for preparing electronic grade chlorine trifluoride as claimed in claim 6, wherein said S1 specifically comprises:
s11, performing S11; fluorine gas is firstly introduced into a precooling tank body (121) for precooling;
s12, performing S12; the pre-cooled fluorine gas passes through a degassing tank (122) with lower temperature to condense and precipitate hydrogen fluoride in the fluorine gas, so that the hydrogen fluoride in the fluorine gas is reduced;
s13, performing S13; the fluoride in the fluorine gas is physically adsorbed by the metal fluoride in the adsorber (123), and hydrogen fluoride in the fluorine gas is reduced again.
8. The method for preparing electronic grade chlorine trifluoride as claimed in claim 7, wherein the temperature in the pre-cooling tank (121) is-80 ℃ to-85 ℃.
9. The method for preparing electronic grade chlorine trifluoride as claimed in claim 7, wherein the temperature in the degassing tank (122) is-85 ℃ to-90 ℃.
10. The method for preparing electronic grade chlorine trifluoride as claimed in claim 6, wherein said S3 further comprises: the condensed and separated impurities are collected by a separate tail gas collecting and treating structure (31) and then used for preparing carbon tetrafluoride.
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