CN115557471B - Method for preparing sulfuryl fluoride and sulfuryl fluoride - Google Patents
Method for preparing sulfuryl fluoride and sulfuryl fluoride Download PDFInfo
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- CN115557471B CN115557471B CN202211259170.2A CN202211259170A CN115557471B CN 115557471 B CN115557471 B CN 115557471B CN 202211259170 A CN202211259170 A CN 202211259170A CN 115557471 B CN115557471 B CN 115557471B
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- sulfuryl fluoride
- fluoride
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- sulfuryl
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- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 239000005935 Sulfuryl fluoride Substances 0.000 title claims abstract description 127
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000007789 gas Substances 0.000 claims abstract description 91
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 68
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 59
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 41
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims abstract description 37
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract description 37
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 29
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 19
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 15
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 claims description 12
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 claims description 10
- 229910000127 oxygen difluoride Inorganic materials 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 8
- 229910001626 barium chloride Inorganic materials 0.000 claims description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 7
- 239000011775 sodium fluoride Substances 0.000 claims description 7
- 235000013024 sodium fluoride Nutrition 0.000 claims description 7
- 150000003462 sulfoxides Chemical class 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 16
- 239000000203 mixture Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 8
- 239000003814 drug Substances 0.000 description 8
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 7
- 238000004821 distillation Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 7
- 229940001584 sodium metabisulfite Drugs 0.000 description 7
- 235000010262 sodium metabisulphite Nutrition 0.000 description 7
- 235000019345 sodium thiosulphate Nutrition 0.000 description 7
- 229940079593 drug Drugs 0.000 description 6
- 238000004817 gas chromatography Methods 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 235000009518 sodium iodide Nutrition 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910018503 SF6 Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 4
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 4
- 229960000909 sulfur hexafluoride Drugs 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002001 electrolyte material Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- -1 fluorosulfonyl imide Chemical class 0.000 description 2
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 2
- PNQBEPDZQUOCNY-UHFFFAOYSA-N trifluoroacetyl chloride Chemical compound FC(F)(F)C(Cl)=O PNQBEPDZQUOCNY-UHFFFAOYSA-N 0.000 description 2
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010941 LiFSI Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- NNTJKSMVNWGFTB-UHFFFAOYSA-N disulfuryl chloride Chemical compound ClS(=O)(=O)OS(Cl)(=O)=O NNTJKSMVNWGFTB-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4561—Compounds containing sulfur, halogen and oxygen only
- C01B17/4576—Sulfuryl fluoride (SO2F2)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application provides a method for preparing sulfuryl fluoride and the prepared sulfuryl fluoride, wherein the method comprises the following steps: s1) reacting sulfur trioxide steam with barium fluoride to obtain mixed gas of barium sulfate and sulfuryl fluoride; s2) carrying out acid washing on the mixed gas obtained in the step S1 through a concentrated sulfuric acid solution with the concentration of 70-98.3%, so as to obtain first-stage purified sulfuryl fluoride gas; s3) passing the primary purified sulfuryl fluoride gas obtained in the step S2 through a sodium sulfite aqueous solution with the concentration of 2-10wt.% or a sodium sulfite aqueous solution with the addition of 0.1-2wt.% of potassium iodide and 2-10wt.% of sodium sulfite; s4) cooling the sulfuryl fluoride gas obtained in the step S3 by liquid nitrogen, and then introducing the cooled sulfuryl fluoride gas into a rectification system for rectification separation, wherein the rectification temperature is-65 to-55 ℃, the reflux ratio is 0.6-0.8, or the rectification temperature is-70 to-50 ℃, and the reflux ratio is 0.5-1. The method has the advantages of low-cost and easily-obtained raw materials, simple process, low cost and high yield and purity of the prepared sulfuryl fluoride, and is suitable for industrial production.
Description
The present application is a divisional application of the invention patent application with the application number 202210111605.2 and the name of "a method for preparing sulfuryl fluoride", which is the application day 2022, 1 and 29.
Technical Field
The present application relates to a process for preparing sulfuryl fluoride, and more particularly, to a process for preparing sulfuryl fluoride having high purity.
Background
Sulfuryl fluoride is an inorganic compound with a chemical formula of SO 2 F 2 . Colorless, odorless and toxic gas at normal temperature and normal pressure. Chemically inert, does not decompose at high temperatures, is stable at 400 ℃, and is less reactive. The sulfuryl fluoride has the advantages of strong diffusion permeability, convenient use at low temperature, fast desorption, less dosage, no pollution to metals,Cotton, leather, plastic and the like have the advantages of no corrosion, no color influence and the like, and become a fumigant with wide application. In addition, as sulfuryl fluoride is further studied, it is increasingly applied to more and more fields as an important intermediate in the field of fluorine chemical industry.
In recent years, sulfuryl fluoride has been used as a raw material for synthesizing lithium difluorosulfonimide. Lithium bis (fluorosulfonyl imide) (chemical formula Li [ N (SO) 2 F) 2 ]The English abbreviation LiFSI) is an important new fluorine-containing material, is a novel lithium salt electrolyte material of a lithium ion battery with wide application prospect, is a key high-performance electrolyte material in the lithium ion battery, a super capacitor and an ionic liquid, and has extremely high industrialized application value. The battery system has the advantages of high electrochemical stability, small probability of side reaction, high thermal stability, proper conductivity and the like after the lithium bis (fluorosulfonyl) imide is added into the lithium ion battery electrolyte, and particularly in a power battery, the cycle performance and the multiplying power performance of the power battery can be improved. However, as a raw material for synthesizing lithium difluorosulfonimide, sulfuryl fluoride is required to have a high purity.
The method for preparing sulfuryl fluoride by taking sulfur trioxide as a raw material is reported at present as follows: US3403144 reports a process for preparing sulfuryl fluoride by reacting barium fluoride or barium fluosilicate with sulfur trioxide at a reaction temperature of 500-650 ℃, but without involving identification and separation of by-products; CN 102351681a reports a method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride, namely, sulfur trioxide and trifluorotrichloroethane are continuously introduced into the middle lower part of a reaction rectifying tower filled with a catalyst and a filler, the temperature of the tower kettle is controlled to be 120-130 ℃, the reflux ratio is controlled to be 2.5-3, trifluoroacetyl chloride is collected from the top of the tower, after the sulfuryl chloride and pyrosulfuryl chloride in the tower kettle are fractionated, sulfuryl chloride and hydrogen fluoride react under the action of palladium/carbon catalyst to generate sulfuryl fluoride, the method is complex, the separation of byproducts is not involved, and the purity of the obtained sulfuryl fluoride is not reported. Therefore, the composition of the sulfuryl fluoride product obtained by the existing method for preparing sulfuryl fluoride by taking sulfur trioxide as a raw material is complex, the reaction yield is not high, and the purity of the sulfuryl fluoride needs to be further improved.
The preparation method needs to be provided, so that the sulfuryl fluoride has low production cost, high purity and high yield, is suitable for industrial production, and is a problem which needs to be solved by the technicians in the field.
Disclosure of Invention
In view of the problems in the prior art, the present application provides a method for preparing sulfuryl fluoride, comprising the steps of:
s1) reacting sulfur trioxide steam with barium fluoride to obtain mixed gas of barium sulfate and sulfuryl fluoride;
s2) carrying out acid washing on the mixed gas obtained in the step S1 through a concentrated sulfuric acid solution with the concentration of 70-98.3%, so as to obtain first-stage purified sulfuryl fluoride gas;
s3) passing the primary purified sulfuryl fluoride gas obtained in step S2 through an aqueous solution having a concentration of 2-10wt.% selected from one of the following: sodium sulfite, sodium bisulphite, sodium metabisulfite and sodium thiosulfate to obtain sulfuryl fluoride gas.
In any embodiment, the method further comprises a step S4, wherein the step S4 is to cool the sulfuryl fluoride gas obtained in the step S3 through liquid nitrogen, and then introduce the sulfuryl fluoride gas into a rectification system for rectification separation, the rectification temperature is between-70 and-50 ℃, preferably between-65 and-55 ℃, and the reflux ratio is between 0.5 and 1, preferably between 0.6 and 0.8.
In any embodiment, potassium iodide or sodium iodide is added to the solution of step S3 at a concentration of 0.1 to 2 wt.%.
In any embodiment, in step S3, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through 2-10wt.% aqueous sodium sulfite solution.
In any embodiment, 0.1 to 2wt.% potassium iodide is added to the 2 to 10wt.% aqueous sodium sulfite solution of step S3.
In any embodiment, in said step S3, the primary purified sulfuryl fluoride gas is bubbled through an aqueous solution of at least one selected from sodium sulfite, sodium bisulfite, sodium metabisulfite, sodium thiosulfate, at a temperature of 20-40 ℃.
In any embodiment, the volume fraction of oxygen difluoride in the sulfuryl fluoride gas obtained in step S3 is less than 0.1%.
In any embodiment, the volume fraction of sulfoxide tetrafluoride in the sulfonyl fluoride gas resulting from step S3 is less than 0.15%.
In any embodiment, the barium fluoride of step S1 is prepared by treating an aqueous solution of barium sulfide with hydrogen fluoride, or by reacting barium chloride with sodium fluoride.
In any embodiment, in step S1, the reaction with barium fluoride is carried out directly using sulfur trioxide vapor or using sulfur trioxide vapor transported by helium as a carrier.
The method for preparing sulfuryl fluoride has the advantages that: the raw materials used are cheap and easy to obtain, the production process is simple, the cost is low, and the prepared sulfuryl fluoride has high yield and high purity and is suitable for industrial production.
Detailed Description
Embodiments of the method of preparing sulfuryl fluoride of the present application are described in detail below. However, unnecessary detailed description may be omitted. For example, detailed descriptions of well-known matters and repeated descriptions of the actual same structure may be omitted. This is to avoid that the following description becomes unnecessarily lengthy, facilitating the understanding of those skilled in the art. Furthermore, the following description is provided for a thorough understanding of the present application by those skilled in the art, and is not intended to limit the subject matter recited in the claims.
The "range" disclosed herein is defined in terms of lower and upper limits, with a given range being defined by the selection of a lower and an upper limit, the selected lower and upper limits defining the boundaries of the particular range. Ranges that are defined in this way can be inclusive or exclusive of the endpoints, and any combination can be made, i.e., any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum range values 3,4 and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In this application, unless otherwise indicated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" have been listed throughout, and "0-5" is simply a shorthand representation of a combination of these values. When a certain parameter is expressed as an integer of 2 or more, it is disclosed that the parameter is, for example, an integer of 2, 3,4, 5, 6, 7, 8, 9, 10, 11, 12 or the like.
All embodiments and alternative embodiments of the present application may be combined with each other to form new solutions, unless specifically stated otherwise.
All technical features and optional technical features of the present application may be combined with each other to form new technical solutions, unless specified otherwise.
Reference herein to "comprising" and "including" means open ended, as well as closed ended, unless otherwise noted. For example, the terms "comprising" and "comprises" may mean that other components not listed may be included or included, or that only listed components may be included or included.
The term "or" is inclusive in this application, unless otherwise specified. For example, the phrase "a or B" means "a, B, or both a and B. More specifically, either of the following conditions satisfies the condition "a or B": a is true (or present) and B is false (or absent); a is false (or absent) and B is true (or present); or both A and B are true (or present).
The present application provides a process for preparing sulfuryl fluoride comprising the steps of:
s1) reacting sulfur trioxide steam with barium fluoride to obtain mixed gas of barium sulfate and sulfuryl fluoride;
s2) carrying out acid washing on the mixed gas obtained in the step S1 through a concentrated sulfuric acid solution with the concentration of 70-98.3%, so as to obtain first-stage purified sulfuryl fluoride gas;
s3) passing the primary purified sulfuryl fluoride gas obtained in step S2 through an aqueous solution having a concentration of 2-10wt.% selected from one of the following: sodium sulfite, sodium bisulphite, sodium metabisulfite and sodium thiosulfate to obtain sulfuryl fluoride gas.
In the method, the temperature is room temperature and the pressure is atmospheric pressure during operation.
In the method of the present application, the amounts of sulfuryl fluoride, sulfur trioxide and by-products in the mixed gas are all obtained by gas chromatography. In the present application, the purity of the sulfuryl fluoride gas is the volume of the sulfuryl fluoride gas in the sulfuryl fluoride mixed gas and the volume percentage of the mixed gas.
In the present application, the barium fluoride used in step S1 may be obtained by a method for preparing barium fluoride known in the art. In some embodiments, the barium fluoride is obtained by treating an aqueous barium sulfide solution with hydrogen fluoride. In other embodiments, the barium fluoride is obtained by reacting barium chloride with sodium fluoride.
In some embodiments, in step S1, the reaction is performed directly with barium fluoride using sulfur trioxide vapor to obtain sulfuryl fluoride. In other embodiments, in step S1, sulfur trioxide vapor delivered by helium as a carrier is used to react with barium fluoride to obtain sulfuryl fluoride. Wherein the sulfur trioxide vapor was produced by heating 65% oleum and phosphorus pentoxide (3H 2 SO 4 +P 2 O 5 →2H 3 PO 4 +3SO 3 The phosphoric acid produced is a non-volatile acid). The sulfur trioxide is present in excess in the sulfuryl fluoride gas obtained in step S1, and oxygen difluoride (OF) is a by-product 2 ) Sulfoxide tetrafluoride (F) 4 OS), sulfur hexafluoride (SF) 6 ) Etc.
In some embodiments, in step S1, the molar ratio of sulfur trioxide vapor to barium fluoride is from 2:1 to 5:1, preferably from 2.5:1 to 3:1; the reaction temperature is 500-600 ℃, preferably 550-600 ℃. In some preferred embodiments, a bubbler structure, such as a porous material made of polytetrafluoroethylene fibers, is added at the sulfur trioxide feed to allow the sulfur trioxide to enter the reactor in a fine foam state, increasing the contact time and contact area with the barium sulfide for better reaction.
In some embodiments, in step S2, the mixed gas obtained in step S1 is subjected to acid washing with a concentrated sulfuric acid solution having a concentration of 70 to 98.3%. In some preferred embodiments, the sulfuryl fluoride mixture obtained in step S1 is acid washed with a concentrated sulfuric acid solution having a concentration of 80-95% to better remove sulfur trioxide from the sulfuryl fluoride mixture, resulting in a first-stage purified sulfuryl fluoride gas having a sulfuryl fluoride purity of about 94%.
In some embodiments, in step S3, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through an aqueous solution having a concentration of 2-10wt.% selected from one of the following: sodium sulfite, sodium bisulfite, sodium metabisulfite, sodium thiosulfate to remove the reaction by-product oxygen difluoride (OF) 2 ) And sulfoxide tetrafluoride (F) 4 OS). In some embodiments, the primary purified sulfuryl fluoride gas obtained in step S2 is bubbled through the above solution at a temperature of 20-40 ℃. Thus, in the sulfuryl fluoride gas obtained through step S3, the volume fraction of oxygen difluoride is less than 0.1%, the volume fraction of sulfoxide tetrafluoride is less than 0.15%, and the volume fractions of oxygen difluoride and sulfoxide tetrafluoride are determined using gas chromatography.
In some preferred embodiments, in step S3, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through an aqueous solution selected from sodium sulfite, sodium bisulfite, sodium metabisulfite, sodium thiosulfate, in a concentration of 4-8wt.%, preferably 5-6wt.%. In some more preferred embodiments, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through an aqueous sodium sulfite solution having a concentration of 2-10wt.%, preferably 4-8wt.%, more preferably 5-6wt.%. More preferably, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through a sodium sulfite solution having a concentration of 5wt.%.
In some more preferred embodiments, potassium iodide or sodium iodide is added to the solution of step S3 at a concentration of 0.1-2 wt%. Preferably, potassium iodide is added to the solution of step S3 at a concentration of 0.1-2 wt%. More preferably, potassium iodide is added to the solution of step S3 at a concentration of 0.5wt.%.
In still other more preferred embodiments, 0.1-2wt.% potassium iodide is added to the aqueous sodium sulfite solution of step S3. Preferably, the primary purified sulfuryl fluoride gas obtained in step S2 is passed through 5. 5 wt% sodium sulfite and 0.5wt.% potassium iodide solution.
In some preferred embodiments, the method further comprises a step S4 of cooling the sulfuryl fluoride gas obtained in step S3 with liquid nitrogen, and then introducing the cooled sulfuryl fluoride gas into a rectification system for rectification separation, wherein the rectification temperature is-70 to-50 ℃, preferably-65 to-55 ℃, and the reflux ratio is 0.5 to 1, preferably 0.6 to 0.8, so as to separate the sulfuryl fluoride from the byproduct sulfur hexafluoride, thereby obtaining high-purity sulfuryl fluoride, i.e. the purity of the sulfuryl fluoride obtained after rectification separation is up to about 99%.
In the application, the barium sulfate obtained in the step S1 is reduced by carbon at the temperature of 600-1200 ℃, and the obtained barium sulfide can be used for preparing the barium fluoride again.
In the application, the obtained sulfuryl fluoride gas is dried, compressed and condensed to obtain the sulfuryl fluoride product.
Examples
Hereinafter, embodiments of the present application are described. The embodiments described below are exemplary only for the purpose of illustrating the present application and are not to be construed as limiting the present application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
I. Raw materials
Hydrogen fluoride (HF, CAS:7664-39-3, available from national pharmaceutical group chemical Co., ltd.)
Barium sulfide (BaS, CAS:21109-95-5, available from national medicine group chemical reagent Co., ltd.)
Barium chloride (BaCl) 2 CAS:10361-37-2, available from the national pharmaceutical group chemical company, inc
Sodium fluoride (NaF, CAS:7681-49-4, available from national pharmaceutical systems and chemical reagents Co., ltd.) sulfur trioxide vapor (SO 3 Prepared by heating 65% oleum with phosphorus pentoxide
65% oleum (from Bo Jianlong chemical Co., ltd.)
Concentrated sulfuric acid (H) 2 SO 4 Concentration ofThe degree of refraction is 70-98.3%, and is purchased from chemical reagent limited company of national medicine group
Sodium sulfite (Na) 2 SO 3 CAS:7757-83-7, available from chemical reagent Co., ltd. In the national drug group
Sodium bisulphite (NaHSO) 3 CAS:7631-90-5 from chemical reagent Co., ltd. From the national drug group
Sodium metabisulfite (Na) 2 S 2 O 5 CAS:7681-57-4 from chemical reagent Co., ltd. From the national drug group
Sodium thiosulfate (Na) 2 S 2 O 3 CAS:7772-98-7 from chemical reagent Co., ltd. From the national drug group
Potassium iodide (KI, CAS:7681-11-0, available from chemical reagents, inc. of the national drug group)
Sodium iodide (NaI, CAS:7681-82-5, available from chemical reagent Co., ltd., from the national drug group)
Liquid nitrogen (from Fujiede and chemical industry Co., ltd.)
Carbon (C, CAS:7440-44-0, available from Country pharmaceutical Chemie Co., ltd.)
Palladium-based catalyst (available from Kang Chi chemical industry Shenzhen Co., ltd.)
II. instrument
The gas composition was detected using a gas chromatograph model 7890B from agilent technologies, usa, and the instrument parameters were set to: the temperature of the column box is 40-260 ℃, the temperature of the detector is 300 ℃, the air pressure is 0.4MPa, the hydrogen flow is 30ml/min, and the air flow is 400ml/min.
III preparation of barium fluoride
(1) Preparation of barium fluoride from hydrogen fluoride and barium sulfide
169.4g of barium sulfide is weighed and dissolved in 1000ml of water, the solution is placed in a reaction kettle at 25 ℃, hydrogen fluoride gas is introduced into the barium sulfide water solution at 10ml/min under stirring, white solid barium fluoride is separated out along with the progress of the reaction, and the obtained barium fluoride is washed by deionized water and dried at 70 ℃.
(2) Preparation of barium fluoride from barium chloride and sodium fluoride
208.2g of barium chloride was weighed and dissolved in 1000ml of water, followed by adding 50.4g of sodium fluoride with stirring, and as the reaction proceeded, white solid-like barium fluoride was precipitated, and after filtration, the obtained barium fluoride was washed with deionized water and dried at 70 ℃.
IV preparation of Sulfur trioxide vapor
65% fuming sulfuric acid and phosphorus pentoxide are heated at 60 ℃ in a molar ratio of 5:1 to produce sulfur trioxide vapor.
V. preparation of barium sulfide from recovered barium sulfate
Barium sulfate and carbon were reacted at a molar ratio of 1:2.5 at a temperature of 1000 ℃ at atmospheric pressure using a palladium-based catalyst.
Comparative example 1
175.3g of solid barium fluoride is placed in a reaction kettle, the device is heated to 580 ℃ by an electric heater, sulfur trioxide steam passes through the solid barium fluoride at a molar ratio of 1:2.5 of the barium fluoride to the sulfur trioxide at 10ml/min, and the sulfuryl fluoride mixed gas obtained by the reaction is dried.
The obtained sulfuryl fluoride mixed gas was subjected to gas chromatography, and the composition and the corresponding ratio of the mixed gas are shown in Table 1.
Comparative example 2
Placing 175.3g of solid barium fluoride into a reaction kettle, heating the device to 580 ℃ by an electric heater, enabling sulfur trioxide steam to pass through the solid barium fluoride at a molar ratio of 1:2.5 at 10ml/min, and reacting to obtain sulfuryl fluoride mixed gas; and (3) pickling the obtained mixed gas by using a concentrated sulfuric acid solution with the concentration of 70% contained in a pickling tank, and drying the obtained primary purified sulfuryl fluoride gas.
The first-order purified sulfuryl fluoride gas subjected to concentrated sulfuric acid washing was subjected to gas chromatography to obtain the sulfuryl fluoride having the purity shown in Table 2.
Comparative example 3
The results are shown in Table 2, except that the sulfuryl fluoride mixture was passed through a concentrated sulfuric acid solution having a concentration of 98.3%, which was the same as comparative example 2.
Example 1
Placing 175.3g of solid barium fluoride into a reaction kettle, heating the device to 580 ℃ by an electric heater, enabling sulfur trioxide steam to pass through the solid barium fluoride at a molar ratio of 1:2.5 at 10ml/min, and reacting to obtain sulfuryl fluoride mixed gas; pickling the obtained mixed gas by using a concentrated sulfuric acid solution with the concentration of 70% contained in a pickling tank to obtain first-stage purified sulfuryl fluoride gas; the first-stage purified sulfuryl fluoride gas was then purified by bubbling a sodium sulfite solution having a concentration of 2wt.%, and the resulting aqueous sulfuryl fluoride gas was dried.
The sulfuryl fluoride gas was tested by gas chromatography to give the sulfuryl fluoride with the purity listed in table 2.
Examples 2 to 6
The results are set forth in table 2, except that the primary purified sulfuryl fluoride gas was purified by passing it through sodium sulfite solutions having concentrations of 4wt.%, 5wt.%, 6wt wt.%, 8wt.%, 10wt.%, respectively.
Examples 7 to 9
The results are shown in Table 2, except that the primary purified sulfuryl fluoride gas was purified by passing it through a sodium bisulphite solution, a sodium metabisulfite solution, and a sodium thiosulfate solution, respectively, each having a concentration of 5wt.%.
Example 10
Placing 175.3g of solid barium fluoride into a reaction kettle, heating the device to 580 ℃ by an electric heater, enabling sulfur trioxide steam to pass through the solid barium fluoride at a molar ratio of 1:2.5 at 10ml/min, and reacting to obtain sulfuryl fluoride mixed gas; pickling the obtained mixed gas by using a concentrated sulfuric acid solution with the concentration of 70% contained in a pickling tank to obtain first-stage purified sulfuryl fluoride gas; then introducing the first-stage purified sulfuryl fluoride gas into sodium sulfite solution with the concentration of 5wt.% for purification treatment; cooling the obtained sulfuryl fluoride gas by liquid nitrogen, introducing the cooled sulfuryl fluoride gas into a rectifying tower for rectifying and separating, controlling the rectifying temperature to be-70 ℃ and the reflux ratio to be 0.5, and drying the obtained sulfuryl fluoride gas.
The obtained sulfuryl fluoride gas was subjected to gas chromatography, and the purity of the obtained sulfuryl fluoride is shown in Table 2.
Examples 11 to 14
The results are shown in Table 2, except that the sulfuryl fluoride gas after sodium sulfite treatment was subjected to distillation separation at a distillation temperature of-65℃and a reflux ratio of 0.6, a distillation temperature of-60℃and a reflux ratio of 0.7, a distillation temperature of-55℃and a reflux ratio of 0.8, and a distillation temperature of-50℃and a reflux ratio of 1, respectively.
Examples 15 to 21
The results are set forth in table 2, except that the primary purified sulfuryl fluoride gas is passed into a sodium sulfite solution having a concentration of 5wt.%, and 0.1wt.%, 0.3wt.%, 0.5wt.%, 1wt.%, 1.5wt.%, 2wt.% potassium iodide, and 0.5wt.% sodium iodide are added to the sodium sulfite solution, respectively.
Example 22
The results are shown in Table 2, except that the first-stage purified sulfuryl fluoride gas was introduced into a sodium sulfite solution having a concentration of 5wt.% and containing 0.5wt.% potassium iodide, and then the resulting sulfuryl fluoride gas was subjected to rectification separation at a rectification temperature of-70℃and a reflux ratio of 0.5.
Example 23
The results are shown in Table 2, except that the obtained sulfuryl fluoride gas was subjected to distillation separation at a distillation temperature of-50℃and a reflux ratio of 1, in the same manner as in example 22.
TABLE 1 composition of gas mixtures
| Composition of the mixed gas | Content (%) |
| SO 2 F 2 | 90.2 |
| SO 3 | 6 |
| OF 2 | 1.2 |
| F 4 OS | 1 |
| SF 6 | 1.5 |
| Others | ＜0.1 |
As can be seen from the results in Table 1, in the untreated mixed gas of sulfuryl fluoride, the purity of sulfuryl fluoride was about 90%, and the mixed gas contained sulfur trioxide vapor as a raw material and by-products such as oxygen difluoride, sulfoxide tetrafluoride, sulfur hexafluoride and the like.
TABLE 2 Experimental related procedure parameters and results
As can be seen from the results in Table 2, the purity of sulfuryl fluoride after only concentrated sulfuric acid washing was 94.5%, the purity of sulfuryl fluoride after further purification treatment with sodium sulfite solution was about 98%, and the purity of sulfuryl fluoride after further separation by rectification was as high as about 99%. As can be seen, the process of the present application allows for the production of high purity sulfuryl fluoride gas.
The present application is not limited to the above embodiment. The above embodiments are merely examples, and embodiments having substantially the same configuration and the same effects as those of the technical idea within the scope of the present application are included in the technical scope of the present application. Further, various modifications that can be made to the embodiments and other modes of combining some of the constituent elements in the embodiments, which are conceivable to those skilled in the art, are also included in the scope of the present application within the scope not departing from the gist of the present application.
Claims (17)
1. A method for preparing sulfuryl fluoride is characterized in that,
the method comprises the following steps:
s1) reacting sulfur trioxide steam with barium fluoride to obtain mixed gas of barium sulfate and sulfuryl fluoride;
s2) carrying out acid washing on the mixed gas obtained in the step S1 through a concentrated sulfuric acid solution with the concentration of 70-98.3wt.% to obtain first-stage purified sulfuryl fluoride gas;
s3) passing the primary purified sulfuryl fluoride gas obtained in the step S2 through an aqueous sodium sulfite solution with the concentration of 2-10 wt.%;
s4) cooling the sulfuryl fluoride gas obtained in the step S3 by liquid nitrogen, and then introducing the cooled sulfuryl fluoride gas into a rectification system for rectification separation, wherein the rectification temperature is-65 to-55 ℃, and the reflux ratio is 0.6-0.8;
or,
the method comprises the following steps:
s1) reacting sulfur trioxide steam with barium fluoride to obtain mixed gas of barium sulfate and sulfuryl fluoride;
s2) carrying out acid washing on the mixed gas obtained in the step S1 through a concentrated sulfuric acid solution with the concentration of 70-98.3wt.% to obtain first-stage purified sulfuryl fluoride gas;
s3) passing the primary purified sulfuryl fluoride gas obtained in the step S2 through a 2-10wt.% aqueous sodium sulfite solution to which 0.1-2wt.% potassium iodide is added;
s4) cooling the sulfuryl fluoride gas obtained in the step S3 by liquid nitrogen, and then introducing the cooled sulfuryl fluoride gas into a rectification system for rectification separation, wherein the rectification temperature is-65 to-55 ℃, and the reflux ratio is 0.6-0.8.
2. The method according to claim 1, characterized in that in both schemes the concentration of sodium sulfite is 4-8wt.%.
3. The method according to claim 1, characterized in that in both schemes the concentration of sodium sulfite is 5-6wt.%.
4. A method according to any one of claims 1 to 3, characterized in that the concentration of potassium iodide is 0.5wt.%.
5. A method according to any one of claims 1 to 3, characterized in that in said step S3 in both schemes, the primary purified sulfuryl fluoride gas is bubbled through an aqueous sodium sulfite solution at a temperature of 20-40 ℃, or 2-10wt.% aqueous sodium sulfite solution with 0.1-2wt.% potassium iodide added.
6. A method according to any one of claims 1 to 3, characterized in that in both variants the volume fraction of oxygen difluoride in the sulfuryl fluoride gas obtained in step S3 is lower than 0.1%.
7. A method according to any one of claims 1 to 3, characterized in that in both variants the volume fraction of sulfoxide tetrafluoride in the sulfuryl fluoride gas obtained in step S3 is lower than 0.15%.
8. A method according to any one of claims 1 to 3, wherein in both versions the barium fluoride of step S1 is obtained by treating an aqueous solution of barium sulphide with hydrogen fluoride or by reacting barium chloride with sodium fluoride.
9. A method according to any one of claims 1 to 3, characterized in that in the step S1 in both schemes, the reaction with barium fluoride is carried out directly with sulfur trioxide vapour or with sulfur trioxide vapour transported by helium as carrier.
10. A method according to any one of claims 1 to 3, characterized in that in step S1 in both variants, the molar ratio of sulfur trioxide vapour to barium fluoride is 2:1-5:1 and the reaction temperature is 500-600 ℃.
11. A method according to any one of claims 1 to 3, characterized in that in step S1 in both variants the molar ratio of sulfur trioxide vapour to barium fluoride is 2.5:1-3:1.
12. A method according to any one of claims 1 to 3, characterized in that in the step S1 in both variants, the reaction temperature of the sulfur trioxide vapour with the barium fluoride is 550-600 ℃.
13. A method according to any one of claims 1 to 3, wherein the barium sulphate obtained in step S1 is reduced with carbon at a temperature of 600-1200 ℃ to obtain barium sulphide.
14. A process according to any one of claims 1 to 3, characterized in that the resulting sulfuryl fluoride is dried, compressed, condensed to obtain a sulfuryl fluoride product.
15. A sulfuryl fluoride obtainable by the process of any one of claims 1 to 14.
16. The sulfuryl fluoride of claim 15, wherein the purity of the sulfuryl fluoride is up to 99%.
17. The sulfuryl fluoride of claim 15, wherein the purity of the sulfuryl fluoride is 99.1%, 99.3%, or 99.8%.
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