CN112536014B - Device and method for continuously preparing lithium bis (trifluoromethanesulfonyl) imide - Google Patents
Device and method for continuously preparing lithium bis (trifluoromethanesulfonyl) imide Download PDFInfo
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- CN112536014B CN112536014B CN202011481539.5A CN202011481539A CN112536014B CN 112536014 B CN112536014 B CN 112536014B CN 202011481539 A CN202011481539 A CN 202011481539A CN 112536014 B CN112536014 B CN 112536014B
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- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 102
- 239000000843 powder Substances 0.000 claims abstract description 47
- 239000002253 acid Substances 0.000 claims abstract description 43
- 238000001694 spray drying Methods 0.000 claims abstract description 39
- 239000012498 ultrapure water Substances 0.000 claims abstract description 28
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 claims abstract description 24
- 230000007246 mechanism Effects 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 59
- 238000006243 chemical reaction Methods 0.000 claims description 27
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 claims description 26
- 238000001914 filtration Methods 0.000 claims description 23
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 15
- -1 lithium imide Chemical class 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 150000002466 imines Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 238000002834 transmittance Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000002608 ionic liquid Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract description 3
- 150000003949 imides Chemical class 0.000 abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 24
- 239000010935 stainless steel Substances 0.000 description 24
- 239000000047 product Substances 0.000 description 22
- 238000001514 detection method Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 12
- 229910003002 lithium salt Inorganic materials 0.000 description 9
- 159000000002 lithium salts Chemical class 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- IMNIECVIVJOTBH-UHFFFAOYSA-N trifluoromethanesulfonyl bromide Chemical compound FC(F)(F)S(Br)(=O)=O IMNIECVIVJOTBH-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007040 multi-step synthesis reaction Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229940124530 sulfonamide Drugs 0.000 description 2
- 150000003461 sulfonyl halides Chemical class 0.000 description 2
- 125000005463 sulfonylimide group Chemical group 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical class [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005695 dehalogenation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006351 sulfination reaction Methods 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- KAKQVSNHTBLJCH-UHFFFAOYSA-N trifluoromethanesulfonimidic acid Chemical compound NS(=O)(=O)C(F)(F)F KAKQVSNHTBLJCH-UHFFFAOYSA-N 0.000 description 1
- SLVAEVYIJHDKRO-UHFFFAOYSA-N trifluoromethanesulfonyl fluoride Chemical compound FC(F)(F)S(F)(=O)=O SLVAEVYIJHDKRO-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/36—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of amides of sulfonic acids
- C07C303/40—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of amides of sulfonic acids by reactions not involving the formation of sulfonamide groups
-
- 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
Abstract
The invention relates to a device and a method for continuously preparing lithium bis (trifluoromethanesulfonyl) imide, and belongs to the technical field of preparation of lithium bis (trifluoromethanesulfonyl) imide. The device comprises a powder storage tank, a powder conveying mechanism, a multifunctional reactor, a double (trifluoromethanesulfonyl) imide acid storage tank, a high-purity water storage tank, a double (trifluoromethanesulfonyl) imide lithium solution storage tank, a feed pump and spray drying equipment, wherein raw materials are added into the multifunctional reactor through each raw material storage tank, mixed and reacted in the multifunctional reactor, and then spray drying treatment is carried out to obtain the product powder. The device has less equipment, can realize continuous production, has high safety, improves the quality stability of products, improves the running efficiency of the equipment and effectively reduces the production cost; the method disclosed by the invention is simple in process, easy to operate, high in production efficiency, high in purity and stable in quality of the prepared product, and can meet the requirements of special industries such as ionic liquid on special indexes of the ionic liquid.
Description
Technical Field
The invention relates to a device and a method for continuously preparing lithium bis (trifluoromethanesulfonyl) imide, and belongs to the technical field of preparation of lithium bis (trifluoromethanesulfonyl) imide.
Background
The lithium fluorosulfonyl imide is an important fluorine-containing organic ion compound, has high voltage resistance and conductivity, and has important industrial application value in a plurality of fields. The bis (trifluoromethanesulfonyl) imide lithium is a typical representative of fluorosulfonyl imide lithium, has good thermal stability, high electrochemical stability and conductivity, and is widely applied to organic electrolyte lithium salts of lithium ion batteries to prepare room-temperature ionic liquids, reaction catalysts, antistatic agents and the like.
The methods reported so far for preparing lithium bis (trifluoromethanesulfonyl) imide are as follows:
US5874616 reports the preparation of fluoroalkyl sulfimide compounds by reacting fluoroalkyl sulfonyl halides with fluoroalkyl sulfonamides in aprotic solvents, acidifying, and reacting with bases or salts in organic solvents. The method adopts more reactant types, has fewer reaction steps, and has higher reaction yield but lower purity.
U.S. Pat. No. 3,182 reports that the yield of the product sulfonylimide metal salt is high (89% or more) and the yield of the lithium salt is low (about 2%) by placing 1mol of anhydrous ammonia, 2mol of sulfonyl halide and 6mol of alkali metal fluoride into a reactor, reacting the mixture in a solvent, or placing 1mol of ammonium salt, 2mol of sulfonyl halide and 7mol of alkali metal fluoride into a reactor, reacting the mixture in a solvent, filtering the hydrogen fluoride after the reaction is completed, and evaporating the solvent to concentrate the product sulfonylimide metal salt. The fluorosulfonyl imide acid is obtained through acidolysis and reacts with lithium carbonate to obtain the product with the purity of 99 percent.
Chinese patent CN200910057888.1 reports that trifluoromethane is subjected to a sulfination dehalogenation reaction to obtain trifluoromethanesulfonyl bromide, the trifluoromethanesulfonyl bromide is added into ammonia water to react to obtain trifluoromethanesulfonyl amide, the trifluoromethanesulfonyl bromide is dissolved in an alkylamine solution, the trifluoromethanesulfonyl bromide is continuously added to react, the solvent is removed under reduced pressure after the reaction is finished, the remainder is dissolved in dichloromethane, an organic phase is collected after washing to obtain bis (trifluoromethanesulfonyl) imine, the obtained bis (trifluoromethanesulfonyl) imine is reacted with lithium salt to obtain a final product, and then the final product is recrystallized and purified by using a mixed solvent of n-hexane and ethers to obtain a purer product. The purification by adopting a recrystallization method has lower purity (about 99 percent) and poor operation environment.
Chinese patent CN200810197929 reports that sulfonamide, thionyl chloride and chlorosulfonic acid are added into a reactor according to a certain ratio to react, after the reaction is finished, an imine compound is distilled off under reduced pressure, sbF3 is added into the imine compound under the protection of argon, after the reaction is finished, an organic solvent is added, carbonate is added to react, the mixture is filtered under reduced pressure, the filtrate is recrystallized to obtain salts, then double decomposition reaction is adopted to prepare lithium salts, and the lithium salts are recrystallized to obtain the product. The method has the advantages of multiple operation steps, toxic and harmful raw materials, poor operation environment and low purity of the final product.
Chinese patent 201310616081.3 reports: preparing lithium salt suspension by using lithium salt and deionized water in a reaction kettle, dropwise adding a exquisite fluorosulfonyl imide acid solution under stirring to obtain a reaction solution, controlling the pH value of the reaction solution, and performing non-vacuum drying and then vacuum drying on the reaction solution. The purity of the obtained product can reach 99.95%, but the pH value of the reaction solution is controlled to easily cause high acidity of the finished product, the fluctuation of the product is large, the transmittance of 75% of bis (trifluoromethanesulfonyl) imide lithium aqueous solution is low, and the method is not suitable for industries with high requirements on ionic liquid and the like.
Several methods for preparing lithium bis (trifluoromethanesulfonyl) imide have been reported at home and abroad, and there are mainly one-step synthesis and multi-step synthesis. The one-step synthesis method is prepared by adopting liquid ammonia, trifluoro methanesulfonyl fluoride and lithium fluoride to react in an organic solvent, and the method has extremely low yield, low purity and difficult industrial application; the multi-step synthesis is to synthesize crude bis (trifluoromethanesulfonyl) imide salt, then acidolyze the bis (trifluoromethanesulfonyl) imide salt, decompress and purify the bis (trifluoromethanesulfonyl) imide salt to obtain bis (trifluoromethanesulfonyl) imide acid, react with excessive lithium salt in organic solvent or water, concentrate and purify the bis (trifluoromethanesulfonyl) imide lithium in the organic solvent after filtering the excessive lithium salt, in the process of the preparation of the method, the purity of the bis (trifluoromethanesulfonyl) imide acid is not high, the quality of the product is not stable under the control of an intermittent method, and the cost is high. In addition, the organic solvent for the product obtained by the method is reacted or purified, most of the organic solvent is inflammable and explosive, the safety and the operation environment are poor, and the lithium fluorosulfonyl imide and the organic solvent are easy to form a complex, so that the subsequent drying and the final purity of the product are affected. The purity of the product obtained by batch process operation can only reach 99%, and although some method indexes can reach higher purity, the special requirements of the ionic liquid industry on the acidity and transmittance of the product can not be met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a device and a method for continuously preparing lithium bis (trifluoromethanesulfonyl) imide, which have fewer devices, can realize continuous production, improve the quality stability of products, improve the operation efficiency of the devices and effectively reduce the production cost; the method has the advantages of simple process, easy operation, high production efficiency, higher purity and stable quality of the prepared product, and can meet the requirements of special industries such as ionic liquid and the like on special indexes of the ionic liquid.
The aim of the invention is achieved by the following technical scheme.
An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide, which comprises a powder storage tank, a powder conveying mechanism, a multifunctional reactor, a bis (trifluoromethanesulfonyl) imide acid storage tank, a high-purity water storage tank, a bis (trifluoromethanesulfonyl) imide lithium solution storage tank, a feed pump and spray drying equipment;
the multifunctional reactor has stirring, filtering and heating functions and is a reaction container comprising stirring equipment, heating equipment and filtering equipment, and the top of the multifunctional reactor is provided with a vent;
the powder conveying mechanism is respectively connected with a discharge port of the powder storage tank and a feed port of the multifunctional reactor, a discharge port of the bis (trifluoromethanesulfonyl) imidic acid storage tank and a discharge port of the high-purity water storage tank are respectively connected with the feed port of the multifunctional reactor, and heat tracing equipment is respectively arranged on the bis (trifluoromethanesulfonyl) imidic acid storage tank and a pipeline connecting the bis (trifluoromethanesulfonyl) imidic acid storage tank and the multifunctional reactor; the discharge port of the multifunctional reactor is connected with the feed port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank, and the feed pump is respectively connected with the discharge port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank and the feed port of the spray drying equipment.
Further, the ratio of the height to the inner diameter of the multi-functional reactor is preferably (1.8 to 3): 1.
Further, the filtration pore diameter of the filtration device in the multi-functional reactor is preferably not more than 10. Mu.m, more preferably 0.01 μm to 10. Mu.m.
Further, the top of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank is provided with a vacuum port which is connected with external vacuumizing equipment.
Further, a dehumidifying device is arranged in the spray drying equipment to dehumidify a drying air source used by the spray drying equipment, so that the moisture content of the drying air source is less than or equal to 10 multiplied by 10 -6 。
The method for preparing the lithium bis (trifluoromethanesulfonyl) imide by adopting the device comprises the following specific steps:
high purity water storage tank, bis (trifluoromethanesulfonyl) imidic acid storage tank and powder storage tank according to high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder= (0.4-3.3): (7.54-7.56) 1 adding raw materials into a multifunctional reactor according to the mass ratio, mixing the raw materials, reacting at 80-120 ℃, filtering the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction, then entering a bis (trifluoromethanesulfonyl) imide solution storage tank, and entering spray drying equipment for spray drying under the action of a feed pump to obtain the bis (trifluoromethanesulfonyl) imide lithium powder with the purity of more than 99.95 weight percent, wherein the water content of the bis (trifluoromethanesulfonyl) imide lithium powder is less than or equal to 50 multiplied by 10 -6 ，F - The content is less than or equal to 25 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 20 multiplied by 10 -6 ，Cl - The content is less than or equal to l5 multiplied by 10 -6 The content of B, na, K, ca, si, fe, mg, pb, al, zn, ni and Cu ions is less than or equal to 1 multiplied by 10 -6 The acidity index is less than or equal to 50ppm, and the transmittance of 75wt percent of the lithium bis (trifluoromethanesulfonyl) imide aqueous solution is more than or equal to 99.5 percent.
Further, the spray drying process parameters were as follows: the temperature of the air inlet is 200-300 ℃, the temperature of the air outlet is 150-180 ℃, the size of the atomizing disk is 52-155 mm, and the rotating speed is 10000-30000 r/min.
Further, the moisture content of the drying air source used in spray drying is less than or equal to 10 multiplied by 10 -6 。
Further, the heating temperature of the heat tracing equipment arranged on the pipeline connecting the bis (trifluoromethanesulfonyl) imidic acid storage tank and the multifunctional reactor is preferably 55-60 ℃.
Further, the purity of the lithium carbonate powder stored in the powder storage tank is more than or equal to 99.999wt percent, and F - The content is less than or equal to 10 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 10 multiplied by 10 -6 ，Cl - The content is less than or equal to 10 multiplied by 10 -6 。
Further, the purity of the bis (trifluoromethanesulfonyl) imide acid stored in the bis (trifluoromethanesulfonyl) imide acid tank is not less than 99.95% by weight, and F - The content is less than or equal to 25 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 20 multiplied by 10 -6 ，Cl - The content is less than or equal to 15 multiplied by 10 -6 The content of B, na, K, ca, si, fe, mg, pb, al, zn, ni and Cu ions is less than or equal to 1 multiplied by 10 -6 。
The beneficial effects are that:
(1) The device has less equipment, can realize continuous production, reduces equipment stop time, reduces personnel participation links, has high safety, improves the quality stability of products, improves the operation efficiency of the equipment and effectively reduces the production cost;
(2) The method disclosed by the invention is simple in process, easy to operate, high in production efficiency, high in purity and stable in quality of the prepared product, can meet the requirements of special industries such as ionic liquid and the like on special indexes of the product, and expands the application field of lithium bis (trifluoromethanesulfonyl) imide.
Drawings
Fig. 1 is a schematic structural view of the device according to the present invention.
The device comprises a 1-powder conveying mechanism, a 2-powder storage tank, a 3-bis (trifluoromethanesulfonyl) imide acid storage tank, a 4-high-purity water storage tank, a 5-multifunctional reactor, a 6-emptying port, a 7-vacuum port, an 8-bis (trifluoromethanesulfonyl) imide lithium solution storage tank, a 9-feed pump and 10-spray drying equipment.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
In the following examples, the lithium carbonate powder used was 5N grade lithium carbonate from Shanghai lithium Utility Co., ltd, and the detection method and apparatus used are shown in Table 1.
TABLE 1
The apparatus involved in the continuous preparation of lithium bis (trifluoromethanesulfonyl) imide in the following examples comprises a powder storage tank 2, a powder conveying mechanism 1, a multifunctional reactor 5, a bis (trifluoromethanesulfonyl) imide acid storage tank 3, a high-purity water storage tank 4, a bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8, a feed pump 9 and a spray drying device 10, as shown in fig. 1;
the multifunctional reactor 5 has stirring, filtering and heating functions and is a reaction vessel containing stirring equipment, heating equipment and filtering equipment, wherein the filtering pore diameter of the filtering equipment is not more than 10 mu m; the top of the multifunctional reactor 5 is provided with an emptying port 6, and the ratio of the height to the inner diameter of the multifunctional reactor 5 is (1.8-3): 1;
the top of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 is provided with a vacuum port 7 which is connected with external vacuum equipment;
the spray drying apparatus 10 is provided with a dehumidifying device, and is used for drying the spray drying apparatus 10Dehumidifying the dry air source to make the water content of the dry air source less than or equal to 10 multiplied by 10 -6 ；
The powder conveying mechanism 1 is respectively connected with a discharge port of the powder storage tank 2 and a feed port of the multifunctional reactor 5 and is used for conveying the powder in the powder storage tank 2 to the multifunctional reactor 5; the discharge port of the double (trifluoromethanesulfonyl) imidic acid storage tank 3 and the discharge port of the high-purity water storage tank 4 are respectively connected with the feed port of the multifunctional reactor 5, heat tracing equipment is respectively arranged on the double (trifluoromethanesulfonyl) imidic acid storage tank 3 and a pipeline connecting the double (trifluoromethanesulfonyl) imidic acid storage tank 3 and the multifunctional reactor 5, and the heating temperature of the heating equipment is controlled within the range of 55-60 ℃; the discharge port of the multifunctional reactor 5 is connected with the feed port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8, the feed pump 9 is respectively connected with the discharge port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 and the feed port of the spray drying equipment 10, and the lithium bis (trifluoromethanesulfonyl) imide solution is conveyed into the spray drying equipment 10 through the feed pump 9.
Example 1
In the device related to the continuous preparation of the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has the volume of 0.5m 3 Weight detection is provided; the powder conveying mechanism 1 is made of stainless steel and is a screw feeding device; the bis (trifluoromethanesulfonyl) imide acid storage tank 3 is made of stainless steel and has weight detection; the high-purity water storage tank 4 is made of stainless steel and has a volume of 0.5m 3 Weight detection is provided; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder is 900mm, the inner diameter of the cylinder is 500mm, the bottom of the cylinder is a conical filtering part, the maximum aperture of a filtering hole is 10 mu m, and the multifunctional reactor 5 has weight detection; the spray drying apparatus 10 is of stainless steel and the size of the atomizing disk is 52mm.
The specific steps for preparing the lithium bis (trifluoromethanesulfonyl) imide are as follows:
firstly, adding lithium carbonate powder in a powder storage tank 2 into a multifunctional reactor 5 through a powder conveying mechanism 1, wherein the adding amount is 1 kg-3 kg; the top vent 6 of the multifunctional reactor 5 is opened, and the high purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imidic acid storage tank 3 are filled with high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powderBody = 0.4: (7.54-7.56) adding high purity water and bis (trifluoromethanesulfonyl) imide acid to the multifunctional reactor 5 in a mass ratio of 1; the reaction materials are mixed in a multifunctional reactor 5 and react at 80-85 ℃, when the net weight of the reaction materials reaches 100-200 kg, the top vacuum port 7 of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is opened, the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is controlled to be minus 0.1MPa to minus 0.03MPa, and the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction is filtered and then enters the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, and conveying the bis (trifluoromethanesulfonyl) imide lithium solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 to the spray drying equipment 10 through a feed pump 9 for spray drying, wherein the temperature of an air inlet is 200-210 ℃, the temperature of an air outlet is 150-160 ℃, the rotating speed is 30000r/min, the discharge amount per hour is 5 kg-6 kg, and LiN (SO) with the bulk density of 0.76kg/L is obtained 2 CF 3 ) 2 The yield of the powder was 99.1%.
Respectively for raw materials Li 2 CO 3 And HN (SO) 2 CF 3 ) 2 And product LiN (SO) 2 CF 3 ) 2 The component contents of (2) were examined, and the results are shown in Table 2.
TABLE 2
Example 2
In the device related to the continuous preparation of the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has the volume of 0.5m 3 Weight detection is provided; the powder conveying mechanism 1 is made of stainless steel and is a screw feeding device; the bis (trifluoromethanesulfonyl) imide acid storage tank 3 is made of stainless steel and has weight detection; the high-purity water storage tank 4 is made of stainless steel and has a volume of 0.5m 3 Weight detection is provided; the multifunctional reactor 5 is made of stainless steel, the height of a cylinder body is 1500mm, the inner diameter of the cylinder body is 500mm, the bottom of the multifunctional reactor is a conical filtering part, and the most filtering holes are formedThe large aperture is 0.01 mu m, and the multifunctional reactor 5 has weight detection; the spray drying apparatus 10 is of stainless steel and the size of the atomizing disk is 155mm.
The specific steps for preparing the lithium bis (trifluoromethanesulfonyl) imide are as follows:
firstly, adding lithium carbonate powder in a powder storage tank 2 into a multifunctional reactor 5 through a powder conveying mechanism 1, wherein the adding amount is 1 kg-3 kg; the top vent 6 of the multifunctional reactor 5 is opened, and the high purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imidic acid storage tank 3 are filled with high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder = 3.3: (7.54-7.56) adding high purity water and bis (trifluoromethanesulfonyl) imide acid to the multifunctional reactor 5 in a mass ratio of 1; the reaction materials are mixed in a multifunctional reactor 5 and react at 90-95 ℃, when the net weight of the reaction materials reaches 100-200 kg, the top vacuum port 7 of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is opened, the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is controlled to be minus 0.1MPa to minus 0.03MPa, and the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction is filtered and then enters the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, and conveying the bis (trifluoromethanesulfonyl) imide lithium solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 to the spray drying equipment 10 through a feed pump 9 for spray drying, wherein the temperature of an air inlet is 290-300 ℃, the temperature of an air outlet is 170-180 ℃, the rotating speed is 10000r/min, the discharge amount per hour is 220 kg-230 kg, and LiN (SO) with the volume bulk density of 0.78kg/L is obtained 2 CF 3 ) 2 The yield of the powder was 99.2%.
Respectively for raw materials Li 2 CO 3 And HN (SO) 2 CF 3 ) 2 And product LiN (SO) 2 CF 3 ) 2 The component contents of (2) were examined, and the results are shown in Table 3.
TABLE 3 Table 3
Example 3
In the device related to the continuous preparation of the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has the volume of 0.5m 3 Weight detection is provided; the powder conveying mechanism 1 is made of stainless steel and is a screw feeding device; the bis (trifluoromethanesulfonyl) imide acid storage tank 3 is made of stainless steel and has weight detection; the high-purity water storage tank 4 is made of stainless steel and has a volume of 0.5m 3 Weight detection is provided; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder is 750mm, the inner diameter of the cylinder is 300mm, the bottom of the cylinder is a conical filtering part, the maximum aperture of a filtering hole is 0.1 mu m, and the multifunctional reactor 5 has weight detection; the spray drying apparatus 10 is of stainless steel and the size of the atomizing disk is 108mm.
The specific steps for preparing the lithium bis (trifluoromethanesulfonyl) imide are as follows:
firstly, adding lithium carbonate powder in a powder storage tank 2 into a multifunctional reactor 5 through a powder conveying mechanism 1, wherein the adding amount is 1 kg-3 kg; the top vent 6 of the multifunctional reactor 5 is opened, and the high purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imidic acid storage tank 3 are filled with high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder = 2.8: (7.54-7.56) adding high purity water and bis (trifluoromethanesulfonyl) imide acid to the multifunctional reactor 5 in a mass ratio of 1; the reaction materials are mixed in a multifunctional reactor 5 and react at 110-115 ℃, when the net weight of the reaction materials reaches 200-300 kg, the top vacuum port 7 of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is opened, the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is controlled to be minus 0.1MPa to minus 0.03MPa, and the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction is filtered and then enters the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, and conveying the bis (trifluoromethanesulfonyl) imide lithium solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 to the spray drying equipment 10 for spray drying through a feed pump 9, wherein the temperature of an air inlet is 280-290 ℃, the temperature of an air outlet is 160-170 ℃, the rotating speed is 16800r/min, the discharge amount per hour is 100 kg-120 kg, and LiN (SO) with the volume bulk density of 0.79kg/L is obtained 2 CF 3 ) 2 The yield of the powder was 99.1%.
Respectively for raw materials Li 2 CO 3 And HN (SO) 2 CF 3 ) 2 And product LiN (SO) 2 CF 3 ) 2 The component contents of (2) were examined, and the results are shown in Table 4.
TABLE 4 Table 4
Example 4
In the device related to the continuous preparation of the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has the volume of 0.5m 3 Weight detection is provided; the powder conveying mechanism 1 is made of stainless steel and is a screw feeding device; the bis (trifluoromethanesulfonyl) imide acid storage tank 3 is made of stainless steel and has weight detection; the high-purity water storage tank 4 is made of stainless steel and has a volume of 0.5m 3 Weight detection is provided; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder is 800mm, the inner diameter of the cylinder is 400mm, the bottom of the cylinder is a conical filtering part, the maximum aperture of a filtering hole is 1 mu m, and the multifunctional reactor 5 has weight detection; the spray drying apparatus 10 is of stainless steel and the size of the atomizing disk is 130mm.
The specific steps for preparing the lithium bis (trifluoromethanesulfonyl) imide are as follows:
firstly, adding lithium carbonate powder in a powder storage tank 2 into a multifunctional reactor 5 through a powder conveying mechanism 1, wherein the adding amount is 1 kg-3 kg; the top vent 6 of the multifunctional reactor 5 is opened, and the high purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imidic acid storage tank 3 are filled with high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder = 2.8: (7.54-7.56) adding high purity water and bis (trifluoromethanesulfonyl) imide acid to the multifunctional reactor 5 in a mass ratio of 1; the reaction materials are mixed in a multifunctional reactor 5 and react at the temperature of 85-90 ℃, when the net weight of the reaction materials reaches 200-300 kg, the top vacuum port 7 of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is opened, the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is controlled to be minus 0.1MPa to minus 0.03MPa, and the lithium bis (trifluoromethanesulfonyl) imide generated by the reaction is dissolvedFiltering the solution, and then, feeding the solution into a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, and conveying the bis (trifluoromethanesulfonyl) imide lithium solution in the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 to the spray drying equipment 10 through a feed pump 9 for spray drying, wherein the temperature of an air inlet is 250-260 ℃, the temperature of an air outlet is 165-175 ℃, the rotating speed is 14700r/min, the discharge amount per hour is 100 kg-120 kg, and LiN (SO) with the bulk density of 0.76kg/L is obtained 2 CF 3 ) 2 The yield of the powder was 99.2%.
Respectively for raw materials Li 2 CO 3 And HN (SO) 2 CF 3 ) 2 And product LiN (SO) 2 CF 3 ) 2 The component contents of (2) were examined, and the results are shown in Table 5.
TABLE 5
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. 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. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide, which is characterized in that: the device comprises a powder storage tank, a powder conveying mechanism, a multifunctional reactor, a bis (trifluoromethanesulfonyl) imide acid storage tank, a high-purity water storage tank, a bis (trifluoromethanesulfonyl) imide lithium solution storage tank, a feed pump and spray drying equipment;
the multifunctional reactor is a reaction vessel containing stirring equipment, heating equipment and filtering equipment, and the top of the multifunctional reactor is provided with a vent;
the powder conveying mechanism is respectively connected with a discharge port of the powder storage tank and a feed port of the multifunctional reactor, a discharge port of the bis (trifluoromethanesulfonyl) imidic acid storage tank and a discharge port of the high-purity water storage tank are respectively connected with the feed port of the multifunctional reactor, and heat tracing equipment is respectively arranged on the bis (trifluoromethanesulfonyl) imidic acid storage tank and a pipeline connecting the bis (trifluoromethanesulfonyl) imidic acid storage tank and the multifunctional reactor; the discharge port of the multifunctional reactor is connected with the feed port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank, and the feed pump is respectively connected with the discharge port of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank and the feed port of the spray drying equipment.
2. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the ratio of the height to the inner diameter of the multifunctional reactor is (1.8-3): 1.
3. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the filtration pore size of the filtration device in the multifunctional reactor is not more than 10 μm.
4. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the spray drying equipment is internally provided with a dehumidifying device.
5. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the top of the double (trifluoro methylsulfonyl) imine lithium solution storage tank is provided with a vacuum port which is connected with external vacuum-pumping equipment.
6. A method for preparing lithium bis (trifluoromethanesulfonyl) imide using the apparatus of any one of claims 1 to 5, characterized in that: the steps of the method are as follows,
high purity water storage tank, bis (trifluoromethanesulfonyl) imidic acid storage tank and powder storage tank according to high purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder= (0.4-3.3): (7.54-7.56) 1 the raw materials are added into a multifunctional reactor according to the mass ratio, and after the raw materials are mixed, the raw materials react at 80-120 ℃ to produce bis (trifluoromethanesulfonyl)) Filtering the lithium imide solution, then feeding the filtered lithium imide solution into a lithium bis (trifluoromethanesulfonyl) imide solution storage tank, feeding the lithium bis (trifluoromethanesulfonyl) imide solution into spray drying equipment under the action of a feed pump, and performing spray drying to obtain lithium bis (trifluoromethanesulfonyl) imide powder with the purity of more than 99.95 weight percent, wherein the water content of the lithium bis (trifluoromethanesulfonyl) imide powder is less than or equal to 50 multiplied by 10 -6 ，F - The content is less than or equal to 25 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 20 multiplied by 10 -6 ，Cl - The content is less than or equal to l5 multiplied by 10 -6 The content of B, na, K, ca, si, fe, mg, pb, al, zn, ni and Cu ions is less than or equal to 1 multiplied by 10 -6 The acidity index is less than or equal to 50ppm, and the transmittance of 75wt percent of the lithium bis (trifluoromethanesulfonyl) imide aqueous solution is more than or equal to 99.5 percent.
7. A method for preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 6, wherein: the process parameters of spray drying are as follows: the temperature of the air inlet is 200-300 ℃, the temperature of the air outlet is 150-180 ℃, the size of the atomizing disk is 52-155 mm, and the rotating speed is 10000-30000 r/min.
8. A method for preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 6, wherein: the moisture content of a drying air source used in spray drying is less than or equal to 10 multiplied by 10 -6 。
9. An apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 6, wherein: the heating temperature of the heat tracing equipment arranged on the pipeline connecting the bis (trifluoromethanesulfonyl) imidic acid storage tank and the multifunctional reactor is 55-60 ℃.
10. A method for preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 6, wherein: the purity of the lithium carbonate powder stored in the powder storage tank is more than or equal to 99.999 weight percent, and F - The content is less than or equal to 10 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 10 multiplied by 10 -6 ，Cl - The content is less than or equal to 10 multiplied by 10 -6 The method comprises the steps of carrying out a first treatment on the surface of the Bis (trifluoromethanesulfonyl) sulfinesThe purity of the bis (trifluoromethanesulfonyl) imide stored in the amine acid tank is not less than 99.95% by weight, and F - The content is less than or equal to 25 multiplied by 10 -6 ，SO 4 2- The content is less than or equal to 20 multiplied by 10 -6 ，Cl - The content is less than or equal to 15 multiplied by 10 -6 The content of B, na, K, ca, si, fe, mg, pb, al, zn, ni and Cu ions is less than or equal to 1 multiplied by 10 -6 。
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| CN1319589A (en) * | 2000-01-31 | 2001-10-31 | 森田化学工业株式会社 | Process for preparing sulfimine compound |
| CN103664712A (en) * | 2013-11-27 | 2014-03-26 | 中国船舶重工集团公司第七一八研究所 | Method for preparing fluorine sulfimide lithium |
| KR20190001092A (en) * | 2017-06-26 | 2019-01-04 | 임광민 | Novel preparing method of very efficient and simple lithium bis(fluorosulfonyl)imide |
| CN111362843A (en) * | 2019-08-22 | 2020-07-03 | 福建永晶科技股份有限公司 | Novel process for synthesizing fluorinated conductive salt for lithium ion battery |
| CN215087056U (en) * | 2020-12-15 | 2021-12-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Device for continuously preparing bis (trifluoromethanesulfonyl) imide lithium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319589A (en) * | 2000-01-31 | 2001-10-31 | 森田化学工业株式会社 | Process for preparing sulfimine compound |
| CN103664712A (en) * | 2013-11-27 | 2014-03-26 | 中国船舶重工集团公司第七一八研究所 | Method for preparing fluorine sulfimide lithium |
| KR20190001092A (en) * | 2017-06-26 | 2019-01-04 | 임광민 | Novel preparing method of very efficient and simple lithium bis(fluorosulfonyl)imide |
| CN111362843A (en) * | 2019-08-22 | 2020-07-03 | 福建永晶科技股份有限公司 | Novel process for synthesizing fluorinated conductive salt for lithium ion battery |
| CN215087056U (en) * | 2020-12-15 | 2021-12-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Device for continuously preparing bis (trifluoromethanesulfonyl) imide lithium |
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