CN112536014A - Device and method for continuously preparing bis (trifluoromethanesulfonyl) imide lithium - Google Patents
Device and method for continuously preparing bis (trifluoromethanesulfonyl) imide lithium Download PDFInfo
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- CN112536014A CN112536014A CN202011481539.5A CN202011481539A CN112536014A CN 112536014 A CN112536014 A CN 112536014A CN 202011481539 A CN202011481539 A CN 202011481539A CN 112536014 A CN112536014 A CN 112536014A
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- trifluoromethanesulfonyl
- imide
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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 79
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000003860 storage Methods 0.000 claims abstract description 106
- 239000000843 powder Substances 0.000 claims abstract description 47
- 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 abstract description 45
- 239000002253 acid Substances 0.000 claims abstract description 40
- 238000001694 spray drying Methods 0.000 claims abstract description 38
- 239000012498 ultrapure water Substances 0.000 claims abstract description 25
- -1 (trifluoromethanesulfonyl) lithium imide Chemical class 0.000 claims abstract description 23
- 230000007246 mechanism Effects 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 64
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 62
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000001914 filtration Methods 0.000 claims description 26
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000002834 transmittance Methods 0.000 claims description 4
- 125000001889 triflyl group Chemical group FC(F)(F)S(*)(=O)=O 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 150000003949 imides Chemical class 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000002608 ionic liquid Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000010924 continuous production Methods 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 19
- 239000000463 material Substances 0.000 description 12
- 238000001514 detection method Methods 0.000 description 8
- 229910003002 lithium salt Inorganic materials 0.000 description 8
- 159000000002 lithium salts Chemical class 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 8
- 229910052808 lithium carbonate Inorganic materials 0.000 description 6
- IMNIECVIVJOTBH-UHFFFAOYSA-N trifluoromethanesulfonyl bromide Chemical compound FC(F)(F)S(Br)(=O)=O IMNIECVIVJOTBH-UHFFFAOYSA-N 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 239000002904 solvent Substances 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
- 238000000746 purification Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 150000003839 salts Chemical class 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
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 239000000203 mixture 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
- 238000001308 synthesis method Methods 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 compound [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
- GUNJVIDCYZYFGV-UHFFFAOYSA-K antimony trifluoride Chemical compound F[Sb](F)F GUNJVIDCYZYFGV-UHFFFAOYSA-K 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
- JHRWWRDRBPCWTF-OLQVQODUSA-N captafol Chemical compound C1C=CC[C@H]2C(=O)N(SC(Cl)(Cl)C(Cl)Cl)C(=O)[C@H]21 JHRWWRDRBPCWTF-OLQVQODUSA-N 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
- 238000004821 distillation Methods 0.000 description 1
- 150000002170 ethers Chemical class 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
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012046 mixed solvent Substances 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
- 238000011085 pressure filtration Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000007921 spray Substances 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
- 230000002194 synthesizing effect Effects 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
Images
Classifications
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- 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 bis (trifluoromethanesulfonyl) lithium imide, belonging to the technical field of preparation of bis (trifluoromethanesulfonyl) lithium imide. 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 feeding pump and spray drying equipment, wherein raw materials are added into the multifunctional reactor through the raw material storage tanks, are mixed and react in the multifunctional reactor, and are subjected to spray drying treatment to obtain product powder. The device provided by the invention has the advantages that the number of devices is small, the continuous production can be realized, the safety is high, the quality stability of products is improved, the operation efficiency of the device is improved, and the production cost is effectively reduced; the method has the advantages of simple process, easy operation, high production efficiency, high purity of the prepared product and stable quality, and can meet the requirements of special industries such as ionic liquid and the like on special indexes of the product.
Description
Technical Field
The invention relates to a device and a method for continuously preparing bis (trifluoromethanesulfonyl) lithium imide, belonging to the technical field of preparation of bis (trifluoromethanesulfonyl) lithium imide.
Background
The lithium fluorosulfonyl imide is an important fluorine-containing organic ionic compound, has high voltage resistance and conductivity, and has important industrial application value in many fields. The bis (trifluoromethanesulfonyl) imide lithium is a typical representative of fluorosulfonyl imide lithium, has good thermal stability, high electrochemical stability and high conductivity, and is widely applied to lithium ion battery organic electrolyte lithium salts to prepare room-temperature ionic liquids, reaction catalysts, antistatic agents and the like.
The methods for preparing lithium bis (trifluoromethanesulfonyl) imide reported so far are as follows:
U.S. Pat. No. 5,5874616 reports that fluoroalkyl sulfonyl halides are reacted with fluoroalkyl sulfonamides in the presence of aprotic solvents to give fluorosulfonyl imines, which are acidified and then reacted with bases or salts in the presence of organic solvents to give fluoroalkyl sulfonyl imines. The method adopts more kinds of reactants, has fewer reaction steps, and has higher reaction yield but lower purity.
U.S. Pat. No. 20010021790 reports that 1mol of anhydrous ammonia, 2mol of sulfonyl halide and 6mol of alkali metal fluoride are put into a reactor, the mixture is reacted in a solvent, or 1mol of ammonium salt, 2mol of sulfonyl halide and 7mol of alkali metal fluoride are put into the reactor, the mixture is reacted in the solvent, after the reaction is finished, hydrogen fluoride is filtered, the solvent is evaporated and concentrated to obtain the product of the metal salt of sulfonimide, the yield is high (more than 89%), and the yield of the lithium salt is low (about 2%). And reacting the fluorosulfonyl imide acid obtained by acidolysis with lithium carbonate to obtain the product with the purity of 99%.
Chinese patent CN200910057888.1 reports that trifluoromethanesulfonyl bromide is subjected to sulfination and dehalogenation reaction to obtain trifluoromethanesulfonyl bromide, trifluoromethanesulfonyl bromide is added into ammonia water to react to obtain trifluoromethanesulfonyl amide, the trifluoromethanesulfonyl bromide is dissolved in alkylamine solution, trifluoromethanesulfonyl bromide is continuously added to react, the solvent is removed under reduced pressure after the reaction is finished, the residue is dissolved in dichloromethane, organic phase is collected after washing with water to obtain bis (trifluoromethanesulfonyl) imide, the obtained bis (trifluoromethanesulfonyl) imide is reacted with lithium salt to obtain final product, and then the final product is obtained after recrystallization and purification by using mixed solvent of n-hexane and ethers. The purification by using a recrystallization method has low purity (about 99 percent) and poor operating environment.
Chinese patent CN200810197929 reports that sulfonamide, thionyl chloride and chlorosulfonic acid are added into a reactor according to a certain proportion for reaction, after the reaction is finished, an imine compound is evaporated out 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 for reaction, the reduced pressure filtration is carried out, the filtrate is recrystallized to obtain salts, then a double decomposition reaction is adopted to prepare lithium salt, and the recrystallization is carried out 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 fine fluorosulfonyl imide acid solution while 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 easily controlled to cause high acidity of the finished product, the product fluctuation is large, the transmittance of 75% lithium bis (trifluoromethanesulfonyl) imide aqueous solution is low, and the method is not suitable for industries such as ionic liquid and the like with high requirements on the lithium bis (trifluoromethanesulfonyl) imide aqueous solution.
Various methods for preparing lithium bis (trifluoromethanesulfonyl) imide have been reported at home and abroad, and mainly comprise a one-step synthesis method and a multi-step synthesis method. The one-step synthesis method is characterized in that liquid ammonia, trifluoromethanesulfonyl fluoride and lithium fluoride are adopted to react in an organic solvent for preparation, and the method is extremely low in yield, low in purity and difficult in industrial application; the multi-step synthesis method comprises the steps of firstly synthesizing crude bis (trifluoromethanesulfonyl) imide salt, then carrying out acidolysis on the crude bis (trifluoromethanesulfonyl) imide salt, carrying out reduced pressure distillation and purification on the crude bis (trifluoromethanesulfonyl) imide salt to obtain bis (trifluoromethanesulfonyl) imide acid, reacting the bis (trifluoromethanesulfonyl) imide acid with excessive lithium salt in an organic solvent or water, filtering out the excessive lithium salt, and concentrating and purifying the bis (trifluoromethanesulfonyl) imide lithium in the organic solvent. In addition, the product obtained by the method is reacted or purified by using an organic solvent, most of the organic solvents are 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 compound, so that the subsequent drying and the final purity of the product are influenced. The purity of the product obtained by the intermittent operation can only reach 99 percent mostly, and the special requirements of the ionic liquid industry on the acidity and the transmittance can not be met although some method indexes can reach higher purity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a device and a method for continuously preparing bis (trifluoromethanesulfonyl) imide lithium, the device has less equipment, can realize continuous production, improves the quality stability of products, improves the operation efficiency of the equipment, and effectively reduces the production cost; the method has the advantages of simple process, easy operation, high production efficiency, high purity of the prepared product and stable quality, and can meet the requirements of special industries such as ionic liquid and the like on special indexes of the product.
The purpose of the invention is realized by the following technical scheme.
The device for continuously preparing the lithium bis (trifluoromethanesulfonyl) imide 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 feeding pump and spray drying equipment;
the multifunctional reactor has stirring, filtering and heating functions, is a reaction container containing stirring equipment, heating equipment and filtering equipment, and is provided with a vent at the top;
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) imide storage tank and a discharge port of the high-purity water storage tank are respectively connected with a feed port of the multifunctional reactor, and heat tracing equipment is respectively arranged on the bis (trifluoromethanesulfonyl) imide storage tank and a pipeline connecting the bis (trifluoromethanesulfonyl) imide storage tank and the multifunctional reactor; the discharge port of the multifunctional reactor is connected with the feed port of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank, and the feed pump is respectively connected with the discharge port of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank and the feed port of the spray drying equipment.
Furthermore, the ratio of the height to the inner diameter of the multifunctional reactor is preferably (1.8-3): 1.
Further, the filtration pore size of the filtration device in the multifunctional reactor is preferably not more than 10 μm, more preferably 0.01 μm to 10 μm.
Furthermore, the top of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank is provided with a vacuum port which is connected with an external vacuum-pumping device.
Furthermore, a dehumidifying device is arranged in the spray drying equipment to dehumidify the 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 10×10-6。
The method for preparing the bis (trifluoromethanesulfonyl) imide lithium by adopting the device provided by the invention comprises the following specific steps:
a high-purity water storage tank, a bis (trifluoromethanesulfonyl) imide acid storage tank and a powder storage tank are arranged according to the following proportion: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder (0.4 to 3.3): (7.54-7.56) adding raw materials into a multifunctional reactor according to the mass ratio of 1, mixing the raw materials, reacting at 80-120 ℃, filtering a bis (trifluoromethanesulfonyl) lithium imide solution generated by the reaction, then feeding the filtered bis (trifluoromethanesulfonyl) lithium imide solution into a bis (trifluoromethanesulfonyl) lithium imide solution storage tank, and feeding the bis (trifluoromethanesulfonyl) lithium imide solution into a spray drying device for spray drying under the action of a feed pump to obtain bis (trifluoromethanesulfonyl) lithium imide powder with the purity of more than 99.95 wt%, wherein the water content of the powder is less than or equal to 50 x 10-6，F-The content is less than or equal to 25 multiplied by 10-6，SO4 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 10-6The contents of B, Na, K, Ca, Si, Fe, Mg, Pb, Al, Zn, Ni and Cu ions are less than or equal to 1 x 10-6The acidity index is less than or equal to 50ppm, and the transmittance of 75 wt% lithium bis (trifluoromethanesulfonyl) imide aqueous solution is more than or equal to 99.5%.
Further, 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 r/min-30000 r/min.
Further, the water content of the drying air source used in the spray drying is less than or equal to 10 multiplied by 10-6。
Further, the heating temperature of the bis (trifluoromethanesulfonyl) imide acid storage tank and the heat tracing equipment arranged on the pipeline connecting the bis (trifluoromethanesulfonyl) imide 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 99.999 wt%, and F-The content is less than or equal to 10 multiplied by 10-6，SO4 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, bis (trifluoromethanesulfonyl) imideThe purity of the bis (trifluoromethanesulfonyl) imide acid stored in the acid storage tank is more than or equal to 99.95 wt%, and F-The content is less than or equal to 25 multiplied by 10-6，SO4 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 10-6The contents of B, Na, K, Ca, Si, Fe, Mg, Pb, Al, Zn, Ni and Cu ions are less than or equal to 1 x 10-6。
Has the advantages that:
(1) the device provided by the invention has fewer devices, can realize continuous production, reduces the device stop time, reduces the personnel participation link, has high safety, improves the quality stability of products, improves the device operation efficiency, and effectively reduces the production cost;
(2) the method has the advantages of simple process, easy operation, high production efficiency, high purity of the prepared product and stable quality, 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 the lithium bis (trifluoromethanesulfonyl) imide.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention.
The device comprises a powder conveying mechanism 1, a powder storage tank 2, a 3-bis (trifluoromethanesulfonyl) imide acid storage tank, a high-purity water storage tank 4, a multifunctional reactor 5, a vent 6, a vacuum port 7, a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8, a feeding pump 9 and spray drying equipment 10.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
In the following examples, lithium carbonate powder used was lithium carbonate of grade 5N from lithium industries ltd in shanghai, and the details of the detection method and apparatus used are shown in table 1.
TABLE 1
The device 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 storage tank 3 for bis (trifluoromethanesulfonyl) imide acid, a storage tank 4 for high-purity water, a storage tank 8 for lithium bis (trifluoromethanesulfonyl) imide solution, a feeding pump 9 and spray drying equipment 10, as shown in fig. 1;
the multifunctional reactor 5 has stirring, filtering and heating functions, and is a reaction container 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 a vent 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 lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is provided with a vacuum port 7 which is connected with external vacuum-pumping equipment;
the spray drying equipment 10 is internally provided with a dehumidifying device which dehumidifies the drying air source used by the spray drying equipment 10 to ensure that the moisture content of the drying air source is less than or equal to 10 multiplied by 10-6；
The powder conveying mechanism 1 is respectively connected with a discharge hole of the powder storage tank 2 and a feed inlet of the multifunctional reactor 5 and is used for conveying the powder in the powder storage tank 2 to the multifunctional reactor 5; a discharge hole of the bis (trifluoromethanesulfonyl) imide acid storage tank 3 and a discharge hole of the high-purity water storage tank 4 are respectively connected with a feed inlet of the multifunctional reactor 5, heat tracing equipment is respectively arranged on the bis (trifluoromethanesulfonyl) imide acid storage tank 3 and a pipeline connecting the bis (trifluoromethanesulfonyl) imide 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 bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8, the feed pump 9 is respectively connected with the discharge port of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank 8 and the feed port of the spray drying equipment 10, and the bis (trifluoromethanesulfonyl) imide lithium solution is conveyed into the spray drying equipment 10 through the feed pump 9.
Example 1
In the device for continuously preparing the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has a volume of 0.5m3Heavy and heavyDetecting the quantity; 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 0.5m3Detecting the weight; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder body is 900mm, the inner diameter of the cylinder body is 500mm, the bottom is a conical filtering part, the maximum aperture of the filtering hole is 10 mu m, and the multifunctional reactor 5 is used for weight detection; the spray drying equipment 10 is made of stainless steel, and the size of the atomizing disk is 52 mm.
The specific steps for preparing 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; opening the top vent 6 of the multifunctional reactor 5, and then filling the high-purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imide acid storage tank 3 with high-purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder 0.4: (7.54-7.56) adding high-purity water and bis (trifluoromethanesulfonyl) imide acid into the multifunctional reactor 5 according to the mass ratio of 1; mixing the reaction materials in a multifunctional reactor 5, reacting at 80-85 ℃, opening a vacuum port 7 at the top of a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 when the net weight of the reaction materials reaches 100-200 kg, controlling the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to be-0.1-0.03 MPa, and filtering the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction and then feeding the lithium bis (trifluoromethanesulfonyl) imide solution into the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, conveying the lithium bis (trifluoromethanesulfonyl) imide solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to the spray drying equipment 10 through a feed pump 9 for spray drying, wherein the air inlet temperature is 200-210 ℃, the air outlet temperature is 150-160 ℃, the rotating speed is 30000r/min, the discharge amount per hour is 5 kg-6 kg, and LiN (SO) with the volume bulk density of 0.76kg/L is obtained2CF3)2Powder, yield 99.1%.
Respectively to raw material Li2CO3And HN (SO)2CF3)2And the product LiN (SO)2CF3)2The component contents of (A) are detected, and the results are detailed in table 2.
TABLE 2
Example 2
In the device for continuously preparing the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has a volume of 0.5m3Detecting the weight; 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 0.5m3Detecting the weight; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder body is 1500mm, the inner diameter of the cylinder body is 500mm, the bottom is a conical filtering part, the maximum aperture of the filtering hole is 0.01 mu m, and the multifunctional reactor 5 is used for weight detection; the spray drying equipment 10 is made of stainless steel, and the size of an atomizing disk is 155 mm.
The specific steps for preparing 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; opening the top vent 6 of the multifunctional reactor 5, and then filling the high-purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imide acid storage tank 3 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 into the multifunctional reactor 5 according to the mass ratio of 1; mixing the reaction materials in a multifunctional reactor 5 and reacting at 90-95 ℃, opening a vacuum port 7 at the top of a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 when the net weight of the reaction materials reaches 100-200 kg, controlling the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to be-0.1-0.03 MPa, and filtering the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction and then feeding the lithium bis (trifluoromethanesulfonyl) imide solution into the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is accumulated to 100 kg-200 kg, the spray drying equipment 10 is startedConveying the lithium bis (trifluoromethanesulfonyl) imide solution in a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to spray drying equipment 10 through a feeding pump 9 for spray drying, wherein the air inlet temperature is 290-300 ℃, the air outlet temperature is 170-180 ℃, the rotating speed is 10000r/min, the hourly discharge amount is 220-230 kg, and LiN (SO) with the volume bulk density of 0.78kg/L is obtained2CF3)2Powder, yield 99.2%.
Respectively to raw material Li2CO3And HN (SO)2CF3)2And the product LiN (SO)2CF3)2The component contents of (A) were measured and the results are detailed in Table 3.
TABLE 3
Example 3
In the device for continuously preparing the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has a volume of 0.5m3Detecting the weight; 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 0.5m3Detecting the weight; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder body is 750mm, the inner diameter of the cylinder body is 300mm, the bottom is a conical filtering part, the maximum aperture of the filtering hole is 0.1 mu m, and the weight of the multifunctional reactor 5 is detected; the spray drying equipment 10 is made of stainless steel, and the size of an atomizing disk is 108 mm.
The specific steps for preparing 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; opening the top vent 6 of the multifunctional reactor 5, and then filling the high-purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imide acid storage tank 3 with high-purity water: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder 2.8: (7.54-7.56) in a mass ratio of 1 to the multifunctional reactor 5High purity water and bis (trifluoromethanesulfonyl) imide acid; mixing the reaction materials in a multifunctional reactor 5, reacting at 110-115 ℃, opening a vacuum port 7 at the top of a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 when the net weight of the reaction materials reaches 200-300 kg, controlling the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to be-0.1-0.03 MPa, and filtering the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction and then feeding the lithium bis (trifluoromethanesulfonyl) imide solution into the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, conveying the lithium bis (trifluoromethanesulfonyl) imide solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to the spray drying equipment 10 through a feed pump 9 for spray drying, wherein the air inlet temperature is 280-290 ℃, the air outlet temperature 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 obtained2CF3)2Powder, yield 99.1%.
Respectively to raw material Li2CO3And HN (SO)2CF3)2And the product LiN (SO)2CF3)2The component contents of (A) were measured, and the results are shown in Table 4.
TABLE 4
Example 4
In the device for continuously preparing the lithium bis (trifluoromethanesulfonyl) imide, the powder storage tank 2 is made of stainless steel material and has a volume of 0.5m3Detecting the weight; 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 0.5m3Detecting the weight; the multifunctional reactor 5 is made of stainless steel, the height of the cylinder body is 800mm, the inner diameter of the cylinder body is 400mm, the bottom is a conical filtering part, the maximum aperture of the filtering hole is 1 mu m, and the multifunctional reactor 5 is used for weight detection; spray dryingThe drying device 10 is made of stainless steel, and the size of the atomizing disk is 130 mm.
The specific steps for preparing 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; opening the top vent 6 of the multifunctional reactor 5, and then filling the high-purity water storage tank 4 and the bis (trifluoromethanesulfonyl) imide acid storage tank 3 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 into the multifunctional reactor 5 according to the mass ratio of 1; mixing the reaction materials in a multifunctional reactor 5, reacting at 85-90 ℃, opening a vacuum port 7 at the top of a lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 when the net weight of the reaction materials reaches 200-300 kg, controlling the pressure of the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to be-0.1-0.03 MPa, and filtering the lithium bis (trifluoromethanesulfonyl) imide solution generated by the reaction and then feeding the lithium bis (trifluoromethanesulfonyl) imide solution into the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8; after the solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 is accumulated to 100 kg-200 kg, starting the spray drying equipment 10, conveying the lithium bis (trifluoromethanesulfonyl) imide solution in the lithium bis (trifluoromethanesulfonyl) imide solution storage tank 8 to the spray drying equipment 10 through a feeding pump 9 for spray drying, wherein the air inlet temperature is 250-260 ℃, the air outlet temperature is 165-175 ℃, the rotating speed is 14700r/min, the discharge amount per hour is 100 kg-120 kg, and LiN (SO) with the volume bulk density of 0.76kg/L is obtained2CF3)2Powder, yield 99.2%.
Respectively to raw material Li2CO3And HN (SO)2CF3)2And the product LiN (SO)2CF3)2The component contents of (A) were measured, and the results are shown in Table 5.
TABLE 5
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement 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, comprising: 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 feeding pump and spray drying equipment;
the multifunctional reactor is a reaction container 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) imide storage tank and a discharge port of the high-purity water storage tank are respectively connected with a feed port of the multifunctional reactor, and heat tracing equipment is respectively arranged on the bis (trifluoromethanesulfonyl) imide storage tank and a pipeline connecting the bis (trifluoromethanesulfonyl) imide storage tank and the multifunctional reactor; the discharge port of the multifunctional reactor is connected with the feed port of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank, and the feed pump is respectively connected with the discharge port of the bis (trifluoromethanesulfonyl) imide lithium solution storage tank and the feed port of the spray drying equipment.
2. The 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) to 1.
3. The apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the filtering pore size of the filtering device in the multifunctional reactor is not more than 10 μm.
4. The 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. The apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 1, wherein: the top of the bis (trifluoromethanesulfonyl) imide 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 device of any one of claims 1 to 5, wherein: the steps of the method are as follows,
a high-purity water storage tank, a bis (trifluoromethanesulfonyl) imide acid storage tank and a powder storage tank are arranged according to the following proportion: bis (trifluoromethanesulfonyl) imide acid: lithium carbonate powder (0.4 to 3.3): (7.54-7.56) adding raw materials into a multifunctional reactor according to the mass ratio of 1, mixing the raw materials, reacting at 80-120 ℃, filtering a bis (trifluoromethanesulfonyl) lithium imide solution generated by the reaction, then feeding the filtered bis (trifluoromethanesulfonyl) lithium imide solution into a bis (trifluoromethanesulfonyl) lithium imide solution storage tank, and feeding the bis (trifluoromethanesulfonyl) lithium imide solution into a spray drying device for spray drying under the action of a feed pump to obtain bis (trifluoromethanesulfonyl) lithium imide powder with the purity of more than 99.95 wt%, wherein the water content of the powder is less than or equal to 50 x 10-6，F-The content is less than or equal to 25 multiplied by 10-6，SO4 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 10-6The contents of B, Na, K, Ca, Si, Fe, Mg, Pb, Al, Zn, Ni and Cu ions are less than or equal to 1 x 10-6The acidity index is less than or equal to 50ppm, and the transmittance of 75 wt% lithium bis (trifluoromethanesulfonyl) imide aqueous solution is more than or equal to 99.5%.
7. The method according to claim 6, wherein the lithium bis (trifluoromethanesulfonyl) imide comprises: the process parameters of spray drying 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 r/min-30000 r/min.
8. A process according to claim 6 for the preparation of lithium bis (trifluoromethanesulfonyl) imideThe method is characterized in that: the water content of the drying air source used in the spray drying is less than or equal to 10 multiplied by 10-6。
9. The apparatus for continuously preparing lithium bis (trifluoromethanesulfonyl) imide according to claim 6, wherein: the heating temperature of the double (trifluoromethanesulfonyl) imide acid storage tank and the heat tracing equipment arranged on the pipeline connecting the double (trifluoromethanesulfonyl) imide acid storage tank and the multifunctional reactor is 55-60 ℃.
10. The method according to claim 6, wherein the lithium bis (trifluoromethanesulfonyl) imide comprises: the purity of the lithium carbonate powder stored in the powder storage tank is more than or equal to 99.999 wt%, and F-The content is less than or equal to 10 multiplied by 10-6，SO4 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(ii) a The purity of the bis (trifluoromethanesulfonyl) imide acid stored in the bis (trifluoromethanesulfonyl) imide acid storage tank is more than or equal to 99.95 wt%, and F-The content is less than or equal to 25 multiplied by 10-6，SO4 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 10-6The contents of B, Na, K, Ca, Si, Fe, Mg, Pb, Al, Zn, Ni and Cu ions are less than or equal to 1 x 10-6。
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| CN115159480A (en) * | 2022-06-24 | 2022-10-11 | 森松（江苏）重工有限公司 | Production system of bis (chlorosulfonyl) imide |
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| 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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| CN1319589A (en) * | 2000-01-31 | 2001-10-31 | 森田化学工业株式会社 | Process for preparing sulfimine compound |
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| KR20190001092A (en) * | 2017-06-26 | 2019-01-04 | 임광민 | Novel preparing method of very efficient and simple lithium bis(fluorosulfonyl)imide |
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