CN116573619B - Preparation device and method of sodium bis (fluorosulfonyl) imide - Google Patents
Preparation device and method of sodium bis (fluorosulfonyl) imide Download PDFInfo
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- CN116573619B CN116573619B CN202310826887.9A CN202310826887A CN116573619B CN 116573619 B CN116573619 B CN 116573619B CN 202310826887 A CN202310826887 A CN 202310826887A CN 116573619 B CN116573619 B CN 116573619B
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- VCCATSJUUVERFU-UHFFFAOYSA-N sodium bis(fluorosulfonyl)azanide Chemical compound FS(=O)(=O)N([Na])S(F)(=O)=O VCCATSJUUVERFU-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 8
- 229910021201 NaFSI Inorganic materials 0.000 claims description 67
- 230000015572 biosynthetic process Effects 0.000 claims description 48
- 238000003786 synthesis reaction Methods 0.000 claims description 48
- 239000002904 solvent Substances 0.000 claims description 37
- -1 alkali metal salt Chemical class 0.000 claims description 35
- 229910052783 alkali metal Inorganic materials 0.000 claims description 25
- 239000010409 thin film Substances 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000010408 film Substances 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- WBUSGNQHRJVPTI-UHFFFAOYSA-N FN(F)S(=O)=O Chemical compound FN(F)S(=O)=O WBUSGNQHRJVPTI-UHFFFAOYSA-N 0.000 claims description 9
- 238000006386 neutralization reaction Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XPVRBHCXMWRJEY-UHFFFAOYSA-N difluoro(imino)-$l^{4}-sulfane Chemical compound FS(F)=N XPVRBHCXMWRJEY-UHFFFAOYSA-N 0.000 claims description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000004537 pulping Methods 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 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 claims description 2
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 claims description 2
- 150000001348 alkyl chlorides Chemical class 0.000 claims 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 12
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910010941 LiFSI Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ATMIHASMQFJNLZ-UHFFFAOYSA-N dichloro(imino)-$l^{4}-sulfane Chemical compound ClS(Cl)=N ATMIHASMQFJNLZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
- C01B21/096—Amidosulfonic acid; Salts thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/06—Evaporators with vertical tubes
- B01D1/065—Evaporators with vertical tubes by film evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- 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
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/1812—Tubular reactors
- B01J19/1818—Tubular reactors in series
-
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/086—Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of sodium ion batteries, and particularly relates to a preparation device and a preparation method of sodium bis (fluorosulfonyl) imide.
Description
Technical Field
The invention belongs to the field of sodium ion batteries, and relates to a preparation device and a preparation method of sodium bis (fluorosulfonyl) imide.
Background
In recent years, as the demand of the lithium ion battery is increased, the lithium resource supply is insufficient, the price of lithium carbonate is continuously increased, the content of sodium element in crust is rich, the cost is lower, the influence of supply and demand on the price is small, and aluminum foils can be used for the anode and cathode current collector materials of the sodium ion battery, so that the low-cost advantage of the sodium ion battery is further expanded. The sodium ion battery has more excellent high-low temperature performance. Compared with the working temperature range of-20 ℃ to 60 ℃ of the lithium ion battery, the sodium ion battery can normally work in the temperature range of-40 ℃ to 80 ℃, the capacity retention rate is approximately 90% in the environment of-20 ℃, and the high-low temperature performance is more excellent. The sodium ion battery has higher safety, and has higher safety due to higher internal resistance, less instant heating value under the short circuit condition and higher thermal runaway temperature than the lithium ion battery. The safety performance of the sodium ion battery is also satisfactory when tested for overcharge, overdischarge, needling, and extrusion. The sodium ion battery has good multiplying power performance and has advantages in the aspect of quick charge. The sodium ion battery has better multiplying power performance, can adapt to response type energy storage and large-scale power supply, and can be better qualified for large-scale energy storage.
Currently, the main stream of sodium battery electrolyte solute products is(sodium hexafluorophosphate),. About.>The higher viscosity affects the kinetic properties. Compared with the sodium ion battery electrolyte solute, the NaFSI has the advantages of small viscosity, good dynamic performance, contribution to improving the energy density of the sodium ion battery, higher capacity retention rate under the high-rate charge and discharge working condition, longer cycle life and better performance.
The synthesis process of NaFSI generally requires three steps: (1) preparation of dichlor sulfimide; (2) Preparing difluoro sulfimide through fluorination reaction of dichloro sulfimide; (3) The neutralization reaction of the difluoro sulfimide and the alkali metal salt is carried out to prepare NaFSI, wherein the neutralization salification reaction in the third step is taken as a key step of the synthesis of the product, the influence on the product index of the NaFSI is large, and how to optimize the salification reaction and make the subsequent product purification is a key factor for improving the product quality.
The current mainstream technology adopts a preparation technology similar to LiFSI, neutralization reaction is carried out by using difluoro sulfimide and alkali metal salt in an organic solvent in a heterogeneous form of a solid-liquid mixture, the reaction time is long, the reaction heat is difficult to take, the reaction temperature is not well controlled, and unreacted alkali metal salt is difficult to separate and can enter into a product to influence the quality of the product.
Disclosure of Invention
In order to solve the problems in the background technology of the invention, the invention provides a high-efficiency, low-energy consumption and high-purity sodium bis-fluorosulfonyl imide preparation device and method, wherein the method selects screened alcohol organic solvent to dissolve alkali metal salt and then react with bis-fluorosulfonyl imide in homogeneous phase, the reaction time is greatly shortened from conventional 25-30h to 6-8h; after homogeneous phase reaction is changed, the heat transfer coefficient of the system is greatly improved, and the reaction temperature is easy to control; the solvent is removed by a film evaporator with higher evaporation efficiency, so that the concentration time is greatly shortened and the energy consumption is reduced compared with that of a kettle type concentrator. And the subsequent vacuum desolventizing and dewatering, pulping and washing, filtering and drying to obtain high-quality NaFSI product with NaFSI purity up to 99.9% and yield over 90%.
The scheme is as follows:
the preparation method of the sodium bis (fluorosulfonyl) imide comprises the following steps:
s10: adding a certain amount of alcohol organic solvent into a NaFSI synthesis kettle, and then adding alkali metal salt into the NaFSI synthesis kettle through an alkali metal salt feeding bin;
s20: starting a chilled water control system of a jacket of the NaFSI synthesis kettle, controlling the temperature in the NaFSI synthesis kettle to be-10-5 ℃, dropwise adding the difluoro sulfonimide into the NaFSI synthesis kettle, controlling the pressure in the NaFSI synthesis kettle to be 3-10Kpa in the reaction process, and reacting for 6-8h to obtain a feed liquid after neutralization salification reaction of the difluoro sulfonimide sodium;
s30: pumping the reacted feed liquid in the NaFSI synthesis kettle into a thin film evaporator by a material transfer pump, controlling the temperature of the thin film evaporator to be 30 ℃, controlling the pressure to be-0.99 Mpa (G), removing the solvent and the water in the feed liquid to obtain concentrated slurry, and enabling the removed solvent to enter a solvent recovery tank for recovery and reuse through a solvent condenser;
s40: placing the concentrated slurry at the bottom of the thin film evaporator into a three-in-one dryer, starting a vacuum unit to control the internal pressure of the three-in-one dryer to be-0.99-0.9 Mpa (G), introducing hot water into a jacket of the three-in-one dryer to control the internal temperature of the three-in-one dryer to be 20-50 ℃, and further concentrating the slurry;
s50: after the concentration is finished, chloralkane is added into a three-in-one dryer to separate out NaFSI crystals, and the metal ion impurities and excessive difluoro sulfonamide are washed clean through pulping and washing of the crystals;
s60: starting a vacuum unit to carry out vacuum drying, controlling the drying temperature to be 20-50 ℃, controlling the drying pressure to be-0.99-0.9 Mpa (G), and drying for 2-6h to obtain a qualified NaFSI product.
Preferably, in S10, the amount of the alcohol organic solvent added in the nafpi synthesis kettle is 2-5 times that of the difluoro sulfonamide.
Preferably, in S10, the alcohol-based organic solvent is methanol or ethanol.
Preferably, in S10, the alkali metal salt is sodium hydroxide or sodium bicarbonate.
Preferably, in S20, the bisfluorosulfonyl imide is added dropwise to the NaFSI synthesis tank via a metering pump.
Preferably, in S20, the amount of the bis-fluorosulfonamide added is 4.5 to 6 times that of the alkali metal.
Preferably, in S50, the chlorinated alkane is added in an amount of 1-3 times that of NaFSI.
The preparation device of the sodium bis (fluorosulfonyl) imide is suitable for the preparation method of the sodium bis (fluorosulfonyl) imide, and comprises an alkali metal salt feeding bin for storing alkali metal salt, and further comprises:
the NaFSI synthesis kettle is communicated with one end of the alkali metal salt feeding bin for feeding;
the input end of the material transferring pump is communicated with the discharge end of the NaFSI synthesis kettle;
the top feed inlet of the thin film evaporator is communicated with the output end of the material transferring pump;
the three-in-one dryer is communicated with the discharge end of the thin film evaporator, and the bottom of the three-in-one dryer is communicated with a pneumatic conveying packaging system;
a solvent condenser in communication with a slurry outlet in the thin film evaporator;
the solvent recovery tank is communicated with the discharge end of the solvent condenser;
the vacuum unit is respectively communicated with the film evaporator and the three-in-one dryer, a pipeline for communicating the vacuum unit with the film evaporator and a pipeline for communicating the vacuum unit with the three-in-one dryer are respectively provided with a switch valve for realizing switching of vacuumizing, and the switch valve is used for controlling the pressure inside the film evaporator and the three-in-one dryer;
the film evaporator and the three-in-one dryer are connected with a vacuum unit after passing through a solvent condenser.
The beneficial effects of the invention are as follows:
1. according to the device and the method for preparing the sodium bis (fluorosulfonyl) imide, the purity of the sodium bis (fluorosulfonyl) imide prepared by the method can reach more than 99.9%, and the yield can reach more than 90%.
2. The neutralization reaction is carried out in a homogeneous system by selecting a specific alcohol organic solvent, so that the reaction time is greatly shortened.
3. The heat transfer coefficient of the reaction system is improved, the reaction temperature is easier to control, and the energy consumption is greatly reduced.
4. The reaction is carried out in a homogeneous system, so that the product is not easy to coat other solid impurities, and the purity is greatly improved.
And 5, the traditional kettle type concentrator is abandoned by NaFSI solvent concentration, the solvent and the water are removed by adopting a film evaporator with higher efficiency, the concentration time is greatly shortened, and the energy consumption is reduced.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic view of a production apparatus in the present invention;
in the figure: 1. alkali metal salt feeding bin; 2. a NaFSI synthesis kettle; 3. a transfer pump; 4. a thin film evaporator 5, a three-in-one dryer; 6. A solvent condenser; 7. a solvent recovery tank; 8. and (5) a vacuum unit.
Detailed Description
The invention is further described in connection with the following detailed description in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Embodiment one:
as shown in fig. 1, the device for preparing the bischlorosulfimide provided by the invention comprises an alkali metal salt feeding bin 1 for storing alkali metal salt, and further comprises:
the NaFSI synthesis kettle 2 is communicated with one feeding end of the alkali metal salt feeding bin 1;
the input end of the material transferring pump 3 is communicated with the discharge end of the NaFSI synthesis kettle 2;
the top feed inlet of the thin film evaporator 4 is communicated with the output end of the material transferring pump 3;
the three-in-one dryer 5 is communicated with the discharge end of the thin film evaporator 4, and the bottom of the three-in-one dryer 5 is communicated with a pneumatic conveying packaging system;
a solvent condenser 6 in communication with the slurry outlet in the thin film evaporator 4;
a solvent recovery tank 7 communicated with the discharge end of the solvent condenser 6;
the vacuum unit 8 is respectively communicated with the film evaporator 4 and the three-in-one dryer 5, a pipeline for communicating the vacuum unit 8 with the film evaporator 4 and a pipeline for communicating the vacuum unit 8 with the three-in-one dryer 5 are respectively provided with a switch valve to realize switching of vacuumizing, and the switch valve is used for controlling the pressure inside the film evaporator 4 and the three-in-one dryer 5;
the film evaporator 4 and the three-in-one dryer 5 are connected with a vacuum unit 8 after passing through a solvent condenser 6.
The preparation method of the invention comprises the following steps:
s10: neutralization and salification reaction of sodium bis (fluorosulfonyl) imide: 1000Kg of ethanol is added into a NaFSI synthesis kettle, and then 100Kg of sodium hydroxide is added into the NaFSI synthesis kettle through an alkali metal salt feeding bin;
s20: starting a chilled water control system of a jacket of the NaFSI synthesis kettle, controlling the temperature in the NaFSI synthesis kettle to be-10 ℃, dropwise adding 500kg of difluoro sulfimide into the NaFSI synthesis kettle through a metering pump, controlling the pressure in the NaFSI synthesis kettle to be 3Kpa in the reaction process, and reacting for 6 hours;
s30: concentration of sodium bis-fluorosulfonyl imide: pumping the reacted feed liquid in the NaFSI synthesis kettle into a thin film evaporator by a material transfer pump, controlling the temperature of the thin film evaporator to be 30 ℃, controlling the pressure to be-0.99 Mpa (G), removing the solvent and the water in the feed liquid to obtain concentrated slurry, and enabling the removed solvent to enter a solvent recovery tank for recovery and reuse through a solvent condenser;
s40: refining and purifying sodium dichlorosulfimide: placing the concentrated slurry at the bottom of the thin film evaporator into a three-in-one dryer, starting a vacuum unit to control the internal pressure of the three-in-one dryer to be-0.99 (G), and introducing hot water into a jacket of the three-in-one dryer to control the internal temperature of the three-in-one dryer to be 20 ℃, so as to further concentrate the slurry;
s50: after the concentration is finished, adding 500kg of dichloromethane into a three-in-one dryer to separate out NaFSI crystals, and washing the crystals to clean metal ion impurities and excessive difluoro sulfonamide through pulping and washing;
s60: starting a vacuum unit to carry out vacuum drying, controlling the drying temperature to be 20 ℃, controlling the drying pressure to be-0.99 (G), and drying for 2 hours to obtain a qualified NaFSI product, wherein the purity of the NaFSI product is 99.92 percent measured by a gas chromatograph.
Embodiment two:
s10: neutralization and salification reaction of sodium bis (fluorosulfonyl) imide: 1500Kg of methanol is added into a NaFSI synthesis kettle, and then 150Kg of sodium hydroxide is added into the NaFSI synthesis kettle through an alkali metal salt feeding bin;
s20: starting a chilled water control system of a jacket of the NaFSI synthesis kettle, controlling the temperature in the NaFSI synthesis kettle to be 0 ℃, dropwise adding 800kg of difluoro sulfimide into the NaFSI synthesis kettle through a metering pump, controlling the pressure in the NaFSI synthesis kettle to be 6Kpa in the reaction process, and reacting for 7 hours;
s30: concentration of sodium bis-fluorosulfonyl imide: pumping the reacted feed liquid in the NaFSI synthesis kettle into a thin film evaporator by a material transfer pump, controlling the temperature of the thin film evaporator to 35 ℃ and the pressure to-0.95 Mpa (G), removing the solvent and the water in the feed liquid to obtain concentrated slurry, and allowing the removed solvent to enter a solvent recovery tank for recovery and reuse by a solvent condenser;
s40: refining and purifying sodium dichlorosulfimide: placing the concentrated slurry at the bottom of the thin film evaporator into a three-in-one dryer, starting a vacuum unit to control the internal pressure of the three-in-one dryer to be-0.95 (G), and introducing hot water into a jacket of the three-in-one dryer to control the internal temperature of the three-in-one dryer to be 30 ℃, so as to further concentrate the slurry;
s50: after the concentration is finished, adding 800kg of dichloroethane into a three-in-one dryer to separate out NaFSI crystals, and washing the crystals to clean metal ion impurities and excessive difluoro sulfonamide through pulping and washing;
s60: starting a vacuum unit to carry out vacuum drying, controlling the drying temperature to be 30 ℃, controlling the drying pressure to be-0.95 (G), and drying for 3 hours to obtain a qualified NaFSI product, wherein the purity of the NaFSI product is 99.95 percent measured by a gas chromatograph.
Embodiment III:
s10: neutralization and salification reaction of sodium bis (fluorosulfonyl) imide: 2000Kg of methanol is added into a NaFSI synthesis kettle, and then 200Kg of sodium bicarbonate is added into the NaFSI synthesis kettle through an alkali metal salt feeding bin;
s20: starting a chilled water control system of a jacket of the NaFSI synthesis kettle, controlling the temperature in the NaFSI synthesis kettle to be-5 ℃, dropwise adding 1000kg of difluoro sulfimide into the NaFSI synthesis kettle through a metering pump, controlling the pressure in the NaFSI synthesis kettle to be 10Kpa in the reaction process, and reacting for 8 hours;
s30: concentration of sodium bis-fluorosulfonyl imide: pumping the reacted feed liquid in the NaFSI synthesis kettle into a thin film evaporator by a material transfer pump, controlling the temperature of the thin film evaporator to 35 ℃ and the pressure to-0.9 Mpa (G), removing the solvent and the water in the feed liquid to obtain concentrated slurry, and allowing the removed solvent to enter a solvent recovery tank for recovery and reuse by a solvent condenser;
s40: refining and purifying sodium dichlorosulfimide: placing the concentrated slurry at the bottom of the thin film evaporator into a three-in-one dryer, starting a vacuum unit to control the internal pressure of the three-in-one dryer to be-0.9 (G), and introducing hot water into a jacket of the three-in-one dryer to control the internal temperature of the three-in-one dryer to be 35 ℃, so as to further concentrate the slurry;
s50: after the concentration is finished, 1000kg of dichloroethane is added into a three-in-one dryer to separate out NaFSI crystals, and the crystals are washed by pulping and washing to clean metal ion impurities and excessive difluoro sulfonamide;
s60: and starting a vacuum unit to perform vacuum drying, controlling the drying temperature to be 35 ℃, controlling the drying pressure to be-0.9 (G), and drying for 4 hours to obtain a qualified NaFSI product, wherein the purity of the NaFSI product is 99.91 percent measured by a gas chromatograph.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. A preparation method of sodium bis (fluorosulfonyl) imide is characterized in that: the method comprises the following steps:
s10: adding a certain amount of alcohol organic solvent into a NaFSI synthesis kettle, and then adding alkali metal salt into the NaFSI synthesis kettle through an alkali metal salt feeding bin;
s20: starting a chilled water control system of a jacket of the NaFSI synthesis kettle, controlling the temperature in the NaFSI synthesis kettle to be-10-5 ℃, dropwise adding the difluoro sulfonimide into the NaFSI synthesis kettle, controlling the pressure in the NaFSI synthesis kettle to be 3-10KPa in the reaction process, and reacting for 6-8h to obtain a feed liquid after neutralization salification reaction of the difluoro sulfonimide sodium;
s30: pumping the reacted feed liquid in the NaFSI synthesis kettle into a thin film evaporator through a material transfer pump, controlling the temperature of the thin film evaporator to be 30 ℃, controlling the pressure to be-0.99 MPa gauge pressure, removing the solvent and the water in the feed liquid to obtain concentrated slurry, and enabling the removed solvent to enter a solvent recovery tank through a solvent condenser for recovery and reuse;
s40: placing the concentrated slurry at the bottom of the thin film evaporator into a three-in-one dryer, starting a vacuum unit to control the internal pressure of the three-in-one dryer to be-0.99-0.9 MPa gauge pressure, introducing hot water into a jacket of the three-in-one dryer to control the internal temperature of the three-in-one dryer to be 20-50 ℃, and further concentrating the slurry;
s50: after the concentration is finished, chloralkane is added into a three-in-one dryer to separate out NaFSI crystals, and the metal ion impurities and excessive difluoro sulfonamide are washed clean through pulping and washing of the crystals;
s60: starting a vacuum unit to carry out vacuum drying, controlling the drying temperature to be 20-50 ℃, controlling the drying pressure to be-0.99-0.9 MPa gauge pressure, and drying for 2-6 hours to obtain a qualified NaFSI product;
in S10, the addition amount of the alcohol organic solvent in the NaFSI synthesis kettle is 2-5 times of that of the difluoro sulfonamide;
in S10, the alcohol-based organic solvent is methanol or ethanol;
in S10, the alkali metal salt is sodium hydroxide or sodium bicarbonate;
in S20, dropwise adding the difluoro sulfimide into a NaFSI synthesis kettle through a metering pump;
in S20, the addition amount of the difluoro sulfonamide is 4.5-6 times of that of alkali metal;
in S50, the chloroalkane is added in an amount of 1 to 3 times that of NaFSI.
2. A device for preparing sodium bis (fluorosulfonyl) imide, which is suitable for the preparation method of sodium bis (fluorosulfonyl) imide in claim 1, and is characterized in that: including the alkali metal salt dosing bin for storing alkali metal salt, still include:
the NaFSI synthesis kettle is communicated with one end of the alkali metal salt feeding bin for feeding;
the input end of the material transferring pump is communicated with the discharge end of the NaFSI synthesis kettle;
the top feed inlet of the thin film evaporator is communicated with the output end of the material transferring pump;
the three-in-one dryer is communicated with the discharge end of the thin film evaporator, and the bottom of the three-in-one dryer is communicated with a pneumatic conveying packaging system;
a solvent condenser in communication with a slurry outlet in the thin film evaporator;
the solvent recovery tank is communicated with the discharge end of the solvent condenser;
the vacuum unit is respectively communicated with the film evaporator and the three-in-one dryer, a pipeline for communicating the vacuum unit with the film evaporator and a pipeline for communicating the vacuum unit with the three-in-one dryer are respectively provided with a switch valve for realizing switching of vacuumizing, and the switch valve is used for controlling the pressure inside the film evaporator and the three-in-one dryer;
the film evaporator and the three-in-one dryer are connected with a vacuum unit after passing through a solvent condenser.
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| WO2015143866A1 (en) * | 2014-03-24 | 2015-10-01 | 深圳新宙邦科技股份有限公司 | Preparation method for bis-fluorosulfonyl imide and alkali metal salts thereof |
| EP3825278A1 (en) * | 2019-11-20 | 2021-05-26 | Shanghai Rolechem Co., Ltd. | Method for preparing high-purity bisfluorosulfonylimide salt |
| CN114572945A (en) * | 2022-04-18 | 2022-06-03 | 湖北万润新能源科技股份有限公司 | Preparation method and application of sodium bis (fluorosulfonyl) imide |
| CN114873571A (en) * | 2022-06-28 | 2022-08-09 | 河南省氟基新材料科技有限公司 | Preparation method of bis (fluorosulfonyl) imide salt |
| KR20220135283A (en) * | 2021-03-29 | 2022-10-07 | 주식회사 천보 | Method for manufacturing sodium bis(fluorosulfonyl)imide |
| CN115818592A (en) * | 2022-10-12 | 2023-03-21 | 多氟多新材料股份有限公司 | Preparation method of sodium bis (fluorosulfonyl) imide |
| CN116354319A (en) * | 2023-03-02 | 2023-06-30 | 多氟多新材料股份有限公司 | Preparation method of difluoro sulfonyl imide salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015143866A1 (en) * | 2014-03-24 | 2015-10-01 | 深圳新宙邦科技股份有限公司 | Preparation method for bis-fluorosulfonyl imide and alkali metal salts thereof |
| EP3825278A1 (en) * | 2019-11-20 | 2021-05-26 | Shanghai Rolechem Co., Ltd. | Method for preparing high-purity bisfluorosulfonylimide salt |
| KR20220135283A (en) * | 2021-03-29 | 2022-10-07 | 주식회사 천보 | Method for manufacturing sodium bis(fluorosulfonyl)imide |
| CN114572945A (en) * | 2022-04-18 | 2022-06-03 | 湖北万润新能源科技股份有限公司 | Preparation method and application of sodium bis (fluorosulfonyl) imide |
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