CN115520875B - Continuous production process of lithium tetrafluoroborate - Google Patents
Continuous production process of lithium tetrafluoroborate Download PDFInfo
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- CN115520875B CN115520875B CN202211293502.9A CN202211293502A CN115520875B CN 115520875 B CN115520875 B CN 115520875B CN 202211293502 A CN202211293502 A CN 202211293502A CN 115520875 B CN115520875 B CN 115520875B
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- lithium tetrafluoroborate
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- -1 lithium tetrafluoroborate Chemical compound 0.000 title claims abstract description 32
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000010924 continuous production Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims abstract description 6
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 30
- 238000003786 synthesis reaction Methods 0.000 claims description 26
- 229910003002 lithium salt Inorganic materials 0.000 claims description 18
- 159000000002 lithium salts Chemical class 0.000 claims description 18
- 239000012074 organic phase Substances 0.000 claims description 18
- 229910015900 BF3 Inorganic materials 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 12
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011268 mixed slurry Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 3
- 239000002000 Electrolyte additive Substances 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 4
- 229910013075 LiBF Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
- C01B35/066—Alkali metal tetrafluoborates
-
- 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
Abstract
The invention provides a continuous production process of lithium tetrafluoroborate, and relates to the field of electrolyte additive production. The continuous production process of lithium tetrafluoroborate comprises a configuration working section, a continuous reaction working section, a filtering and concentrating working section and a drying working section of reaction raw materials. The continuous production process of lithium tetrafluoroborate has the effect of continuous reaction, can greatly improve the productivity of a device, changes the traditional kettle type reactor into a tower type reactor, changes the form of air blowing feeding into the form of liquid phase spraying into gas phase in the production process, improves the contact area of gas and liquid, thereby improving the conversion rate and the yield of raw materials, has large heat exchange area of the tower type reactor, reduces the temperature of a self-circulation pipeline through an external heat exchanger, further improves the heat exchange effect of the reaction device, improves the reaction efficiency, has high purity of the prepared product, does not need purification, uses a thin film evaporator to replace the traditional concentration crystallization, and has simple process route.
Description
Technical Field
The invention relates to the technical field of electrolyte additive production, in particular to a continuous production process of lithium tetrafluoroborate.
Background
In the background of the strong development of global new energy automobiles in main countries such as China, europe, japanese and Korean, the global power lithium battery market has a trend of keeping the output to be increased at a high speed in recent years. In the next few years, with implementation of double integration system of new energy automobile in China and acceleration of electric automobile in European Union and UK, the trend of high growth of power lithium battery is kept under the drive of new energy automobile terminal, and lithium tetrafluoroborate (LiBF) is used as lithium battery additive 4 ) The demand in the future is also increasing.
Lithium tetrafluoroborate (LiBF) 4 ) The appearance is white powder, the melting point is 293-300 ℃, the decomposition temperature is 390 ℃, and the powder has better chemical stability and thermal stability and is mainly used as LiBF 6 The base electrolyte system additive is used for improving the cycle life, widening the working temperature range of the battery and improving the high-low temperature discharge performance of the battery.
The presently disclosed preparation method of lithium tetrafluoroborate has low yield and purity, is kettle type batch reaction, and has low productivity.
The current methods for producing lithium tetrafluoroborate mainly comprise a lithium salt method, a solid phase reaction method, an aqueous solution method and the like. The existing lithium salt method device has low production efficiency and low conversion rate of raw materials; the solid phase reaction method has high reaction conditions, high energy consumption, lower purity of products and complicated process flow caused by subsequent purification; the aqueous solution method can lead to the combination of the product and water, on the one hand, the difficulty in drying and dewatering the product, and on the other hand, the hydrolysis of the product can lead to the reduction of the yield and the product quality, and the reduction of the cycle performance of the battery in the use process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a continuous production process of lithium tetrafluoroborate, solves the prior technical problems, can realize continuous synthesis reaction, saves cost, and improves the yield and the purity of products.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a continuous production process of lithium tetrafluoroborate, comprising the following steps:
s1, preparation working section of reaction raw materials
Adding an organic solvent into a premixing tank, then adding lithium salt, and starting stirring and uniformly mixing to obtain mixed slurry;
s2, continuous reaction section
Mixing slurry and boron trifluoride gas in a premixing tank are added into a synthesis reaction tower simultaneously and continuously in proportion, wherein the boron trifluoride gas enters from the tower top in two ways, one way is continuously added from the tower top, the pressure in the reaction tower is kept stable through a regulating valve, the second way is added from the middle part of the tower, the reaction is thoroughly carried out, the organic slurry is continuously added from the tower top, the reaction temperature is controlled to be 10-70 ℃, and the reaction pressure is controlled to be 1-200kpa;
s3, filtering
Completely reacting solid lithium salt to generate lithium tetrafluoroborate in the process that the organic phase falls from the top of the tower, collecting at the bottom of the tower, removing insoluble substances from the organic phase after the reaction, and concentrating and crystallizing in a concentrating section;
s4, concentration working section
Transferring the organic phase after the reaction to a thin film evaporator for concentration, condensing the gasified organic solvent for repeated use, and discharging the solid of the evaporator to obtain a lithium tetrafluoroborate wet product;
s5, drying section
And transferring the wet product into a dryer for drying, wherein the drying temperature is 50-150 ℃, the pressure is-0.08 to-0.1 MPa, and the lithium tetrafluoroborate product is obtained after the drying is completed.
Preferably, in the step S1, the molar ratio of the lithium salt to the organic solvent is 1:1-4.5.
Preferably, in the step S2, the molar ratio of the lithium salt to the boron trifluoride is 1-2:1.
Preferably, in the step S1, the organic solvent is one or two of dimethyl carbonate, diethyl carbonate and ethylmethyl carbonate.
Preferably, in the step S1, the lithium salt is one or two of lithium fluoride, lithium carbonate and lithium hydroxide.
Preferably, in the step S2, the height of the synthesis reaction tower is 10-40m, and the diameter of the synthesis reaction tower is 0.5-2.5m, and in the step S2, the synthesis reaction tower is distributed with one organic phase feed inlet and two gas phase feed inlets.
Preferably, in the step S2, the mass ratio of the mixed slurry to the boron trifluoride gas feed is 1-9:1, the synthesis reaction time of the synthesis reaction tower is controlled to be 60-300s, and the shell side medium of the synthesis reaction tower is low-temperature water with the temperature of 5-20 ℃.
Preferably, in the step S4, the temperature of the thin film evaporator is controlled to be 10-70 ℃ and the pressure is controlled to be-0.08 to-0.1 MPa.
The invention provides a continuous production process of lithium tetrafluoroborate. The beneficial effects are as follows:
1. the continuous production process of lithium tetrafluoroborate provided by the invention has the effect of continuous reaction, can greatly improve the productivity of a device, changes a traditional kettle type reactor into a tower type reactor in the production process, changes the form of air blowing feeding into the form of liquid phase spraying into gas phase, and improves the contact area of gas and liquid, thereby improving the conversion rate and the yield of raw materials.
2. In the continuous production process of lithium tetrafluoroborate, the heat exchange area of the tower reactor is large, the self-circulation pipeline is cooled through the external heat exchanger, the heat exchange effect of the reaction device is further improved, the reaction efficiency is improved, meanwhile, the prepared product is high in purity, purification is not needed, a thin film evaporator is used for replacing the traditional concentration crystallization, and the process route is simple.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
as shown in fig. 1, the embodiment of the invention provides a continuous production process of lithium tetrafluoroborate, comprising the following steps:
s1, preparation working section of reaction raw materials
Adding an organic solvent into a premixing tank, then adding lithium salt, and starting stirring and uniformly mixing to obtain mixed slurry;
s2, continuous reaction section
Mixing slurry and boron trifluoride gas in a premixing tank are added into a synthesis reaction tower simultaneously and continuously in proportion, wherein the boron trifluoride gas enters from the tower top in two ways, one way is continuously added from the tower top, the pressure in the reaction tower is kept stable through a regulating valve, the second way is added from the middle part of the tower, the reaction is thoroughly carried out, the organic slurry is continuously added from the tower top, the reaction temperature is controlled to be 10-70 ℃, and the reaction pressure is controlled to be 1-200kpa;
s3, filtering
Completely reacting solid lithium salt to generate lithium tetrafluoroborate in the process that the organic phase falls from the top of the tower, collecting at the bottom of the tower, removing insoluble substances from the organic phase after the reaction, and concentrating and crystallizing in a concentrating section;
s4, concentration working section
Transferring the organic phase after the reaction to a thin film evaporator for concentration, condensing the gasified organic solvent for repeated use, and discharging the solid of the evaporator to obtain a lithium tetrafluoroborate wet product;
s5, drying section
And transferring the wet product into a dryer for drying, wherein the drying temperature is 50-150 ℃, the pressure is-0.08 to-0.1 MPa, and the lithium tetrafluoroborate product is obtained after the drying is completed.
In the step S1, the molar ratio of the lithium salt to the organic solvent is 1:1-4.5.
In the step S2, the molar ratio of the lithium salt to the boron trifluoride is 1-2:1.
In the step S1, the organic solvent is one or two of dimethyl carbonate, diethyl carbonate and ethylmethyl carbonate.
In the step S1, the lithium salt is one or two of lithium fluoride, lithium carbonate and lithium hydroxide.
In the step S2, the height of the synthesis reaction tower is 10-40m, the diameter is 0.5-2.5m, in the step S2, an organic phase feed inlet and two gas phase feed inlets are distributed in the synthesis reaction tower, wherein the gas phase boron trifluoride is provided with the two feed inlets, the lateral direction of the tower top is the main feed inlet, and the pressure in the tower is controlled through a regulating valve; the middle part of the tower is provided with an auxiliary feed inlet, so that lithium salt in the organic slurry is completely converted into lithium tetrafluoroborate. The organic slurry feeding port is arranged at the top of the tower, and the discharge port in the organic slurry tower is of a rotary spray header structure, so that the slurry can be uniformly distributed in the tower.
In the step S2, the mass ratio of the mixed slurry to the boron trifluoride gas feed is 1-9:1, the synthesis reaction time of the synthesis reaction tower is controlled to be 60-300s, a jacket is arranged outside the synthesis reaction tower, a circulating pump is arranged at the bottom of the reaction tower, and a heat exchanger is externally connected, so that heat released by the reaction can be timely transferred, and the shell side medium of the synthesis reaction tower is low-temperature water with the temperature of 5-20 ℃.
In the S4 step, the temperature of the film evaporator is controlled at 10-70 ℃, the pressure is-0.08 to-0.1 MPa, the dryer has a jacket temperature control function, and the dryer is connected with a vacuum system, and the drying temperature is controlled at 50-150 ℃ and the drying pressure is-0.1 MPa.
Embodiment two:
adding 100kg of lithium fluoride and 1500kg of dimethyl carbonate into a premixing tank, starting stirring and mixing uniformly to prepare organic slurry, adding the organic slurry into a synthesis reaction tower at a speed of 660kg/h, starting a jacket and an external heat exchanger, then introducing boron trifluoride gas into the synthesis reaction tower at a speed of 110kg/h, controlling the reaction temperature to 30 ℃ by adjusting the flow of cooling water, filtering an organic phase of a tower kettle through a precise filter after the reaction is finished, pumping the organic phase into a buffer tank, and pumping the organic phase from the buffer tank into a thin film evaporator; and (3) heating the film evaporator to 50 ℃ by hot water, then starting a vacuum pumping system to carry out negative pressure operation, repeatedly applying dimethyl carbonate after gasification and condensation, discharging a solid lithium tetrafluoroborate wet product from the bottom, transferring the wet product into a dryer to carry out vacuum drying, controlling the drying temperature to 125 ℃, sampling and detecting at intervals of 3 hours, and discharging after the wet product is qualified. Through testing, the purity of the product reaches 99.99 percent, and the yield is 93 percent.
Embodiment III:
150kg of lithium fluoride and 2500kg of diethyl carbonate are added into a premixing tank, and stirring and mixing are started to prepare organic slurry; adding organic slurry into a synthesis reaction tower at the speed of 600kg/h, simultaneously opening a jacket and an external heat exchanger, then introducing boron trifluoride gas into the synthesis reaction tower at the speed of 100kg/h, controlling the reaction temperature to 45 ℃ by adjusting the flow of cooling water, filtering an organic phase of a tower kettle after the reaction is finished, pumping the organic phase into a buffer tank through a precise filter, and pumping the organic phase into a thin film evaporator from the buffer tank; and (3) heating the film evaporator to 65 ℃ by hot water, then starting a vacuum pumping system to perform negative pressure operation, repeatedly applying dimethyl carbonate after gasification and condensation, discharging a solid lithium tetrafluoroborate wet product from the bottom, transferring the wet product into a dryer to perform vacuum drying, controlling the drying temperature to 130 ℃, sampling and detecting at intervals of 3 hours, and discharging after the wet product is qualified. Through testing, the purity of the product reaches 99.98 percent, and the yield is 91 percent.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A continuous production process of lithium tetrafluoroborate is characterized in that: the method comprises the following steps:
s1, preparation working section of reaction raw materials
Adding an organic solvent into a premixing tank, then adding lithium salt, and starting stirring and uniformly mixing to obtain mixed slurry;
s2, continuous reaction section
Mixing slurry and boron trifluoride gas in a premixing tank are added into a synthesis reaction tower simultaneously and continuously in proportion, wherein the boron trifluoride gas enters from the tower top in two ways, one way is continuously added from the tower top, the pressure in the reaction tower is kept stable through a regulating valve, the second way is added from the middle part of the tower, the reaction is thoroughly carried out, the organic slurry is continuously added from the tower top, the reaction temperature is controlled to be 10-70 ℃, and the reaction pressure is controlled to be 1-200kpa;
s3, filtering
Completely reacting solid lithium salt to generate lithium tetrafluoroborate in the process that the organic phase falls from the top of the tower, collecting at the bottom of the tower, removing insoluble substances from the organic phase after the reaction, and concentrating and crystallizing in a concentrating section;
s4, concentration working section
Transferring the organic phase after the reaction to a thin film evaporator for concentration, condensing the gasified organic solvent for repeated use, and discharging the solid of the evaporator to obtain a lithium tetrafluoroborate wet product;
s5, drying section
Transferring the wet product into a dryer for drying at the temperature of 50-150 ℃ and the pressure of-0.08 to-0.1 MPa, and obtaining a lithium tetrafluoroborate product after the drying is completed;
in the step S1, the molar ratio of the lithium salt to the organic solvent is 1:1-4.5;
in the step S2, the molar ratio of the lithium salt to the boron trifluoride is 1-2:1;
in the step S1, the organic solvent is one or two of dimethyl carbonate, diethyl carbonate and ethylmethyl carbonate;
in the step S1, the lithium salt is one or two of lithium fluoride, lithium carbonate and lithium hydroxide.
2. The continuous production process of lithium tetrafluoroborate according to claim 1, wherein: in the step S2, the height of the synthesis reaction tower is 10-40m, the diameter of the synthesis reaction tower is 0.5-2.5m, and in the step S2, an organic phase feed inlet and two gas phase feed inlets are distributed in the synthesis reaction tower.
3. The continuous production process of lithium tetrafluoroborate according to claim 1, wherein: in the step S2, the mass ratio of the mixed slurry to the boron trifluoride gas feed is 1-9:1, the synthesis reaction time of the synthesis reaction tower is controlled to be 60-300s, and the shell side medium of the synthesis reaction tower is low-temperature water with the temperature of 5-20 ℃.
4. The continuous production process of lithium tetrafluoroborate according to claim 1, wherein: in the step S4, the temperature of the thin film evaporator is controlled at 10-70 ℃ and the pressure is-0.08 to-0.1 MPa.
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Citations (1)
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| CN102803142A (en) * | 2009-06-19 | 2012-11-28 | 斯泰拉化工公司 | Method for producing tetrafluoroborate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102803142A (en) * | 2009-06-19 | 2012-11-28 | 斯泰拉化工公司 | Method for producing tetrafluoroborate |
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