CN112397781B - Preparation method of vinylene carbonate additive for lithium battery car electrolyte - Google Patents
Preparation method of vinylene carbonate additive for lithium battery car electrolyte Download PDFInfo
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- CN112397781B CN112397781B CN202011287859.7A CN202011287859A CN112397781B CN 112397781 B CN112397781 B CN 112397781B CN 202011287859 A CN202011287859 A CN 202011287859A CN 112397781 B CN112397781 B CN 112397781B
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- triethylamine
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- carbonate
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- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 title claims abstract description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000654 additive Substances 0.000 title claims description 7
- 230000000996 additive effect Effects 0.000 title claims description 7
- 239000003792 electrolyte Substances 0.000 title claims description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 156
- 239000007788 liquid Substances 0.000 claims abstract description 120
- 238000000926 separation method Methods 0.000 claims abstract description 30
- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 8
- 239000012265 solid product Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims description 45
- 238000004140 cleaning Methods 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 15
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical class O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 239000012263 liquid product Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 210000003141 lower extremity Anatomy 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 11
- 239000002000 Electrolyte additive Substances 0.000 abstract description 7
- 238000010924 continuous production Methods 0.000 abstract description 3
- 238000006386 neutralization reaction Methods 0.000 abstract description 3
- 238000011403 purification operation Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 10
- 238000009835 boiling Methods 0.000 description 5
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 238000005194 fractionation Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/88—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices
- B01D29/94—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices for discharging the filter cake, e.g. chutes
-
- 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
- B01J19/0086—Processes carried out with a view to control or to change the pH-value; Applications of buffer salts; Neutralisation reactions
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- 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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Abstract
The invention discloses a preparation method of vinylene carbonate serving as an electrolyte additive of a lithium battery car, which comprises the steps of reacting a solid product obtained after solid-liquid separation with a sodium hydroxide solution, distilling, drying, condensing and the like the reactant to reduce triethylamine, rectifying and condensing the separated liquid to obtain chloroethylene carbonate, triethylamine and vinylene carbonate again, and continuously using the obtained triethylamine, chloroethylene carbonate and vinylene carbonate as raw materials for producing the vinylene carbonate, so that the utilization rate of the raw materials is improved, and clean production is realized; and the solid-liquid separation device is improved, so that the separated solid substances can be neutralized in the solid-liquid separation device to obtain mixed liquid containing triethylamine raw materials, the mixed liquid is discharged through a liquid discharge pipe to perform the next purification operation, the solid substances are not manually separated for neutralization, and the continuous production of the whole production line is realized.
Description
Technical Field
The invention relates to the technical field of fine chemical synthesis. More particularly, the invention relates to a preparation method of vinylene carbonate serving as an electrolyte additive of a lithium battery car.
Background
The electrolyte additive is a small amount of additive added into the electrolyte for improving the electrochemical performance of the electrolyte and improving the quality of cathode precipitates, wherein vinylene carbonate is an additive commonly added into the electrolyte of a lithium battery car.
In industry, during the production process of preparing vinylene carbonate by reacting triethylamine and chloroethylene carbonate, some byproducts are generated, so that the utilization rate of raw materials is reduced.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a preparation method of vinylene carbonate serving as an electrolyte additive of a lithium battery car, which can improve the utilization rate of raw materials.
To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a method for preparing vinylene carbonate as an additive for lithium battery vehicles, comprising: the method for preparing vinylene carbonate comprises the following steps:
s1: uniformly mixing chlorinated ethylene carbonate and ethylene carbonate to obtain a mixed solution;
s2: introducing the mixed solution and triethylamine into a tubular reactor according to a certain proportion, transferring heat through a jacket of the tubular reactor to control axial temperature distribution in the reactor, and reacting to obtain a mixture;
s3: carrying out solid-liquid separation on the mixture to obtain a solid product and a liquid product;
s4: fractionating the liquid product to obtain gaseous vinylene carbonate, gaseous triethylamine, gaseous chloroethylene carbonate and liquid vinylene carbonate;
s5: respectively condensing gaseous vinylene carbonate, gaseous triethylamine and gaseous chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: and (3) reacting the obtained solid product with a proper amount of sodium hydroxide solution to obtain a triethylamine mixed solution:
s7: distilling, drying and condensing the triethylamine mixed solution to obtain liquid triethylamine;
s8: the liquid ethylene chlorocarbonate obtained in S5 and the liquid ethylene carbonate obtained in S4 were added as reactants to the reaction in the S1 step, and the liquid triethylamine obtained in S5 and S7 were added as reactants to the reaction in the S2 step.
Preferably, the apparatus for preparing vinylene carbonate comprises: with the solid-liquid separation equipment of tubular reactor output intercommunication, with the fractionating device of the first output intercommunication of solid-liquid separation equipment, with the distillation plant of solid-liquid separation equipment second output intercommunication, with the drying device of distillation plant output intercommunication, the fractionating device with through three pipeline intercommunications between the tubular reactor, three pipelines are gaseous chlorinated ethylene carbonate pipeline, gaseous triethylamine pipeline, liquid ethylene carbonate pipeline respectively, be equipped with first condensing equipment on the gaseous chlorinated ethylene carbonate pipeline, be equipped with second condensing equipment on the gaseous triethylamine pipeline, wherein, the drying device output with second condensing equipment input intercommunication, be equipped with third condensing equipment on the pipeline of fractionating device output gaseous vinylene carbonate.
Preferably, the solid-liquid separation apparatus includes:
the device comprises a first tank body, a second tank body and a liquid inlet pipe, wherein the inner space of the first tank body is in a square shape, the upper part of one side of the first tank body is provided with the liquid inlet pipe, the middle part of the other opposite side of the first tank body is provided with the liquid outlet pipe, the lower part of the liquid outlet pipe is provided with a discharge outlet, and the discharge outlet horizontally penetrates through the side wall of the first tank body and two side walls adjacent to the side wall;
the telescopic mechanism is vertically arranged and fixedly connected with the bottom of the first tank body, the output end of the telescopic mechanism is connected with the sealing block, four sides of the sealing block are respectively abutted against the inner side wall of the first tank body, the top surface of the sealing block is inclined, and the sealing block is inclined downwards from the liquid inlet pipe to the liquid outlet pipe;
the filter screens are arranged at intervals along the liquid inlet pipe towards the liquid outlet pipe, any filter screen is vertical to the liquid inlet pipe, and two sides of each filter screen are fixedly connected with the inner side wall of the first tank body;
the cleaning box is fixedly arranged in the middle of one side of the first tank body and is communicated with the inner space of the first tank body, a first air cylinder is arranged in the cleaning box, a cleaning brush is arranged at the output end of the first air cylinder, the output end of the first air cylinder is parallel to the top surface of the sealing block, the first air cylinder is arranged in such a way that when the first air cylinder is completely contracted, the cleaning brush is positioned in the cleaning box, and when the first air cylinder is extended out, the cleaning brush can extend into the inner part of the first tank body;
the second tank body is cylindrical, the inner space of the second tank body is fixedly connected to the bottom of the first tank body, the horizontal projection of the first tank body falls into the second tank body, the side wall, positioned below the discharge port, of the second tank body extends upwards to a height higher than the discharge port, and forms a closed space with the outer side wall of the first tank body, the bottom of the closed space is provided with an inlet port in a penetrating mode, the side wall of the second tank body is provided with an alkali inlet pipe, the bottom of the second tank body is provided with a liquid discharge pipe, and a stirring device is arranged in the second tank body;
wherein, telescopic machanism sets up to, when it stretches out completely, the low side of sealed piece is located the drain pipe with between the bin outlet, the bottom of filter screen with the top surface butt of sealed piece, work as when telescopic machanism contracts completely, the low side of sealed piece with the lower limb of bin outlet flushes, the high end of sealed piece is located the below of the output of first cylinder, the cleaning brush is in stretch out under the drive of first cylinder the cleaning box with the top surface butt of sealed piece, and follow the top surface reciprocating motion of sealed piece.
Preferably, the telescopic mechanism is a cylinder.
Preferably, the stirring device comprises a stirring shaft arranged in the second tank body, a plurality of stirring paddles arranged on the stirring shaft at intervals, and a servo motor fixedly arranged on the outer side of the bottom of the second tank body, wherein the servo motor is connected with the bottom of the second tank body through the stirring shaft.
Preferably, the mesh of the filter screen close to the side wall of the first tank body provided with the discharge opening is smaller than the mesh of the filter screen far from the side wall of the first tank body provided with the discharge opening.
The invention at least comprises the following beneficial effects:
firstly, reacting a solid product obtained after solid-liquid separation with a sodium hydroxide solution, reducing triethylamine through the steps of distilling, drying, condensing and the like on a reactant, rectifying, condensing and the like on liquid obtained after separation to obtain chloroethylene carbonate, triethylamine and ethylene carbonate again, and continuously using the obtained triethylamine, chloroethylene carbonate and ethylene carbonate as raw materials for producing vinylene carbonate, so that the utilization rate of the raw materials is improved, and clean production is realized.
Secondly, the solid-liquid separation device is improved, so that the separated solid substances can be neutralized in the solid-liquid separation device to obtain mixed liquid containing triethylamine raw materials, the mixed liquid is discharged through a liquid discharge pipe to perform the next purification operation, the solid substances are not manually separated for neutralization, and the continuous production of the whole production line is realized.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic diagram of a production device of a preparation method of vinylene carbonate as an electrolyte additive for a lithium battery car according to one embodiment of the invention;
FIG. 2 is a sectional view of a solid-liquid separation device according to one embodiment of the present invention;
FIG. 3 is a sectional view of a solid-liquid separator according to one embodiment of the present invention in use.
Reference numerals: the device comprises a tubular reactor 1, a solid-liquid separation device 2, a fractionation device 3, a distillation device 4, a drying device 5, a first condensing device 6, a gas chloroethylene carbonate conveying pipeline 7, a gas triethylamine conveying pipeline 8, a liquid chloroethylene carbonate conveying pipeline 9, a second condensing device 10, a third condensing device 11, a first tank body 12, a liquid inlet pipe 13, a liquid outlet pipe 14, a discharge outlet 15, a telescopic mechanism 16, a sealing block 17, a filter screen 18, a cleaning box 19, a first air cylinder 20, a cleaning brush 21, a second tank body 22, a closed space 23, an inlet port 24, an alkali inlet pipe 25, a liquid discharge pipe 26 and a stirring device 27.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
As shown in fig. 1 to 3, the present invention provides a method for preparing vinylene carbonate as an electrolyte additive for lithium vehicles, comprising: vinylene carbonate, and the preparation method of the vinylene carbonate comprises the following steps:
s1: mixing ethylene carbonate serving as a solvent with chloroethylene carbonate to obtain a mixed solution;
s2: introducing the mixed solution and triethylamine into a tubular reactor 1 according to a certain molar ratio, and transferring heat through a jacket of the tubular reactor 1 to control axial temperature distribution in the reactor so that the mixed solution and triethylamine fully react to obtain a mixture, wherein the mixed species comprise solid triethylamine hydrochloride, liquid vinylene carbonate, ethylene carbonate, chloroethylene carbonate and triethylamine;
s3: carrying out solid-liquid separation on the mixture to obtain a solid product and a liquid product;
s4: because the boiling points of the liquid products are different, the liquid products can be fractionated according to the respective boiling points to obtain gaseous vinylene carbonate, gaseous triethylamine, gaseous chloroethylene carbonate and liquid ethylene carbonate, wherein the boiling point of the liquid ethylene carbonate is the highest, so that the temperature can not be increased to exceed the boiling point of the liquid ethylene carbonate during fractionation, and the aim of separating the ethylene carbonate from other components is fulfilled;
s5: respectively condensing gaseous vinylene carbonate, gaseous triethylamine and gaseous chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: and (3) reacting the obtained solid product triethylamine hydrochloride with a proper amount of sodium hydroxide solution to obtain a triethylamine mixed solution:
s7: the triethylamine mixed solution contains components such as triethylamine, sodium chloride, sodium hydroxide, water and the like, and the boiling point of the triethylamine is lower than that of other components, so the triethylamine can be separated out through distillation, and the separated triethylamine contains part of water, the water is removed through drying, and then the triethylamine solution serving as a target product is obtained through condensation;
s8: the liquid chloroethylene carbonate obtained from S5 and the liquid ethylene carbonate obtained from S4 are added to the reaction in the step S1 as reactants, and the liquid triethylamine obtained from S5 and S7 are added to the reaction in the step S2 as reactants, so that the raw materials can be recycled, the utilization rate of the raw materials is improved, and the clean production is realized.
In another embodiment, the apparatus for preparing vinylene carbonate comprises: a solid-liquid separation device 2 communicated with the output end of the tubular reactor 1, a fractionating device 3 communicated with the first output end of the solid-liquid separation device 2, a distillation device 4 communicated with the second output end of the solid-liquid separation device 2, and a drying device 5 communicated with the output end of the distillation device 4, the fractionating device 3 is communicated with the tubular reactor 1 through three pipelines which are respectively a gas chloroethylene carbonate conveying pipeline 7, a gas triethylamine conveying pipeline 8 and a liquid chloroethylene carbonate conveying pipeline 9, a first condensing device 6 is arranged on the gas chloroethylene carbonate conveying pipeline 7, a second condensing device 10 is arranged on the gas triethylamine conveying pipeline 8, the output end of the drying device 5 is communicated with the input end of the second condensing device 10, and a third condensing device 11 is arranged on a pipeline for outputting gas vinylene carbonate from the fractionating device 3.
By adopting the technical scheme, the tubular reactor 1 is used for reacting raw materials, triethylamine hydrochloride is separated from other liquid substances in the solid-liquid separation device 2, the liquid substances enter the next production link, the separated triethylamine hydrochloride is reacted with a sodium hydroxide solution in the solid-liquid separation device 2 to obtain a triethylamine mixed solution, the triethylamine mixed solution is sent to the next production link for reaction, the fractionating device 3 is used for separating liquid products generated by the reaction of the production raw materials, the distilling device 4 is used for separating triethylamine gas, the separated triethylamine gas is dried by the drying device 5 and condensed by the condensing device to obtain the triethylamine solution, the triethylamine solution is sent back to the tubular reactor 1 as the raw materials for production, and after all the gases separated by fractionation are condensed by the condensing tube, the obtained target products are left, the obtained raw material product is sent back to the tubular reactor 1 for reaction.
In another embodiment, the solid-liquid separation apparatus 2 includes:
the device comprises a first tank body 12, a second tank body 12 and a liquid inlet pipe 13, wherein the inner space of the first tank body 12 is square, a liquid outlet pipe 14 is arranged in the middle of the other opposite side of the first tank body 12, a discharge port 15 is arranged below the liquid outlet pipe 14, and the discharge port 15 horizontally penetrates through the side wall of the first tank body 12 and two side walls adjacent to the side wall;
the telescopic mechanism 16 is vertically arranged and fixedly connected with the bottom of the first tank 12, the output end of the telescopic mechanism is connected with the sealing block 17, four sides of the sealing block 17 are respectively abutted against the inner side wall of the first tank 12, the top surface of the sealing block 17 is inclined, and the sealing block is inclined downwards from the liquid inlet pipe 13 to the liquid outlet pipe 14;
a plurality of filter screens 18 are arranged at intervals along the liquid inlet pipe 13 towards the liquid outlet pipe 14, any filter screen 18 is perpendicular to the liquid inlet pipe 13, and two sides of each filter screen 18 are fixedly connected with the inner side wall of the first tank body 12;
a cleaning box 19 fixedly arranged at the middle part of one side of the first tank body 12 and communicated with the inner space of the first tank body 12, wherein a first air cylinder 20 is arranged in the cleaning box 19, a cleaning brush 21 is arranged at the output end of the first air cylinder 20, the output end of the first air cylinder 20 is parallel to the top surface of the sealing block 17, the first air cylinder 20 is arranged in such a way that when the first air cylinder 20 is completely contracted, the cleaning brush 21 is positioned in the cleaning box 19, and when the first air cylinder 20 is extended out, the cleaning brush 21 can be extended into the inner part of the first tank body 12;
the inner space of the second tank body 22 is cylindrical and is fixedly connected to the bottom of the first tank body 12, the horizontal projection of the first tank body 12 falls into the second tank body 22, the side wall of the second tank body 22, which is positioned below the discharge port 15, extends upwards to a height greater than the height of the discharge port 15 and forms a closed space 23 with the outer side wall of the first tank body 12, an inlet port 24 is arranged at the bottom of the closed space 23 in a penetrating manner, an alkali inlet pipe 25 is arranged on the side wall of the second tank body 22, a liquid discharge pipe 26 is arranged at the bottom of the second tank body, and a stirring device 27 is arranged in the closed space 23;
when the telescopic mechanism 16 is completely extended, the lower end of the sealing block 17 is located between the liquid outlet pipe 14 and the material outlet 15, the bottom of the filter screen 18 is abutted to the top surface of the sealing block 17, when the telescopic mechanism 16 is completely retracted, the lower end of the sealing block 17 is flush with the lower edge of the material outlet 15, the higher end of the sealing block 17 is located below the output end of the first cylinder 20, and the cleaning brush 21 is driven by the first cylinder 20 to extend out of the cleaning box 19 to be abutted to the top surface of the sealing block 17 and reciprocate along the top surface of the sealing block 17.
In the above technical solution, the solid-liquid separation device 2 includes a first tank 12, a telescopic mechanism 16, a plurality of filter screens 18, a cleaning box 19, and a second tank 22, the internal space of the first tank 12 is cube-shaped, a liquid inlet pipe 13 is arranged above one side wall, a switch valve is arranged on the liquid inlet pipe 13, the valve is opened when liquid is required to be introduced, the valve is closed when liquid is not required to be introduced, a liquid outlet pipe 14 is arranged in the middle of the other opposite side wall, the switch valve is also arranged on the liquid outlet pipe 14, when liquid is required to flow out, the valve is opened, and in order to enable the liquid in the tank to flow out as completely as possible, a device similar to a water pump can be connected to the end of the liquid outlet pipe 14, a discharge opening 15 is arranged below the liquid outlet pipe 14, and the discharge opening 15 horizontally penetrates through the side wall of the first tank 12 and the two side walls adjacent to the side wall; the telescopic mechanism 16 is arranged in the first tank body 12, the output end of the telescopic mechanism 16 is connected with a sealing block 17, four sides of the sealing block 17 are respectively abutted against the inner side wall of the first tank body 12, the sealing block 17 can vertically slide in the first tank body 12 under the driving of the telescopic mechanism 16, the top surface of the sealing block 17 is a slope, the high end of the sealing block 17 is contacted with the side wall of the first tank body 12 provided with a liquid inlet pipe 13, the bottom end of the sealing block 17 is contacted with the side wall of the first tank body 12 provided with a liquid outlet pipe 14, wherein the type of the telescopic mechanism 16 is not limited, the telescopic mechanism 16 can be an air cylinder or a structure formed by combining a servo motor, a screw rod and the like, and the telescopic mechanism can be used as long as the sealing block 17 can be driven to vertically slide in the first tank body 12; the plurality of filter screens 18 are arranged at intervals along the direction from the liquid inlet pipe 13 to the liquid outlet pipe 14, the number of the filter screens 18 is not limited in the invention, 3 or more filter screens 18 can be provided, but when too many filter screens 18 occupy too much space of the first tank body 12, the number of the filter screens 18 is preferably 3-4, any filter screen 18 is perpendicular to the liquid inlet pipe 13, two sides of the filter screen 18 are fixedly connected with the inner side wall of the first tank body 12, when the telescopic mechanism 16 drives the sealing block 17 to move upwards until the top surface is contacted with the plurality of filter screens 18, the top surface of the sealing block 17 can be abutted against the bottom end of each filter screen 18, at the moment, the lower end of the sealing block 17 is positioned between the liquid outlet pipe 14 and the discharge port 15, and the aim is that after a solid-liquid mixture enters the first tank body 12 from the liquid inlet pipe 13, the solid can fall on the top surface of the sealing block 17, and the liquid can be discharged from the liquid outlet pipe 14 through the filter screens 18; the cleaning box 19 is fixedly arranged in the middle of one side of the first tank body 12 and is communicated with the inner space of the first tank body 12, a first air cylinder 20 and a cleaning brush 21 connected with the output end of the first air cylinder 20 are arranged in the cleaning box 19, the output end of the first air cylinder 20 is parallel to the top surface of the sealing block 17, the first air cylinder 20 is arranged in such a way that when the first air cylinder 20 is completely contracted, the cleaning brush 21 is positioned in the cleaning box 19, when the first air cylinder 20 is extended out, the cleaning brush 21 can extend into the first tank body 12, when the telescopic mechanism 16 is completely contracted, the lower end of the sealing block 17 is flush with the lower edge of the discharge port 15, the high end of the sealing block 17 is positioned below the output end of the first air cylinder 20, the cleaning brush 21 is driven by the first air cylinder 20 to extend out of the cleaning box 19 to be abutted to the top surface of the sealing block 17 and to reciprocate along the top surface of the sealing block 17, the purpose is that when the sealing block 17 with the solid substance moves downwards to the lower end of the sealing block 17 to be flush with the lower edge of the discharge port 15, the cleaning brush 21 in the cleaning box 19 pushes the solid substance under the driving of the first cylinder 20 to push the solid substance down from the top surface of the sealing block 17; the inner space of the second tank 22 is cylindrical and fixed at the bottom of the first tank 12, the horizontal projection of the first tank 12 falls into the second tank 22, the side wall of the second tank 22 below the discharge opening 15 extends upwards to a height greater than the discharge opening 15, and forms a closed space 23 with the outer side wall of the first tank 12, the bottom of the closed space 23 is provided with an inlet 24, the solid matters pushed down from the top surface of the sealing block 17 by the cleaning brush 21 enter the second tank 22 through the inlet 24, after a certain amount of solid matters in the second tank 22 are accumulated, alkali liquor is put into the alkali inlet 25, the solid matters are completely reacted under the stirring of the stirring device 27, and after the complete reaction, the mixed liquid is discharged from the discharge pipe 26 for the next operation.
In the using process, when solid-liquid separation is carried out, the telescopic mechanism 16 is completely extended out, solid matters stay on the top surface of the sealing block 17, liquid matters pass through the filter screen 18 and then are discharged from the liquid outlet pipe 14, after the liquid matters are completely discharged, the telescopic mechanism 16 is completely contracted, the first air cylinder 20 in the cleaning box 19 is started, the first air cylinder 20 drives the cleaning brush 21 to push out the solid matters on the top surface of the sealing block 17, the solid matters enter the second tank body 22 through the discharge port 15 and the inlet port 24, after the solid matters in the second tank body 22 are accumulated to a certain amount, alkali liquor is put into the alkali inlet pipe 25, the solid matters are completely reacted under the stirring of the stirring device 27, after the solid matters are completely reacted, mixed liquid is discharged from the liquid discharge pipe 26, the next operation is carried out, the solid-liquid separation device 2 is modified by adopting the technical scheme, so that the separated solid matters can be neutralized in the solid-liquid separation device 2 to obtain mixed liquid containing triethylamine raw materials, the mixed liquid is discharged through the liquid discharge pipe 26 to be used for the next purification operation instead of manually separating solid substances for neutralization, thereby realizing the continuous production of the whole production line.
In another technical scheme, the telescopic mechanism 16 is an air cylinder, and the air cylinder drives the sealing block 17 to slide in the first tank 12.
In another technical scheme, the stirring device 27 comprises a stirring shaft arranged in the second tank 22, a plurality of stirring paddles arranged on the stirring shaft at intervals, and a servo motor fixedly arranged on the outer side of the bottom of the second tank 22, wherein the servo motor and the stirring shaft penetrate through the bottom of the second tank 22 to be connected, and the stirring device 27 is used for enabling object substances to fully react.
In another technical scheme, the meshes of the filter screen 18 close to the side wall of the first tank 12 provided with the discharge opening 15 are smaller than the meshes of the filter screen 18 far away from the side wall of the first tank 12 provided with the discharge opening 15, so that the filtration is more thorough in a step-by-step filtration mode.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. The use, modifications and variations of the method of making vinylene carbonate, an additive for lithium-vehicle electrolytes, of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, described and illustrated herein, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed, and to such extent that such modifications are readily available to those skilled in the art, and it is not intended to be limited to the details shown and described herein without departing from the general concept as defined by the appended claims and their equivalents.
Claims (4)
1. The preparation method of the vinylene carbonate additive for the lithium battery car electrolyte is characterized by comprising the following steps of:
s1: uniformly mixing chlorinated ethylene carbonate and ethylene carbonate to obtain a mixed solution;
s2: introducing the mixed solution and triethylamine into a tubular reactor according to a certain proportion, transferring heat through a jacket of the tubular reactor to control axial temperature distribution in the reactor, and reacting to obtain a mixture;
s3: carrying out solid-liquid separation on the mixture to obtain a solid product and a liquid product;
s4: fractionating the liquid product to obtain gaseous vinylene carbonate, gaseous triethylamine, gaseous chloroethylene carbonate and liquid vinylene carbonate;
s5: respectively condensing gaseous vinylene carbonate, gaseous triethylamine and gaseous chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: and (3) reacting the obtained solid product with a proper amount of sodium hydroxide solution to obtain a triethylamine mixed solution:
s7: distilling, drying and condensing the triethylamine mixed solution to obtain liquid triethylamine;
s8: adding liquid chloroethylene carbonate obtained from S5 and liquid ethylene carbonate obtained from S4 as reactants to the reaction in the step S1, and adding liquid triethylamine obtained from S5 and S7 as reactants to the reaction in the step S2;
wherein, the equipment for preparing the vinylene carbonate comprises: the system comprises a solid-liquid separation device communicated with the output end of a tubular reactor, a fractionating device communicated with the first output end of the solid-liquid separation device, a distillation device communicated with the second output end of the solid-liquid separation device, and a drying device communicated with the output end of the distillation device, wherein the fractionating device is communicated with the tubular reactor through three pipelines which are respectively a gas chloroethylene carbonate conveying pipeline, a gas triethylamine conveying pipeline and a liquid ethylene carbonate conveying pipeline;
the solid-liquid separation device comprises:
the device comprises a first tank body, a second tank body and a liquid inlet pipe, wherein the inner space of the first tank body is in a square shape, the upper part of one side of the first tank body is provided with the liquid inlet pipe, the middle part of the other opposite side of the first tank body is provided with the liquid outlet pipe, the lower part of the liquid outlet pipe is provided with a discharge outlet, and the discharge outlet horizontally penetrates through the side wall of the first tank body and two side walls adjacent to the side wall;
the telescopic mechanism is vertically arranged and fixedly connected with the bottom of the first tank body, the output end of the telescopic mechanism is connected with the sealing block, four sides of the sealing block are respectively abutted against the inner side wall of the first tank body, the top surface of the sealing block is inclined, and the sealing block is inclined downwards from the liquid inlet pipe to the liquid outlet pipe;
the filter screens are arranged at intervals along the liquid inlet pipe towards the liquid outlet pipe, any filter screen is vertical to the liquid inlet pipe, and two sides of each filter screen are fixedly connected with the inner side wall of the first tank body;
the cleaning box is fixedly arranged in the middle of one side of the first tank body and is communicated with the inner space of the first tank body, a first air cylinder is arranged in the cleaning box, a cleaning brush is arranged at the output end of the first air cylinder, the output end of the first air cylinder is parallel to the top surface of the sealing block, the first air cylinder is arranged in such a way that when the first air cylinder is completely contracted, the cleaning brush is positioned in the cleaning box, and when the first air cylinder is extended out, the cleaning brush can extend into the inner part of the first tank body;
the second tank body is cylindrical, the inner space of the second tank body is fixedly connected to the bottom of the first tank body, the horizontal projection of the first tank body falls into the second tank body, the side wall, located below the discharge port, of the second tank body extends upwards to a height greater than the height of the discharge port, and forms a closed space with the outer side wall of the first tank body, an inlet port is formed in the bottom of the closed space in a penetrating mode, an alkali inlet pipe is arranged on the side wall of the second tank body, a liquid discharge pipe is arranged at the bottom of the second tank body, and a stirring device is arranged inside the second tank body;
wherein, telescopic machanism sets up to, when it stretches out completely, the low side of sealed piece is located the drain pipe with between the bin outlet, the bottom of filter screen with the top surface butt of sealed piece, work as when telescopic machanism contracts completely, the low side of sealed piece with the lower limb of bin outlet flushes, the high end of sealed piece is located the below of the output of first cylinder, the cleaning brush is in stretch out under the drive of first cylinder the cleaning box with the top surface butt of sealed piece, and follow the top surface reciprocating motion of sealed piece.
2. The method of claim 1, wherein the telescoping mechanism is a cylinder.
3. The method for preparing vinylene carbonate serving as an additive of lithium battery car electrolyte of claim 1, wherein the stirring device comprises a stirring shaft arranged in the second tank, a plurality of stirring paddles arranged on the stirring shaft at intervals, and a servo motor fixedly arranged on the outer side of the bottom of the second tank, and the servo motor and the stirring shaft penetrate through the bottom of the second tank to be connected.
4. The method of claim 1, wherein the mesh openings of the screen adjacent to the side wall of the first can having the discharge opening are smaller than the mesh openings of the screen remote from the side wall of the first can having the discharge opening.
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| CN202011287859.7A CN112397781B (en) | 2020-11-17 | 2020-11-17 | Preparation method of vinylene carbonate additive for lithium battery car electrolyte |
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| CN202011287859.7A CN112397781B (en) | 2020-11-17 | 2020-11-17 | Preparation method of vinylene carbonate additive for lithium battery car electrolyte |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101481613B1 (en) * | 2013-07-08 | 2015-01-12 | 주식회사 포스코 | Apparatus for recycling sealing water of coke oven draft pipe |
| CN104744423A (en) * | 2015-03-17 | 2015-07-01 | 沈阳化工大学 | Method for continuously producing vinylene carbonate |
| CN104844556A (en) * | 2015-04-30 | 2015-08-19 | 荣成青木高新材料股份有限公司 | Method for continuously preparing vinylene carbonate by tubular reactor |
| CN204661588U (en) * | 2015-03-17 | 2015-09-23 | 沈阳化工大学 | A kind of device of continuous prodution vinylene carbonate |
| CN206285596U (en) * | 2016-12-06 | 2017-06-30 | 科斗（苏州）脑机科技有限公司 | A kind of portable chemical spent material solid-liquid separation treatment device |
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2020
- 2020-11-17 CN CN202011287859.7A patent/CN112397781B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101481613B1 (en) * | 2013-07-08 | 2015-01-12 | 주식회사 포스코 | Apparatus for recycling sealing water of coke oven draft pipe |
| CN104744423A (en) * | 2015-03-17 | 2015-07-01 | 沈阳化工大学 | Method for continuously producing vinylene carbonate |
| CN204661588U (en) * | 2015-03-17 | 2015-09-23 | 沈阳化工大学 | A kind of device of continuous prodution vinylene carbonate |
| CN104844556A (en) * | 2015-04-30 | 2015-08-19 | 荣成青木高新材料股份有限公司 | Method for continuously preparing vinylene carbonate by tubular reactor |
| CN206285596U (en) * | 2016-12-06 | 2017-06-30 | 科斗（苏州）脑机科技有限公司 | A kind of portable chemical spent material solid-liquid separation treatment device |
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