CN112436187B - Gel electrolyte for lithium battery - Google Patents
Gel electrolyte for lithium battery Download PDFInfo
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- CN112436187B CN112436187B CN202011328597.4A CN202011328597A CN112436187B CN 112436187 B CN112436187 B CN 112436187B CN 202011328597 A CN202011328597 A CN 202011328597A CN 112436187 B CN112436187 B CN 112436187B
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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
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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
- H01M10/052—Li-accumulators
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of 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 gel electrolyte of a lithium battery, which comprises: when the vinylene carbonate additive is prepared, a solid product obtained after solid-liquid separation reacts with a sodium hydroxide solution, a reactant is subjected to distillation, drying, condensation and other steps to reduce triethylamine, and the separated liquid is subjected to rectification, condensation and other steps to obtain chloroethylene carbonate, triethylamine and ethylene carbonate raw materials again, so that the utilization rate of the raw materials is improved, and clean production is realized; a solid-liquid separation device is improved, so that separated solid substances can be neutralized inside the solid-liquid separation device to obtain mixed liquid containing triethylamine raw materials instead of manually separating the solid substances for neutralization, and 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 present invention relates to a gel electrolyte for a lithium battery.
Background
The lithium battery gel electrolyte comprises a gel factor, an electrolyte solvent, an electrolyte lithium salt and a functional additive, wherein the functional 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, and vinylene carbonate is an additive commonly added into the lithium battery gel electrolyte.
Industrially, during the process of preparing vinylene carbonate by reacting triethylamine and chloroethylene carbonate, some byproducts are generated, and 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 the gel electrolyte of the lithium battery, which is prepared by reducing the by-product obtained in the process of producing the additive vinylene carbonate and then continuously using the reduced by-product as the raw material, so that the utilization rate of the raw material is improved, and clean production is realized.
The invention also aims to provide a device for preparing the gel electrolyte of the lithium battery, which realizes the continuous production of the whole production line.
To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a gel electrolyte for a lithium battery including
The gel factor comprises a gel monomer, a cross-linking agent and an initiator;
the electrolyte solvent comprises a mixture of two of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, ethylene carbonate and propylene carbonate;
the electrolyte lithium salt includes LiPF 6 、LiBF 4 、LiClO 4 、LiCF 3 SO 3 、LiN(CF 3 O 2 ) 2 、LiN(CF 2 CF 3 SO 2 ) 2 One or a mixture of two;
the functional additive comprises vinylene carbonate, and the preparation method of the vinylene carbonate comprises the following steps:
s1: uniformly mixing chloroethylene 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 the gas vinylene carbonate, the gas triethylamine and the gas chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: reacting the obtained solid product with a proper amount of sodium hydroxide solution to obtain triethylamine mixed solution;
s7: distilling, drying and condensing the triethylamine mixed solution to obtain liquid triethylamine;
s8: the liquid chloroethylene carbonate obtained in the step S5 and the liquid ethylene carbonate obtained in the step S4 are used as reactants to be added into the reaction in the step S1, and the liquid triethylamine obtained in the step S5 and the liquid triethylamine obtained in the step S7 are used as reactants to be added into the reaction in the step S2.
Still provide a preparation facilities of gel electrolyte of lithium cell, including tubular reactor, 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, 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 the gaseous vinylene carbonate of fractionating device output.
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 cuboid, 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 filtering mechanism comprises a first baffle and a second baffle which are arranged along the liquid inlet pipe to the liquid outlet pipe at intervals, the first baffle and the second baffle are symmetrical about a straight line which passes through the center of the first tank body and is perpendicular to the top surface of the first tank body, the first baffle comprises an inclined plate which is gradually far away from the liquid inlet pipe from top to bottom, the top end of the inclined plate is fixedly connected with the inner side wall, below the liquid inlet of the liquid inlet pipe, of the first tank body in a sealing manner, the two sides of the inclined plate are fixedly connected with the inner side wall of the first tank body, the bottom end of the inclined plate vertically extends downwards to form a vertical plate, and the vertical plate is provided with filtering holes all over;
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 downwards inclined from the liquid inlet pipe to the liquid outlet pipe, the middle parts of two opposite side walls of the sealing block penetrate through the filtering mechanism and are vertically and upwardly extended to be provided with a pair of connecting plates, the length of each connecting plate is greater than that of each vertical plate, and cleaning brushes matched with the two vertical plates are fixedly arranged at the top ends of the connecting plates;
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, filter machanism's bottom with the top surface butt of sealed piece works 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, the bottom surface of cleaning brush with filter machanism's the least significant end flushes.
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 plurality of paddles have a triangular longitudinal cross-section.
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.
Thirdly, the longitudinal section of the shape formed by the first baffle plate and the second baffle plate of the filtering mechanism is the same as the longitudinal section of the funnel, namely the longitudinal section of the filtering mechanism is in a shape with a large upper part and a small lower part, when the mixture flows from the upper part to the lower part of the filtering mechanism, the flow velocity of the mixture is increased, a flushing effect is exerted on the vertical plate, so that solid matters adhered to the vertical plate are flushed to the top surface of the sealing block, and in the process that the sealing block moves downwards, a cleaning brush connected with the sealing block also moves downwards to clean the vertical plate, further the vertical plate is cleaned, and the solid matters are prevented from being adhered to the vertical plate to block a filter hole.
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 gel electrolyte production apparatus for a lithium battery according to one embodiment of the present 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 separation apparatus according to one embodiment of the present invention in use;
FIG. 4 is a side view of the seal block according to one embodiment of the present invention;
fig. 5 is a top view of the sealing block according to one embodiment of the present invention.
Reference numerals are as follows: 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 filtering mechanism 16, a first baffle 17, a second baffle 18, an inclined plate 19, a vertical plate 20, a telescopic mechanism 21, a sealing block 22, a connecting plate 23, a cleaning brush 24, a cleaning box 25, a first cylinder 26, a cleaning brush 27, a second tank body 28, a closed space 29, an inlet port 30, an alkali inlet pipe 31, a liquid discharge pipe 32, a stirring device 33, a stirring shaft 34, a stirring paddle 35 and a servo motor 36.
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 combinations thereof.
As shown in fig. 1, the invention provides a gel electrolyte of a lithium battery, which comprises a gel factor, an electrolyte solvent, an electrolyte lithium salt and a functional additive, wherein the gel factor, the electrolyte solvent, the electrolyte lithium salt and the functional additive are only required to be mixed according to a certain proportion when the gel electrolyte is prepared, so that the lithium battery gel electrolyte can be obtained, the gel factor comprises a gel monomer, a cross-linking agent and an initiator, the gel monomer comprises an acrylic acid isocyano ester compound, the cross-linking agent comprises an acrylate compound, and the initiator comprises one of dibenzoyl peroxide, acetyl peroxide, di-tert-butyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile;
the electrolyte solvent comprises a mixture of two of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, ethylene carbonate and propylene carbonate;
the electrolyte lithium salt includes LiPF 6 、LiBF 4 、LiClO 4 、LiCF 3 SO 3 、LiN(CF 3 O 2 ) 2 、LiN(CF 2 CF 3 SO 2 ) 2 One or a mixture of two;
the functional additive comprises vinylene carbonate, and the preparation method of the vinylene carbonate comprises the following steps:
s1: mixing ethylene carbonate 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, chlorinated ethylene 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 the gas vinylene carbonate, the gas triethylamine and the gas chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: reacting the obtained solid product with a proper amount of sodium hydroxide solution to obtain 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: and (3) adding the liquid chloroethylene carbonate obtained in the step (S5) and the liquid ethylene carbonate obtained in the step (S4) as reactants into the reaction in the step (S1), and adding the liquid triethylamine obtained in the step (S5) and the liquid triethylamine obtained in the step (S7) as reactants into the reaction in the step (S2), so that the raw materials can be recycled, the utilization rate of the raw materials is improved, and clean production is realized.
As shown in fig. 2 to 5, the present invention provides an apparatus for preparing a gel electrolyte for a lithium battery, comprising: tubular reactor 1, with tubular reactor 1 output intercommunication's solid-liquid separation equipment 2, with the fractionating device 3 of the first output intercommunication of solid-liquid separation equipment 2, with the distillation plant 4 of the second output intercommunication of solid-liquid separation equipment 2, with the drying device 5 of the 4 output intercommunications of distillation plant, fractionating device 3 with through three pipeline intercommunications between the tubular reactor 1, three pipelines are gaseous chlorinated ethylene carbonate pipeline 7, gaseous triethylamine pipeline 8, liquid ethylene carbonate pipeline 9 respectively, be equipped with first condensing equipment 6 on the gaseous chlorinated ethylene carbonate pipeline 7, be equipped with second condensing equipment 10 on the gaseous triethylamine pipeline 8, wherein, drying device 5 output with the input of second condensing equipment 10 communicates, be equipped with third condensing equipment 11 on the pipeline of gaseous vinylene carbonate of fractionating device 3 output.
When the technical scheme is adopted to produce the lithium battery gel electrolyte, the tubular reactor 1 carries out the reaction of 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 reacts with sodium hydroxide solution in the solid-liquid separation device 2 to obtain 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 in the triethylamine mixed solution, 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 raw materials for production, all the gases obtained by fractionation are condensed by the condensing tube, the obtained target products are left, and the obtained raw material products are sent back to the tubular reactor 1 for reaction. The obtained target product, namely the functional additive vinylene carbonate, is used as a production raw material of lithium battery electrolyte, the functional additive vinylene carbonate, the gel factor, the electrolyte solvent and the electrolyte lithium salt are put into a glove box (with the moisture content less than 10ppm and the oxygen content less than 1 ppm) filled with argon, and the functional additive, the gel factor, the electrolyte solvent and the electrolyte lithium salt are mixed according to a certain proportion to obtain the lithium battery gel electrode solution.
In another embodiment, the solid-liquid separation apparatus 2 includes:
a first tank 12, the inner space of which is cuboid, wherein a liquid inlet pipe 13 is arranged above one side of the first tank 12, a liquid outlet pipe 14 is arranged in the middle of the other opposite side, a discharge outlet 15 is arranged below the liquid outlet pipe 14, and the discharge outlet 15 horizontally penetrates through the side wall of the first tank 12 and two side walls adjacent to the side wall;
the filtering mechanism 16 comprises a first baffle 17 and a second baffle 18 which are arranged along the liquid inlet pipe 13 to the liquid outlet pipe 14 at intervals, the first baffle 17 and the second baffle 18 are symmetrical about a straight line which passes through the center of the first tank body 12 and is perpendicular to the top surface of the first tank body 12, the first baffle 17 comprises an inclined plate 19 which is gradually far away from the liquid inlet pipe 13 from top to bottom, the top end of the inclined plate 19 is fixedly connected with the inner side wall of the first tank body 12 below the liquid inlet of the liquid inlet pipe 13 in a sealing manner, the two sides of the inclined plate are fixedly connected with the inner side wall of the first tank body 12, the bottom end of the inclined plate 19 is vertically extended downwards to form a vertical plate 20, and the vertical plate 20 is provided with filter holes all over;
the telescopic mechanism 21 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 22, four sides of the sealing block 22 are respectively abutted against the inner side wall of the first tank 12, the top surface of the sealing block 22 is inclined and is inclined downwards from the liquid inlet pipe 13 to the liquid outlet pipe 14, the middle parts of two opposite side walls of the sealing block 22 penetrate through the filtering mechanism 16 and are vertically and upwardly extended to be provided with a pair of connecting plates 23, the length of each connecting plate 23 is greater than that of each vertical plate 20, and the top ends of the pair of connecting plates 23 are fixedly provided with cleaning brushes 24 matched with the two vertical plates 20;
a cleaning box 25 fixedly arranged at the middle part of one side of the first tank 12 and communicated with the inner space of the first tank 12, wherein a first cylinder 26 is arranged in the cleaning box 25, a cleaning brush 27 is arranged at the output end of the first cylinder 26, the output end of the first cylinder 26 is parallel to the top surface of the sealing block 22, the first cylinder 26 is arranged such that when the first cylinder 26 is completely contracted, the cleaning brush 27 is positioned in the cleaning box 25, and when the first cylinder 26 is extended, the cleaning brush 27 can be extended into the inner part of the first tank 12;
a second tank 28, the inner space of which is cylindrical and is fixedly connected to the bottom of the first tank 12, the horizontal projection of the first tank 12 falls into the second tank 28, the side wall of the second tank 28, which is located below the discharge opening 15, extends upward to a height greater than the discharge opening 15, and forms a closed space 29 with the outer side wall of the first tank 12, the bottom of the closed space 29 is provided with an inlet opening 30 in a penetrating manner, wherein the side wall of the second tank 28 is provided with an alkali inlet pipe 31, the bottom of the second tank is provided with a liquid discharge pipe 32, and a stirring device 33 is arranged inside the second tank;
wherein, telescopic machanism 21 sets up to, when it stretches out completely, the low end of sealed piece 22 is located between drain pipe 14 and the bin outlet 15, the bottom of filter equipment 16 with the top surface butt of sealed piece 22, when telescopic machanism 21 contracts completely, the low end of sealed piece 22 with the lower limb of bin outlet 15 flushes, the high end of sealed piece 22 is located the below of the output of first cylinder 26, cleaning brush 27 stretches out under the drive of first cylinder 26 cleaning box 25 with the top surface butt of sealed piece 22, and along the top surface reciprocating motion of sealed piece 22, the bottom surface of cleaning brush 24 with the lowest end of filter equipment 16 flushes.
In the above technical solution, the solid-liquid separation device 2 includes a first tank 12, a filtering mechanism 16, a telescopic mechanism 21, a cleaning box 25 and a second tank 28, the internal space of the first tank 12 is cuboid, 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 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 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 12 and the two side walls adjacent to the side wall; the filtering mechanism 16 comprises a first baffle 17 and a second baffle 18, the first baffle 17 and the second baffle 18 are arranged at intervals along the liquid inlet pipe 13 towards the liquid outlet pipe 14, the first baffle 17 and the second baffle 18 are symmetrical about a straight line which passes through the center of the first tank 12 and is perpendicular to the top surface of the first tank 12, the first baffle 17 comprises an inclined plate 19 which is gradually far away from the liquid inlet pipe 13 from top to bottom, the top end of the inclined plate 19 is fixedly connected with the inner side wall of the first tank 12 below the liquid inlet of the liquid inlet pipe 13 in a sealing way, two sides of the inner side wall of the first tank 12 are fixedly connected with the inner side wall of the first tank, the bottom end of the inclined plate 19 extends vertically downwards to form a vertical plate 20, two sides of the vertical plate 20 are fixedly connected with the inner side wall of the first tank 12 in a sealing way, the longitudinal section of the first baffle 17 and the second baffle 18 of the filtering mechanism 16 and the longitudinal section of the funnel are the same in shape, namely, the channel formed by the first baffle 17 and the second baffle 18 is in a shape which is large at the bottom, when the mixture flows from the upper part to the lower part towards the lower part of the filtering mechanism 16, the flow speed of the mixture is increased, and the vertical plate 20 has a washing effect, so that the solid substance is adhered on the vertical plate 20, and the vertical plate 20 is adhered to be washed on the filtering block 20, and filtered on the filtering plate 20, and the filtering block 20 is adhered on the filtering block 20; the telescopic mechanism 21 is arranged at the bottom in the first tank body 12, the output end of the telescopic mechanism 21 is connected with a sealing block 22, four sides of the sealing block 22 are respectively abutted against the inner side wall of the first tank body 12, the sealing block 22 can vertically slide in the first tank body 12 under the driving of the telescopic mechanism 21, the top surface of the sealing block 22 is a slope surface, the high end of the sealing block 22 is in contact with the side wall of the first tank body 12 provided with a liquid inlet pipe 13, the low end of the sealing block 22 is in contact with the side wall of the first tank body 12 provided with a liquid outlet pipe 14, wherein the type of the telescopic mechanism 21 is not limited, the telescopic mechanism 21 can be an air cylinder or a structure formed by combining a servo motor 36 and a screw rod, and the like, as long as the sealing block 22 can be driven to vertically slide in the first tank body 12, a pair of connecting plates 23 vertically extend upwards from the two opposite side walls of the sealing block 22, the connecting plates 23 pass through the filtering mechanism 16, the top end of the connecting plates 23 is fixedly provided with a cleaning brush 24 for cleaning the vertical plate 20 of the filtering mechanism 16, when the sealing block 22 moves upwards and downwards, the lower end of the sealing block 22 is flush with the filtering mechanism 16, the lower end of the filtering mechanism 16 is in parallel to the lower end of the lower filtering mechanism 16, and the lower end of the lower filtering mechanism 16, the lower end of the lower sealing block 16, the lower sealing block 22 is flush with the filtering mechanism 16, and the lower end of the filtering mechanism 16, and the lower end of the filtering mechanism 16 are flush with the lower end of the filtering mechanism 16; the cleaning box 25 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 26 and a cleaning brush 27 connected with the output end of the first air cylinder 26 are arranged in the cleaning box 25, the output end of the first air cylinder 26 is parallel to the top surface of the sealing block 22, the first air cylinder 26 is arranged such that when the first air cylinder 26 is completely contracted, the cleaning brush 27 is positioned in the cleaning box 25, when the first air cylinder 26 is extended out, the cleaning brush 27 can be extended into the first tank body 12, when the telescopic mechanism 21 is completely contracted, the lower end of the sealing block 22 is flush with the lower edge of the discharge port 15, the upper end of the sealing block 22 is positioned below the output end of the first air cylinder 26, the cleaning brush 27 is extended out of the cleaning box 25 under the driving of the first air cylinder 26 to abut against the top surface of the sealing block 22 and reciprocates along the top surface of the sealing block 22, and the purpose is that when the sealing block 22 with solid substances moves down to the lower end of the discharge block 22 and is flush with the lower edge of the lower end of the discharge port 15, the cleaning brush 27 in the sealing block 25, the sealing block 22 pushes the solid substances down from the sealing block 22 to push the sealing block 22 to drop down from the sealing block 22; the second tank 28 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 28, the side wall of the second tank 28 below the discharge opening 15 extends upwards to a height greater than the discharge opening 15, and forms a closed space 29 with the outer side wall of the first tank 12, the bottom of the closed space 29 is provided with an inlet opening 30, the solid matters pushed down from the top surface of the sealing block 22 by the cleaning brush 27 enter the second tank 28 through the inlet opening 30, after a certain amount of solid matters in the second tank 28 are accumulated, alkali liquor is put into the alkali inlet pipe 31, the solid matters are completely reacted under the stirring of the stirring device 33, after the complete reaction, the mixed liquid is discharged from the liquid discharge pipe 32, and the next operation is carried out.
In the using process, when solid-liquid separation is carried out, the telescopic mechanism 21 is fully extended, solid matters stay on the top surface of the sealing block 22, liquid matters are discharged from the liquid outlet pipe 14 after passing through meshes of the vertical plate 20, after the liquid matters are fully discharged, the telescopic mechanism 21 is fully contracted, the first air cylinder 26 in the cleaning box 25 is started, the first air cylinder 26 drives the cleaning brush 27 to push out the solid matters on the top surface of the sealing block 22, the solid matters enter the second tank body 28 through the discharge port 15 and the inlet port 30, after the solid matters in the second tank body 28 are accumulated to a certain amount, alkali liquor is put into the alkali inlet pipe 31, the solid matters are fully reacted under the stirring of the stirring device 33, after the full reaction, mixed liquid is discharged from the liquid outlet pipe 32, the next step of operation is carried out, the solid-liquid separation device 2 is modified by adopting the technical scheme, 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 can be discharged through the liquid outlet pipe 32, the next step of purification operation can be carried out, the solid matters can be carried out, and the solid matters can be separated out by non-liquid neutralization by a non-liquid separation, and the continuous production line of the whole production is realized.
In another technical solution, the telescopic mechanism 21 is an air cylinder, and the air cylinder drives the sealing block 22 to slide in the first tank 12.
In another technical solution, the stirring device 33 includes a stirring shaft 34 disposed in the second tank 28, a plurality of stirring paddles 35 disposed on the stirring shaft 34 at intervals, and a servo motor 36 fixedly disposed at the outer side of the bottom of the second tank 28, wherein the servo motor 36 and the stirring shaft 34 penetrate through the bottom of the second tank 28, and the stirring device 33 is used to fully react the substance.
In another technical solution, the longitudinal sections of the stirring paddles 35 are triangular, so as to prevent solid matters from sticking to the top surfaces of the stirring paddles 35.
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 lithium vehicle electrolyte additive 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 limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (4)
1. The preparation method of the gel electrolyte of the lithium battery comprises the steps of preparing a gel electrolyte of the lithium battery, wherein the gel electrolyte of the lithium battery comprises a gel factor, an electrolyte solvent, an electrolyte lithium salt and a functional additive, and is characterized in that the gel factor comprises a gel monomer, a cross-linking agent and an initiator;
the electrolyte solvent comprises a mixture of two of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, ethylene carbonate and propylene carbonate;
the describedThe lithium salt of the electrolyte includes LiPF 6 、LiBF 4 、LiClO 4 、LiCF 3 SO 3 、LiN(CF 3 SO 2 ) 2 、LiN(CF 2 CF 3 SO 2 ) 2 One or a mixture of two;
the functional additive comprises vinylene carbonate, and the preparation method of the 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 the gas vinylene carbonate, the gas triethylamine and the gas chloroethylene carbonate to obtain target products of vinylene carbonate, liquid triethylamine and liquid chloroethylene carbonate;
s6: reacting the obtained solid product with a 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 in the step S5 and liquid chloroethylene carbonate obtained in the step S4 as reactants into the reaction in the step S1, and adding liquid triethylamine obtained in the steps S5 and S7 as reactants into the reaction in the step S2;
wherein, a preparation facilities for preparing vinylene carbonate includes: the system comprises a tubular reactor, a solid-liquid separation device communicated with the output end of the 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 chlorinated ethylene carbonate conveying pipeline, a gas triethylamine conveying pipeline and a liquid ethylene carbonate conveying pipeline, a first condensing device is arranged on the gas chlorinated ethylene carbonate conveying pipeline, a second condensing device is arranged on the gas triethylamine conveying pipeline, the output end of the drying device is communicated with the input end of the second condensing device, and a third condensing device is arranged on a pipeline for outputting gaseous vinylene carbonate by the fractionating device;
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 cuboid, 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 filtering mechanism comprises a first baffle and a second baffle which are arranged along the liquid inlet pipe to the liquid outlet pipe at intervals, the first baffle and the second baffle are symmetrical about a straight line which passes through the center of the first tank body and is perpendicular to the top surface of the first tank body, the first baffle comprises an inclined plate which is gradually far away from the liquid inlet pipe from top to bottom, the top end of the inclined plate is fixedly connected with the inner side wall, below the liquid inlet of the liquid inlet pipe, of the first tank body in a sealing manner, the two sides of the inclined plate are fixedly connected with the inner side wall of the first tank body, the bottom end of the inclined plate vertically extends downwards to form a vertical plate, and filtering holes are formed in the vertical plate in a spreading manner;
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 downwards inclined from the liquid inlet pipe to the liquid outlet pipe, the middle parts of two opposite side walls of the sealing block penetrate through the filtering mechanism and are vertically and upwards extended to be provided with a pair of connecting plates, the length of each connecting plate is greater than that of each vertical plate, and cleaning brushes matched with the two vertical plates are fixedly arranged at the top ends of the connecting plates;
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, filter machanism's bottom with the top surface butt of sealed piece, works 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, the bottom surface of cleaning brush with filter machanism's the lowest end flushes.
2. The method for preparing gel electrolyte for lithium battery as claimed in claim 1, wherein the telescopic mechanism is a cylinder.
3. The method for preparing gel electrolyte of lithium battery as claimed in claim 2, wherein said stirring device comprises a stirring shaft disposed in said second tank, stirring paddles disposed on said stirring shaft at intervals, and a servo motor fixedly disposed outside the bottom of said second tank, said servo motor and said stirring shaft penetrating the bottom of said second tank to be connected.
4. The method for preparing gel electrolyte for lithium battery as claimed in claim 3, wherein the paddle has a triangular longitudinal section.
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| CN101400667A (en) * | 2006-03-20 | 2009-04-01 | 三菱化学株式会社 | Method of purifying ethylene carbonate, process for producing purified ethylene carbonate and ethylene carbonate |
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| CN107819150A (en) * | 2017-08-07 | 2018-03-20 | 天津金牛电源材料有限责任公司 | A kind of gel electrolyte of lithium ion battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005021964A1 (en) * | 2005-05-12 | 2006-11-16 | Lanxess Deutschland Gmbh | Process for the preparation of vinylene carbonate |
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| CN101400667A (en) * | 2006-03-20 | 2009-04-01 | 三菱化学株式会社 | Method of purifying ethylene carbonate, process for producing purified ethylene carbonate and ethylene carbonate |
| CN204502555U (en) * | 2015-03-04 | 2015-07-29 | 邯郸市同达矿用电器有限公司 | Equipment for separating liquid from solid |
| CN104744423A (en) * | 2015-03-17 | 2015-07-01 | 沈阳化工大学 | Method for continuously producing vinylene carbonate |
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