CN109806831B - Preparation process of energy storage material of lithium battery - Google Patents
Preparation process of energy storage material of lithium battery Download PDFInfo
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- CN109806831B CN109806831B CN201910204406.4A CN201910204406A CN109806831B CN 109806831 B CN109806831 B CN 109806831B CN 201910204406 A CN201910204406 A CN 201910204406A CN 109806831 B CN109806831 B CN 109806831B
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation process of a lithium battery energy storage material, which comprises the steps of cleaning a storage tank, dehydrating a solvent, mixing raw materials and filling. In the invention, in the process of solvent dehydration, the raw materials are beaten by the material beating machine, so that the raw materials can be fully crushed, and the time and the economic cost of solvent dehydration are reduced by setting the molecular sieve to adsorb moisture in the solvent; in the process of cleaning the storage tank, the quick-opening structure and the screw are washed, and meanwhile, the sealing washer is replaced and the leakage test is carried out, so that the whole sealing performance of the storage tank is ensured; the inside at reation kettle's stirring rake is provided with the first cooling tube and the second cooling tube of establishing ties through the stirring frame like this at the in-process of stirring rake normal rotation, can cool off the stirring rake through external cooling water to improve cooling efficiency, shorten the cool time.
Description
Technical Field
The invention relates to the technical field of lithium battery production, in particular to a preparation process of a lithium battery energy storage material.
Background
A "lithium battery" is a type of battery using a nonaqueous electrolyte solution with lithium metal or a lithium alloy as a negative electrode material. Lithium batteries can be broadly classified into two types: lithium metal batteries and lithium ion batteries. Lithium ion batteries do not contain lithium in the metallic state and are rechargeable. The safety, specific capacity, self-discharge rate and cost performance ratio of the lithium ion battery are all superior to those of the lithium ion battery. The energy storage material is a functional material which stores energy by utilizing physical or chemical changes of substances, and the stored energy can be electric energy, mechanical energy, chemical energy, thermal energy or other forms of energy. The energy storage material can not be separated from an energy storage technology, the forms of energy sources are various, and materials used for electricity storage, heat storage, hydrogen storage, solar cells and the like belong to the energy storage materials in a broad sense.
In the production process of the existing lithium battery electrolyte, the production period and the production cost are high for the dehydration of a solvent, the sealing performance of the storage tank after cleaning is affected, and the problem that the existing reaction kettle has a long period for the cooling of the mixed ethylene carbonate and diethyl carbonate is solved.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a preparation process of a lithium battery energy storage material, wherein in the solvent dehydration process, a material beating machine is used for beating the raw materials, so that the raw materials can be fully crushed, and the molecular sieve is arranged for adsorbing the moisture in the solvent, so that the time and the economic cost for solvent dehydration are reduced; in the process of cleaning the storage tank, the quick-opening structure and the screw are washed, and meanwhile, the sealing washer is replaced and the leakage test is carried out, so that the whole sealing performance of the storage tank is ensured; the first cooling pipe and the second cooling pipe which are connected in series and pass through the stirring frame are arranged in the stirring paddle of the reaction kettle, so that the stirring paddle can be cooled by externally connected cooling water in the normal rotating process of the stirring paddle, the cooling efficiency is improved, and the cooling time is shortened; the bottom at stirring rake main shaft pole closes soon and is connected with the bottom, and the inside of bottom rotates through rotating the seat and is connected with the U type pipe that cup joints first cooling tube and second cooling tube, and this kind of structure makes things convenient for the later stage to empty the inside ponding of stirring rake, novel structure, and the practicality is strong.
The purpose of the invention can be realized by the following technical scheme:
the preparation process of the energy storage material of the lithium battery comprises the steps of cleaning a storage tank, dehydrating a solvent, mixing raw materials and filling, and comprises the following specific steps:
(1) cleaning a storage tank: washing the inner wall of the storage tank by deionized water, filling the deionized water to test the conductivity of the inner wall of the storage tank, washing until the conductivity meets the requirement, drying the inner wall of the storage tank to remove water stains, washing the quick-opening joint and the screw by the deionized water, washing the flange cover and the barrel cover by the deionized water, baking the flange cover to remove the water stains, replacing the sealing washer, testing whether the replaced sealing washer leaks, continuously replacing the sealing washer if the sealing washer leaks, assembling the storage tank if the sealing washer does not leak, filling argon into the assembled storage tank to replace internal gas, and testing the water and the pressure in the storage tank;
(2) solvent dehydration: respectively liquefying ethylene carbonate and diethyl carbonate, respectively beating the liquefied ethylene carbonate and diethyl carbonate by a beating machine, respectively adsorbing internal water by the ethylene carbonate and the diethyl carbonate treated by the beating machine through molecular sieves, respectively distilling and dehydrating the ethylene carbonate and the diethyl carbonate, respectively filtering the distilled ethylene carbonate and the distilled diethyl carbonate, removing impurities doped in the ethylene carbonate and the diethyl carbonate, and finally respectively storing the obtained ethylene carbonate and the diethyl carbonate;
(3) mixing raw materials: confirming the specification of a reaction kettle according to the processing amount, injecting deionized water into the reaction kettle to wash the inner wall of the reaction kettle, sequentially injecting ethylene carbonate and diethyl carbonate solvents with specified weight into the reaction kettle, stirring the ethylene carbonate and the diethyl carbonate through a stirring paddle in the reaction kettle to fully mix the ethylene carbonate and the diethyl carbonate, adding an additive into the reaction kettle, cooling the mixed ethylene carbonate and the diethyl carbonate, adding lithium hexafluorophosphate with specified weight into the reaction kettle, stirring, checking the moisture and the conductivity of the electrolyte to judge whether the electrolyte meets the specification;
(4) filling: and (4) filling the finished electrolyte prepared in the step (3) into the storage tank cleaned in the step (1) for storage.
Further, the method comprises the following steps: the additive in the step (3) is anisole and alumina.
Further, the method comprises the following steps: the moisture and conductivity specifications of the electrolyte in the step (3) are respectively that the moisture content is lower than 10 x 10-6Conductivity of 10-3—2*10-3s/cm。
Further, the method comprises the following steps: the reaction kettle in the step (3) comprises a kettle body and an upper cover connected with the top of the kettle body through a bolt, four supporting legs are welded on the side wall of the bottom of the kettle body at equal angles, a bottom sealing cover is fixed at the center of the bottom of the kettle body through a bolt, an external cooling water outlet pipe is arranged on the side wall of the kettle body and is communicated with one end of a third cooling pipe spirally wound in the kettle body, the other end of the third cooling pipe is communicated with an external cooling water inlet pipe fixed at the bottom of the kettle body, and a discharge pipe communicated with the inner cavity of the kettle body is arranged on the side wall of the bottom of the kettle body;
the stirring device comprises an upper cover, a kettle body and a stirring paddle, wherein the top of the upper cover is movably connected with the stirring paddle extending into the kettle body through a bearing, the stirring paddle comprises a main shaft rod, three pairs of stirring frames are symmetrically welded on the outer wall of the main shaft rod, an outer water collecting cover is welded on the top of the main shaft rod, an inner water collecting cover is welded inside the outer water collecting cover, the bottom of the inner water collecting cover is communicated with a first cooling pipe which is connected with the stirring frames on one side in series and extends to the bottom of the main shaft rod, the bottom of the outer water collecting cover is communicated with a second cooling pipe which is connected with the stirring frames on the other side in series and extends to the bottom of the main shaft rod, the bottom of the main shaft rod is connected with a bottom cover in a screwing mode, the center of the bottom cover is;
the lateral wall of upper cover is provided with the dog-house, the top surface that the upper cover is close to the main shaft pole is fixed with the motor through motor support frame, the motor shaft joint of motor is fixed with first sprocket, first sprocket passes through the chain and is connected with the second sprocket drive of main shaft pole outer wall joint, the top of upper cover has the anti-overflow lid of covering the cover of establishing outer water collecting cover through the welding of iron stand, cover and outer water collecting cover position weld respectively and have interior cooling outlet pipe and the interior cooling inlet tube that extends to its inside in the top surface correspondence of anti-overflow lid.
Further, the method comprises the following steps: the stirring frame is a U-shaped structure which is horizontally placed, wherein the side wall of the upper part of the stirring frame is horizontally arranged, and the side wall of the lower part of the stirring frame is downwards inclined towards the direction of the main shaft rod.
Further, the method comprises the following steps: the inner diameter of the U-shaped pipe is in transition fit with the outer diameters of the first cooling pipe and the second cooling pipe, and rubber rings are sleeved on the outer walls of the ports, connected with the U-shaped pipe in a clamped mode, of the first cooling pipe and the second cooling pipe.
Further, the method comprises the following steps: the first cooling pipe and the second cooling pipe have the same inner diameter.
Further, the method comprises the following steps: the reaction kettle comprises the following specific using operation steps:
the method comprises the following steps: connecting an external cooling water inlet pipe and an internal cooling water inlet pipe with the water outlet end of an external circulating water pump, and connecting an internal cooling water outlet pipe and an external cooling water outlet pipe with the water inlet end of the external circulating water pump;
step two: injecting deionized water into the reaction kettle, and washing the inner wall of the reaction kettle;
step three: ethylene carbonate and diethyl carbonate solvents with specified weight are injected into the reaction through a feeding port in sequence, then a motor is controlled to rotate, and a stirring paddle is driven to rotate through the transmission action of a first chain wheel and a second chain wheel, so that the ethylene carbonate and the diethyl carbonate are stirred, and the ethylene carbonate and the diethyl carbonate can be fully mixed;
step four: adding an additive to the interior of the reaction through a feed port;
step five: cooling water is injected into a third cooling pipe in the kettle body and a first cooling pipe and a second cooling pipe in the stirring paddle through a circulating water pump, so that the inner wall of the kettle body contacted with the third cooling pipe and the stirring paddle contacted with the first cooling pipe and the second cooling pipe can quickly cool the mixture of ethylene carbonate and diethyl carbonate;
step six: after the mixture of the ethylene carbonate and the diethyl carbonate is cooled to a specified temperature, adding lithium hexafluorophosphate with specified weight into the reaction kettle through a feeding port and stirring;
step seven: and discharging the electrolyte fully stirred through a discharge pipe.
The invention has the beneficial effects that:
1. in the process of solvent dehydration, the raw materials are beaten by the beater so that the raw materials can be fully crushed, and the molecular sieve is arranged to adsorb moisture in the solvent, so that the combination mode can improve the speed of the molecular sieve for adsorbing the moisture in the solvent, and meanwhile, the molecular sieve can be repeatedly used, thereby reducing the time and economic cost of solvent dehydration;
2. in the process of cleaning the storage tank, the quick-opening structure and the screw are washed, the sealing washer is replaced at the same time, and then the storage tank with the sealing washer replaced is subjected to leakage test, so that the whole sealing performance of the storage tank is ensured;
3. a first cooling pipe and a second cooling pipe which are connected in series and pass through a stirring frame are arranged in a stirring paddle of a reaction kettle, an outer water collecting cover is welded at the top of a main shaft rod of the stirring paddle, an inner water collecting cover is fixed in the outer water collecting cover and is communicated with the first cooling pipe, the outer water collecting cover is communicated with the second cooling pipe, an anti-overflow cover is covered at the top of the outer water collecting cover, and an inner cooling water outlet pipe and an inner cooling water inlet pipe which extend into the outer water collecting cover and the inner water collecting cover are welded at the top of the anti-overflow cover, so that the stirring paddle can be cooled by external cooling water in the normal rotating process of the stirring paddle, the cooling efficiency is improved, and the cooling time is shortened;
4. the bottom at stirring rake main shaft pole closes soon and is connected with the bottom, and the inside of bottom rotates through rotating the seat and is connected with the U type pipe that cup joints first cooling tube and second cooling tube, and this kind of structure makes things convenient for the later stage to empty the inside ponding of stirring rake, novel structure, and the practicality is strong.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic view of the internal structure of the reaction vessel in the present invention.
FIG. 3 is a schematic view of the structure of the stirring paddle of the present invention.
Fig. 4 is a partial enlarged view of fig. 3 a according to the present invention.
In the figure: 1. a bottom sealing cover; 2. an external cooling water inlet pipe; 3. supporting legs; 4. a discharge pipe; 5. a stirring paddle; 51. a stirring frame; 52. a main shaft rod; 53. a first cooling pipe; 54. an outer water collection cover; 55. an inner water collecting cover; 56. a second cooling pipe; 57. a bottom cover; 58. a rotating seat; 59. a U-shaped pipe; 6. a first sprocket; 7. a motor support frame; 8. a motor; 9. cooling the water outlet pipe internally; 10. cooling the water inlet pipe internally; 11. an anti-overflow cover; 12. a second sprocket; 13. a feeding port; 14. an upper cover; 15. an external cooling water outlet pipe; 16. a third cooling pipe; 17. a kettle body.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the preparation process of the energy storage material for the lithium battery includes the steps of cleaning a storage tank, dehydrating a solvent, mixing raw materials, and filling, and includes the following specific steps:
(1) cleaning a storage tank: washing the inner wall of the storage tank by deionized water, filling the deionized water to test the conductivity of the inner wall of the storage tank, washing until the conductivity meets the requirement, drying the inner wall of the storage tank to remove water stains, washing the quick-opening joint and the screw by the deionized water, washing the flange cover and the barrel cover by the deionized water, baking the flange cover to remove the water stains, replacing the sealing washer, testing whether the replaced sealing washer leaks, continuously replacing the sealing washer if the sealing washer leaks, assembling the storage tank if the sealing washer does not leak, filling argon into the assembled storage tank to replace internal gas, and testing the water and the pressure in the storage tank;
(2) solvent dehydration: respectively liquefying ethylene carbonate and diethyl carbonate, respectively beating the liquefied ethylene carbonate and diethyl carbonate by a beating machine, respectively adsorbing internal water by the ethylene carbonate and the diethyl carbonate treated by the beating machine through molecular sieves, respectively distilling and dehydrating the ethylene carbonate and the diethyl carbonate, respectively filtering the distilled ethylene carbonate and the distilled diethyl carbonate, removing impurities doped in the ethylene carbonate and the diethyl carbonate, and finally respectively storing the obtained ethylene carbonate and the diethyl carbonate;
(3) mixing raw materials: confirming the specification of a reaction kettle according to the processing amount, injecting deionized water into the reaction kettle to wash the inner wall of the reaction kettle, sequentially injecting ethylene carbonate and diethyl carbonate solvents with specified weight into the reaction kettle, stirring the ethylene carbonate and the diethyl carbonate through a stirring paddle in the reaction kettle to fully mix the ethylene carbonate and the diethyl carbonate, adding an additive into the reaction kettle, cooling the mixed ethylene carbonate and the diethyl carbonate, adding lithium hexafluorophosphate with specified weight into the reaction kettle, stirring, checking the moisture and the conductivity of the electrolyte to judge whether the electrolyte meets the specification;
(4) filling: and (4) filling the finished electrolyte prepared in the step (3) into the storage tank cleaned in the step (1) for storage.
The additives in the step (3) are anisole and alumina, and the moisture content and the conductivity specification of the electrolyte in the step (3) are respectively that the moisture content is less than 10 x 10-6Conductivity of 10-3—2*10-3s/cm。
Referring to fig. 2-4, in the preparation process of the energy storage material for the lithium battery, the reaction kettle in step (3) includes a kettle body 17 and an upper cover 14 connected to the top of the kettle body by bolts, four support legs 3 are welded to the bottom side wall of the kettle body 17 at equal angles, a bottom sealing cover 1 is fixed to the bottom center of the kettle body 17 by bolts, an external cooling water outlet pipe 15 is arranged on the side wall of the kettle body 17, the external cooling water outlet pipe 15 is communicated with one end of a third cooling pipe 16 spirally wound inside the kettle body 17, the other end of the third cooling pipe 16 is communicated with an external cooling water inlet pipe 2 fixed to the bottom of the kettle body 17, and a discharge pipe 4 communicated with the inner cavity of the kettle body 17 is arranged on the bottom side;
the top of the upper cover 14 is movably connected with a stirring paddle 5 extending into the kettle body 17 through a bearing, the stirring paddle 5 comprises a main shaft rod 52, three pairs of stirring frames 51 are symmetrically welded on the outer wall of the main shaft rod 52, an outer water collecting cover 54 is welded on the top of the main shaft rod 52, an inner water collecting cover 55 is welded inside the outer water collecting cover 54, the bottom of the inner water collecting cover 55 is communicated with a first cooling pipe 53 which is connected with the stirring frame 51 on one side in series and extends to the bottom of the main shaft rod 52, the bottom of the outer water collecting cover 54 is communicated with a second cooling pipe 56 which is connected with the stirring frame 51 on the other side in series and extends to the bottom of the main shaft rod 52, the bottom of the main shaft rod 52 is rotatably connected with a bottom cover 57, the center of the bottom cover 57 is rotatably connected with a rotating base 58, and a U-shaped pipe 59;
the lateral wall of upper cover 14 is provided with dog-house 13, the top surface that upper cover 14 is close to main shaft 52 is fixed with motor 8 through motor support frame 7, the motor shaft joint of motor 8 is fixed with first sprocket 6, first sprocket 6 passes through the chain and is connected with the second sprocket 12 transmission of main shaft 52 outer wall joint, the top of upper cover 14 has the anti-overflow lid 11 that covers outer water collecting cover 54 through the welding of iron stand, the position of water collecting cover 55 and outer water collecting cover 54 in the top surface of anti-overflow lid 11 corresponds welds respectively and has extended to its inside interior cooling outlet pipe 9 and interior cooling inlet pipe 10.
The stirring frame 51 is of a horizontally placed U-shaped structure, wherein the upper side wall of the stirring frame 51 is horizontally arranged, and the lower side wall of the stirring frame 51 is inclined downwards towards the main shaft rod 52, so that water is prevented from being accumulated in the stirring paddle 5, and the accumulated water in the first cooling pipe 53 and the second cooling pipe 56 in the stirring paddle 5 can be conveniently discharged from the bottom of the main shaft rod 52 in the later period; the inner diameters of the first cooling pipe 53 and the second cooling pipe 56 are the same, the inner diameter of the U-shaped pipe 59 is in transition fit with the outer diameters of the first cooling pipe 53 and the second cooling pipe 56, and rubber rings are sleeved on the outer walls of the ports, clamped with the U-shaped pipe 59, of the first cooling pipe 53 and the second cooling pipe 56, so that the sealing performance of connection between the inner wall of the U-shaped pipe 59 and the outer walls of the first cooling pipe 53 and the second cooling pipe 56 is improved.
The specific using operation steps of the reaction kettle are as follows:
the method comprises the following steps: the external cooling water inlet pipe 2 and the internal cooling water inlet pipe 10 are connected with the water outlet end of an external circulating water pump, and the internal cooling water outlet pipe 9 and the external cooling water outlet pipe 15 are connected with the water inlet end of the external circulating water pump;
step two: injecting deionized water into the reaction kettle, and washing the inner wall of the reaction kettle;
step three: ethylene carbonate and diethyl carbonate solvents with specified weight are injected into the reaction through a feeding port 13 in sequence, then a motor 8 is controlled to rotate, and a stirring paddle 5 is driven to rotate through the transmission action of a first chain wheel 6 and a second chain wheel 12, so that the ethylene carbonate and the diethyl carbonate are stirred, and the ethylene carbonate and the diethyl carbonate can be fully mixed;
step four: adding an additive to the inside of the reaction through a feed port 13;
step five: cooling water is injected into the third cooling pipe 16 in the kettle body 17 and the first cooling pipe 53 and the second cooling pipe 56 in the stirring paddle 5 through a circulating water pump, so that the inner wall of the kettle body 17 contacted with the third cooling pipe 16 and the stirring paddle 5 contacted with the first cooling pipe 53 and the second cooling pipe 56 can rapidly cool the mixture of ethylene carbonate and diethyl carbonate;
step six: after the mixture of the ethylene carbonate and the diethyl carbonate is cooled to the specified temperature, adding lithium hexafluorophosphate with the specified weight into the reaction kettle through the feeding port 13 and stirring;
step seven: the electrolyte fully stirred is discharged outwards through a discharge pipe 4.
The invention has the beneficial effects that:
1. in the process of solvent dehydration, the raw materials are beaten by the beater so that the raw materials can be fully crushed, and the molecular sieve is arranged to adsorb moisture in the solvent, so that the combination mode can improve the speed of the molecular sieve for adsorbing the moisture in the solvent, and meanwhile, the molecular sieve can be repeatedly used, thereby reducing the time and economic cost of solvent dehydration;
2. in the process of cleaning the storage tank, the quick-opening structure and the screw are washed, the sealing washer is replaced at the same time, and then the storage tank with the sealing washer replaced is subjected to leakage test, so that the whole sealing performance of the storage tank is ensured;
3. a first cooling pipe 53 and a second cooling pipe 56 which are connected in series and pass through a stirring frame 51 are arranged inside a stirring paddle 5 of a reaction kettle, an outer water collecting cover 54 is welded at the top of a spindle rod 52 of the stirring paddle 5, an inner water collecting cover 55 is fixed inside the outer water collecting cover 54, the inner water collecting cover 55 is communicated with the first cooling pipe 53, the outer water collecting cover 54 is communicated with the second cooling pipe 56, an anti-overflow cover 11 is covered at the top of the outer water collecting cover 54, and an inner cooling water outlet pipe 9 and an inner cooling inlet water 10 which extend into the outer water collecting cover 54 and the inner water collecting cover 55 are welded at the top of the anti-overflow cover 11, so that the stirring paddle 5 can be cooled by external cooling water in the normal rotation process of the stirring paddle 5, the cooling efficiency is improved, and the cooling time is shortened;
4. the bottom of 5 main shaft rods 52 at stirring rake closes soon and is connected with bottom 57, and the inside of bottom 57 rotates through rotating seat 58 and is connected with the U type pipe 59 that cup joints first cooling tube 53 and second cooling tube 56, and this kind of structure makes things convenient for the later stage to empty the inside ponding of stirring rake 5, novel structure, and the practicality is strong.
The working principle is as follows: when the device is used, the external cooling water inlet pipe 2 and the internal cooling water inlet pipe 10 are connected with the water outlet end of an external circulating water pump, the internal cooling water outlet pipe 9 and the external cooling water outlet pipe 15 are connected with the water inlet end of the external circulating water pump, then deionized water is injected into the reaction kettle to wash the inner wall of the reaction kettle, then ethylene carbonate and diethyl carbonate solvents with specified weight are sequentially injected into the reaction kettle through the feeding port 13, then the motor 8 is controlled to rotate, the stirring paddle 5 is driven to rotate through the transmission action of the first chain wheel 6 and the second chain wheel 12, so that ethylene carbonate and diethyl carbonate are stirred, the ethylene carbonate and diethyl carbonate can be fully mixed, then additives are added into the reaction kettle through the feeding port 13, then cooling water is injected into the third cooling pipe 16 in the kettle body 17 and the first cooling pipe 53 and the second cooling pipe 56 in the stirring paddle 5 through the circulating water pump, the inner wall of the kettle body 17 contacted with the third cooling pipe 16 and the stirring paddle 5 contacted with the first cooling pipe 53 and the second cooling pipe 56 can rapidly cool the mixture of the ethylene carbonate and the diethyl carbonate, then after the mixture of the ethylene carbonate and the diethyl carbonate is cooled to a specified temperature, lithium hexafluorophosphate with specified weight is added into the reaction kettle through the feeding port 13 and stirred, then the electrolyte fully stirred is discharged outwards through the discharging pipe 4, after the use is finished, the ground sealing cover 1 is opened, the bottom cover 57 is unscrewed and taken down, and accumulated water in the first cooling pipe 53 and the second cooling pipe 56 in the stirring paddle 5 is emptied.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (3)
1. The preparation process of the energy storage material of the lithium battery is characterized by comprising the steps of cleaning a storage tank, dehydrating a solvent, mixing raw materials and filling, and comprises the following specific steps:
(1) cleaning a storage tank: washing the inner wall of the storage tank by deionized water, filling the deionized water to test the conductivity of the inner wall of the storage tank, washing until the conductivity meets the requirement, drying the inner wall of the storage tank to remove water stains, washing the quick-opening joint and the screw by the deionized water, washing the flange cover and the barrel cover by the deionized water, baking the flange cover to remove the water stains, replacing the sealing washer, testing whether the replaced sealing washer leaks, continuously replacing the sealing washer if the sealing washer leaks, assembling the storage tank if the sealing washer does not leak, filling argon into the assembled storage tank to replace internal gas, and testing the water and the pressure in the storage tank;
(2) solvent dehydration: respectively liquefying ethylene carbonate and diethyl carbonate, respectively beating the liquefied ethylene carbonate and diethyl carbonate by a beating machine, respectively adsorbing internal water by the ethylene carbonate and the diethyl carbonate treated by the beating machine through molecular sieves, respectively distilling and dehydrating the ethylene carbonate and the diethyl carbonate, respectively filtering the distilled ethylene carbonate and the distilled diethyl carbonate, removing impurities doped in the ethylene carbonate and the diethyl carbonate, and finally respectively storing the obtained ethylene carbonate and the diethyl carbonate;
(3) mixing raw materials: confirming the specification of a reaction kettle according to the processing amount, injecting deionized water into the reaction kettle to wash the inner wall of the reaction kettle, sequentially injecting ethylene carbonate and diethyl carbonate solvents with specified weight into the reaction kettle, stirring the ethylene carbonate and the diethyl carbonate through a stirring paddle in the reaction kettle to fully mix the ethylene carbonate and the diethyl carbonate, adding an additive into the reaction kettle, cooling the mixed ethylene carbonate and the diethyl carbonate, adding lithium hexafluorophosphate with specified weight into the reaction kettle, stirring, checking the moisture and the conductivity of the electrolyte to judge whether the electrolyte meets the specification;
(4) filling: filling the finished electrolyte prepared in the step (3) into the clean storage tank in the step (1) for storage;
the reaction kettle in the step (3) comprises a kettle body (17) and an upper cover (14) connected with the top of the kettle body through a bolt, four supporting legs (3) are welded on the side wall of the bottom of the kettle body (17) at equal angles, a bottom sealing cover (1) is fixed at the center of the bottom of the kettle body (17) through a bolt, an external cooling water outlet pipe (15) is arranged on the side wall of the kettle body (17), the external cooling water outlet pipe (15) is communicated with one end of a third cooling pipe (16) spirally wound in the kettle body (17), the other end of the third cooling pipe (16) is communicated with an external cooling water inlet pipe (2) fixed at the bottom of the kettle body (17), and a discharge pipe (4) communicated with an inner cavity of the kettle body (17) is arranged on the side wall of the bottom of;
the top of upper cover (14) has stirring rake (5) that extends to the cauldron body (17) inside through bearing swing joint, stirring rake (5) include main shaft pole (52), the outer wall symmetrical welding of main shaft pole (52) has three pairs of stirring frame (51), the top welding of main shaft pole (52) has outer cover (54) that catchments, the inside welding of outer cover (54) that catchments has interior cover (55) that catchments, the bottom intercommunication of interior cover (55) that catchments has series connection one side stirring frame (51) and extends to first cooling tube (53) of main shaft pole (52) bottom, the bottom intercommunication of outer cover (54) that catchments has series connection opposite side stirring frame (51) and extends to second cooling tube (56) of main shaft pole (52) bottom, the bottom closure of main shaft pole (52) is connected with bottom (57), the center of bottom (57) is rotated and is connected with and is rotated seat (58), a U-shaped pipe (59) communicated with the first cooling pipe (53) and the second cooling pipe (56) is fixed in the rotating seat (58);
a feeding port (13) is formed in the outer side wall of the upper cover (14), a motor (8) is fixed to the top surface, close to the spindle rod (52), of the upper cover (14) through a motor support frame (7), a first chain wheel (6) is fixedly clamped to a motor shaft of the motor (8), the first chain wheel (6) is in transmission connection with a second chain wheel (12) clamped to the outer wall of the spindle rod (52) through a chain, an anti-overflow cover (11) covering the outer water collecting cover (54) is welded to the top of the upper cover (14) through an iron frame, and an inner cooling water outlet pipe (9) and an inner cooling water inlet pipe (10) extending to the inner portion of the anti-overflow cover (11) are respectively welded to positions corresponding to the inner water collecting cover (55) and the outer water collecting cover (54;
the stirring frame (51) is of a horizontally placed U-shaped structure, wherein the side wall of the upper part of the stirring frame (51) is horizontally arranged, and the side wall of the lower part of the stirring frame (51) is downwards inclined towards the direction of the main shaft rod (52);
the inner diameter of the U-shaped pipe (59) is in transition fit with the outer diameters of the first cooling pipe (53) and the second cooling pipe (56), and rubber rings are sleeved on the outer walls of the ports, clamped with the U-shaped pipe (59), of the first cooling pipe (53) and the second cooling pipe (56);
the inner diameters of the first cooling pipe (53) and the second cooling pipe (56) are the same;
the specific using operation steps of the reaction kettle are as follows:
the method comprises the following steps: the external cooling water inlet pipe (2) and the internal cooling water inlet pipe (10) are connected with the water outlet end of an external circulating water pump, and the internal cooling water outlet pipe (9) and the external cooling water outlet pipe (15) are connected with the water inlet end of the external circulating water pump;
step two: injecting deionized water into the reaction kettle, and washing the inner wall of the reaction kettle;
step three: ethylene carbonate and diethyl carbonate solvents with specified weight are injected into the reaction through a feeding port (13) in sequence, then a motor (8) is controlled to rotate, and a stirring paddle (5) is driven to rotate through the transmission action of a first chain wheel (6) and a second chain wheel (12), so that the ethylene carbonate and the diethyl carbonate are stirred, and the ethylene carbonate and the diethyl carbonate can be fully mixed;
step four: adding an additive to the interior of the reaction through a feed port (13);
step five: cooling water is injected into a third cooling pipe (16) in the kettle body (17) and a first cooling pipe (53) and a second cooling pipe (56) in the stirring paddle (5) through a circulating water pump, so that the inner wall of the kettle body (17) contacted with the third cooling pipe (16) and the stirring paddle (5) contacted with the first cooling pipe (53) and the second cooling pipe (56) can rapidly cool the mixture of the ethylene carbonate and the diethyl carbonate;
step six: after the mixture of the ethylene carbonate and the diethyl carbonate is cooled to a specified temperature, adding lithium hexafluorophosphate with specified weight into the reaction kettle through a feeding port (13) and stirring;
step seven: and discharging the electrolyte fully stirred through a discharge pipe (4) to the outside.
2. The process for preparing an energy storage material for a lithium battery as claimed in claim 1, wherein the additive in the step (3) is anisole and alumina.
3. The process for preparing an energy storage material for a lithium battery according to claim 1, wherein the electrolyte of step (3) has moisture and conductivity specifications of less than 10 x 10 moisture content-6Conductivity of 10-3—2*10-3s/cm。
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