CN207856912U - A kind of lithium battery tertiary precursor synthesis apparatus system - Google Patents

A kind of lithium battery tertiary precursor synthesis apparatus system Download PDF

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Publication number
CN207856912U
CN207856912U CN201721902855.9U CN201721902855U CN207856912U CN 207856912 U CN207856912 U CN 207856912U CN 201721902855 U CN201721902855 U CN 201721902855U CN 207856912 U CN207856912 U CN 207856912U
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reaction kettle
lithium battery
ternary precursor
clarification
mother liquor
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CN201721902855.9U
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赵林
但勇
赵澎
陈雪风
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Sichuan Compliance Power Battery Materials Co ltd
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Meishan Compliance Power Battery Material Co Ltd
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Abstract

The utility model discloses a kind of lithium battery tertiary precursor synthesis apparatus system, including reaction kettle, division box and circular clarifying device;The reaction kettle is closed tank structure, which, which matches, is arranged with agitating device;It is connected to inside the division box and reaction kettle, for carrying out solid sedimentation and mother liquor separating treatment to the material mixture liquid out of reaction kettle;The circular clarifying device is external clarification case, connects into circulation loop by pipeline with division box and reaction kettle successively, for the recycling to carrying out material after secondary settlement separating treatment and deposition from the mother liquor isolated in the division box.The apparatus system can not influence material in reactor synthesis while realize efficiently separating for mother liquor and solid material, solid content in reaction kettle is improved to 20% or more, make ternary precursor crystallized product size distribution evenly, and it controls entrained solids in last discharge mother liquor and is less than 0.1%, loss of material is reduced, material utilization and product qualification rate are improved.

Description

Lithium battery ternary precursor synthesis device system
Technical Field
The utility model relates to a lithium cell ternary precursor synthesizer, especially a mother liquor separation circulating device system in lithium cell ternary precursor synthesis.
Background
The key material of the lithium ion battery is a positive electrode material, which accounts for about 30% of the cost of the lithium ion battery, and lithium cobaltate, a ternary material, lithium manganate and lithium iron phosphate are mainly applied in the current market. The lithium nickel cobalt manganese oxide material is a novel lithium battery positive electrode material; compared with other anode materials, the anode material has the advantages of high mass specific capacity, low cost, good thermal stability and high energy density, and is widely applied to the fields of digital electronic products, electric tools, electric bicycles and the like. The ternary material is prepared by mixing a ternary precursor and a lithium source and then sintering at high temperature. Nickel cobalt manganese hydroxide is a widely used ternary precursor material with a chemical general formula of NixCoyMnz(OH)2Specifically, nickel salt, cobalt salt and manganese salt are used as raw materials, and the synthesis is carried out by adjusting the specific dosage ratio (x: y: z) of nickel, cobalt and manganese according to actual needs.
At present, the nickel-cobalt-manganese hydroxide ternary precursor is usually prepared by a crystallization coprecipitation method, and specifically, in a single-kettle continuous production mode, a nickel-cobalt-manganese soluble salt aqueous solution, a sodium hydroxide aqueous solution and an ammonia aqueous solution are subjected to overflow design and feeding design of a reaction kettle, and material feeding and discharging speed control are combined, so that materials in the reaction kettle reach a stable state, small crystal nucleus generation and large particle growth are performed simultaneously, the production continuity is good, material particles with a certain particle size width can be generated, and the method is widely used. However, since the nickel, cobalt and manganese hydroxides generated in the preparation process are very easily oxidized after contacting with air, the whole reaction kettle needs to be kept in a sealed state, for the sake of production safety, in the existing reaction process, the concentrations of the nickel, cobalt and manganese salt solution and sodium hydroxide in the reaction kettle cannot be too high, the content of crystalline solids generated in the reaction kettle can only reach about 10% at most, the output efficiency of crystalline particles is low, and the problems that the granularity of the prepared crystalline particles is too fine or too large, part of the crystalline particles are immature, the surface structures of the particles are loose and the like often occur, thereby causing the serious waste of production materials.
SUMMERY OF THE UTILITY MODEL
The invention of the utility model aims to: aiming at the problems in the prior art, the lithium battery ternary precursor reaction synthesizer system can effectively improve the solid content in a reaction kettle, enables the prepared ternary precursor to be more uniform in crystal size distribution, and greatly improves the yield and the qualification rate of the crystalline solid.
In order to realize the purpose, the utility model discloses a technical scheme be:
a lithium battery ternary precursor synthesis device system comprises a reaction kettle, a water distribution device and a circulating clarification device; wherein,
the reaction kettle is of a closed tank structure, and a stirring device is arranged inside the reaction kettle tank body in a matched manner and is used for fully mixing materials in the reaction kettle;
the water diversion device is of an inverted cone structure with a large upper part and a small lower part, and the bottom of the water diversion device is communicated with the inside of the reaction kettle tank body and is used for carrying out solid settlement and mother liquor separation treatment on a material mixed solution flowing out of the reaction kettle tank body;
the circulating clarification device is an external clarification tank, the top of the clarification tank is connected with a feed pipe, and the other end of the feed pipe is connected with a water outlet arranged on the side wall of the upper part of the water distribution device and used for carrying out secondary sedimentation separation treatment on the mother liquor separated from the water distribution device; a water outlet is formed in the side face of the clarification tank and used for discharging the clarified mother liquor; the material outlet at the bottom of the clarification tank and the feed inlet at the top of the reaction kettle are connected with a return pipeline, and a pumping device is arranged on the return pipeline and used for pumping and returning the material deposited at the bottom of the clarification tank to the reaction kettle for recycling.
According to the technical scheme, solid-liquid mixed fluid formed after materials in the reaction kettle tank body are fully stirred, mixed and reacted for a period of time enters a water distribution device communicated with the solid-liquid mixed fluid; the inverted cone structure setting of the water diversion device big-end-up makes the solid-liquid mixed fluid follow the water diversion device bottom flow in-process reduces the velocity of flow gradually to make solid material in the solid-liquid mixed liquid freely settle in the water diversion device of inverted cone and return to the reaction kettle tank internally, the mother liquor of separating is from setting up the delivery port discharge back on the lateral wall at water diversion device top, inside the inlet pipe inflow external circulation clarification device, in the clarification tank, a small amount of material that the mother liquor smugglied secretly continues sedimentation separation, the mother liquor after the complete clarification is discharged from the discharge port of clarification tank side. When the material in the external clarifying tank is deposited to a certain amount, the material is circularly pumped back to the reaction kettle through the pump to continue to react.
By the device system, the solid content of the synthesized ternary precursor produced in the reaction kettle is increased to more than 20%, solid particles carried by the finally discharged mother liquor are less than 0.1%, and the product yield is remarkably improved. And, the foundation synthesizer system has effectively prolonged the dwell time of solid particle in reation kettle, increases the probability of looks mutual friction between the solid particle to effectively improve the particle size distribution and the topography structure of ternary precursor crystal particle product, the ternary precursor crystal particle size distribution that makes the preparation is more even, greatly improves crystallization solid yield and qualification rate.
Preferably, the water diversion device mainly comprises a lower conical cylinder and an upper cylinder, and the bottom of a lower conical through hole of the water diversion device is communicated with the inside of the reaction kettle tank body; a plurality of baffle plates which are arranged in a staggered mode are arranged in the cylinder at the upper portion of the water distribution device. Preferably, the baffles are vertically staggered near the water outlet of the water diversion device, and more preferably, the baffles are horizontally staggered near the water outlet of the water diversion device.
According to the preferable scheme, in the process that solid materials in the solid-liquid mixed fluid in the reaction kettle enter the water diversion device along the conical cylinder at the bottom, the solid materials return to the reaction kettle through free settling, and meanwhile, after the solid materials meet the baffles which are arranged in the cylinder at the upper part of the water diversion device and are staggered with each other, the solid-liquid mixed fluid forms baffling state roundabout flow under the action of the baffles, so that the flow path of the fluid is increased on one hand, and the effects of settling the solid materials and separating the solid from the liquid are facilitated; on the other hand, the disturbance effect of the baffle on the flow state of the solid-liquid mixed fluid is utilized, the flow velocity of the fluid is reduced, the solid-liquid separation effect is enhanced, and meanwhile, the treated mother liquor can be effectively drained to the position near the water outlet, so that the treated mother liquor is discharged.
Preferably, a plurality of baffle plates which are arranged in a staggered mode are arranged inside the clarifying tank of the circulating clarifying device, and the baffle plates which are arranged in the staggered mode form a circuitous flow channel for promoting the separation of solid and liquid in feed liquid, so that the settling and separating efficiency of materials in mother liquid in the clarifying tank is further improved.
Preferably, the number of the baffles is more than one.
Further, the stirring device comprises a motor, a stirring shaft and stirring blades; the motor sets up at reation kettle cauldron body top, and the output of motor is connected with the upper end of (mixing) shaft, the lower extreme of (mixing) shaft stretches into reation kettle cauldron internal to be equipped with a plurality of stirring vane at the (mixing) shaft lower extreme.
Preferably, the water diversion device is communicated with the side wall of the bottom of the reaction kettle.
Preferably, the bottom of the reaction kettle is conical. Is beneficial to the slow and effective discharge of mature ternary precursor crystal particles produced in the reaction kettle.
Further, a feed inlet is formed in the top of the reaction kettle, and a discharge outlet is formed in the bottom of the reaction kettle.
Preferably, plastic layers are arranged on the inner wall surfaces of the reaction kettle, the water distribution device and the circulating clarification device. Further preferably, the water diversion device and the circulating clarification device are both of closed structures.
Because in the process of the ternary precursor synthesis reaction, other metal elements are required to be prevented from being doped, the existing commonly used reaction kettle needs a lining nonmetal plastic layer, and the influence of introducing other impurity metals due to the direct contact of materials and reaction equipment made of metal materials is avoided. Therefore, it is preferred the utility model discloses a spoiler surface set up the non-metal film layer, play the separation guard action. Meanwhile, the spoiler is embedded into the plastic film layer, so that the fixing property is good, and the spoiler cannot fall off in high-speed stirring. More preferably, the non-metal plastic film layer is made of one or more materials of PP, PPT, PPS and ABS. Furthermore, the water diversion device and the circulating clarification device are both of a closed structure, and the barrier protection effect on reaction materials in the whole device system is facilitated.
To sum up, the beneficial effects of the utility model are that:
1. lithium cell ternary precursor synthesizer system, combine the water knockout drum device that sets up with reation kettle intercommunication, and in proper order with water knockout drum device and reation kettle pass through the circulation clarification device of pipe connection into circulation loop, can be when not influencing reation kettle interior material synthesis, realize the effective separation of mother liquor and solid material, improve solid content in the reation kettle to more than 20%, the dwell time of solid particle in reation kettle has effectively been prolonged, increase the probability of mutual friction between the solid particle, thereby effectively improve the particle size distribution and the appearance structure of ternary precursor crystal particle product, the ternary precursor crystal particle size distribution that makes the preparation is more even, granule crystal maturity is high, greatly improve material utilization efficiency and product percent of pass.
2. The foundation the utility model provides a lithium cell ternary precursor synthesizer system combines circulation clarification device carries out the secondary sedimentation separation to the mother liquor that water separator separated, realizes the recycle to tiny material in the mother liquor, makes final exhaust mother liquor solid content be less than 0.1%, reduces the loss that solid particle was taken out by the mother liquor, improves the product yield.
3. The foundation the utility model provides a lithium cell ternary precursor synthesizer system, whole device system device is simple compact, and the cooperation is inseparable each other, combines current intelligence control system, can realize the full automatic cycle operation of whole mother liquor separation and material recycle procedure, and industrial practical value is high.
Drawings
Fig. 1 is a schematic structural diagram of a ternary precursor synthesizer system according to embodiment 1 of the present invention.
Fig. 2 is a schematic top view of the upper cylindrical portion (202) of the water diversion apparatus of fig. 1.
Fig. 3 is a schematic structural diagram of a ternary precursor synthesizer system according to embodiment 2 of the present invention.
The labels in the figure are: 1-a reaction kettle tank body, 101-a first feeding port, 102-a second feeding port, 103-a third feeding port, 104-a discharging port, 105-a fourth feeding port, 2-a water distribution device and 201-a cylinder; 202-cone, 202 a-baffle, 202 b-water outlet, 3-circulation clarifying device, 301-baffle, 302-material outlet, 303-material inlet; 304-a water outlet; 4-pump, 6-stirring device, 601-motor, 602-stirring shaft, 603-stirring blade.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
As shown in fig. 1-2, a novel lithium battery ternary precursor synthesizer system comprises a reaction kettle 1, a water diversion device 2 and a circulating clarification device 3; wherein,
the reaction kettle 1 is of a closed conical tank structure, the top of the reaction kettle 1 is provided with a first feed inlet 101, a second feed inlet 102, a third feed inlet 103 and a fourth feed inlet 105, and the bottom of the reaction kettle 1 is provided with a discharge outlet 104. The stirring device 6 is arranged inside the tank body of the reaction kettle 1 in a matching manner, and the stirring device 6 comprises a motor 601, a stirring shaft 602 and stirring blades 603; the motor 601 is arranged on the top of the tank body of the reaction kettle 1, the output end of the motor 601 is connected with the upper end of the stirring shaft 602, the lower end of the stirring shaft 602 extends into the tank body of the reaction kettle 1, and two stirring blades 603 are arranged at the lower end of the stirring shaft 602.
The water diversion device 2 mainly comprises an inner through closed container consisting of a lower conical cylinder 201 and an upper cylinder 202, and the bottom of the lower conical cylinder 201 of the water diversion device 2 is communicated with the inner part of the tank body of the reaction kettle 1; a plurality of baffles 202a arranged in a staggered manner in the transverse direction are arranged in the upper cylinder 202 of the water diversion device 2, as shown in fig. 2, the baffles 202a in the upper cylinder 202 of the water diversion device 2 are sequentially staggered from left to right in the transverse direction to form a baffling channel, so that the solid-liquid mixed fluid flows in a tortuous manner in a baffling state under the action of the baffles 202 a. A water outlet 202b is arranged on the side surface of the upper cylinder 202 of the water diversion device 2.
The circulating clarification device 3 is an external clarification tank, the top of the clarification tank is connected with a feed pipe 303, and the other end of the feed pipe 303 is connected with a water outlet 202b arranged on the side wall of the top of the water diversion device; a plurality of baffles 301 which are vertically staggered are arranged in the clarification tank and are used for carrying out secondary sedimentation separation treatment on the mother liquor separated from the water diversion device 1; a water outlet 304 is arranged on the upper side surface of the clarification tank and used for discharging the clarified mother liquor; and a backflow pipeline is connected between the material outlet 302 at the bottom of the clarification tank and the four feeding holes 105 at the top of the reaction kettle, and a pump 4 is arranged on the backflow pipeline and used for pumping and refluxing the material deposited at the bottom of the clarification tank to the reaction kettle 1 for recycling.
And, be provided with the plastic layer on reation kettle 1, water diversion device 2 and 3 inner wall surfaces of circulation clarification device, avoid the material to contact with the response equipment direct contact of metal material, introduce other impurity metal influences, play the separation guard action.
According to the utility model provides a pair of novel synthetic reation kettle of lithium cell ternary precursor, reaction material are respectively from feed inlet 101, and feed inlet two 102 and feed inlet three 103 get into reation kettle 1 in, motor 601 drive among the agitating unit 6 has stirring vane 603's (mixing) shaft 602 rotatory, makes the abundant rotatory flow mixed reaction of the internal material of reation kettle 1 jar. The method is characterized in that solid-liquid mixed fluid formed after materials in the tank body of the reaction kettle 1 are fully stirred, mixed and reacted for a period of time is fed into the water distribution device 2 from the conical cylinder 201 at the bottom of the water distribution device 2 under the action of pressure, the flow velocity of the fluid is gradually reduced, partial solid materials in the solid-liquid mixed fluid return to the tank body of the reaction kettle 1 through free settling under the action of vertical gravity to continue to react, and meanwhile, the material fluid flows in a circuitous way along a baffling channel formed by the baffles 202a and the inner wall of the cylinder 202 after encountering the baffles 202a which are arranged in the cylinder 202 at the upper part of the water distribution device 2 and staggered with each other, so that the flow path of the fluid is; on the other hand, by means of the disturbance effect of the baffle 202a on the flow state of the solid-liquid mixed fluid, the treated mother liquor is guided to the water outlet 202b and flows into the external circulating clarification device 3 through the feeding pipe 303, the mother liquor flows in a circuitous way along a baffling channel formed by the baffles 301 which are vertically staggered and the inner wall of the tank body in the clarification tank, so that a small amount of materials carried in the mother liquor are continuously settled and separated, and the completely clarified mother liquor is discharged from a discharge port 304 on the side surface of the clarification tank; after a certain amount of materials are deposited in the external clarifying tank, the materials are circularly pumped back into the reaction kettle 1 through the pump 4 to continue to react, so that the material loss is effectively reduced, and the material utilization rate is improved. And the whole device system can realize continuous full-automatic mother liquor separation and material recycling production by combining the existing control system.
Example 2
As shown in fig. 3, the structure of the ternary precursor synthesis device system for a lithium battery shown in this embodiment 2 is only that in the ternary precursor synthesis device system for a lithium battery disclosed in embodiment 1, the arrangement of a plurality of baffles 202a in the upper cylinder 202 of the water distribution device 2 is changed from the horizontal staggered arrangement to the vertical staggered arrangement, and the bottoms of the baffles are sealed to form a baffling channel, as shown in 203 in fig. 3, so that water flows in a vertically circuitous manner under the action of the baffles 202a, thereby performing a solid-liquid separation function.
Through detection, by using the novel lithium battery ternary precursor synthesizer system described in embodiment 1 and embodiment 2, the solid content of the synthesized ternary precursor produced in the reaction kettle 1 is increased to more than 20%, the particle size distribution of the prepared ternary precursor crystal particles is uniform, the crystallization maturity is high, the product yield reaches more than 99.4%, the solid particles carried by the finally discharged mother liquor is less than 0.1%, and the product yield can reach more than 98.5%.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A lithium battery ternary precursor synthesis device system is characterized by comprising a reaction kettle, a water distribution device and a circulating clarification device; wherein,
the reaction kettle is of a closed tank structure, and a stirring device is arranged inside the reaction kettle tank body in a matched manner and is used for fully mixing materials in the reaction kettle;
the water diversion device is of an inverted cone structure with a large upper part and a small lower part, and the bottom of the water diversion device is communicated with the inside of the reaction kettle tank body and is used for carrying out solid settlement and mother liquor separation treatment on a material mixed solution flowing out of the reaction kettle tank body;
the circulating clarification device is an external clarification tank, the top of the clarification tank is connected with a feed pipe, and the other end of the feed pipe is connected with a water outlet arranged on the side wall of the upper part of the water distribution device and used for carrying out secondary sedimentation separation treatment on the mother liquor separated from the water distribution device; a water outlet is formed in the side face of the upper part of the clarification tank and used for discharging the clarified mother liquor; the material outlet at the bottom of the clarification tank and the feed inlet at the top of the reaction kettle are connected with a return pipeline, and a pumping device is arranged on the return pipeline and used for pumping and returning the material deposited at the bottom of the clarification tank to the reaction kettle for recycling.
2. The lithium battery ternary precursor synthesis device system according to claim 1, wherein the water diversion device mainly comprises a lower conical cylinder and an upper cylindrical cylinder, and the bottom of a lower conical through of the water diversion device is communicated with the inside of the reaction kettle tank; a plurality of baffle plates which are arranged in a staggered mode are arranged in the cylinder at the upper portion of the water diversion device, and the baffle plates which are arranged in the staggered mode form a circuitous flow passage which is used for promoting separation of solid and liquid in feed liquid.
3. The lithium battery ternary precursor synthesis device system according to claim 1, wherein a plurality of staggered baffles are arranged inside the circulating clarification device, and the staggered baffles form a circuitous flow channel for promoting separation of solid and liquid in the feed liquid.
4. The lithium battery ternary precursor synthesis device system according to claim 3, wherein the number of the baffles is more than one.
5. The lithium battery ternary precursor synthesis device system according to claim 1, wherein the stirring device comprises a motor, a stirring shaft and stirring blades; the motor sets up at reation kettle cauldron body top, and the output of motor is connected with the upper end of (mixing) shaft, the lower extreme of (mixing) shaft stretches into reation kettle cauldron internal to be equipped with a plurality of stirring vane at the (mixing) shaft lower extreme.
6. The lithium battery ternary precursor synthesis device system according to claim 1 or 2, wherein the water diversion device is communicated with the side wall of the reaction kettle bottom.
7. The lithium battery ternary precursor synthesis device system according to claim 1, wherein the bottom of the reaction kettle is tapered.
8. The lithium battery ternary precursor synthesis device system according to claim 1 or 7, wherein a feed inlet is formed in the top of the reaction kettle, and a discharge outlet is formed in the bottom of the reaction kettle.
9. The lithium battery ternary precursor synthesis device system as claimed in claim 1, wherein a plastic layer is disposed on the inner wall surfaces of the reaction kettle, the water diversion device and the circulating clarification device.
10. The lithium battery ternary precursor synthesis device system according to claim 1, wherein the water diversion device and the circulation clarification device are both of closed structures.
CN201721902855.9U 2017-12-29 2017-12-29 A kind of lithium battery tertiary precursor synthesis apparatus system Active CN207856912U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109675513A (en) * 2018-12-26 2019-04-26 柳州申通汽车科技有限公司 A kind of preparation method of continous way narrow ditribution lithium battery ternary precursor
CN110586017A (en) * 2019-11-01 2019-12-20 常州市正元干燥工程有限公司 Purifier
CN112387236A (en) * 2020-11-19 2021-02-23 安徽国祯生态科技有限公司 Soil repairing agent granulator auxiliary assembly
CN112933730A (en) * 2021-01-28 2021-06-11 山东口天环保设备科技有限责任公司 Full-automatic sediment filtration chip cleaning device and method for numerical control machining center

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109675513A (en) * 2018-12-26 2019-04-26 柳州申通汽车科技有限公司 A kind of preparation method of continous way narrow ditribution lithium battery ternary precursor
CN110586017A (en) * 2019-11-01 2019-12-20 常州市正元干燥工程有限公司 Purifier
CN112387236A (en) * 2020-11-19 2021-02-23 安徽国祯生态科技有限公司 Soil repairing agent granulator auxiliary assembly
CN112933730A (en) * 2021-01-28 2021-06-11 山东口天环保设备科技有限责任公司 Full-automatic sediment filtration chip cleaning device and method for numerical control machining center

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