CN112316881A - Multistage reaction kettle - Google Patents
Multistage reaction kettle Download PDFInfo
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- CN112316881A CN112316881A CN202011574697.5A CN202011574697A CN112316881A CN 112316881 A CN112316881 A CN 112316881A CN 202011574697 A CN202011574697 A CN 202011574697A CN 112316881 A CN112316881 A CN 112316881A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
The invention relates to the technical field of reaction kettle design, and discloses a multistage reaction kettle which comprises N-stage kettle bodies sleeved from top to bottom and from inside to outside in sequence, wherein an overflow port is formed in the side wall of each stage kettle body close to the top cover of the kettle body, the end part of each stage kettle body provided with the overflow port is exposed as a non-sleeved end, and a material receiving port for receiving a material output from the overflow port of the last kettle body is formed in each stage kettle body from the second stage kettle body; each stage of kettle body is provided with a feeding hole. Through arranging the overflow ports on each stage of reaction kettle, continuous reaction is realized, and the yield can be greatly improved; meanwhile, a backflow pipeline is arranged between the last-stage kettle body and the first-stage kettle body, so that the particle size distribution of the product can be effectively regulated and controlled; for the preparation of the ternary precursor, the single kettle is enabled to continuously synthesize the narrowly distributed ternary precursor with the same component or different components in the core-shell structure, the particle size distribution of the ternary precursor is effectively improved, the micro powder in the product is reduced, the utilization rate of small particle waste in a reaction system is improved, the production cost is saved, and the product performance is optimized.
Description
Technical Field
The invention relates to the technical field of reaction kettle design, in particular to a multistage reaction kettle.
Background
With the rapid development of the lithium ion battery industry, the requirement for the performance of the precursor of the ternary cathode material in the industry is higher and higher. With the continuous improvement of the energy density requirement of the vehicle-mounted lithium ion power battery, the nickel-cobalt-manganese ternary cathode material is continuously developed towards the directions of high nickel content, high voltage, high compaction density and high safety. The nickel-cobalt-manganese ternary precursor is important for the production of the ternary cathode material, and the quality of the ternary precursor directly determines the performance exertion of the ternary cathode material. The high-performance nickel-cobalt-manganese ternary precursor is a basis for producing a ternary cathode material for a lithium ion power battery, and the synthesis process for preparing the high-performance nickel-cobalt-manganese ternary precursor is a key point.
At present, the main domestic methods for synthesizing the ternary cathode material precursor mainly comprise a batch method synthesis process and a single-kettle continuous synthesis process. Wherein, although the productivity of the single-kettle continuous synthesis process is higher than that of the batch synthesis process, the particle size distribution of the single-kettle continuous synthesis process is wider than that of the batch synthesis process. The industry provides a novel multi-kettle series continuous synthesis process, successfully improves the particle size distribution of the product, and synthesizes the ternary cathode material precursor with better sphericity and less micro powder. However, the multi-kettle series synthesis process needs to use a plurality of reaction kettles at the same time, which causes resource waste and is not beneficial to improving the production efficiency.
The patent with publication number CN205084734U discloses a two-stage reaction kettle, which is suitable for staged reaction, simple in structure, convenient to manufacture, and low in cost, but only one bottom discharge port is reserved in the two-stage reaction kettle, which is still a rotary kettle reaction essentially, the production efficiency still cannot be substantially improved, and the number of stages is small, and the two-stage reaction kettle is not suitable for the production of products with product granularity increased by more stages of reactions.
Disclosure of Invention
The invention solves the technical problem of overcoming the defects of the prior art and provides a multistage reaction kettle which can realize continuous reaction and select the stage number of the reaction kettle according to actual requirements.
The purpose of the invention is realized by the following technical scheme:
a multi-stage reaction kettle comprises N-stage kettle bodies which are sequentially sleeved from top to bottom and from inside to outside, wherein an overflow port is formed in the side wall of each stage of kettle body close to the top cover of the kettle body, the end part of each stage of kettle body provided with the overflow port is exposed as a non-sleeved end, and a material receiving port for receiving materials output from the overflow port of the last kettle body is formed in each stage of kettle body from the second stage of kettle body; each stage of kettle body is provided with a feeding hole.
Further, still include the agitating unit who stirs respectively to each internal material of cauldron, agitating unit includes (mixing) shaft and stirring rake.
Furthermore, all the kettle bodies share one stirring device, the stirring shaft penetrates through the bottom of each kettle body, and the stirring paddles are arranged on shaft sections of the stirring shaft in the space of each kettle body.
And furthermore, the stirring paddle is arranged close to the bottom of the kettle body.
Furthermore, the feed inlet and the overflow outlet of each kettle body are respectively arranged on the different sides of the stirring shaft.
Further, a discharging port is arranged at the bottom of each kettle body or close to the bottom.
Furthermore, the discharge port and the overflow port of each kettle body are respectively arranged on the opposite sides of the stirring shaft.
Furthermore, a return pipeline is arranged between the Nth-stage kettle body and the first-stage kettle body.
Compared with the prior art, the invention has the following beneficial effects:
through arranging the overflow ports on each stage of reaction kettle, continuous reaction is realized, and the yield can be greatly improved; meanwhile, a backflow pipeline is arranged between the last-stage kettle body and the first-stage kettle body, so that the particle size distribution of the product can be effectively regulated and controlled; for the preparation of the ternary precursor, the single kettle is enabled to continuously synthesize the narrowly distributed ternary precursor with the same component or different components in the core-shell structure, the particle size distribution of the ternary precursor is effectively improved, the micro powder in the product is reduced, the utilization rate of small particle waste in a reaction system is improved, the production cost is saved, and the product performance is optimized.
Drawings
FIG. 1 is a schematic structural view of a multistage reaction vessel described in example 1.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the drawings are provided for illustrative purposes only and are not intended to be limiting; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
Example 1
A multistage reaction kettle for preparing a narrow-distribution ternary precursor takes three stages as an example, as shown in figure 1, the multistage reaction kettle comprises three kettle bodies which are sequentially sleeved from top to bottom and from inside to outside, an overflow port 2 is formed in the side wall of each stage of kettle body close to the top cover of the kettle body, the end part of each stage of kettle body provided with the overflow port is exposed outside as a non-sleeved end, namely, the part below an overflow port 11 of the first stage of kettle body is embedded in a second stage of kettle body 12, and the part below an overflow port 12 of the second stage of kettle body is embedded in a third stage of kettle body 13 when viewed from inside to outside. A material receiving port 3 for receiving the material output from the overflow port 2 of the last kettle body is arranged on each kettle body from the second-stage kettle body 12, and the overflow ports 2 and the material receiving ports 3 between two adjacent kettle bodies are communicated through overflow pipelines 4; each stage of kettle body is provided with a feeding hole 5, the feeding holes are generally arranged at the edge of the top cover of the kettle body, the number of the feeding holes of each stage of kettle body can be determined according to the number of reaction media, and one or more feeding holes can be used.
In order to accelerate the reaction of the materials in each kettle body, the multistage reaction kettle is also provided with a stirring device for stirring the materials in each kettle body respectively, and the stirring device comprises a stirring shaft 61, a stirring paddle 62 and a driving mechanism 63 for controlling the rotation of the stirring shaft. For simplifying multistage reation kettle's overall structure, also for promoting production efficiency simultaneously, the three cauldron bodies of the reation kettle of this embodiment share a agitating unit, and wherein (mixing) shaft 61 runs through each cauldron body bottom surface, and each cauldron body is arranged the bearing seal in (mixing) shaft run-through position department, and stirring rake 62 sets up on the shaft section that (mixing) shaft 61 is located each cauldron internal space, and the preferred setting that is close to cauldron body bottom of stirring rake.
The feed inlet 5 and the overflow outlet 2 of each kettle body are respectively arranged at the opposite sides of the stirring shaft 61 so as to ensure that the overflowing or discharging materials are fully reacted and stirred.
In addition, each cauldron body has still seted up drain hole 7 on the bottom lateral wall to discharge residual material when the reaction is close to finishing, wherein the drain hole 7 and the overflow mouth 2 of each cauldron body also set up respectively in the (mixing) shaft 61 heteropleural.
In the reaction kettle of the embodiment, a reflux device (not shown) for guiding relevant materials to the first-stage kettle body 11 is further arranged on the third-stage kettle body 13, the two kettle bodies are communicated through a reflux pipeline of the reflux device, a feed inlet of the reflux device is arranged at any position, close to the bottom, on the side wall of the third-stage kettle body 13, and a pump, a flow regulating valve, a flowmeter and other elements are arranged on the reflux pipeline, so that the relevant materials can smoothly reflux and the reflux condition can be monitored; the backflow pipeline is a detachable pipeline, and the backflow device determines whether to start or not according to the actual production requirement; the reflux device is arranged to ensure that the material flows back according to a certain flow, so that the distribution of the reaction particle size of the produced product can be effectively adjusted.
The process for preparing the ternary precursor by using the multistage reaction kettle is described as follows: before preparation, reaction media are respectively introduced into the three kettles through the feed inlets, parameters such as pH and ammonia concentration in each kettle are set, the rotating speed of the stirring shaft is set, then the nickel-cobalt-manganese salt with the prepared proportion is introduced into the first-stage kettle body 11, the first-stage kettle body 11 is set to be in a high-pH reaction condition, the method is characterized in that only nucleation and no growth are carried out in the first-stage kettle body, when the liquid level in the first-stage kettle body 11 is high, the nuclei overflow to the second-stage kettle body 12, in the second-stage kettle body, particles only carry out primary growth and nucleation is avoided, the second-stage kettle body 12 can obtain a ternary precursor intermediate product with the same or different component core-shell structure by regulating and controlling the proportion of introduced salt, when the liquid level in the second-stage kettle body 12 is high, the ternary precursor intermediate product overflows to the third-stage kettle body 13, in the third-stage kettle body, the particles optimally grow, and similarly, the ternary precursor with the same or different components can be obtained by regulating and controlling the proportion of introduced salt; after the materials reach the third-stage kettle body, if the reaction particle size distribution needs to be adjusted, the materials of the third-stage kettle body flow back through the reflux device to enter the first-stage kettle body, and the operation is repeated.
If more stages of reaction are needed, reaction kettles with more stages are selected for reaction, and finally precursor particles reaching the Nth-stage kettle body overflow to the aging kettle to form a final product. When the reaction in the reaction kettle is close to termination, the discharge ports of the kettle bodies at all levels are opened in sequence, and the residual materials are discharged.
Aiming at the preparation of the ternary precursor, the overflow ports of the kettle bodies at all levels are newly added, so that continuous reaction can be realized, the preparation of the narrowly distributed ternary precursor with the same or different core-shell structures becomes possible, the operation is simpler and more convenient, and the yield is greatly improved; according to the concept that the higher the grade number is, the narrower the product particle size distribution is, when the grade number of the reaction kettle is less, the reflux device is arranged on the kettle body of the last grade, so that the particle size distribution of the product can be effectively regulated and controlled; in general, the multistage reaction kettle can improve the particle size distribution of the ternary precursor, reduce micro powder in the product, improve the utilization rate of small particle waste in a reaction system, obviously save the production cost and optimize the product performance. The number of reaction kettle stages can be selected according to actual requirements during actual production.
It should be understood that the above examples are only for clearly illustrating the technical solutions of the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A multi-stage reaction kettle is characterized by comprising N stages of kettle bodies which are sequentially sleeved from top to bottom and from inside to outside, wherein an overflow port is formed in the side wall of each stage of kettle body close to the top cover of the kettle body, the end part of each stage of kettle body provided with the overflow port is exposed as a non-sleeved end, and a material receiving port for receiving materials output from the overflow port of the last kettle body is formed in each stage of kettle body from the second stage of kettle body; each stage of kettle body is provided with a feeding hole.
2. The multi-stage reaction kettle according to claim 1, further comprising a stirring device for stirring the materials in each kettle body, wherein the stirring device comprises a stirring shaft and a stirring paddle.
3. The multi-stage reaction kettle of claim 2, wherein all kettle bodies share one stirring device, the stirring shaft penetrates through the bottom of each kettle body, and the stirring paddle is arranged on the shaft section of the stirring shaft in each kettle body space.
4. The multi-stage reactor of claim 3, wherein the paddles are disposed proximate the bottom of the body.
5. The multistage reaction kettle of claim 2, 3 or 4, wherein the feed inlet and the overflow outlet of each kettle body are respectively arranged at the opposite sides of the stirring shaft.
6. The multi-stage reaction kettle according to claim 1, wherein a discharge port is arranged at or near the bottom of each kettle body.
7. The multistage reaction kettle of claim 6, wherein the discharge port and the overflow port of each kettle body are respectively arranged on the opposite sides of the stirring shaft.
8. The multistage reaction kettle of claim 1, wherein a return pipeline is further arranged between the Nth stage kettle body and the first stage kettle body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011574697.5A CN112316881A (en) | 2020-12-28 | 2020-12-28 | Multistage reaction kettle |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011574697.5A CN112316881A (en) | 2020-12-28 | 2020-12-28 | Multistage reaction kettle |
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| CN112316881A true CN112316881A (en) | 2021-02-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522209A (en) * | 2021-07-02 | 2021-10-22 | 中冶瑞木新能源科技有限公司 | Synthesis equipment for producing narrow-particle-size ternary precursor by continuous method |
| CN113694873A (en) * | 2021-09-14 | 2021-11-26 | 朱枫 | Production and processing equipment and process of polyurethane waterproof coating |
Citations (7)
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| EP1015123A1 (en) * | 1997-09-19 | 2000-07-05 | Valmet Corporation | Apparatus for cleaning a suspension, preferably a fiber mass suspension |
| CN205084734U (en) * | 2015-08-31 | 2016-03-16 | 宣城市聚源精细化工有限公司 | Second order reaction cauldron |
| CN207169687U (en) * | 2017-06-06 | 2018-04-03 | 陕西科技大学 | A kind of high efficient gas and liquid reaction kettle device based on multistage venturi mixer |
| CN107986338A (en) * | 2017-11-23 | 2018-05-04 | 清远佳致新材料研究院有限公司 | The process units and its technique of a kind of nickel-cobalt-manganese ternary hydroxide |
| CN209271412U (en) * | 2018-11-05 | 2019-08-20 | 山东润博生物科技有限公司 | A kind of two phase flow reaction system |
| WO2019173893A1 (en) * | 2018-03-12 | 2019-09-19 | Xianggen Wu | A bioreactor comprising an internal resonant vibratory motor for agitation of biodegradable waste comprising horizontal and diagonal extension springs |
| CN111330523A (en) * | 2020-03-07 | 2020-06-26 | 宋青 | Synthetic reation kettle of resin |
-
2020
- 2020-12-28 CN CN202011574697.5A patent/CN112316881A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1015123A1 (en) * | 1997-09-19 | 2000-07-05 | Valmet Corporation | Apparatus for cleaning a suspension, preferably a fiber mass suspension |
| CN205084734U (en) * | 2015-08-31 | 2016-03-16 | 宣城市聚源精细化工有限公司 | Second order reaction cauldron |
| CN207169687U (en) * | 2017-06-06 | 2018-04-03 | 陕西科技大学 | A kind of high efficient gas and liquid reaction kettle device based on multistage venturi mixer |
| CN107986338A (en) * | 2017-11-23 | 2018-05-04 | 清远佳致新材料研究院有限公司 | The process units and its technique of a kind of nickel-cobalt-manganese ternary hydroxide |
| WO2019173893A1 (en) * | 2018-03-12 | 2019-09-19 | Xianggen Wu | A bioreactor comprising an internal resonant vibratory motor for agitation of biodegradable waste comprising horizontal and diagonal extension springs |
| CN209271412U (en) * | 2018-11-05 | 2019-08-20 | 山东润博生物科技有限公司 | A kind of two phase flow reaction system |
| CN111330523A (en) * | 2020-03-07 | 2020-06-26 | 宋青 | Synthetic reation kettle of resin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113522209A (en) * | 2021-07-02 | 2021-10-22 | 中冶瑞木新能源科技有限公司 | Synthesis equipment for producing narrow-particle-size ternary precursor by continuous method |
| CN113694873A (en) * | 2021-09-14 | 2021-11-26 | 朱枫 | Production and processing equipment and process of polyurethane waterproof coating |
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Application publication date: 20210205 |