CN207507478U - A kind of preparation facilities of ternary precursor - Google Patents
A kind of preparation facilities of ternary precursor Download PDFInfo
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- CN207507478U CN207507478U CN201721517444.8U CN201721517444U CN207507478U CN 207507478 U CN207507478 U CN 207507478U CN 201721517444 U CN201721517444 U CN 201721517444U CN 207507478 U CN207507478 U CN 207507478U
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Abstract
本实用新型涉及一种三元前驱体的制备装置,包括反应釜体和与其配合的反应釜盖,所述反应釜体连通有两根液碱进液管和一根金属盐进液管,其中一根液碱进液管的出液口高于另一根液碱进液管的出液口;在所述反应釜体内贴近反应釜盖处和反应釜体的溢流口处均设置有液位传感器,所述溢流口安装有溢流阀,所述液位传感器的信号传送至控制器,控制器根据信号控制所述溢流阀的开启与关闭。本实用新型采用一高一低两根液碱进液管,其中一根液碱进液管主要负责调节整个体系的pH值,另一根液碱进液管主要负责与氨水和金属盐的直接合成反应,达到明显减少晶核的目的。
The utility model relates to a preparation device for a ternary precursor, comprising a reactor body and a reactor cover matched with it, and the reactor body is connected with two liquid alkali inlet pipes and a metal salt inlet pipe, wherein The liquid outlet of one liquid alkali inlet pipe is higher than the liquid outlet of the other liquid alkali inlet pipe; in the reactor body close to the reactor lid and the overflow port of the reactor body, there are liquid A level sensor, the overflow port is equipped with an overflow valve, the signal of the liquid level sensor is sent to the controller, and the controller controls the opening and closing of the overflow valve according to the signal. The utility model adopts two liquid alkali inlet pipes, one high and one low, one of which is mainly responsible for adjusting the pH value of the whole system, and the other liquid alkali inlet pipe is mainly responsible for direct contact with ammonia water and metal salts. Synthesis reaction, to achieve the purpose of significantly reducing crystal nuclei.
Description
技术领域technical field
本实用新型涉及三元前驱体的制备装置。The utility model relates to a preparation device of a ternary precursor.
背景技术Background technique
镍钴锰三元材料广泛应用于数码电子产品、电动工具、电动自行车等的锂离子电池上。目前镍钴锰三元前躯体的生产方法主要采用金属盐、液碱、氨水同时加入反应釜体中制备生成。在连续法制备过程中,由于边进液边出料,使得物料在反应釜体内的停留时间各不相同,从而产生了最终产品的大小颗粒的正态分布。但在后续烧结过程中,晶核(也叫极小颗粒)容易出现过烧,因而是正极材料厂商所不愿意看到的。前躯体厂商一般采用过滤时滤布穿滤或者烘干时抽风分离掉部分晶核,虽能满足正极材料厂商的要求(D0>3μm),但这样必然会导致物料损失,收率下降,从而造成成本上升,这也是目前不得已的主流方法。Nickel-cobalt-manganese ternary materials are widely used in lithium-ion batteries of digital electronic products, electric tools, electric bicycles, etc. At present, the production method of nickel-cobalt-manganese ternary precursor is mainly prepared by adding metal salt, liquid caustic soda and ammonia water into the reactor body at the same time. In the process of continuous preparation, due to the liquid feeding and discharging, the residence time of the materials in the reactor body varies, resulting in a normal distribution of the size of the final product. However, in the subsequent sintering process, the crystal nuclei (also called extremely small particles) are prone to overburning, which is what the cathode material manufacturers do not want to see. Precursor manufacturers generally use filter cloth to filter through or dry to separate part of the crystal nuclei. Although it can meet the requirements of cathode material manufacturers (D0>3μm), this will inevitably lead to material loss and yield decline, resulting in This is also the mainstream method of last resort.
实用新型内容Utility model content
针对上述问题,本实用新型提供一种可在制备过程中减少晶核的三元前驱体的制备装置。In view of the above problems, the utility model provides a preparation device for a ternary precursor that can reduce crystal nuclei during the preparation process.
本实用新型解决上述技术问题所采用的技术方案为:一种三元前驱体的制备装置,包括反应釜体和与其配合的反应釜盖,所述反应釜体连通有两根液碱进液管和一根金属盐进液管,其中一根液碱进液管的出液口高于另一根液碱进液管的出液口;在所述反应釜体内贴近反应釜盖处和反应釜体的溢流口处均设置有液位传感器,所述溢流口安装有溢流阀,所述液位传感器的信号传送至控制器,控制器根据信号控制所述溢流阀的开启与关闭。The technical scheme adopted by the utility model to solve the above-mentioned technical problems is: a preparation device of a ternary precursor, including a reactor body and a reactor cover matched with it, and the reactor body is connected with two liquid alkali inlet pipes and a metal salt liquid inlet pipe, wherein the liquid outlet of one liquid alkali liquid inlet pipe is higher than the liquid outlet of another liquid alkali liquid inlet pipe; The overflow port of the body is equipped with a liquid level sensor, and the overflow port is equipped with an overflow valve. The signal of the liquid level sensor is transmitted to the controller, and the controller controls the opening and closing of the overflow valve according to the signal. .
作为优选,所述反应釜体内设置有上下两层搅拌浆,所述其中一根液碱进液管的出液口靠近上层搅拌浆,另一根液碱进液管的出液口靠近下层搅拌桨。As a preference, the reactor body is provided with upper and lower two layers of stirring blades, the liquid outlet of one of the liquid alkali inlet pipes is close to the upper stirring blade, and the liquid outlet of the other liquid alkali inlet pipe is close to the lower stirring blade. paddle.
作为优选,所述另一根液碱进液管的出液口和金属盐进液管的出液口平齐。As a preference, the liquid outlet of the other liquid caustic soda inlet pipe is flush with the liquid outlet of the metal salt liquid inlet pipe.
作为优选,所述反应釜体还连通有氨水进液管。Preferably, the reactor body is also connected with an ammonia water inlet pipe.
作为优选,当反应釜盖处的液位传感器感应到反应液时,该传感器将信号传送至控制器控制溢流阀开启;当溢流口处的液位传感器没有感应到反应液时,该传感器将信号传送至控制器控制溢流阀关闭。As preferably, when the liquid level sensor at the reaction kettle cover senses the reaction liquid, the sensor sends a signal to the controller to control the overflow valve to open; when the liquid level sensor at the overflow port does not sense the reaction liquid, the sensor Send a signal to the controller to control the overflow valve to close.
从以上技术方案可知,本实用新型采用一高一低两根液碱进液管,其中一根液碱进液管主要负责调节整个体系的pH值,另一根液碱进液管主要负责与氨水和金属盐的直接合成反应,由于直接参与反应的液碱量减少,局部pH变低,一旦形成了新的晶核,都会以比原来明显更快地速度迅速长大,从而达到明显减少晶核的目的。It can be seen from the above technical scheme that the utility model adopts two liquid alkali inlet pipes, one high and one low, one of which is mainly responsible for adjusting the pH value of the whole system, and the other liquid alkali inlet pipe is mainly responsible for adjusting the pH value of the whole system. In the direct synthesis reaction of ammonia water and metal salts, due to the decrease in the amount of liquid alkali directly participating in the reaction, the local pH becomes lower. Once new crystal nuclei are formed, they will grow rapidly at a significantly faster rate than before, thereby achieving a significant reduction in crystal nuclei. nuclear purpose.
附图说明Description of drawings
图1是本实用新型一种优选方式的结构示意图。Fig. 1 is a structural schematic diagram of a preferred mode of the utility model.
具体实施方式Detailed ways
下面将结合图1详细说明本实用新型,在此本实用新型的示意性实施例以及说明用来解释本实用新型,但并不作为对本实用新型的限定。The utility model will be described in detail below in conjunction with FIG. 1 . Here, the schematic embodiment and description of the utility model are used to explain the utility model, but not as a limitation to the utility model.
本实用新型解决上述技术问题所采用的技术方案为:一种三元前驱体的制备装置,包括反应釜体1和与其配合的反应釜盖6,所述反应釜体连通有两根液碱进液管2和一根金属盐进液管3,两根液碱进液管可向反应釜体内通入液碱,金属盐进液管可向反应釜体内通入金属盐;其中一根液碱进液管的出液口高于另一根液碱进液管的出液口,从其中一根液碱进液管流入反应釜体内的液碱可调节整个反应体系的pH值,从另一根液碱进液管流入反应釜体内的液碱可与氨水和金属盐直接进行合成反应,实现镍钴锰三元前驱体的制备。The technical scheme adopted by the utility model to solve the above-mentioned technical problems is: a preparation device of a ternary precursor, comprising a reactor body 1 and a reactor cover 6 matched therewith, and the reactor body is connected with two liquid caustic inlets Liquid pipe 2 and a metal salt liquid inlet pipe 3, two liquid alkali liquid inlet pipes can pass into liquid alkali in the reactor body, and metal salt liquid inlet pipes can pass into metal salt in the reactor body; one of the liquid alkali The liquid outlet of the liquid inlet pipe is higher than the liquid outlet of another liquid alkali inlet pipe, and the liquid alkali that flows into the reactor body from one of the liquid alkali inlet pipes can adjust the pH value of the whole reaction system, and the other The liquid caustic soda that flows into the reaction kettle through the root liquid caustic inlet pipe can directly carry out a synthetic reaction with ammonia water and metal salts to realize the preparation of nickel-cobalt-manganese ternary precursors.
本实用新型在所述反应釜体内贴近反应釜盖处和反应釜体的溢流口7处均设置有液位传感器8,所述溢流口安装有溢流阀9,所述液位传感器的信号传送至控制器10,控制器根据信号控制所述溢流阀的开启与关闭。具体来说,当反应釜盖处的液位传感器感应到反应液时,该传感器将信号传送至控制器控制溢流阀开启;当溢流口处的液位传感器没有感应到反应液时,该传感器将信号传送至控制器控制溢流阀关闭。本实用新型将溢流阀门由常开状态调整为间歇开启状态。由于溢流口距反应釜盖还有一段距离,关闭溢流口并不会马上导致反应釜冒槽。关闭溢流口,延长小颗粒在反应釜的停留时间,待反应釜液位上升至接近反应釜盖时,开启溢流阀直至釜内液位与溢流阀平齐,此时再关闭溢流阀,如此循环进行。由于小颗粒在反应釜内的平均停留时间得到了显著延长,这将大大降低最终产品中小颗粒的数量。The utility model is provided with a liquid level sensor 8 at the place close to the reactor cover and the overflow port 7 of the reactor body in the reactor body, and an overflow valve 9 is installed at the overflow port, and the liquid level sensor The signal is sent to the controller 10, and the controller controls the opening and closing of the overflow valve according to the signal. Specifically, when the liquid level sensor at the cover of the reaction kettle senses the reaction liquid, the sensor sends a signal to the controller to control the overflow valve to open; when the liquid level sensor at the overflow port does not sense the reaction liquid, the The sensor sends a signal to the controller to control the overflow valve to close. The utility model adjusts the overflow valve from a normally open state to an intermittently open state. Since the overflow port is still some distance away from the reactor cover, closing the overflow port will not immediately cause the reactor tank to leak. Close the overflow port to prolong the residence time of small particles in the reactor. When the liquid level of the reactor rises to close to the lid of the reactor, open the overflow valve until the liquid level in the reactor is equal to the overflow valve, and then close the overflow valve, and so on. This significantly reduces the number of small particles in the final product, since the average residence time of the small particles in the reactor is significantly increased.
作为优选,所述反应釜体内设置有上下两层搅拌浆4,对反应溶液进行搅拌,所述其中一根液碱进液管的出液口靠近上层搅拌浆,另一根液碱进液管的出液口靠近下层搅拌桨,使得溶液更加均匀;所述另一根液碱进液管的出液口和金属盐进液管的出液口平齐,可保证反应在反应釜体下部快速进行。本实用新型的所述反应釜体还连通有氨水进液管5,通过氨水进液管可向反应釜体内通入氨水。As preferably, the upper and lower layers of stirring paddles 4 are arranged in the reactor body to stir the reaction solution. The liquid outlet of one of the liquid alkali inlet pipes is close to the upper stirring blade, and the other liquid alkali inlet pipe The liquid outlet of the liquid alkali inlet pipe is close to the lower stirring paddle, so that the solution is more uniform; the liquid outlet of the other liquid alkali inlet pipe is flush with the liquid outlet of the metal salt liquid inlet pipe, which can ensure the rapid reaction in the lower part of the reaction kettle body. conduct. The reactor body of the utility model is also connected with an ammonia water inlet pipe 5, and ammonia water can be passed into the reactor body through the ammonia water inlet pipe.
本实用新型采用四根进液管,可实现液碱、金属盐、氨水的同时输送,提高生产效率,同时利用了高低的两根液碱进液管,不仅可明显减少反应过程中的晶核,还可使合成过程D0至少大于1.5μm,再经过后续的陈化工艺,可以让D0提高到3μm以上。The utility model adopts four liquid inlet pipes, which can realize the simultaneous transportation of liquid alkali, metal salt and ammonia water, and improve production efficiency. At the same time, the utility model utilizes two liquid alkali liquid inlet pipes with high and low heights, which can not only significantly reduce the crystal nuclei in the reaction process , can also make the synthesis process D0 greater than 1.5 μm at least, and then through the subsequent aging process, D0 can be increased to more than 3 μm.
以上对本实用新型实施例所提供的技术方案进行了详细介绍,本文中应用了具体个例对本实用新型实施例的原理以及实施方式进行了阐述,以上实施例的说明只适用于帮助理解本实用新型实施例的原理;同时,对于本领域的一般技术人员,依据本实用新型实施例,在具体实施方式以及应用范围上均会有改变之处,综上所述,本说明书内容不应理解为对本实用新型的限制。The technical solutions provided by the embodiments of the present invention have been introduced in detail above. In this paper, specific examples have been used to illustrate the principles and implementation methods of the embodiments of the present invention. The descriptions of the above embodiments are only applicable to help understand the present invention. The principle of the embodiment; at the same time, for those of ordinary skill in the art, according to the embodiment of the present invention, there will be changes in the specific implementation and the scope of application. Utility model restrictions.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336192A (en) * | 2018-10-11 | 2019-02-15 | 新乡天力锂能股份有限公司 | A kind of lithium ion battery cathode material precursor and ultrasonic vibration reactor and method for preparing the precursor |
| CN109354077A (en) * | 2018-10-16 | 2019-02-19 | 中伟新材料有限公司 | A kind of polycrystalline ternary precursor and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336192A (en) * | 2018-10-11 | 2019-02-15 | 新乡天力锂能股份有限公司 | A kind of lithium ion battery cathode material precursor and ultrasonic vibration reactor and method for preparing the precursor |
| CN109336192B (en) * | 2018-10-11 | 2021-06-25 | 新乡天力锂能股份有限公司 | An Ultrasonic Oscillation Reactor for Preparing Lithium-ion Battery Cathode Material Precursor |
| CN109354077A (en) * | 2018-10-16 | 2019-02-19 | 中伟新材料有限公司 | A kind of polycrystalline ternary precursor and preparation method thereof |
| CN109354077B (en) * | 2018-10-16 | 2021-05-07 | 中伟新材料股份有限公司 | A kind of polycrystalline ternary precursor and preparation method thereof |
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