Preparation method of high-nickel ternary precursor

文档序号:1650717 发布日期:2019-12-24 浏览:32次 中文

阅读说明:本技术 一种高镍三元前驱体的制备方法 (Preparation method of high-nickel ternary precursor ) 是由 刘奇 于 2019-09-25 设计创作,主要内容包括:本发明涉公开了一种高镍三元前驱体的制备方法,其包括配制一定浓度的金属盐溶液、液碱、氨水溶液;将上述加入反应釜中反应,高镍前驱体在合成过程中由于一次粒子偏小,结晶过程中由于颗粒的碰撞容易发生开裂现象,造成正极材料循环性能的恶化,传统方式采用缩短反应停留时间来解决开裂现象。本发明采用有机絮凝剂添加的方式,通过形成絮凝形成的网状保护结构,在颗粒之间形成保护网,金属离子可顺利通过保护网,而颗粒与颗粒之间的碰撞由之前的刚性碰撞转变为柔性碰撞,从而杜绝颗粒开裂现象,从而提高正极材料的颗粒完整度,显著改善电池循环性能。(The invention discloses a preparation method of a high-nickel ternary precursor, which comprises the steps of preparing a metal salt solution with a certain concentration, liquid caustic soda and an ammonia water solution; the high nickel precursor is added into a reaction kettle for reaction, the high nickel precursor is easy to crack due to the collision of particles in the crystallization process because primary particles are smaller, so that the cycle performance of the anode material is deteriorated, and the cracking phenomenon is solved by shortening the reaction retention time in the traditional mode. According to the invention, the organic flocculant is added, a mesh-shaped protection structure formed by flocculation is formed, the protection net is formed among particles, metal ions can smoothly pass through the protection net, and the collision between the particles is changed from rigid collision to flexible collision, so that the particle cracking phenomenon is avoided, the particle integrity of the anode material is improved, and the cycle performance of the battery is obviously improved.)

1. A preparation method of a high-nickel ternary precursor is characterized by comprising the following steps:

s1, preparing a metal salt solution, liquid caustic soda, an ammonia water solution and a PAM flocculating agent with certain concentration;

s2 enabling the metal salt solution, the liquid caustic soda, the ammonia water solution and the PAM flocculating agent to flow into the reaction kettle in parallel through the liquid inlet pipe;

s3 circularly linking the material in the ripening tank with the material in the reaction kettle, and conveying the material in the ripening tank to a filter pressing buffer tank when the liquid level in the ripening tank rises to a certain liquid level;

and S4, washing and drying the aged reactant to obtain the nickel-cobalt-manganese ternary precursor.

2. The method for preparing the high-nickel ternary precursor according to claim 1, wherein the concentration of the ammonia water solution is 12-25g/L, and the pH in the reaction kettle is controlled to be 10-12.

3. The method for preparing the high-nickel ternary precursor according to claim 1, wherein the feed flow ratio of the flocculating agent to the metal salt solution is controlled to be 1: 20.

4. the preparation method of the high-nickel ternary precursor according to claim 1, characterized by introducing inert gas with a stable flow into the reaction kettle for atmosphere protection, starting stirring paddles inside the reaction kettle for stirring, wherein the stirring paddles are axial flow paddles with an upper layer and a middle layer, the lower layer is a turbine blade, and controlling the stirring speed of the stirring paddles to be 50-200 r/min.

5. The method for preparing the high-nickel ternary precursor according to claim 4, wherein an outlet for delivering the metal salt solution and the PAM flocculant is positioned obliquely above the third layer of the blades, and a liquid inlet pipe for delivering the liquid caustic soda solution and the aqueous ammonia solution is positioned right opposite to the outlet for delivering the metal salt solution and the PAM flocculant.

6. The method for preparing the high-nickel ternary precursor according to claim 1, wherein the temperature of the reaction kettle is controlled to be 40-80 ℃ during the reaction in the reaction kettle, and the average residence time of the materials in the reaction kettle is 10-25 hours.

7. The method for preparing a high-nickel ternary precursor as claimed in claim 1, wherein the aging time is 60-180min, the washing time is 60-200min, and the drying time is 4-6 hours.

8. The method for preparing the high-nickel ternary precursor according to claim 1, wherein radar liquid level sensors are arranged at the upper head in the reaction kettle and the upper head of the ripening tank, an overflow valve is arranged at the overflow port, when the liquid level of the ripening tank reaches a first set value, a ripening tank bottom valve and a slurry return pump are automatically opened, when the liquid level of the ripening tank reaches a second set value, the slurry return pump is opened, an automatic valve of the buffer tank is subjected to filter pressing, and when the first liquid level set value is reached, the automatic valve is closed, so that the continuous and automatic control of the reaction is realized.

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