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Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate

A hydroxide and carbonate technology, applied in the preparation of carbonate/acid carbonate, oxygen/ozone/oxide/hydroxide, nickel oxide/nickel hydroxide, etc., can solve pipeline blockage , unsatisfactory, low solubility and other problems, to achieve the effect of solving pipeline blockage, improving tap density and good sphericity

Active Publication Date: 2017-02-15
TIANJIN B&M SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the nickel sulfate ammonium and cobalt ammonia sulfate produced by combining ammonia with nickel sulfate and cobalt sulfate have low solubility, and it is easy to precipitate and block the pipeline after adding ammonia
Although raising the temperature of the solution can improve the solubility of nickel ammonium sulfate and cobalt ammonium sulfate, it will still cause a certain degree of blockage in the pipeline, which cannot meet the needs of actual production.
Therefore, this pre-complexation process has not been widely promoted in actual production.

Method used

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  • Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate
  • Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate
  • Preparation method of mono-/multi-metal coprecipitation hydroxide or carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In the nickel sulfate solution that concentration is 0.1mol / L, add urea in the ratio of 3g / L, at this moment, urea and metal Ni in the solution 2+ The substance mass ratio is 0.5:1. The precipitation agent is sodium hydroxide with a concentration of 6mol / L, and the complexing agent is ammonia water with a concentration of 20wt%. Add deionized water to the reactor in advance until the bottom paddle is submerged, then add ammonia water to adjust the pH value to 10.5-11.0, and then raise the temperature in the reactor to 60-70°C. With the silicone rubber tube with an inner diameter of 10mm as the delivery pipeline, the nickel sulfate solution is pumped into the reaction kettle at a speed of 5ml / min, and the length of the pipeline entering the water bath is adjusted to be 6.5cm. The residence time of the nickel sulfate solution in the water bath is The time is 1min. Ammonia is pumped into the reaction kettle simultaneously at a speed of 2.8ml / min (ammonia is divided into ...

Embodiment 2

[0034] In the nickel-manganese sulfate solution that concentration is 1mol / L, add urea by the ratio of every liter 6g, Ni / Mn=1 in the solution, at this moment, the amount of urea in the solution is equal to that of metal Ni 2+ with Mn 2+ The total mass ratio of the substance is 2:1. The precipitation agent is sodium hydroxide with a concentration of 4mol / L, and the complexing agent is ammonia water with a concentration of 20wt%. Add deionized water to the reactor in advance until the bottom paddle is submerged, then add ammonia water to adjust the pH value to 10.5-11.0, and then raise the temperature in the reactor to 60-70°C. With a silicone rubber tube with an inner diameter of 10mm as the delivery pipeline, the salt solution is pumped into the reaction kettle at a speed of 50ml / min, and the length of the pipeline entering the water bath is adjusted to 200cm, and the residence time of the salt solution in the water bath is 3.1 min. Ammonia water is pumped into the reactio...

Embodiment 3

[0036] In the nickel-cobalt-manganese sulfate solution that concentration is 2mol / L, add urea in the ratio of every liter 360g, Ni / Co / Mn=1 in the solution, now in the solution, the amount of urea and metal (Ni 2+ +Co 2+ +Mn 2+ ) The total substance mass ratio is 2:1. The precipitation agent is sodium hydroxide with a concentration of 10mol / L, and the complexing agent is ammonia water with a concentration of 20wt%. Add deionized water to the reactor in advance until the bottom paddle is covered, then add ammonia water to adjust the pH value to 10.5-11.0, and then raise the temperature in the reactor to 50-60°C. Use a silicone rubber tube with an inner diameter of 10mm as the delivery pipeline, pump the salt solution into the reaction kettle at a speed of 100ml / min, adjust the length of the pipeline entering the water bath to 1275cm, and the residence time of the salt solution in the water bath is 10min . Ammonia water is pumped into the reaction kettle simultaneously with t...

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Abstract

The invention discloses a preparation method of mono- / multi-metal coprecipitation hydroxide or carbonate. The preparation method includes the steps of firstly, preparing a mono- / multi-metal soluble salt solution, and adding urea to obtain a solution I; secondly, preparing a precipitator solution; thirdly, adding deionized water and ammonia water into a reaction kettle to allow the pH of purified water in the reaction kettle to be 10.5-11.0, using a metering pump to pump the solution I, the precipitator solution and a complexing agent solution into the reaction kettle so as to perform coprecipitation reaction, wherein the solution I is heated before being pumped into the reaction kettle to allow the decomposition rate of the urea to be 30-100%; fourthly, performing solid-liquid separation on substances in the reaction kettle after the reaction, collecting filter cake, and washing to remove impurity ions; drying to obtain the mono- / multi-metal coprecipitation hydroxide or carbonate. The preparation method has the advantages that the feature that the high-temperature decomposition of the urea releases ammonia is utilized to achieve the pre-complexing of metal ions in the metal salt solution, the reaction efficiency of the controllable crystallization reaction is increased, and accordingly product density and particle spheroidization degree are increased.

Description

technical field [0001] The invention relates to the field of preparation of battery electrode materials, in particular to a method for preparing single / multi-metal coprecipitated hydroxides or carbonates. Background technique [0002] Metal hydroxides or carbonates are widely used in the battery industry. For example, the positive electrode material of nickel metal hydride batteries is spherical nickel hydroxide Ni(OH) 2 , whose additive is cobaltous hydroxide Co(OH) 2 or cobalt hydroxide Co(OH) 3 , Many materials in lithium-ion battery positive electrode materials use single or metal co-precipitated hydroxides or carbonates as precursors, such as cobalt lithium oxide materials use spherical cobalt oxyhydroxide CoOOH or cobalt carbonate CoCO3 as precursors, nickel-cobalt binary or Nickel-cobalt-aluminum ternary material is Ni x co 1-x (OH) 2 and Ni 1-x-y co x al y (OH) 2 As a precursor, the nickel-cobalt-manganese ternary material is nickel, cobalt-manganese co-prec...

Claims

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Application Information

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IPC IPC(8): C01B13/36C01B32/60C01G53/04
CPCC01B13/36C01B13/363C01G53/04C01P2004/32C01P2004/60C01P2006/11C01P2006/12
Inventor 陈勃涛唐淼李征玉徐宁吴孟涛
Owner TIANJIN B&M SCI & TECH
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