Preparation method of manganese phosphate and manganese phosphate product

A manganese phosphate and manganese source technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of complex composition, high price, high production cost, etc., and achieve high product purity, uniform particle size distribution, and high purity Effect

Inactive Publication Date: 2016-05-25
SINOSTEEL ANHUI TIANYUAN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When manganese phosphate is prepared by the existing hydrothermal synthesis method, excessive manganese sources are used, and the manganese precipitation rate is only about 50%, or even lower. Compared with phosphorus sources, the manganese source is expensive, the utilization rate of manganese resources is low, and the production cost is high. ; When manganese phosphate is prepared by oxidation-precipitation, it is carried out under a single aqueous phase system, the product purity is difficult to control, the amount of crystal water is unknown, and the particle size distribution is uneven, thereby affecting the electrical properties of the product; when manganese phosphate is prepared by solvothermal synthesis , the composition of the reaction system is complex, the composition and structure of manganese phosphate products are complex, and it is not easy to scale production

Method used

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  • Preparation method of manganese phosphate and manganese phosphate product
  • Preparation method of manganese phosphate and manganese phosphate product
  • Preparation method of manganese phosphate and manganese phosphate product

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In the acid-resistant reaction kettle, a manganese sulfate monohydrate solution with a concentration of 0.5 mol / L is configured, a phosphoric acid solution with a concentration of 1 mol / L is added to the reaction kettle, and hydrogen peroxide with a concentration of 0.5 mol / L is then added to the reaction kettle, Wherein the weight ratio of deionized water, manganese source, phosphorus source, organic solvent is 100: 8.45 : 9.80 : 100 , adding nitric acid to adjust the pH value of the solution to be 2.0, the reaction temperature is 60 ° C, the stirring speed is 200r / min, and finally the concentration is 0.5mol / L ethanol solution added to the system, reacted for 5 hours, washed with water, filtered and dried to obtain manganese phosphate ( MnPO 4 ·H 2 O) Products.

Embodiment 2

[0028] In the acid-resistant reaction kettle, a manganese nitrate solution with a concentration of 0.5 mol / L was prepared, a phosphoric acid solution with a concentration of 0.75 mol / L was added to the reaction kettle, and hydrogen peroxide with a concentration of 0.5 mol / L was added to the reaction kettle. , wherein the weight ratio of deionized water, manganese source, phosphorus source, organic solvent is 100: 12.50 : 7.35 : 50 , add sodium hydroxide to adjust the pH value of the solution to 3.0, the reaction temperature is 80 ° C, the stirring speed is 200 r / min, and finally add a concentration of 0.5 mol / L ethylene glycol solution to the system, react for 3 hours, wash with water, filter, and dry, Obtain manganese phosphate (MnPO 4 ·H 2 O) Products.

Embodiment 3

[0030] In the acid-resistant reaction kettle, a manganese sulfate monohydrate solution with a concentration of 0.5 mol / L is configured, a sodium phosphate solution with a concentration of 0.5 mol / L is added to the reaction kettle, and then a sodium phosphate solution with a concentration of 0.5 mol / L is added into the reaction kettle Sodium nitrate, wherein the weight ratio of deionized water, manganese source, phosphorus source, organic solvent is 100: 8.45 : 19.01 : 200 , add sodium hydroxide to adjust the pH value of the solution to 5.0, the reaction temperature is 30 ° C, the stirring speed is 200 r / min, and finally acetone solution with a concentration of 0.5 mol / L is added to the system, react for 2 hours, wash with water, filter, and dry to obtain phosphoric acid Manganese (MnPO 4 ·H 2 O) Products.

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Abstract

The invention discloses a preparation method of manganese phosphate and a manganese phosphate product. The method comprises the following steps: weighing a soluble phosphorus source compound and a soluble manganese source compound at the molar ratio of P to Mn being (1-2) to 1, dissolving the soluble phosphorus source compound and the soluble manganese source compound into deionized water to prepare solutions; feeding a manganese source solution to an acid-resistant reaction kettle by a metering pump, and then adding a phosphorus source solution for stirring; feeding an oxidant to the acid-resistant reaction kettle by the metering pump, and adjusting the pH value of a system; adding the organic solvent to the acid-resistant reaction kettle, and carrying out stirring reaction at 30-90 DEG C; and naturally cooling the obtained manganese phosphate slurry to a room temperature, carrying out washing, filtering and drying to obtain a manganese phosphate (MnPO<4>.H<2>O) product. According to the method, the manganese deposition rate reaches over 99%; the manganese resource is fully utilized; the product purity is high; the Mn content is greater than 32%; the P content is 18%-19%; the content of a main impurity S is smaller than 0.5%; the content of Na is smaller than 0.02%; the particle size distribution is uniform; and the mean particle size is smaller than 1micron.

Description

technical field [0001] The invention belongs to the technical field of preparation of positive electrode materials for lithium ion batteries, and in particular relates to a method and product for preparing manganese phosphate by oxidation-precipitation process in a liquid phase system. Background technique [0002] Manganese phosphate is a widely used chemical raw material. It is mainly used as a phosphating agent for iron and steel products, especially for the phosphating treatment of large machinery and equipment. agent. In recent years, manganese phosphate has important application value as a high-quality raw material for lithium manganese phosphate, a cathode material for lithium-ion batteries. [0003] At present, there are relatively few researches on the preparation method of manganese phosphate at home and abroad, and the existing preparation methods are mainly: (1) oxidation-precipitation method / hydrothermal synthesis method, such as the invention patent with publi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525C01B25/37
CPCC01B25/377H01M4/5825H01M10/0525Y02E60/10
Inventor 钱有军裴晓东程露露骆艳华佘世杰刘晨王凡陈静
Owner SINOSTEEL ANHUI TIANYUAN TECH
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