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Method for preparing battery-grade lithium dihydrogen phosphate

A lithium dihydrogen phosphate, battery-level technology, applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of inapplicable lithium iron phosphate production, uneven product particle size, complicated process, etc., and achieve shortened crystallization Effects of time, small particle size, and inhibition of growth

Active Publication Date: 2011-07-20
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The conventional production method of lithium dihydrogen phosphate is acid-base neutralization followed by evaporation and crystallization, but since the solubility of lithium dihydrogen phosphate is not greatly affected by temperature changes, the time for crystal precipitation and growth varies, so the particle size of the obtained product is Inhomogeneous, not suitable for the production of lithium iron phosphate
Patent CN101327919A discloses a synthesis method of lithium dihydrogen phosphate, that is, an aqueous solution of lithium dihydrogen phosphate is obtained through an acid-base neutralization reaction, and then the pure product of lithium dihydrogen phosphate is obtained by evaporation and extraction. CN101311108 discloses a lithium dihydrogen phosphate Lithium separation and preparation methods, that is, after obtaining the lithium dihydrogen phosphate aqueous solution, obtain lithium dihydrogen phosphate suitable for the production of lithium iron phosphate by quenching and extractant washing, the above two methods have introduced the extractant, and Processes such as crystallization and separation are required, which complicates the process while increasing costs

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh industrial grade LiOH·H 2 O 428.3g, be dissolved in deionized water, filter to remove insoluble matter, measure wherein Na + 、K + According to the corresponding stoichiometric ratio, add the purifying agent lithium sulfate, cool the LiOH solution with lithium sulfate to a certain temperature, filter and remove the insoluble matter, and obtain a colorless and clear solution, and measure the SO in the solution. 4 2- According to the stoichiometric ratio, the purifying agent barium hydroxide octahydrate was added to the solution, and the insoluble matter was removed by filtration to obtain the refined LiOH solution. Adjust the concentration of LiOH to 10%, and put it in the high-level tank, weigh 1164.5g of industrial phosphoric acid, adjust its concentration to about 40%, add the LiOH solution to the phosphoric acid dropwise, and the feeding time is 1 hour. After the reaction, the pH value of the solution is 2.5, and the solution is colorless and transparent, the...

Embodiment 2

[0032] Weigh industrial grade LiOH·H 2 O 441.2g, be dissolved in deionized water, filter to remove insoluble matter, measure wherein Na + 、K + According to the corresponding stoichiometric ratio, add dilute sulfuric acid as a purifying agent, cool down the LiOH solution added with dilute sulfuric acid to a certain temperature, filter to remove insoluble matter, and obtain a colorless and clear solution, and measure SO in the solution 4 2- content, add barium hydroxide octahydrate to the solution according to the stoichiometric ratio, and filter to remove insoluble matter to obtain LiOH refined solution. Adjust the concentration of LiOH to 8%, and place it in the high-level tank, weigh 1176g of industrial phosphoric acid, adjust its concentration to about 50%, add the LiOH solution dropwise to the phosphoric acid, and the feeding time is 1.5 hours. After the reaction, the pH of the solution is 2. The solution is colorless and transparent. Spray-dry the colorless and transpar...

Embodiment 3

[0034] Weigh industrial grade LiOH·H 2 O 432.6g, be dissolved in deionized water, filter to remove insoluble matter, measure wherein Na + 、K + According to the corresponding stoichiometric ratio, add the purifying agent lithium sulfate, cool the LiOH solution with lithium sulfate to a certain temperature, filter and remove the insoluble matter, and obtain a colorless and clear solution, and measure the SO in the solution. 4 2-content, add barium hydroxide octahydrate to the solution according to the stoichiometric ratio, and filter to remove insoluble matter to obtain LiOH refined solution. Adjust the concentration of LiOH to 5%, and place it in the high-level tank, weigh 1187g of industrial phosphoric acid, adjust its concentration to about 60%, add the LiOH solution dropwise to the phosphoric acid, and the feeding time is 2 hours. After the reaction, the pH of the solution is 3.5, and the solution is colorless and transparent, spray-dry the colorless and transparent solut...

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Abstract

The invention discloses a method for preparing battery-grade lithium dihydrogen phosphate, characterized by comprising the technological steps: (1) purifying industrial lithium hydroxide monohydrate; (2) acid-base neutralization reaction; (3) spray-drying products; and (4) deeply dewatering the products to obtain the products of battery-grade lithium dihydrogen phosphate with the purity being notless than 99.5% and the grain diameter D50 being equal to 3-15 microns.

Description

technical field [0001] The invention relates to the technical field of lithium-ion batteries, and relates to a method for preparing battery-grade lithium dihydrogen phosphate, which is a raw material of a novel lithium-ion battery anode material, lithium iron phosphate. technical background [0002] In today's world, secondary batteries have become one of the important directions for the development of new energy sources. In this context, lithium batteries with great advantages stand out, especially after Sony developed lithium-ion secondary batteries in 1990, in just a dozen years, because of their high energy density, good cycle performance and The ability to hold electricity has developed into a rapidly growing secondary battery system, and has attracted worldwide attention due to its incomparable advantages with other secondary batteries. [0003] With the development of lithium-ion batteries, the iron-based positive electrode has become an expected candidate material. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/1397H01M4/58
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 宁延生许寒郭西凤赵庆云赵洪
Owner CHINA NAT OFFSHORE OIL CORP
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