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Method of preparing battery-grade lithium dihydrogen phosphate by recrystallized lithium hydroxide

A technology of lithium dihydrogen phosphate and lithium hydroxide, which is applied in the direction of phosphorus compounds, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of impurity enrichment, long process, and cumbersome impurity removal, so as to improve recovery rate and reduce energy consumption. Consumption and cost, the effect of shortening the process flow

Active Publication Date: 2012-05-09
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention belongs to the neutralization method, and its purpose is to solve the problems of long process flow, impurity enrichment, and cumbersome impurity removal in the existing process, and to remove soluble impurities by recrystallizing lithium hydroxide, so as to prevent soluble impurities from entering dihydrogen phosphate The above-mentioned problems are caused by the lithium production system, which can simplify the process, reduce the cost and stabilize the quality of the output product

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  • Method of preparing battery-grade lithium dihydrogen phosphate by recrystallized lithium hydroxide
  • Method of preparing battery-grade lithium dihydrogen phosphate by recrystallized lithium hydroxide
  • Method of preparing battery-grade lithium dihydrogen phosphate by recrystallized lithium hydroxide

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Embodiment 1

[0014] see figure 2 , the method for preparing battery-grade lithium dihydrogen phosphate in the present embodiment 1 includes the following steps:

[0015] (1) 800kg of industrial lithium hydroxide was added to 4000L of pure water, fully stirred, and after the lithium hydroxide was completely dissolved, filtered to remove insoluble impurities to obtain a pure lithium hydroxide solution;

[0016] (2) Evaporate the obtained clean liquid, and control the evaporation vapor pressure at 0.1-0.3Mp to prevent the lithium hydroxide solution from overflowing at an excessively fast evaporation rate. After the clean liquid is evaporated and concentrated to 1000L, it is cooled, and the cooling temperature is controlled at 20-30 Degree Celsius, after cooling is completed, separate with a centrifuge, obtain 640kg of recrystallized lithium hydroxide and a lithium hydroxide mother liquor after the separation, and the lithium hydroxide mother liquor returns to the dissolving filtration proces...

Embodiment 2

[0022] see figure 2 , the method for preparing battery-grade lithium dihydrogen phosphate in this embodiment 2 includes the following steps:

[0023] (1) 800kg of industrial lithium hydroxide was added to 4000L of pure water, fully stirred, and after the lithium hydroxide was completely dissolved, filtered to remove insoluble impurities to obtain a pure lithium hydroxide solution;

[0024] (2) Evaporate the obtained clean liquid, and control the evaporation vapor pressure at 0.1-0.3Mp to prevent the lithium hydroxide solution from overflowing at an excessively fast evaporation rate. After the clean liquid is evaporated and concentrated to 1000L, it is cooled, and the cooling temperature is controlled at 20-30 Degree Celsius, after cooling is completed, separate with a centrifuge, obtain 640kg of recrystallized lithium hydroxide and a lithium hydroxide mother liquor after the separation, and the lithium hydroxide mother liquor returns to the dissolving filtration process;

[...

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Abstract

The invention relates to a method for producing battery-grade lithium dihydrogen phosphate, belonging to the manufacturing technical field of the lithium dihydrogen phosphate. As commercially available industrial-grade lithium hydroxide has higher impurity content soluble impurities, the invention provides a new method for producing the battery-grade lithium dihydrogen phosphate aiming at the problem that the soluble impurities in the prior art are easily enriched, comprising the steps of: (1) preparation of recrystallized lithium hydroxide; (2) neutral reaction: reacting phosphoric acid withthe recrystallized lithium hydroxide according to a mol ratio of LiOH to H3PO4 being 1 : (1-1.1), adjusting a PH value to be 1-3, and obtaining a lithium dihydrogen phosphate solution; (3) evaporating concentration; (4) cooling, crystallization and separation; and (5) drying and packaging to obtain lithium dihydrogen phosphate products. The method of preparing the battery-grade lithium dihydrogenphosphate by the recrystallized lithium hydroxide has the advantages of a short technical process, a simple operation and low cost. The obtained battery-grade lithium dihydrogen phosphate products have few impurities (Na, K, SO4(2-) and Cl(1-) in the products are all less than 20 ppm) and stable quality, and can be suitable for preparing a cathode material of a lithium ion battery.

Description

1. Technical field [0001] The invention relates to a method for producing battery-grade lithium dihydrogen phosphate, and belongs to the technical field of lithium dihydrogen phosphate manufacturing. 2. Background technology [0002] Lithium batteries are a new type of battery that emerged in the 1990s, including lithium primary batteries and lithium secondary batteries. With the popularization and application of portable small electrical appliances such as mobile phones and notebook computers, lithium secondary batteries have also developed and popularized. The cathode materials mainly include lithium cobaltate, lithium manganate, lithium nickelate and ternary materials. Since 1996, Japan's NTT first disclosed AyMPO4 (A is an alkali metal, M is a combination of CoFe: LiFeCOPO4) as an olivine-structured lithium battery cathode material. In 1997, John.B.Goodenough, Texas State University, USA and other research groups, and then reported the characteristics of lithium iron p...

Claims

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Application Information

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IPC IPC(8): C01B25/30
Inventor 吕新新赵正红陈力范黎
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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