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Method for producing anhydrous lithium perchlorate

A technology of lithium perchlorate and production method, applied in perchloric acid, perchlorate and other directions, can solve the problems of high energy consumption, high water content, large equipment investment, etc., and achieves easy control, simple process and stable pH value. Effect

Active Publication Date: 2011-08-03
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation of lithium perchlorate has three kinds of methods at present: a) neutralization method, obtain lithium perchlorate solution with lithium hydroxide or lithium carbonate and perchloric acid reaction, obtain lithium perchlorate crystal through concentrated crystallization again, present technology exists High impurity content and high moisture content; b) sodium perchlorate decomposition method, lithium hydroxide or lithium salt is added to the concentrated sodium perchlorate solution, and the double decomposition reaction is carried out to generate lithium perchlorate crystals. The content is higher, and the product purity is lower; c) lithium chlorate aqueous solution electrolysis method, lithium chlorate aqueous solution is electrolyzed, obtains lithium perchlorate, and this method consumes a lot of energy, and equipment investment is big

Method used

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  • Method for producing anhydrous lithium perchlorate
  • Method for producing anhydrous lithium perchlorate
  • Method for producing anhydrous lithium perchlorate

Examples

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Effect test

Embodiment 1

[0021] see figure 1 , a kind of production method of anhydrous lithium perchlorate, the steps are as follows:

[0022] 1. Add 75kg of industrial lithium hydroxide to 150L pure water and stir, then slowly add 252kg of perchloric acid under stirring, after the addition, adjust the pH value of the reaction system to 7 with lithium hydroxide or perchloric acid, wait for 5 Minutes, after detecting that the pH value has no change, filter while hot, remove insoluble impurities, and obtain lithium perchlorate clean solution;

[0023] 2. Heating and evaporating the obtained lithium perchlorate clean liquid, the evaporation end temperature is 120°C, then stirring and cooling to 20°C, after the cooling is completed, use a centrifuge to separate, and after separation, 199kg of primary lithium perchlorate trihydrate crystals and 131L primary mother liquor, the primary mother liquor can be kept for returning to the neutralization process;

[0024] 3. Add 199kg of primary trihydrate lithiu...

Embodiment 2

[0028] see figure 1 , a kind of production method of anhydrous lithium perchlorate, the steps are as follows:

[0029] 1. Add 75kg of industrial lithium hydroxide to 150L of pure water and stir, then slowly add 252kg of perchloric acid under stirring, after the addition, adjust the pH value of the reaction system to 7.2 with lithium hydroxide or perchloric acid, wait for 5 Minutes, after detecting that the pH value has no change, filter while hot, remove insoluble impurities, and obtain lithium perchlorate clean solution;

[0030] 2. Heat and evaporate the obtained lithium perchlorate clean liquid, the evaporation end point temperature is 130°C, then stir and cool to 30°C, after the cooling is completed, separate with a centrifuge to obtain 206kg primary trihydrate lithium perchlorate crystals and 113L primary mother liquor, the primary mother liquor can be retained to be returned to the neutralization process;

[0031] 3. Add 206kg primary trihydrate lithium perchlorate cry...

Embodiment 3

[0035] see figure 1 , a kind of production method of anhydrous lithium perchlorate, the steps are as follows:

[0036] 1. Add 66kg of industrial lithium carbonate to 198L of pure water and stir, then slowly add 252kg of perchloric acid under stirring, after the addition, adjust the pH value of the reaction system to 7.2 with lithium hydroxide or perchloric acid, and wait for 5 minutes , filter while hot after detecting that the pH value has no change, remove insoluble impurities, and obtain lithium perchlorate clean solution;

[0037] 2. Heating and evaporating the obtained lithium perchlorate clean liquid, the evaporation end point temperature is 130°C, then stirring and cooling to 30°C, after the cooling is completed, use a centrifuge to separate, and after separation, 207kg of primary lithium perchlorate trihydrate crystals and 110L primary mother liquor, the primary mother liquor can be kept for returning to the neutralization process;

[0038] 3. Add 207kg primary trihy...

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Abstract

The invention belongs to the technical field of electrolyte preparation of lithium battery electrolyte and discloses a method for producing anhydrous lithium perchlorate. The water content of anhydrous lithium perchlorate sold in the market is about 3,000ppm, so a factory using the anhydrous lithium perchlorate needs to remove water from the anhydrous lithium perchlorate before preparing electrolyte from the anhydrous lithium perchlorate. But the water is not completely removed and fluctuation frequently exists, the yield and the quality of the electrolyte are restricted. At the same time, with the development of lithium batteries, the requirements on the impurity content and the stability of a pH value of lithium perchlorate are higher and higher. The method, namely reaction between lithium hydroxide or lithium carbonate and perchloric acid, solves the problems. The method sequentially comprises the following steps of: neutralizing, filtering, evaporating for the first time, cooling for crystallization, performing centrifugal separation to obtain a solid, dissolving, evaporating for the second time, cooling for crystallization, performing centrifugal separation to obtain a solid,melting and evaporating, cooling and crushing, and drying and packing. The produced anhydrous lithium perchlorate has low impurity content and the water content of lower then 200ppm; the pH value of aqueous solution of the anhydrous lithium perchlorate is stable; and the anhydrous lithium perchlorate can be directly used for producing the electrolyte.

Description

technical field [0001] The invention relates to the technical field of electrolyte preparation for lithium battery electrolyte, in particular to a production method of anhydrous lithium perchlorate. Background technique [0002] Lithium battery is a new type of battery that emerged in the 1990s, including lithium primary batteries and lithium secondary batteries. Lithium perchlorate is mainly used in the electrolyte of lithium primary batteries. Lithium primary batteries have high voltage and active negative electrode materials, so non-aqueous electrolytes must be used. Generally, organic solvents have limited conductivity. Lithium salts with high conductivity must be dissolved in organic solvents to meet the requirements of lithium batteries. Due to its high conductivity, anhydrous lithium perchlorate can meet the requirements of lithium batteries, and its water content is the key to quality assurance. The preparation of lithium perchlorate has three kinds of methods at p...

Claims

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Application Information

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IPC IPC(8): C01B11/18
Inventor 纪东海顾元霞陈力赵正红
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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