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Preparation method of high-purity cerium hydroxide

A technology of cerium hydroxide and cerium oxide, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of impure product quality, poor solubility of nitric acid, etc., and achieve good filtration performance and good clarification effect , The effect of high product yield

Inactive Publication Date: 2010-01-27
甘肃稀土新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein potassium permanganate oxidation method and ammonium persulfate oxidation method produce cerium hydroxide impurity on the high side, resulting in impure product quality, and the solubility of nitric acid is not good, while ozone oxidation method and electrochemical oxidation method are limited by equipment. Enter industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 256KgCe(NO 3 ) 3 ·6H 2 O and 1250L deionized water are made into cerium nitrate solution, add 700 grams of n-amyl alcohol therein, and then add 100 grams of rare earth accelerator; get industrial 35% hydrogen peroxide and be mixed with 27% hydrogen peroxide 190L, then get 6.5mol / L industrial ammonia 245L under the condition of stirring, add hydrogen peroxide and ammonia water to the cerium salt solution dropwise at the same time, control the reaction time for 120 minutes, and control the reaction temperature at 32°C. After the hydrogen peroxide is added dropwise, adjust the pH of the system to 8.5 with ammonia water. Generate a brownish-red precipitate, stir for another 30 minutes, and heat the precipitate to decompose. The decomposition time is 40 minutes, and the temperature is greater than 95°C. After the decomposition is completed, add water to clarify, extract the supernatant and wash it with deionized water for 4 times, and then press filter. Dry at 70°C to obta...

Embodiment 2

[0020] 512KgCe(NO 3 ) 3 ·6H 2 O and 2500L deionized water are made into cerium nitrate solution, add 1400 grams of n-amyl alcohol therein, and then add 200 grams of rare earth accelerator; get industrial 35% hydrogen peroxide and be mixed with 27% hydrogen peroxide 380L, then get 7.0mol / L industrial ammonia water 480L, under the condition of stirring, add hydrogen peroxide and ammonia water dropwise to the cerium salt solution at the same time, control the reaction time for 110 minutes, and control the reaction temperature at 30°C. After the hydrogen peroxide is added dropwise, use ammonia water to adjust the system pH to 8.5. Generate a brownish-red precipitate, stir for another 30 minutes, and heat the precipitate to decompose. The decomposition time is 40 minutes, and the temperature is greater than 95°C. After the decomposition is completed, add water to clarify, extract the supernatant and wash it with deionized water for 4 times, and then press filter. Dry at 70°C to o...

Embodiment 3

[0022] 769KgCe(NO 3 ) 3 ·6H 2 O and 3750L deionized water are made into cerium nitrate solution, add 2100 grams of n-amyl alcohol therein, and then add 300 grams of rare earth accelerator; get industrial 35% hydrogen peroxide and be mixed with 27% hydrogen peroxide 570L, then get 7.0mol / L industrial ammonia 720L, while stirring, add hydrogen peroxide and ammonia water dropwise to the cerium salt solution at the same time, control the reaction time for 120 minutes, and control the reaction temperature at 35°C. Generate a brownish-red precipitate, stir for another 30 minutes, and heat the precipitate to decompose. The decomposition time is 40 minutes, and the temperature is greater than 95°C. After the decomposition is completed, add water to clarify, extract the supernatant and wash it with deionized water for 4 times, and then press filter. Dry at 70°C to obtain bright yellow product cerium hydroxide, product TREO≥70.0%, CeO 2 / TREO≥99.9%, CeO 4+ / ∑Ce≥97.0%, Ce(OH) 4 ≥83....

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Abstract

The invention discloses a preparation method of high-purity cerium hydroxide, comprising the following steps: taking liquid cerium nitrate as a raw material, hydrogen peroxide as oxidant and ammonia water as neutralizer, oxidizing trivalent cerium into tetravalent cerium in cerium nitrate solution in a weak acidic medium with the PH value being equal to 5 to 6 so as to form precipitate, then carrying out thermal decomposition, washing pressure filtration and drying on the precipitate to obtain high-purity cerium hydroxide product. The high-purity cerium hydroxide product prepared by the invention has high purification, wherein, the Ce ratio CeO / TREO is greater than or equal to 99.9%, the oxidation rate CeO<4+> / sigma Ce is greater than or equal to 97.0%, non-rare earth impurity magnesium oxide MgO is less than or equal to 2.5PPm, and the solubility of nitric acid is good. The process flow is short, the operation is convenient, and scale production is easy to be realized. The obtained Ce(OH)4 nitric acid is dissolved clearly, the oxidation rate of cerium is high, the content of non-rare earth impurities is low, thereby meeting the requirement of clients on quality of Ce(OH)4 products.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth compounds, in particular to a preparation method of high-purity cerium hydroxide. Background technique [0002] The common methods for producing cerium hydroxide are: precipitation oxidation method and oxidation precipitation method. The precipitation oxidation method mainly uses NH 3 .H 2 O is directly precipitated, because the precipitate is a colloid, and there are problems such as difficulty in filtration. The methods of oxidation precipitation mainly include: potassium permanganate oxidation method, ammonium persulfate oxidation method, ozone oxidation method, electrochemical oxidation method and hydrogen peroxide oxidation method. Wherein potassium permanganate oxidation method and ammonium persulfate oxidation method produce cerium hydroxide impurity on the high side, resulting in impure product quality, and the solubility of nitric acid is not good, while ozone oxidatio...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 方中心李月红王学荣杨小凤魏周菊
Owner 甘肃稀土新材料股份有限公司
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