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Preparation method of electronic grade ceric sulfate

A cerium sulfate, electronic-grade technology, applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems of low product oxidation rate, low product purity, long filtration time, etc., and achieve high product oxidation rate, The effect of high product purity and high product fineness

Active Publication Date: 2015-11-04
乐山沃耐稀电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method has the following disadvantages: 1, the filtration time is long, and the yield is not high; 2, the product oxidation rate is low; 3, the product purity is low

Method used

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  • Preparation method of electronic grade ceric sulfate

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Effect test

specific Embodiment 1

[0028] Such as figure 1 As shown, a method for preparing electronic grade cerium sulfate includes the following steps:

[0029] (1) Add 1 part of cerium carbonate to 2 parts of dilute nitric acid solution and stir for 1 hour to obtain cerium nitrate solution;

[0030] (2). Add 1mol / L ammonium carbonate aqueous solution to the cerium nitrate solution obtained in step (1) until the pH of the cerium nitrate solution is 4.0, and then heat the cerium nitrate solution to 90°C for 150 minutes , Until the mass concentration of the cerium nitrate solution is 220g / L;

[0031] (3), filter

[0032] Filter the mixed liquid obtained in step (2) through a 1000-mesh sieve to obtain a filtrate;

[0033] (4). Add the filtrate obtained in step (3) to a microporous filter to obtain a filtrate;

[0034] (5). Add 30% hydrogen peroxide to the filtrate obtained in step (4), and then add ammonia aqueous solution dropwise to the filtrate until the pH of the filtrate is 6.0. Control the reaction temperature at 3...

specific Embodiment 2

[0043] A preparation method of electronic grade cerium sulfate includes the following steps:

[0044] (1) Add 1 part of cerium carbonate to 5 parts of dilute nitric acid solution and stir for 2 hours to obtain cerium nitrate solution;

[0045] (2) Add dropwise an aqueous solution of ammonium carbonate with a concentration of 5mol / L to the cerium nitrate solution obtained in step (1) until the pH of the cerium nitrate solution is 4.5, and then heat the cerium nitrate solution to 95°C for 90 minutes , Until the mass concentration of the cerium nitrate solution is 240g / L;

[0046] (3), filter

[0047] Filter the mixed liquid obtained in step (2) through a 1000-mesh sieve to obtain a filtrate;

[0048] (4) Add the filtrate obtained in step (3) to a microporous (pore size 0.5-1.0um) filter to obtain a filtrate;

[0049] (5). Add 30% hydrogen peroxide to the filtrate obtained in step (4), and then add dropwise ammonia solution to the filtrate until the pH of the filtrate is 7.0. Control the r...

specific Embodiment 3

[0058] A preparation method of electronic grade cerium sulfate includes the following steps:

[0059] (1) Add 1 part of cerium carbonate to 3 parts of dilute nitric acid solution, and stir for 1.5 hours to obtain a cerium nitrate solution;

[0060] (2) Add dropwise an aqueous solution of ammonium carbonate with a concentration of 3mol / L to the cerium nitrate solution obtained in step (1) until the pH of the cerium nitrate solution is 4.3, and then heat the cerium nitrate solution to 92°C for 120 minutes , Until the mass concentration of the cerium nitrate solution is 230g / L;

[0061] (3), filter

[0062] Filter the mixed liquid obtained in step (2) through a 1000-mesh sieve to obtain a filtrate;

[0063] (4). Add the filtrate obtained in step (3) to a microporous filter to obtain a filtrate;

[0064] (5). Add 30% hydrogen peroxide to the filtrate obtained in step (4), and then add ammonia solution dropwise to the filtrate until the pH of the filtrate is 6.5. Control the reaction tempera...

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Abstract

The invention relates to a preparation method of electronic grade ceric sulfate, which comprises the following steps: 1)adding a dilute nitric acid solution in cerous carbonate to obtain a cerium nitrate solution; 2)dropping an ammonium carbonate aqueous solution in the solution, heating until the mass concentration of the cerium nitrate solution is 220-240g / L; 3)filtering; 4)adding a filtrate in a micropore filter for filtering; 5)adding hydrogen peroxide with volume concentration being 30% in the filtrate, dropping aqueous ammonia in the filtrate, controlling the reaction temperature being 30-35 DEG C; 6)performing plate filtration to obtain the sediment; 7)adding a cerium hydroxide filter cake in excessive concentrated sulfuric acid; 8)adding concentrated sulfuric acid in the solution, concentrating for reacting for 5 hours, filtering to obtain the ceric sulfate crystal; and 9)dehydrating the ceric sulfate crystal to obtain the electronic grade ceric sulfate. The preparation method has the following beneficial effect that 1)filtering time is short, yield is high; 2)product oxidation rate is high; 3)products purity is high; 4)products fineness is high; and 5)products non rare earth metal impurity is low.

Description

Technical field [0001] The invention belongs to the field of chemical product preparation, and specifically relates to a preparation method of electronic grade cerium sulfate. Background technique [0002] Cerium sulfate is soluble in water, and at the same time it reacts with water to decompose into basic salt, which is soluble in dilute sulfuric acid. It dissolves into light pink in water and has strong oxidizing properties. Cerium sulfate is used as an oxidant in analytical chemistry and industry, as well as in the production of water-repellent agents and anti-mold agents. [0003] The current method for preparing cerium sulfate is mainly to dissolve cerium carbonate with nitric acid to prepare Ce(NO 3 ) 3 , Filtration, the filtrate is added with hydrogen peroxide and ammonia water for precipitation and filtered, the filter cake Ce(OH) 4 Then add sulfuric acid to dissolve, concentrate and crystallize cerium sulfate Ce(SO 4 ) 2 , Dehydration to obtain cerium sulfate. However, t...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 杨青
Owner 乐山沃耐稀电子材料有限公司
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