Method for preparing big-compensating forcing white carbon black and high concentration ammonium fluoride through aminating of fluosilicic acid

A technology of ammonium fluorosilicate and ammonium fluoride, which is applied in the direction of ammonium halide, silicon oxide, etc., can solve the problems of increasing equipment investment, waste of fluorine and silicon resources, pollution of the environment, etc., and achieve the effect of reducing energy consumption

Active Publication Date: 2008-03-12
YUNNAN YUNTIANHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Fluorosilicic acid is usually a by-product of the production of wet-process phosphoric acid and general calcium. In 2005, my country's phosphate fertilizer output was 100% P 2 o 5 Calculated at 11.25 million tons, the by-product fluosilicic acid can be converted into 100% H 2 SiF 6 In my country, most of the fluosilicate is recovered in the form of sodium fluosilicate, but the use of sodium fluosilicate is narrow, the economic benefit is poor, and it is often unsalable, which seriously affects the enthusiasm of manufacturers to recycle fluosilicate. This restricts the development of the phosphate fertilizer industry, which not only causes a serious waste of fluorine and silicon resources, but also pollutes the environment to a large extent
At present, there is a method for preparing white carbon black through sodium fluorosilicate, a by-product of phosphate fertilizer, but sodium fluorosilicate is an indirect by-product of the phosph...

Method used

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  • Method for preparing big-compensating forcing white carbon black and high concentration ammonium fluoride through aminating of fluosilicic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 293.7g of 12% fluosilicic acid solution to the stirred reactor at a temperature of 27-32°C, first add 109.4g of 16% ammonia water to the fluosilicic acid solution, after the dropwise addition , the temperature is 45-50°C, the pH is 6.5-7.2, and it is aged for 30 minutes, and then the first step is filtered, and the filter cake is washed and dried to obtain a white carbon black product with a specific surface area of ​​265m 2 / g; Add ammonium fluorosilicate to the filtrate obtained by filtering in the first step, so that the content of ammonium fluorosilicate in the filtrate is 16%, and the temperature is 30-35°C. Add 35.4g of 28% ammonium fluoride to the filtrate Ammonia water, after the dropwise addition, the temperature is 42-47°C, and it is aged for 30 minutes, and the second step of filtration is carried out. The filter cake is washed and dried to obtain a white carbon black product with a specific surface area of ​​240m 2 / g, carry out the third-step ammoniatio...

Embodiment 2

[0022] Operation is with embodiment 1. The first step of ammoniation is the same as that of Example 1 with filtration. Add ammonium fluorosilicate to the filtrate obtained by filtering in the first step, so that the content of ammonium fluorosilicate in the filtrate is 12%, and the temperature is 20 to 25°C. Add 41.1g of ammonia solution with a concentration of 18%, drop After the addition is completed, the temperature of the solution is 30-35°C, and it is aged for 20-40 minutes, followed by the second step of filtration, and the filter cake is washed and dried to obtain a white carbon black product with a specific surface area of ​​260m 2 / g, carry out the third-step ammoniation of the filtrate obtained by the second-step filtration, the temperature is 20-25°C, add 41.4g of ammonia water with a concentration of 18% to it, after the dropwise addition, the temperature is 28-32°C, the pH >8.0, and aged for 20-40 minutes, then filtered in the third step, the filter cake was wash...

Embodiment 3

[0024] Operation is with embodiment 1. The first step of ammoniation is the same as that of Example 1 with filtration. Add ammonium fluorosilicate to the filtrate obtained by filtering in the first step, so that the content of ammonium fluorosilicate in the filtrate is 18%, and the temperature is 30 to 35°C. Add 35.1g of ammonia solution with a concentration of 28%, drop After the addition is completed, the temperature of the solution is 40-45°C, and it is aged for 20-40 minutes, followed by the second step of filtration, and the filter cake is washed and dried to obtain a white carbon black product with a specific surface area of ​​190m 2 / g, carry out the third-step ammoniation of the filtrate obtained in the second step of filtration, the temperature is 30-35°C, add 52.6g of ammonia water with a concentration of 28% to it, after the dropwise addition, the temperature is 38-42°C, and the pH >8.0, and aged for 20-40 minutes, then filtered in the third step, the filter cake w...

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Abstract

A preparation method of highly reinforced white carbon black and high concentration ammonium fluoride through fluosilicic acid ammoniation relates to a preparation method of chemical product, in particular relating to a preparation method of inorganic power material. The invention carries through ammoniation reaction by steps with the fluosilicic acid and ammonia. The white carbon black is acquired after filtrating, washing and drying. The invention is characterized in that the ammonia is added in by steps and the filter is carried through by steps. The steps are that a, 30 to 70 percent of the total ammonia is added in the fluosilicic acid to carry through ammoniation reaction, the reaction liquid is aged, filtrated to acquire a filter cake and a filter liquid; the ammonium fluorosilicate is added in the filter liquid acquired in step a and then the ammonia is added to carry through ammoniation reaction, the reaction liquid is aged, filtrated to acquire the filter cake and the filter liquid; c, the left ammonia is added in the filter liquid acquired in step b and then the reaction liquid is aged and the aged liquid is filtrated to acquire the filter cake and high concentration ammonium fluoride mother liquid; d, the filter cakes acquired by filtrating are respectively washed and dried to prepare the white carbon black.

Description

technical field [0001] The present invention relates to a preparation method of chemical products, in particular to a preparation method of inorganic powder materials, more specifically, it utilizes fluorosilicic acid, a by-product of the phosphate fertilizer industry, to prepare highly reinforcing white carbon black and co-produce high-concentration fluoride ammonium method. Background technique [0002] White carbon black is hydrated silicon dioxide, the general molecular formula is: SiO 2 ·nH 2 O is a widely used chemical product, which can be used in rubber, plastic, paint, ink, pesticide, medicine, food, feed, paper and other industries. Its largest use is as a reinforcing filler for rubber, and its consumption accounts for more than 75% of its total output. Fluorosilicic acid is usually a by-product of the production of wet-process phosphoric acid and general calcium. In 2005, my country's phosphate fertilizer output was 100% P 2 o 5 Calculated at 11.25 million to...

Claims

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Application Information

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IPC IPC(8): C01B33/113C01C1/16
Inventor 明大增李志祥薛河南
Owner YUNNAN YUNTIANHUA
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