Method for producing high reinforced carbon white by aminating fluorosilicic acid

A technology of ammonia fluorosilicate and white carbon black, which is applied in the field of chemical product preparation, can solve the problems of limited rubber reinforcement effect, narrow use of sodium fluorosilicate, restriction of enthusiasm, etc., and achieves obvious economic and environmental benefits, operation The effect of easy control of conditions and mild reaction conditions

Inactive Publication Date: 2007-10-10
云南云天化国际化工有限公司
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AI Technical Summary

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 phosphate fertilizer industry after all, and its production cost must be higher than that of directly preparing white carbon black through fluorosilicic acid. There are reports on the preparation of white carbon black by the reaction of fluosilicic acid and soda ash or ammonium bicarbonate, but the disadvantage of these two processes is that a large amount of carbon dioxide gas is produced in the reaction. If it is not recycled, it will inevitably pollute the environment, and recycling will prolong the process route. Increase the equipment investment, and at the same time, due to the acidification operation on the filter cake, a large amount of acid waste water will inevitably be produced in the washing process, polluting the environment, and the quality of the produced white carbon black product is not high, and the specific surface area is on the low side, which is harmful to rubber. Reinforcing effect is limited, it is difficult to use as highly reinforcing silica

Method used

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  • Method for producing high reinforced carbon white by aminating fluorosilicic acid

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Experimental program
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Effect test

Embodiment 1

[0026] Add 440.5g of 8% fluosilicic acid solution to the stirred reactor at a temperature of 20-25°C, first add 83.1g of 16% ammonia water to the fluosilicic acid solution, and age for 20 ~40 minutes, and then continue to add 46.0g of ammonia water with a concentration of 16% to the solution. After the dropwise addition, the temperature is 30~40°C, the pH is 6.5~7.4, and it is aged for 20~40 minutes, and the first step of filtration is performed. , the filter cake is washed and dried to obtain a white carbon black product with a specific surface area of ​​185m 2 / g; The filtrate obtained from the first step of filtration is ammoniated again at a temperature of 20-25°C, 54.7g of ammonia water with a concentration of 16% is added to it, and it is aged for 20-40 minutes, and then 35.0g is added to it , Ammonia water with a concentration of 16%, after the dropwise addition, the temperature is 25-35°C, pH>8.0, aging for 20-40 minutes, and the second step of filtration is carried ou...

Embodiment 2

[0028] Add 355.4g of 10% fluosilicic acid solution to the stirred reactor at a temperature of 20-25°C, first add 103.3g of 20% ammonia water to the fluosilicic acid solution, after the dropwise addition , the temperature is 35-40°C, the pH is 6.8-7.3, and it is aged for 20-40 minutes, and the first 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 ​​160m 2 / g; Ammonify the filtrate obtained in the first step of filtration again at a temperature of 20-25°C, add 71.8g of ammonia water with a concentration of 20% to it, after the addition is completed, the temperature is 30-35°C, and the pH>8.0 , and aged for 20 to 40 minutes, and then filtered in the second step. The filter cake was washed and dried to obtain a white carbon black product with a specific surface area of ​​204m 2 / g.

Embodiment 3

[0030] 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 ​​255m 2 / g; the filtrate obtained from the first step of filtration is ammoniated again at a temperature of 27-32°C, and 109.4g of ammonia water with a concentration of 16% is added thereto. After the addition is completed, the temperature is 35-40°C and the pH>8.0 , and aged for 30 minutes, and carried out the second step of filtration. The filter cake was washed and dried to obtain a white carbon black product with a specific surface area of ​​209m 2 / g.

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Abstract

This invention relates to a method for preparing white carbon black with high reinforcing ability by ammoniation of fluorosilicic acid. The method comprises: (1) adding ammoniation agent (30-70% of the total amount) into fluorosilicic acid, and ammoniating at 20-65 deg.C; (2) aging the ammoniation solution, and filtering to obtain filtrate and filter cake; (3) adding the rest ammoniation agent into the filtrate, ammoniating at 20-55 deg.C, aging the ammoniation solution, filtering to obtain mother liquor and filter cake, and sending the mother liquor to the following process; (4) washing the filter cakes, and drying to obtain white carbon black. The method has a high profit, and is environmentally friendly.

Description

technical field [0001] The invention relates to a method for preparing chemical products, in particular to a method for preparing inorganic powder materials, and more specifically to a method for preparing high-reinforcing white carbon black by utilizing fluosilicic acid, a by-product of the phosphate fertilizer industry. 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 tons, the by-product fluosilicic acid can be converted int...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/113C01B33/18
Inventor 明大增李志祥薛河南杨跃华杨建中
Owner 云南云天化国际化工有限公司
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