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Sodium fluorosilicate ammoniating process of producing high reinforcing silica white

A technology of sodium fluorosilicate and white carbon black, applied in the field of powder material preparation, can solve the problems of long production process, low specific surface area of ​​white carbon black, poor transparency and reinforcement, etc., and achieve the effect of high specific surface

Inactive Publication Date: 2005-01-12
TIANJIN CHEM RES & DESIGN INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The white carbon black specific surface area obtained by this process method is on the low side (100m 2 / g), poor transparency and reinforcement in rubber compounds, it is difficult to use as high reinforcement silica
Therefore, the products produced by this process can only be used as fillers
Moreover, SiO after ammoniation 2 The filter cake has strong gelatinity and is not easy to filter and wash
After drying, the product needs to be pulverized, which not only lengthens the production process, but also increases the NH produced by the recovered filter cake. 4 Difficulty of F+NaF mixed solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 5L stirred reactor, add 2300ml of water and 75g of sodium fluorosilicate to make a slurry, heat up to 45°C, add 90ml of ammonia water with a concentration of 16% under stirring, continue to heat up to 65°C, and add fluorosilicic acid in parallel 175g of sodium, 450ml of ammonia water, during which the pH value of the reaction material is around 8.0. After the feeding is completed, the pH value of the reaction slurry is 8.0 to 8.5. After the reaction slurry is filtered, washed and dried, it becomes a powder product with a specific surface area of ​​172m 2 / g.

Embodiment 2

[0021] In a 5L stirred reactor, add 2300ml of mother liquor (containing a small amount of fluorine salt and 1-2% free ammonia) returned from cryolite produced by sodium fluorosilicate-sodium aluminate method, raise the temperature to 40°C, and add 80g of fluorosilicon under stirring Add 55ml of ammonia water with a concentration of 16%, continue to heat up to 60°C, add 170g of sodium fluorosilicate, and add 490ml of ammonia with a concentration of 16% at the same time to maintain pH8.0~8.5, then filter, wash, and dry to obtain the product. Specific surface area 200m 2 / g.

Embodiment 3

[0023] In a 5L stirred reactor, add 2300ml of the mother liquor returned from cryolite produced by the sodium fluorosilicate-sodium aluminate method, raise the temperature to 40°C, add 70g of sodium fluorosilicate under stirring, and add 40ml of ammonia water with a concentration of 16%, and the reaction slurry Continue to heat up the material to 50°C, add 30g of sodium fluorosilicate and 80ml of ammonia water with a concentration of 16% at the same time, age for 10 minutes, then add 150g of sodium fluorosilicate, and simultaneously add 380ml of ammonia water with a concentration of 16%, filter, wash, and dry The obtained product has a specific surface area of ​​150m 2 / g.

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Abstract

The method for preparing high reinforced white carbon black by means of ammonization of sodium fluorosilicate incldues the following steps: firstly, making 25-50% of Na2SiF6 and 5-20% of ammonia water produce reaction at 30-45 deg.C, it is favourable for production of small colloidal kernel, then adding other Na2SiF6 and ammonia water at 50-70 deg.C by once or several times to make them produce reaction, ageing, filtering, washing and drying to obtain the invented white carbon black. Its specific surface area is high, and can be regulated in the range of 130-220 sq.m / g, and its DBP oil-absorbing value also can be regulated in the range of 2.0-3.3. Said product can be used as reinforcing material for making shoes and tyres.

Description

[0001] The invention belongs to the technical field of powder material preparation, in particular to a preparation process for preparing white carbon black by using sodium fluorosilicate, a by-product of phosphate fertilizer. Background technique [0002] At present, a large amount of fluorine-containing waste gas escapes in the process of phosphate fertilizer production, escapes in the form of silicon tetrafluoride, and reacts with NaCl solution after absorption to obtain sodium fluorosilicate. Sodium fluorosilicate can be used directly as a product in some fields, and can also be used as an intermediate raw material for the preparation of fluoride salts. Sodium fluorosilicate is ammoniated, and after desiliconization, the solution is reacted with sodium aluminate to obtain cryolite. Reaction formula: [0003] <chemistry num="001"> <chem file="01141442_cml001.xml" / > < / chemistry> [0004] <chemistry num="002"> <chem fil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/021C01B33/113
Inventor 宁延生朱春雨
Owner TIANJIN CHEM RES & DESIGN INST