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Method of utilizing caprolactam waste alkalis to prepare sodium fluoride and white carbon black

A technology of caprolactam and sodium fluoride, applied in the directions of alkali metal fluoride, silicon oxide, silicon dioxide, etc., can solve the problems of narrow use of sodium fluorosilicate, high cost, waste of fluorine resources, etc., and achieve easy washing, removal, adsorption, etc. Moderate effect and high stability

Inactive Publication Date: 2020-04-10
湖北三宁碳磷基新材料产业技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, a large amount of waste caustic soda is produced in the production process of caprolactam in our country. The spent caustic soda contains a large amount of sodium sulfate impurities, which is poor in quality, low in purity, and difficult to separate. Therefore, enterprises generally sell it as a burden at a very low price, which is economical. extremely low value
On the other hand, a large amount of fluosilicic acid is produced by-product in my country's phosphate fertilizer industry, most of which are recovered in the form of sodium fluosilicate, and sodium fluosilicate has narrow uses, low price, and low economic benefits, which seriously restricts The enthusiasm of enterprises to recycle fluosilicic acid and the development of phosphate fertilizer industry have also caused the waste of fluorine resources in my country
[0003] CN104030317A discloses utilizing sodium carbonate and fluorosilicic acid to prepare sodium fluorosilicate, and then further prepares the technology of sodium fluoride and white carbon black, but wherein directly adopts sodium carbonate decahydrate raw material to produce, and cost is higher, and the obtained fluorine Sodium chloride and white carbon black are easy to form co-precipitation, and the separation effect is poor

Method used

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  • Method of utilizing caprolactam waste alkalis to prepare sodium fluoride and white carbon black

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] like figure 1 As shown, weigh 100g of spent caustic soda (80wt% of sodium carbonate and 18wt% of sodium sulfate), add 120g of desalted water and mix, heat to 60°C, stir and dissolve into spent caustic soda. Keep warm at 60°C, filter while hot, remove insoluble impurities, and obtain filtrate A. The filtrate A was cooled to 20°C for cooling and crystallization for 2 hours, and the fine slurry formed by cooling and crystallization was filtered under reduced pressure to obtain 45 g of sodium carbonate decahydrate crystals and filtrate B.

[0032] Add 20g of fluorosilicic acid to the filtrate B while stirring, and the sodium carbonate and sodium sulfate in the filtrate B react with the fluorosilicic acid to generate sodium fluorosilicate and the corresponding acid. After the reaction, grow crystals, wash and separate 26 g of sodium fluorosilicate crystals and filtrate C, and filtrate C is recycled for reuse.

[0033] Mix the sodium fluorosilicate crystals and sodium carbo...

Embodiment 2

[0041]Weigh 100g of spent caustic soda (including 75% sodium carbonate and 24% sodium sulfate), add 180g of desalted water and mix, heat to 45°C, stir and dissolve to form spent caustic soda. Keep warm at 45°C, filter while hot, remove insoluble impurities, and obtain filtrate A. The filtrate A was cooled to 15°C for cooling and crystallization for 2 hours, and the fine slurry formed by cooling and crystallization was filtered under reduced pressure to obtain 27 g of sodium carbonate decahydrate crystals and filtrate B.

[0042] Add 25g of fluorosilicic acid to the filtrate B under stirring, and the sodium carbonate and sodium sulfate in the filtrate B react with the fluorosilicic acid to generate sodium fluorosilicate and the corresponding acid. After the reaction, grow crystals, wash and separate 30 g of sodium fluorosilicate crystals and filtrate C, and filtrate C is recycled for reuse.

[0043] Mix the sodium fluorosilicate crystals obtained in the above steps with the so...

Embodiment 3

[0046] Weigh 100g of spent caustic soda (including 67% sodium carbonate and 30% sodium sulfate), add 150g desalted water and mix, heat to 55°C, stir and dissolve to form spent caustic lye. Keep warm at 55°C, filter while hot, remove insoluble impurities, and obtain filtrate A. The filtrate A was cooled to 12°C for cooling and crystallization for 2 hours, and the fine slurry formed by cooling and crystallization was filtered under reduced pressure to obtain 20 g of sodium carbonate decahydrate crystals and filtrate B.

[0047] Add 18g of fluorosilicic acid to the filtrate B under stirring, and the sodium carbonate and sodium sulfate in the filtrate B react with the fluorosilicic acid to generate sodium fluorosilicate and the corresponding acid. After the reaction, grow crystals, wash and separate 22 g of sodium fluorosilicate crystals and filtrate C, and filtrate C is recycled for reuse.

[0048] Mix the sodium fluorosilicate crystals obtained in the above steps with the sodiu...

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Abstract

The invention discloses a method of utilizing caprolactam waste alkalis to prepare sodium fluoride and white carbon black. The method comprises following steps: (1) mixing waste alkalis with desalinated water, heating to dissolve waste alkalis, filtering the solution when the solution is still hot to remove insoluble impurities to obtain a filtrate (A), and cooling and re-crystallizing the filtrate (A) to obtain sodium carbonate decahydrate and a filtrate (B); (2) adding fluoro-silicic acid into the filtrate (B), after reactions, growing the grains, filtering to obtain sodium fluorosilicate crystals and a filtrate (C); (3) mixing sodium fluorosilicate obtained in the step (2) and sodium carbonate decahydrate obtained in the step (1), adding water, stirring to carry out reactions, finally adding a surfactant, and evenly mixing; and (4) settling the stock solution obtained in the step (3), removing the supernate, separating sodium fluoride and white carbon black, carrying out centrifugation, and drying to obtain sodium fluoride crystals and white carbon black. The caprolactam waste alkalis and the byproduct namely fluoro-silicic acid of the phosphate fertilizer industry are comprehensively utilized, the wastes are converted into valuable resources, and a high environment protection value and economic value are generated.

Description

technical field [0001] The invention relates to the recycling of spent caprolactam alkali and fluosilicic acid, in particular to a method for preparing sodium fluoride and white carbon black by utilizing spent caprolactam alkali and fluosilicic acid by-product of phosphorus chemical industry. Background technique [0002] At present, a large amount of waste caustic soda is produced in the production process of caprolactam in our country. The spent caustic soda contains a large amount of sodium sulfate impurities, which is poor in quality, low in purity, and difficult to separate. Therefore, enterprises generally sell it as a burden at a very low price, which is economical. Extremely low value. On the other hand, a large amount of fluosilicic acid is produced by-product in my country's phosphate fertilizer industry, most of which are recovered in the form of sodium fluosilicate, and sodium fluosilicate has narrow uses, low price, and low economic benefits, which seriously res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C01D3/02
CPCC01B33/12C01D3/02C01P2006/80
Inventor 魏天荣李慧李善华张小元
Owner 湖北三宁碳磷基新材料产业技术研究院有限公司
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