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A method for producing high-quality sodium fluoride using fluorine-containing wastewater as raw material

A sodium fluoride, high-quality technology, applied in the purification of alkali metal fluorides and alkali metal halides, etc., can solve the problems of waste of fluorine resources, low fluorine concentration, and economic uneconomical

Active Publication Date: 2021-04-06
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the concentration of fluorine in the solution is low, the production process of sodium fluoride requires a large amount of evaporation and concentration, which is economically uneconomical
At present, low-concentration fluorine-containing wastewater at home and abroad, and complex fluorine-containing wastewater are generally treated by lime precipitation, which not only causes a serious waste of fluorine resources, but also produces a large amount of fluorine-containing solid waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Take tantalum and niobium neutralization mother liquor 2.5m from the tantalum and niobium smelter 3 , heat up to 95°C, stir and slowly add sodium carbonate to crystallize the fluorine in the form of sodium fluoride. After the bubbles in the solution gradually disappear, continue to add sodium carbonate to make the Na in the solution 2 CO 3 The concentration of the mixture rose to 350g / L, and then stirred for 1.5h to obtain a sodium fluoride filter cake and a solution containing sodium carbonate. The ammonia-containing gas generated during the reaction was purified by a lime column and returned to the tantalum-niobium neutralization process for recycling. The obtained sodium fluoride filter cake is added with 185g / L NH 4 In solution F, stir and wash at 65°C for 1.5h, filter to obtain refined sodium fluoride and ammonium fluoride solution, return the ammonium fluoride solution to the filter cake washing process for continued use, and dry the refined sodium fluoride to ob...

Embodiment 2

[0062] Take tantalum-niobium ore extract raffinate 2m 3 , stir at room temperature and feed ammonia gas, adjust the pH to 8.7 inversion, continue to stir for 2h, filter to obtain inversion slag filter cake and NH-containing 4 Filtrate of F. The resulting NH 4 Heat the filtrate of F to 85°C, stir and slowly add sodium carbonate to crystallize the fluorine in the solution in the form of sodium fluoride, and volatilize the ammonium in the form of ammonia gas. After the bubbles in the solution gradually disappear, continue to add sodium carbonate to make the Na in the solution 2 CO 3Concentration rises to 200g / L, then stir for 2 hours, filter to obtain sodium fluoride filter cake and sodium carbonate solution, and the ammonia-containing gas generated during the reaction process is returned to the cleaning and extraction raffinate transformation process for recycling. The obtained sodium fluoride filter cake is added with 89g / L NH 4 In solution F, stir and wash at 85°C for 0.5h...

Embodiment 3

[0065] Processing of titanium materials produces 3 m of washing waste liquid containing nitric acid to hydrofluoric acid 3 , first use diffusion dialysis to recover the free nitric acid and hydrofluoric acid in it, the resulting diffusion dialysis raffinate is passed through ammonia gas to adjust the pH to 8.5, stir at room temperature for 2 hours, and filter to obtain metatitanic acid filter cake and NH-containing 4 Filtrate of F. Heat the obtained filtrate to 90°C, stir and slowly add sodium carbonate to crystallize the fluorine in the form of sodium fluoride, and volatilize the ammonium in the form of ammonia gas. After the bubbles in the solution gradually disappear, continue to add sodium carbonate to make the Na in the solution 2 CO 3 Concentration rises to 400g / L, then stir for 1.5h, filter to obtain sodium fluoride filter cake and sodium carbonate solution, and the ammonia-containing gas generated during the reaction process is returned to the diffusion dialysis raffi...

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Abstract

A method for producing high-quality sodium fluoride using fluorine-containing wastewater as a raw material, which includes directly adding excess sodium carbonate salt to fluoride-containing wastewater, so that the fluorine in the solution is completely crystallized in the form of sodium fluoride, or first Ammonium fluoride solution is obtained by adding ammonia to the fluorine-containing wastewater solution, or the fluorine precipitation and enrichment in the fluorine-containing wastewater is firstly enriched, and then the fluorine in the fluoride precipitation enrichment is converted into an ammonium fluoride solution with an ammonium salt solution, and then fluoride Add excess sodium carbonate salt to the ammonium solution to completely crystallize the fluorine in the form of sodium fluoride, and filter to obtain sodium fluoride filter cake and fluorine sinking liquid; the sodium fluoride filter cake is washed and dried by ammonium fluoride solution A high-quality sodium fluoride product with a purity of more than 99.25% is obtained. The sodium carbonate salt in the liquid after fluoride sinking is crystallized and recovered, and the mother liquid of sodium carbonate salt crystallization is further desalted and reused as reclaimed water. The invention has the advantages of simple operation, high recovery rate of fluorine, low production cost, good quality of sodium fluoride product, no fluorine-containing waste and the like.

Description

technical field [0001] The invention belongs to the fields of chemical industry and metallurgy, and in particular relates to a method for producing high-quality sodium fluoride by using fluorine-containing wastewater as a raw material. Background technique [0002] Sodium fluoride is an important chemical raw material, widely used in chemical industry, metallurgy, wood preservatives, agricultural pesticides, brewing fungicides, pharmaceutical preservatives, welding flux, alkaline zincate galvanizing additives and enamel , Paper industry and other industries. At present, the main production methods of sodium fluoride are: melting leaching method, neutralization method, sodium fluorosilicate method, ion exchange method, etc. [0003] The immersion method is to calcinate fluorite, soda ash and quartz sand at a temperature of 800-1000 ° C, then leaching with water, and then evaporate, crystallize, and dry to obtain the finished product of sodium fluoride; the neutralization met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D3/02C01D3/14
CPCC01D3/02C01D3/14C01P2006/80
Inventor 王学文王明玉葛奇孟钰麒
Owner CENT SOUTH UNIV
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