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Recycling method of fluorine-containing sulfuric acid waste liquid

A sulfuric acid waste liquid and recycling technology, which is applied in the field of resource recycling of fluorine-containing sulfuric acid waste liquid, can solve problems such as difficult separation of calcium sulfate and calcium fluoride, waste of resources, etc.

Pending Publication Date: 2021-05-18
盛隆资源再生(无锡)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has low cost, but it is difficult to further separate calcium sulfate and calcium fluoride, resulting in waste of resources

Method used

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  • Recycling method of fluorine-containing sulfuric acid waste liquid
  • Recycling method of fluorine-containing sulfuric acid waste liquid
  • Recycling method of fluorine-containing sulfuric acid waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 1000mL of a fluorine-containing sulfuric acid waste liquid (fluorine content 12g / L, sulfuric acid content 30%), add milk of lime to the waste liquid, adjust the pH of the solution to 8, stir well and then filter to obtain a filter cake, which is calcium fluoride and calcium sulfate mixture. Add 10wt% hydrochloric acid to the mixture of calcium fluoride and calcium sulfate with a mass volume ratio of 1:0.02g / L, then heat and stir at 80°C, then add 0.675g of mixed crystal aid (stearic acid: magnesium chloride mass The ratio is 1:1), after stirring for 1 hour, filter while hot, the obtained filter cake is washed with water, filtered, and dried to obtain 22.62g of calcium fluoride product, the filtrate is cooled at room temperature for 4 hours, filtered, the obtained filter cake is washed with water, filtered , and dried at 50°C to obtain 313.47g of calcium sulfate whisker product.

Embodiment 2

[0037] Take 1000mL of a fluorine-containing sulfuric acid waste liquid (fluorine content 12g / L, sulfuric acid content 30%), add milk of lime to the waste liquid, adjust the pH of the solution to 8, stir well and then filter to obtain a filter cake, which is calcium fluoride and calcium sulfate mixture. Add 15wt% hydrochloric acid to the mixture of calcium fluoride and calcium sulfate with a mass volume ratio of 1:0.02g / L, then heat and stir at 80°C, then add 0.675g of mixed crystal aid (stearic acid: magnesium chloride mass The ratio is 1:1), after stirring for 1 hour, filter while hot, the obtained filter cake is washed with water, filtered, and dried to obtain 23.17g of calcium fluoride product, the filtrate is cooled at room temperature for 4 hours, filtered, the obtained filter cake is washed with water, filtered , dried at 50°C to obtain 351.85g of calcium sulfate whisker product.

Embodiment 3

[0039]Take 1000mL of a fluorine-containing sulfuric acid waste liquid (fluorine content 12g / L, sulfuric acid content 30%), add milk of lime to the waste liquid, adjust the pH of the solution to 8, stir well and then filter to obtain a filter cake, which is calcium fluoride and calcium sulfate mixture. Add 20wt% hydrochloric acid to the mixture of calcium fluoride and calcium sulfate with a mass volume ratio of 1:0.02g / L, then heat and stir at 80°C, then add 0.675g of mixed crystal aid (stearic acid: magnesium chloride mass The ratio is 1:1), after stirring for 1 hour, filter while hot, the obtained filter cake is washed with water, filtered, and dried to obtain 22.36g of calcium fluoride product, the filtrate is cooled at room temperature for 4 hours, filtered, the obtained filter cake is washed with water, filtered , dried at 50°C to obtain 441.41g of calcium sulfate whisker product.

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Abstract

The invention provides a recycling method of fluorine-containing sulfuric acid waste liquid, and belongs to the technical field of waste liquid recycling treatment. The method comprises the following steps: adding lime milk into the fluorine-containing sulfuric acid waste liquid to obtain a filtrate 1 and a precipitate 1, adding hydrochloric acid into the obtained precipitate 1, heating and stirring, then adding a mixed crystallization aid, dissolving, and filtering while hot to obtain a precipitate 2 and a filtrate 2; washing the precipitate 2 to be neutral, filtering and drying to obtain calcium fluoride; cooling, crystallizing and filtering the filtrate 2 at room temperature to obtain precipitate 3 and filtrate 3; washing the obtained precipitate 3 to be neutral, filtering and drying to obtain the calcium sulfate whisker; and circulating the obtained filtrate 3 to the preparation of the precipitate 2, supplementing hydrochloric acid, distilling the filtrate 3 to obtain hydrochloric acid, and recycling the obtained hydrochloric acid. According to the method, calcium sulfate and calcium fluoride are separated in an economical and effective mode, meanwhile, calcium fluoride purification and high-value calcium sulfate whisker product conversion are achieved, and the purpose of resource utilization of fluorine-containing sulfuric acid is achieved.

Description

technical field [0001] The invention belongs to the technical field of waste liquid resource recovery treatment, and in particular relates to a resource recovery method of fluorine-containing sulfuric acid waste liquid. Background technique [0002] The existing hydrogen fluoride recovery process mostly adopts concentrated sulfuric acid replacement method, while the preparation of anhydrous hydrofluoric acid adopts the reaction of concentrated sulfuric acid and fluorspar at high temperature, and it is obtained after crude distillation and rectification. Both preparations will produce A large amount of fluorine-containing waste sulfuric acid waste liquid contains a small amount of heavy metals, which is difficult to handle. It will not only bring huge environmental protection treatment costs to enterprises, but also cause great pollution to the environment. In addition, fluorine is a non-metal chemical element with active chemical properties and widely distributed in minerals...

Claims

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Application Information

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IPC IPC(8): C02F1/58C02F101/14
CPCC02F1/583C02F2101/14
Inventor 张皖秋陈琪马斌斌曹羽芹
Owner 盛隆资源再生(无锡)有限公司
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