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Method for preparing high-quality ammonium bifluoride from fluorine-silicone compound

A technology of ammonium bifluoride and compounds, which is applied in the field of preparation of inorganic fluoride salts, can solve problems such as ammonium fluoride instability and fluorine-containing ammonium wastewater, and achieve the effect of reducing costs

Inactive Publication Date: 2018-06-26
QINGDAO XIANGZHI ELECTRONICS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the technology of using fluorine-containing waste absorption liquid or fluosilicic acid to produce ammonium bifluoride is to carry out one-step ammonium decomposition into ammonium fluoride and silicon dioxide, filter and remove silicon dioxide to obtain ammonium fluoride solution, and convert ammonium fluoride to ammonium fluoride. The solution is heated and concentrated to obtain ammonium bifluoride, or hydrogen fluoride is added after concentration to obtain ammonium bifluoride, or hydrogen fluoride is added to produce ammonium bifluoride and then concentrated. Since ammonium fluoride is unstable in hot water, a large amount of fluorine-containing ammonium wastewater will be produced during evaporation and concentration.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add NH4F-NH with a pH value of 2 to 4 into a closed reactor lined with fluoroplastics 4 HF 2 350g of the reaction solution, add 60g of ammonium fluoride solid with NH4F mass fraction of 95%, set the rotation speed of the stirrer to be above 500r / min, add 31g of hydrogen fluoride, 9g of pure water, and allow the temperature of the material to rise and fall naturally during the feeding process After the addition of hydrogen fluoride is completed, the reaction material is cooled to the ambient temperature, filtered to obtain ammonium bifluoride crystals, and ammonium bifluoride product is obtained after drying. The filtrate is NH4F-NH with a pH value of 1 to 5 4 HF 2 The reaction solution and the filtrate are recycled. Experiment obtains about 100g of ammonium bifluoride filter cake, about 350g of filtrate. After drying the ammonium fluoride filter cake, NH 4 HF 2 Content is 90.5g of the ammonium bifluoride product of 97%.

Embodiment 2

[0018] Add NH4F-NH with a pH value of 1 to 5 in a closed reactor lined with fluoroplastics 4 HF 2 350g of the reaction solution, adding NH4F mass fraction is 95% ammonium fluoride solid 60g, setting the rotating speed of the stirrer is more than 500r / min, adding hydrogen fluoride 22g, HF content is 18g of hydrofluoric acid of 50%, the temperature of the material during the feeding process Allow it to rise and fall naturally, and after the addition of hydrogen fluoride, cool the reaction material to the ambient temperature, filter to obtain ammonium bifluoride crystals, and obtain ammonium bifluoride product after drying. The filtrate is NH4F-NH with a pH value of 1 to 5 4 HF 2The reaction solution and the filtrate are recycled. Experiment obtains about 98g of ammonium bifluoride filter cake, about 352g of filtrate. After drying the ammonium fluoride filter cake, NH 4 HF 2 Content is 90g of the ammonium bifluoride product of 97%.

Embodiment 3

[0020] Add NH4F-NH with a pH value of 2 to 4 into a closed reactor lined with fluoroplastics 4 HF 2 350g of the reaction solution, add NH4F mass fraction and be 60g of ammonium fluoride solids of 95%, set the rotating speed of the agitator to be more than 500r / min, add 26g of hydrogen fluoride, 14g of hydrofluoric acid with HF content of 35%, the material temperature during the feeding process Allow it to rise and fall naturally, and after the addition of hydrogen fluoride, cool the reaction material to the ambient temperature, filter to obtain ammonium bifluoride crystals, and obtain ammonium bifluoride product after drying. The filtrate is NH4F-NH with a pH value of 1 to 5 4 HF 2 The reaction solution and the filtrate are recycled. Experiment obtains about 100g of ammonium bifluoride filter cake, about 350g of filtrate. After drying the ammonium fluoride filter cake, NH 4 HF 2 Content is 90.5g of the ammonium bifluoride product of 97%.

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Abstract

The invention provides a method for preparing high-quality ammonium bifluoride from a fluorine-silicone compound, and relates to an inorganic villiaumite preparation technology in a fluorine chemicalindustry of the chemical industry field. The method provided by the invention comprises the following steps: adding solid fluorosilicic acid or silicon tetrafluoride gas into a saturated ammonium fluoride solution, introducing excess ammonia at the same time, carrying out an ammonolysis reaction so as to respectively obtain an ammonium fluoride crystal mush and a silicon dioxide suspension after completion of the reaction, and successively carrying out six steps as described in the specification so as to obtain a high-quality ammonium bifluoride product, wherein a reaction solution returns a system for cyclic utilization. With the process technology of the invention, impurities contained in raw materials are mainly reserved in silicon dioxide, so the high-quality ammonium bifluoride product can be easier to be produced. Meanwhile, the problem of fluorine pollution from production in phosphorus fertilizer enterprises is solved; fluorine resources are recycled; and three wastes are not additionally generated in cyclic operation of the system.

Description

technical field [0001] The invention relates to the preparation technology of inorganic fluorine salts in the fluorine chemical industry in the chemical industry, in particular to a technical method for preparing ammonium bifluoride by using fluorine-containing waste absorption liquid or fluosilicic acid. Background technique [0002] Ammonium bifluoride is mainly used as glass etchant, preservative, solvent for metal beryllium made of beryllium oxide, chemical reagent, cleaning agent for boiler feed water system and steam generation system, disinfectant for fermentation industry and surface treatment agent for silicon steel plate, manufacturing ceramics and aluminum magnesium Alloy oxidant, organic synthetic fluorinating agent, electroplating solution, solvent for extracting rare elements, acid treatment agent for oil field sand, surface treatment agent for silicon steel plate and corrosive agent for surface treatment of aluminum profiles, etc. High-purity ammonium bifluori...

Claims

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Application Information

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IPC IPC(8): C01C1/16
CPCC01C1/162C01P2006/80
Inventor 不公告发明人
Owner QINGDAO XIANGZHI ELECTRONICS TECH CO LTD
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