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A method for producing anhydrous hydrogen fluoride from ammonium fluoride acidolysis mixed liquor

An anhydrous hydrogen fluoride, ammonium fluoride technology, applied in the direction of fluorine/hydrogen fluoride, hydrogen fluoride, etc., can solve the problems of unsatisfactory hydrogen fluoride yield, low hydrogen fluoride yield, corrosion of production equipment, etc., to improve equipment utilization, The effect of solving equipment corrosion resistance and reducing equipment corrosion problems

Active Publication Date: 2018-09-25
GUIYANG KAILIN FERTILIZER CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method of producing anhydrous hydrogen fluoride from fluosilicic acid is to react solid ammonium fluosilicate with 92%-99% concentrated sulfuric acid to produce SiF 4 Mixed gas with HF; the amount of sulfuric acid added is H 2 SO 4 Calculated as 100%-150% of the theoretical amount; analyze and volatilize SiF under vacuum conditions 4 and HF, the vacuum degree is controlled at 55kPa-85kPa, and the temperature is controlled at 120°C-140°C; 4 and HF, the temperature is controlled at 140°C-175°C; the mixed gas is washed, purified, and condensed to obtain anhydrous hydrogen fluoride, SiF 4 For the preparation of ammonium fluorosilicate, such as patent number 201210565361.1, "A method for preparing anhydrous hydrogen fluoride from fluorine-containing waste liquid or fluorosilicic acid of a phosphate fertilizer enterprise", which discloses the use of fluorine-containing waste gas absorption liquid or water in fluorosilicic acid Excluded by concentrated ammonium fluorosilicate, and then use concentrated sulfuric acid to acidify the solid ammonium fluorosilicate stage to produce a mixed gas of hydrogen fluoride and silicon tetrafluoride with a very low water content; but in the above scheme, the yield of hydrogen fluoride is not as good as satisfactory
[0004] At present, although there are many production methods of anhydrous hydrogen fluoride, most of them have the problems of low yield of hydrogen fluoride and serious corrosion of production equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for producing anhydrous hydrogen fluoride from ammonium fluoride acidolysis mixed liquor, comprising the following steps:

[0018] 1) Ammonium fluoride crystals and concentrated sulfuric acid with a volume concentration of 96% are subjected to an acidolysis reaction under a slight negative pressure, wherein the amount of concentrated sulfuric acid is 1.3 times the amount of concentrated sulfuric acid required to generate ammonium bisulfate;

[0019] 2) sending 20-25% of the total amount of crude hydrogen fluoride gas obtained from the acidolysis reaction into a refining system, and dissolving the remaining crude hydrogen fluoride gas in the liquid after the acidolysis reaction to obtain a mixed solution of ammonium fluoride acidolysis;

[0020] 3) Control the temperature of the ammonium fluoride acidolysis mixture at 100°C, and immediately spray it into the concentrated sulfuric acid circulating liquid, wherein the concentrated sulfuric acid circulating liquid i...

Embodiment 2

[0023] A method for producing anhydrous hydrogen fluoride from ammonium fluoride acidolysis mixed liquor, comprising the following steps:

[0024] 1) Ammonium fluoride crystals and concentrated sulfuric acid with a volume concentration of 94% are subjected to an acidolysis reaction under a slight negative pressure, wherein the amount of concentrated sulfuric acid is 1.5 times the amount of concentrated sulfuric acid required to generate ammonium bisulfate;

[0025] 2) sending 20-25% of the total amount of crude hydrogen fluoride gas obtained from the acidolysis reaction into a refining system, and dissolving the remaining crude hydrogen fluoride gas in the liquid after the acidolysis reaction to obtain a mixed solution of ammonium fluoride acidolysis;

[0026] 3) Control the temperature of the ammonium fluoride acidolysis mixture at 90°C, and immediately spray it into the concentrated sulfuric acid circulating liquid, wherein the concentrated sulfuric acid circulating liquid is...

Embodiment 3

[0029] A method for producing anhydrous hydrogen fluoride from ammonium fluoride acidolysis mixed liquor, comprising the following steps:

[0030] 1) Ammonium fluoride crystals and concentrated sulfuric acid with a volume concentration of 98% are subjected to an acidolysis reaction under a slight negative pressure, wherein the amount of concentrated sulfuric acid is 1.2 times the amount of concentrated sulfuric acid required to generate ammonium bisulfate;

[0031] 2) sending 20-25% of the total amount of crude hydrogen fluoride gas obtained from the acidolysis reaction into a refining system, and dissolving the remaining crude hydrogen fluoride gas in the liquid after the acidolysis reaction to obtain a mixed solution of ammonium fluoride acidolysis;

[0032] 3) Control the temperature of the ammonium fluoride acid hydrolysis mixture at 130°C, and immediately spray it into the concentrated sulfuric acid circulating liquid, wherein the concentrated sulfuric acid circulating liq...

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PUM

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Abstract

The invention relates a fluorine-containing compound, in particular to a method for producing anhydrous hydrogen fluoride from an acid hydrolysis mixed solution of ammonium fluoride. The method comprises the following steps: 1) heating concentrated sulfuric acid to 170-220 DEG C, and keeping circulation; 2) spraying the acid hydrolysis mixed solution of ammonium fluoride to the surface of the circulating concentrated sulfuric acid, collecting gas, and performing cooling to obtain a hydrogen fluoride crude product; and 3) performing rectification and degassing on the hydrogen fluoride crude product to obtain an anhydrous hydrogen fluoride product. By use of the method provided by the invention, the anhydrous hydrogen fluoride product of which the content is more than 99.9% can be obtained, and the recovery rate of hydrogen fluoride is more than 92%. The method provided by the invention has the characteristics of simple process, low energy consumption, and safe and reliable operation, solves the problem of corrosion resistance of equipment, and improves the utilization rate of the equipment.

Description

technical field [0001] The invention relates to fluorine-containing compounds, in particular to a method for producing anhydrous hydrogen fluoride from ammonium fluoride acidolysis mixed liquor. Background technique [0002] In recent years, with the advancement of technology and the growth of demand, the application of fluorine products has penetrated into new industries such as construction, electronics, energy, environmental protection, information, and biomedicine. Fluorine resins, fluorine rubber, fluorine coatings, fluorine-containing fine chemicals, The demand for inorganic fluoride and other products is growing rapidly. However, with the rapid development of China's fluorine chemical industry, fluorite resources are becoming more and more depleted. Recycling and utilizing the rich fluorine resources in phosphate rock is not only beneficial to control fluorine pollution, but also helps to reduce the pressure on fluorite resources. . [0003] The traditional method of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/19
CPCC01B7/194C01B7/195
Inventor 何润林石寅丁慧玲
Owner GUIYANG KAILIN FERTILIZER CO LTD
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