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

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...

Examples

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...

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...

Examples

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...