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Method for preparing fluorine hydride from acidic mixture of inorganic fluoride and sulphuric acid

A technology of fluoride and mixture, which is applied in the recycling of fluoride, and in the field of recovery in the form of hydrogen fluoride, which can solve problems such as short service life, narrowing the selection range of equipment structure and materials, and demanding equipment structure and materials.

Inactive Publication Date: 2009-01-28
GUIZHOU RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disadvantages of the existing technical solutions are: due to the high operating pressure and temperature of the reaction volatilization, distillation separation, or rectification separation process and the long residence time of the material in the equipment, the requirements for the equipment structure and materials are very strict. , so the selection range of equipment structure and materials is greatly reduced, and the equipment also has disadvantages such as short service life and low operation safety, especially for fluorine such as ammonium fluoride, sodium fluoride, potassium fluoride, magnesium fluoride, etc. The heating reaction volatilization of the acidic mixture of compound salts and sulfuric acid, or the process of distillation and separation, there is no suitable equipment structure and material to meet the requirements of its large-scale production under the current industrial technology level.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Take NH respectively 4 80g of solid ammonium fluoride with 95% F content, H 2 SO 4 320g of concentrated sulfuric acid with a content of 96%; slowly add the two raw materials into the reactor simultaneously or successively to obtain an acidic mixture of ammonium fluoride and sulfuric acid, control the absolute pressure of the gas phase in the reactor space to 0.02MPa or vacuum degree -0.08MPa, and control the fluorine The temperature of the acidic mixture of ammonium chloride and sulfuric acid is 120°C to 130°C, and the reaction is stopped after 30 minutes of heat preservation and reaction distillation. The gas mixture of 43g of hydrogen fluoride and water was volatilized during the reaction, distillation and separation, leaving 357g of raffinate. After testing, the volatilization rate of HF is 97.1%.

Embodiment 2

[0026] Embodiment 2: take by weighing respectively the solid sodium fluoride 88g of NaF content 98%, H 2 SO 4 320g of concentrated sulfuric acid with a content of 96%; slowly add the two raw materials into the reactor simultaneously or successively to obtain an acidic mixture of sodium fluoride and sulfuric acid. The temperature of the acidic mixture of sodium chloride and sulfuric acid is 140°C to 150°C, and the reaction is stopped after 60 minutes of heat preservation and reaction distillation. The gas mixture of 47g of hydrogen fluoride and water was volatilized during the reaction, distillation and separation, leaving 361g of raffinate. After testing, the volatilization rate of HF is 98.4%.

Embodiment 3

[0027]Embodiment 3: take by weighing respectively the hydrofluoric acid 93g of HF content 40%, H 2 SO 4 214.5g of concentrated sulfuric acid with a content of 96%; slowly add the two raw materials into the reactor simultaneously or successively to obtain an acidic mixture of hydrogen fluoride and sulfuric acid, control the temperature of the acidic mixture of hydrogen fluoride and sulfuric acid at 90°C to 100°C, and control the reactor space The absolute pressure of the gas phase is 0.01~0.02MPa or the vacuum degree is -0.08~-0.09MPa, and the reaction is stopped after 60min of heat preservation and distillation. A total of 38.5 g of a gaseous mixture of hydrogen fluoride and water was volatilized by distillation and separation, leaving 269 g of raffinate. After testing, the volatilization rate of HF is 94.5%.

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PUM

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Abstract

The invention discloses a method for preparing hydrogen fluoride with an acid mixture of inorganic fluoride and sulfuric acid and relates to a fluoride. The hydrogen fluoride gas is prepared by controlling operating conditions of the reaction volatilization, or distillation separation, or rectification separation process of the acid mixture of the inorganic fluoride and the sulfuric acid in a conventional equipment space, especially the pressure condition and the temperature condition, and carrying out a heat and mass transfer process to cause the water and sulfuric acid and sulfate in the acid mixture to be kept on a liquid phase. When the hydrogen fluoride is purified, a 40% hydrofluoric acid or anhydrous hydrogen fluoride is prepared. The method is suitable for recovering and preparing the hydrogen fluorine from the fluorine of the fluorine-containing intermediate materials or 'three industrial wastes' with the fluorine produced in the processes of chemical industry, electronics industry, glass machining industry, aluminum alloy machining industry and the like to make hydrogen. The method is especially suitable for enterprises to recover the materials with fluorine separated from the phosphoric acid, phosphate fertilizer and other phosphate chemical products produced by the wet process and make the hydrogen fluoride, or for the comprehensive utilization of the 'three industrial wastes' with fluorine.

Description

technical field [0001] The present invention relates to fluorides, in particular to the recovery and utilization of fluorides from inorganic or organic materials in the chemical industry, electronics industry, glass processing and aluminum alloy processing industries, especially a method for recycling in the form of hydrogen fluoride. Background technique [0002] As we all know, in the production process of fluorine chemical industry, phosphorus chemical industry, electronics industry, glass processing and aluminum alloy processing and other industries, waste gas, waste liquid and waste residue containing fluorine elements will be generated, which can be converted into waste liquid through purification and washing of waste gas or waste residue. At present, these waste liquids and waste residues containing fluorine elements have not been efficiently recycled, and only simple treatment is carried out to meet environmental protection requirements. For example, the phosphorus ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/19
Inventor 唐波陈文兴张筑楠丁禹
Owner GUIZHOU RES INST OF CHEM IND
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