Method for preparing hydrogen fluoride from flousper powder and sulfuric acid

A technology for sulfuric acid production and fluorite powder, which is applied in the direction of fluorine/hydrogen fluoride, calcium/strontium/barium sulfate, etc., can solve the problems of high refining cost of hydrogen fluoride products, no industrialized production line, and high production cost of hydrogen fluoride, and achieve novel process routes , Obvious energy saving and pollution reduction effect

Active Publication Date: 2013-01-23
衢州市鼎盛化工科技有限公司
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AI Technical Summary

Problems solved by technology

However, glacial acetic acid is a volatile raw material, so it is difficult to recover and the cost is high. Moreover, the miscibility between glacial acetic acid and hydrogen fluoride is very high, which makes the cost of refining hydrogen fluoride products high. When phosphoric acid is used as the medium, phosphoric acid reacts with fluorite powder and hydrogen fluoride , generate fluorophosphoric acid and fluorophosphate, both phosphoric acid and hydrogen fluoride are consumed; it also makes the refining of hydrogen fluoride difficult or expensive, and the price of phosphoric acid is also expensive, which will make the production cost of hydrogen fluoride very high; therefore, no industrialized production line has been formed at present

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  • Method for preparing hydrogen fluoride from flousper powder and sulfuric acid
  • Method for preparing hydrogen fluoride from flousper powder and sulfuric acid

Examples

Experimental program
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Effect test

Embodiment 1

[0031] 1. Using fluorite powder with a mass percentage of 97% of calcium fluoride and sulfuric acid with a mass percentage of 93% as raw materials. Crush the fluorite powder from about 90 mesh to 280-320 mesh.

[0032] 2. Set up a 500L jacketed and agitated reactor, with 0.6MPa steam in the jacket; by controlling the amount of steam, the reaction temperature can be controlled.

[0033] 3. Put 132kg of sulfuric acid with a mass percentage of 93% into the reaction kettle; open the steam valve to heat the sulfuric acid to 120°C, and slowly add 20kg of fluorite powder under stirring; at this time, the molar ratio of calcium fluoride to sulfuric acid is about fluoride Calcium:sulfuric acid=1:5. Stir; control the reaction temperature at 90°C to 120°C; fully react. After the reaction, hydrogen fluoride gas and calcium sulfate solid (gypsum) are produced, and the produced hydrogen fluoride gas is purified and condensed to become hydrogen fluoride liquid. Then the sulfuric acid and ...

Embodiment 2

[0036] 1. Using fluorite powder with a mass percentage of 97% of calcium fluoride and sulfuric acid with a mass percentage of 93% as raw materials. Crush the fluorite powder from about 90 mesh to 480-520 mesh.

[0037] 2. Set up a 500L jacketed and agitated reactor, with 0.6MPa steam in the jacket; by controlling the amount of steam, the reaction temperature can be controlled.

[0038]3. Put 264kg of sulfuric acid with a mass percentage of 98% into the reaction kettle; open the steam valve to heat the sulfuric acid to 150°C, and slowly add 20kg of fluorite powder under stirring; at this time, the molar ratio of calcium fluoride to sulfuric acid is about fluoride Calcium:sulfuric acid=1:10. Stir; control the reaction temperature at 120°C to 150°C; fully react. After the reaction, hydrogen fluoride gas and calcium sulfate solid (gypsum) are produced, and the produced hydrogen fluoride gas is purified and condensed to become hydrogen fluoride liquid. Then the sulfuric acid and...

Embodiment 3

[0041] 1. Using fluorite powder with a mass percentage of 97% of calcium fluoride and sulfuric acid with a mass percentage of 93% as raw materials. Crush the fluorite powder from about 90 mesh to 780-820 mesh.

[0042] 2. Set up a 500L jacketed and agitated reactor, with heat transfer oil inside the jacket; the reaction temperature of the materials in the reactor is controlled by electrically heating the heat transfer oil.

[0043] 3. Put 395kg of sulfuric acid with a mass percentage of 98% into the reaction kettle; start the electric heating system, raise the temperature of sulfuric acid to 180°C, and slowly add 20kg of fluorite powder under stirring; at this time, the molar ratio of calcium fluoride to sulfuric acid About calcium fluoride: sulfuric acid = 1:15. Stir; control the reaction temperature at 150°C to 180°C; fully react. After the reaction, hydrogen fluoride gas and calcium sulfate solid (gypsum) are produced, and the produced hydrogen fluoride gas is purified an...

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Abstract

The invention discloses a method for preparing hydrogen fluoride from flousper powder and sulfuric acid. The method comprises the following specific steps of: adding solution of sulfuric acid and the flousper powder into a reactor with a stirrer respectively, wherein the molar ratio of calcium fluoride to the sulfuric acid is 1:3-1:30, the granularity of the flousper powder is 280 to 1,220 meshes, and the reaction temperature is controlled to between 90 and 300 DEG C; generating hydrogen fluoride gas and calcium sulfate solid after the reaction; purifying, condensing and rectifying the hydrogen fluoride gas to obtain anhydrous hydrogen fluoride, or purifying and absorbing the hydrogen fluoride gas to obtain hydrofluoric acid; transferring the calcium sulfate solid and the sulfuric acid toa filtering system from the reactor to perform solid-liquid separation; returning the separated solution of sulfuric acid to the reactor; and washing and drying the calcium sulfate solid separated from the sulfuric acid to form a by-product. The method has the advantages of simple equipment, high reaction efficiency, low cost and easy industrialized production.

Description

technical field [0001] The invention relates to a method for producing hydrogen fluoride, more specifically a method for producing hydrogen fluoride with fluorite powder and sulfuric acid as raw materials. Background technique [0002] Hydrogen fluoride is the basic raw material of fluorine chemical industry, molecular formula HF; hydrogen fluoride and its aqueous solution can be used to manufacture organic or inorganic fluorides, such as fluorocarbons, various fluorine refrigerants, fluororesins, aluminum fluoride, potassium fluoride, cryolite etc., can be used for glass etching, electroplating, ceramic treatment, petroleum industry catalyst, frosted bulb manufacturing, metal casting desanding, graphite ash removal, metal cleaning (brass, stainless steel) and semiconductor (germanium, silicon) manufacturing, etc.; The main raw material for the manufacture of elemental fluorine. [0003] The traditional production method of hydrogen fluoride is to use fluorite powder and su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/19C01F11/46
Inventor 应盛荣周贞锋徐建国叶文龙应学来姜战
Owner 衢州市鼎盛化工科技有限公司
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