Method for producing ammonium bifluoride by recovering fluorine resource from fluorine-containing silicon slag

A technology of ammonium bifluoride and fluorine-containing silicon slag, which is applied in the chemical industry, can solve the problems of high production cost, high energy consumption, and large amount of hydrogen fluoride, and achieve the effects of low production cost, reduced pollution, and reduced consumption

Active Publication Date: 2012-06-13
WENGFU (GRP) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent 200610017486.5 discloses "a method for producing ammonium bifluoride and co-production of white carbon black", in which white carbon black and ammonium fluoride are prepared from fluorosilicic acid or ammonium fluorosilicate and ammonia water, and the ammonium fluoride solution is concentrated, Pyrolysis produces liquid ammonium bifluoride and ammonia gas. The decomposition temperature is 130-180°C. Liquid ammonium bifluoride is cooled to produce solid ammonium bifluoride. During the proces

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for recovering fluorine resources in fluorine-containing silicon slag to produce ammonium bifluoride, comprising the steps of:

[0022] (1) Precipitate the fluorine in the fluorine-containing silicon slag and convert it into ammonium fluoride:

[0023] Dissolve silicon slag with a mass concentration of 5% fluorine and an ammonium fluoride solution with a mass concentration of 18% at a temperature of 90°C to 102°C and a pressure of -3KPa (gauge pressure); the obtained ammonium fluorosilicate solution After cooling, feed ammonia gas, control the temperature at 30°C to 60°C, and precipitate white carbon black; filter and wash to obtain white carbon black solids and ammonium fluoride solution with a mass concentration of 16%;

[0024] (2) Reaction: The reaction between ammonium fluoride and anhydrous hydrogen fluoride is a rapid exothermic reaction. Using this property, anhydrous hydrogen fluoride is passed into a reaction tank with a water cooling jacket, and the ...

Embodiment 2

[0030] A method for recovering fluorine resources in fluorine-containing silicon slag to produce ammonium bifluoride, comprising the steps of:

[0031] (1) Precipitate the fluorine in the fluorine-containing silicon slag and convert it into ammonium fluoride:

[0032] Dissolve silicon slag with a mass concentration of 10% fluorine and ammonium fluoride solution with a mass concentration of 25% at a temperature of 95°C to 105°C and a pressure of -10KPa (gauge pressure); the resulting ammonium fluorosilicate solution After cooling, feed ammonia, control the temperature at 40°C to 70°C, and precipitate white carbon black; filter and wash to obtain white carbon black solids and ammonium fluoride solution with a mass concentration of 23%;

[0033] (2) Reaction: The reaction between ammonium fluoride and anhydrous hydrogen fluoride is a rapid exothermic reaction. Using this property, anhydrous hydrogen fluoride is passed into a reaction tank with a water cooling jacket, and the liqu...

Embodiment 3

[0039] A method for recovering fluorine resources in fluorine-containing silicon slag to produce ammonium bifluoride, comprising the steps of:

[0040] (1) Precipitate the fluorine in the fluorine-containing silicon slag and convert it into ammonium fluoride:

[0041]Dissolve silicon slag with a mass concentration of 15% fluorine and ammonium fluoride solution with a mass concentration of 30% at a temperature of 98°C to 108°C and a pressure of -15KPa (gauge pressure); the resulting ammonium fluorosilicate solution After cooling, feed ammonia gas, control the temperature at 40°C to 80°C, and precipitate white carbon black; filter and wash to obtain white carbon black solids and ammonium fluoride solution with a mass concentration of 28%;

[0042] (2) Reaction: The reaction between ammonium fluoride and anhydrous hydrogen fluoride is a rapid exothermic reaction. Using this property, anhydrous hydrogen fluoride is passed into a reaction tank with a water cooling jacket, and the l...

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Abstract

The invention discloses a method for producing ammonium bifluoride by recovering a fluorine resource from fluorine-containing silicon slag. The method comprises the following steps of: dissolving fluorine-containing silicon slag and an ammonium fluoride solution, cooling an obtained ammonium fluosilicate solution, introducing gas ammonia, and precipitating white carbon black out; filtering and washing to obtain a white carbon black solid and an ammonium fluoride solution; introducing anhydrous hydrogen fluoride into the ammonium fluoride solution, uniformly mixing the anhydrous hydrogen fluoride with the ammonium fluoride solution, and fully reacting till the pH of the solution is 2-4 to obtain an ammonium hydrogen fluoride of which the mass concentration is 21-37 percent; mixing with a crystallized ammonium hydrogen fluoride mother solution, and performing triple-effect evaporation and concentration till the mass concentration of the ammonium hydrogen fluoride is 60-80 percent; feeding into a crystallizer, and cooling and crystallizing for 3-7 hours to obtain an ammonium hydrogen fluoride solid-liquid mixture; and separating to obtain an ammonium bifluoride product and an ammonium bifluoride mother solution. The method has the advantages of low using amount of fluorine hydride, high concentration of ammonium bifluoride, low energy consumption in a concentrating process, low production cost, easiness and convenience for operating, and easiness for realizing industrialization.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for recovering fluorine resources in fluorine-containing silicon slag to produce ammonium bifluoride. [0002] Background technique [0003] During the production process of phosphate fertilizer industry, a large amount of fluosilicic acid is produced as a by-product. When anhydrous hydrogen fluoride is produced by using concentrated sulfuric acid as a raw material, a large amount of fluorine-containing silicon slag is produced by-product. Forms exist, including free fluorine and lattice fluorine. How to make good use of the fluorine resource in the fluorine-containing silicon slag is a major subject to be studied. [0004] Ammonium bifluoride is mainly used as glass etchant, chemical reagent, boiler cleaning agent, fermentation industry disinfectant, steel plate surface treatment agent, oil mining plugging agent, fine ceramic filler, etc. [0005] The tradi...

Claims

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Application Information

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IPC IPC(8): C01C1/16B09B3/00
Inventor 何浩明骆吉林汤仁恒刘松林
Owner WENGFU (GRP) CO LTD
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