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Method for producing ammonium fluoride by recovering fluorine resources

A technology of ammonium fluoride and resources, applied in the chemical industry, can solve the problems of low ammonium fluoride concentration and high energy consumption, and achieve the effects of reducing pollution, reducing energy consumption and increasing concentration

Inactive 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

[0005] The above-mentioned technologies all directly use fluosilicic acid and ammonia water as raw materials by-products of wet-process phosphoric acid, and the resulting filtrate has a low concentration of ammonium fluoride, and the energy consumption is high during the concentration process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A method for recovering fluorine resources to produce ammonium fluoride, comprising the following steps:

[0017] (1) Preparation of ammonium fluoride: Dissolve silicon slag with a mass concentration of 8% fluorine and ammonium fluoride at a mass concentration of 22% at 105°C. The amount of ammonium fluoride is 1.3 times the theoretical amount to obtain a transparent The ammonium fluorosilicate solution was cooled to 30°C and passed through ammonia gas until the pH value was 9.0, and the white carbon black was precipitated, and the white carbon black solid and the ammonium fluoride solution with a mass concentration of 21% were obtained by filtration. The ammonium fluoride solution Return in the amount needed to react with silicon slag;

[0018] (2) Concentration: The remaining ammonium fluoride solution is mixed with the mother liquor after ammonium fluoride crystallization, preheated by a heat exchanger, enters the concentration device, and is concentrated under the p...

Embodiment 2

[0022] A method for recovering fluorine resources to produce ammonium fluoride, comprising the following steps:

[0023] (1) Preparation of ammonium fluoride: Dissolve silicon slag with a mass concentration of 15% fluorine and ammonium fluoride at a mass concentration of 18% at 108°C. The amount of ammonium fluoride is 1.5 times the theoretical amount to obtain a transparent The ammonium fluorosilicate solution was cooled to 50°C and passed through ammonia gas until the pH value was 9.8, and the white carbon black was precipitated, and the white carbon black solid and the ammonium fluoride solution with a mass concentration of 16% were obtained by filtration. The ammonium fluoride solution Return in the amount needed to react with silicon slag;

[0024] (2) Concentration: The remaining ammonium fluoride solution is mixed with the mother liquor after ammonium fluoride crystallization, preheated by a heat exchanger, enters the concentration device, and is concentrated under the ...

Embodiment 3

[0028] A method for recovering fluorine resources to produce ammonium fluoride, comprising the following steps:

[0029] (1) Preparation of ammonium fluoride: Dissolve silicon slag with a mass concentration of 5% fluorine and ammonium fluoride at a mass concentration of 25% at 95°C. The amount of ammonium fluoride is twice the theoretical amount to obtain a transparent The ammonium fluorosilicate solution was cooled to 40°C and passed through ammonia gas until the pH value was 9.5, and the white carbon black was precipitated, and the white carbon black solid and the ammonium fluoride solution with a mass concentration of 23% were obtained by filtration. The ammonium fluoride solution Return in the amount needed to react with silicon slag;

[0030] (2) Concentration: The remaining ammonium fluoride solution is mixed with the mother liquor after ammonium fluoride crystallization, preheated by a heat exchanger, enters the concentration device, and is concentrated under the pressu...

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PUM

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Abstract

The invention discloses a method for producing ammonium fluoride by recovering fluorine resources. The method comprises the following steps of: dissolving fluorine-containing silicon dregs and ammonium fluoride at the temperature of between 95 and 108 DEG C to obtain a transparent ammonium fluosilicate solution, cooling, introducing ammonia gas until the pH value is between 9.0 and 9.8, precipitating to separate white carbon black out, filtering to obtain a white carbon black solid and an ammonium fluoride solution, and returning the ammonium fluoride solution according to the quantity required by reacting with silicon dregs; mixing the residual ammonium fluoride solution with a mother solution formed by crystallizing ammonium fluoride, and concentrating the mixture in a concentration device until the mass concentration of the ammonium fluoride is between 60 and 80 percent; conveying the ammonium fluoride into a cooling crystallizer, cooling and crystallizing for 4 to 7 hours, and precipitating ammonium fluoride crystals to obtain an ammonium fluoride solid-liquid mixture; and filtering and separating the ammonium fluoride solid-liquid mixture to obtain the ammonium fluoride crystals. By the method, the concentration of the ammonium fluoride can be improved, the energy consumption in the concentration process can be reduced, fluorine in the fluorine-containing silicon dregs is recovered, phosphorite associated fluorine resources are utilized fully, and the pollution of the fluorine-containing silicon dregs to environment is reduced.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for producing ammonium fluoride by recovering fluorine resources in fluorine-containing silicon slag. [0002] Background technique [0003] In the process of producing phosphoric acid from phosphate rock, a large amount of silicon tetrafluoride gas is produced. At present, the most commonly used method is to absorb silicon tetrafluoride with water to generate fluorosilicic acid, and then use fluorosilicic acid to produce other products, and recover fluorine associated with phosphate rock. resource. [0004] At present, the methods for producing ammonium fluoride by recovering the associated fluorine resources of phosphate rock are: 200710066136.2 Use fluosilicic acid and ammonia water as raw materials for step-by-step ammoniation reaction, filter, wash, and dry to obtain white carbon black and high-concentration ammonium fluoride mother liquor. 200610017485....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16C01B33/12
Inventor 何浩明刘松林汤仁恒骆吉林
Owner WENGFU (GRP) CO LTD
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