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Process for preparing potassium fluoride and co-producing white carbon black from fluosilicic acid

A technology of fluorosilicic acid and potassium fluoride, which is applied in the technical field of preparing potassium fluoride from fluorosilicic acid and co-producing white carbon black, can solve the problems of ineffective removal of silicon, high content of silicon dioxide, poor product quality and the like , to achieve the effect of reducing production cost, high activity and realizing recycling.

Inactive Publication Date: 2013-01-23
湖南有色金属投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its production cost is relatively low, but due to the low reaction rate, the silicon in potassium fluorosilicate cannot be effectively removed, resulting in high silicon dioxide content and poor product quality in the resulting potassium fluoride product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] This embodiment includes the following steps:

[0019] (1) Ammonolysis: Add 275mL of fluorosilicic acid with a mass concentration of 30% to a 1L reactor, gradually introduce 2.46mol of ammonia gas within half an hour, and then add 354mL of a mass concentration of 25% (as NH 3 ) concentrated ammonia water, stirred for 30 minutes, vacuum filtered, and washed with 500mL of water to obtain silica precipitate and ammonium fluoride solution;

[0020] (2) Alkaline hydrolysis: Add 7.4 mol of potassium hydroxide to the ammonium fluoride solution obtained in step (1), evaporate and concentrate until the mass concentration of potassium fluoride is 38%, and spray dry the potassium fluoride solution to obtain Potassium fluoride product; the ammonia gas released by evaporation is condensed and absorbed, and the obtained ammonia water is used as the ammonia water required for ammonolysis for cyclic reaction, and the unabsorbed ammonia gas is directly passed into fluorosilicic acid for...

Embodiment 2

[0023] This embodiment includes the following steps:

[0024] (1) Ammonolysis: Add 236mL of fluorosilicic acid with a mass concentration of 35% to a 1L reactor, gradually introduce 2.81mol of ammonia gas within 30 minutes, then add 410mL of ammonia water with a mass concentration of 20%, and stir the reaction After 30 minutes, vacuum filter and wash the filter cake with 500mL of water to obtain silica precipitate and ammonium fluoride solution;

[0025] (2) Alkaline hydrolysis: Add 7.4 mol of potassium hydroxide to the ammonium fluoride solution obtained in step (1), evaporate and concentrate until the mass concentration of potassium fluoride is 40%, and spray dry the potassium fluoride solution to obtain Potassium fluoride product; the ammonia gas released by evaporation is condensed and absorbed, and the obtained ammonia water is used as the ammonia water required for ammonolysis for cyclic reaction, and the unabsorbed ammonia gas is directly passed into fluorosilicic acid f...

Embodiment 3

[0028] This embodiment includes the following steps:

[0029] (1) Ammonolysis: Add 206mL of fluorosilicic acid with a mass concentration of 40% to a 1L reactor, gradually introduce 3.52mol of ammonia gas within half an hour, and then add 450mL of a mass concentration of 15% (as NH 3 ) ammonia water, stirred and reacted for 30 minutes, vacuum filtered, and washed the filter cake with 500mL water to obtain silica precipitate and ammonium fluoride solution;

[0030] (2) Alkaline hydrolysis: Add 7.6 mol of potassium hydroxide to the ammonium fluoride solution obtained in step (1), evaporate and concentrate until the potassium fluoride mass concentration is 36%, and spray dry the potassium fluoride solution to obtain Potassium fluoride product; the ammonia gas released by evaporation is condensed and absorbed, and the obtained ammonia water is used as the ammonia water required for ammonolysis for cyclic reaction, and the unabsorbed ammonia gas is directly passed into fluorosilicic...

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Abstract

The invention discloses a process for preparing potassium fluoride and co-producing white carbon black from fluosilicic acid. The process comprises the following steps of: 1, ammonolysis: sequentially adding ammonia gas and ammonia water in the fluosilicic acid with the mass concentration of 20-45 percent, stirring for reacting for 25-35min, and then filtering and washing to obtain a silica sediment and an ammonium fluoride solution; 2, alkaline hydrolysis: adding potassium hydroxide in the ammonium fluoride solution obtained in the step 1 under the condition that the mol ratio of the potassium hydroxide to the ammonium fluoride solution is (1.05-1.10):1.00, reacting the ammonium fluoride with the potassium hydroxide to generate potassium fluoride, evaporating and concentrating until the mass concentration of the potassium fluoride is not less than 35 percent, and spraying the potassium fluoride solution to be dried to obtain a potassium fluoride product; and 3, drying the silica sediment to obtain the white carbon black. The process has the advantages of low production cost and good product quality.

Description

technical field [0001] The invention relates to a process for preparing potassium fluoride and co-producing white carbon black with fluosilicic acid. Background technique [0002] Fluosilicic acid is a by-product produced during the production of phosphate fertilizers and anhydrous hydrofluoric acid. At present, the silicon dioxide content in acid-grade fluorite powder is 1.0-1.6%. Every ton of anhydrous hydrogen fluoride produced will produce 0.2t of fluorosilicic acid by-product. (33.5%). Compared with the by-product of phosphate fertilizer, fluosilicic acid, its impurity content is lower, and the concentration of fluosilicic acid is higher, which has higher recycling value. However, the products produced with fluosilicic acid as raw materials generally have the problem that the silicon content in the product is too high and the product quality is not high, which seriously affects the recycling of fluosilicic acid. In this way, not only will it cause a serious waste of fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/02C01B33/12
Inventor 李程文廖志辉刘东晓曹崇高彭颂生段立山梁雅娟
Owner 湖南有色金属投资有限公司
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