Method for preparing ammonium hydrogen fluoride by circularly treating fluosilicic acid through sylvite

A technology for ammonium bifluoride and cyclic treatment, which is applied in the field of phosphorus chemical industry, can solve the problems of low one-time yield of ammonium bifluoride, high equipment requirements and investment, and restricted application, so as to reduce production costs, reduce production energy consumption, and operate with greater flexibility Effect

Active Publication Date: 2018-08-24
HUBEI XIANGYUN GROUP CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of the above two process routes are as follows: (1) the first process route requires a large amount of expensive hydrogen fluoride, and the amount of hydrogen fluoride accounts for 35% of the total mass of ammonium bifluoride; (2) the second process route uses decomposition technology, A decomposition temperature of 130-180°C is required, high energy consumption, high equipment requirements and investment, and low one-time yield of ammonium bifluoride
These technical defects have greatly restricted the application of the above-mentioned process route in industrial production

Method used

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  • Method for preparing ammonium hydrogen fluoride by circularly treating fluosilicic acid through sylvite

Examples

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Effect test

Embodiment 1

[0042] Add 220g of potassium fluorosilicate to ammonia water (347g) with a mass concentration of 20%, stir and react at 40°C for 40 minutes, let it stand for 10 minutes, and filter to obtain a silica filter cake and potassium fluoride-ammonium fluoride solution. The silicon filter cake is washed and dried to obtain a white carbon black product. The washing filtrate was combined with potassium fluoride-ammonium fluoride solution, and fluorosilicic acid (1200g) with a mass concentration of 12% was added, stirred and reacted at 40°C for 20 minutes, left to stand for 10 minutes, and filtered to obtain potassium fluorosilicate and ammonium bifluoride-fluoride ammonium chloride solution. Add hydrogen fluoride to the ammonium bifluoride-ammonium fluoride solution at 30°C to adjust the pH of the solution to 3 to obtain an ammonium bifluoride solution, which is concentrated and dried at an absolute pressure of 35kPa (drying temperature is 80°C) to obtain ammonium bifluoride product. ...

Embodiment 2

[0045] Add 220g of potassium fluorosilicate to ammonia water (463g) with a mass concentration of 15%, stir and react at 30°C for 30min, let it stand for 10min, and filter to obtain a silica filter cake and potassium fluoride-ammonium fluoride solution. The silicon filter cake is washed and dried to obtain a white carbon black product. The washing filtrate was combined with potassium fluoride-ammonium fluoride solution, and fluorosilicic acid (1030g) with a mass concentration of 14% was added, stirred and reacted at 40°C for 15 minutes, left to stand for 10 minutes, and then filtered to obtain potassium fluorosilicate and ammonium bifluoride-fluoride ammonium chloride solution. Add hydrogen fluoride to the ammonium bifluoride-ammonium fluoride solution at 50°C to adjust the pH of the solution to 3 to obtain an ammonium bifluoride solution, which is concentrated and dried at an absolute pressure of 80kPa (drying temperature is 100°C) to obtain ammonium bifluoride product.

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Embodiment 3

[0048] Add 220g of potassium fluorosilicate to ammonia water (694g) with a mass concentration of 10%, stir and react at 70°C for 30min, let it stand for 10min, and filter to obtain a silica filter cake and potassium fluoride-ammonium fluoride solution. The silicon filter cake is washed and dried to obtain a white carbon black product. The washing filtrate was combined with the potassium fluoride-ammonium fluoride solution, and fluorosilicic acid (800g) with a mass concentration of 18% was added, stirred and reacted at 50°C for 30 minutes, left to stand for 10 minutes, and then filtered to obtain potassium fluorosilicate and ammonium bifluoride-fluorine ammonium chloride solution. Add hydrogen fluoride to the ammonium bifluoride-ammonium fluoride solution at 30°C to adjust the pH of the solution to 3 to obtain an ammonium bifluoride solution, which is concentrated and dried at an absolute pressure of 50kPa (the drying temperature is 90°C) to obtain ammonium bifluoride product....

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Abstract

The invention discloses a method for preparing ammonium hydrogen fluoride by circularly treating fluosilicic acid through sylvite, and belongs to the technical field of phosphorus chemical industry. The method comprises the following steps: reacting potassium fluosilicate with ammonia water, after reaction is finished, carrying out solid-liquid separation to obtain a potassium fluoride-ammonium fluoride solution and a silicon dioxide filter cake, and preparing white carbon black from the silicon dioxide filter cake; reacting the potassium fluoride-ammonium fluoride solution with the fluosilicic acid, after reaction is finished, carrying out solid-liquid separation to obtain an ammonium hydrogen fluoride-ammonium fluoride solution and potassium fluosilicate, and returning the potassium fluosilicate into step (1) as a raw material; and feeding hydrogen fluoride in the ammonium hydrogen fluoride-ammonium fluoride solution to enable ammonium fluoride to be completely converted into ammonium hydrogen fluoride so as to obtain an ammonium hydrogen fluoride solution, and carrying out concentration and drying to obtain ammonium hydrogen fluoride. The method has the economic value that the ammonium hydrogen fluoride and the white carbon black which have high value can be obtained simultaneously, and fluorosilicone resources are comprehensively and effectively utilized.

Description

technical field [0001] The invention belongs to the technical field of phosphorus chemical industry, and in particular relates to a method for preparing ammonium bifluoride by recycling fluosilicic acid with potassium salts. Background technique [0002] During the production process of wet-process phosphoric acid, a large amount of dilute fluorosilicic acid will be produced by-product. This substance has certain toxicity and corrosiveness, and its direct discharge will cause serious pollution to the environment. If it can be used effectively, it can not only reduce pollution, but also convert the contained fluorine into fluorine products with high economic value, so that the utilization of fluorosilicic acid in enterprises can be raised to a new level, and the output value and profit can be increased. The selection of the target fluorine product determines the technical route of the utilization of fluosilicic acid. Ammonium bifluoride is one of the better target products. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05C01B33/18
CPCC01B33/186C01C1/162C01P2006/12C01P2006/80
Inventor 黄忠何俊胡挺余双强饶济高开元查炎华
Owner HUBEI XIANGYUN GROUP CHEM
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