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Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production

A technology of anhydrous hydrogen fluoride and ammonium fluorosilicate, applied in the chemical industry, can solve the problems of clogging, poor fluorine absorption effect, and large silica precipitation, etc., and achieve the effect of simple process flow, less equipment, and low production cost

Active Publication Date: 2012-09-19
WENGFU (GRP) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There will be clogging during the washing and absorption process, the fluorine absorption effect will be poor after the concentration of fluorine-containing rich solution is high, and a large amount of silica will be precipitated if the subsequent ammoniation control is not good.

Method used

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  • Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production
  • Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production
  • Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A method for preparing ammonium fluorosilicate by utilizing fluorine-containing silicon slag in the production of anhydrous hydrogen fluoride, comprising the steps of:

[0027] (1) Dissolution reaction: In a dissolution reaction kettle with a stirrer and a heating device, according to SiO 2 The calculated molar ratio of ammonium fluoride to fluorine-containing silicon slag is 12, add fluorine-containing silicon slag and ammonium fluoride solution with a mass concentration of 40%, under the conditions of temperature 90-100°C and pressure -15--10kpa A dissolution reaction occurs until the silicon slag is completely dissolved to obtain a high-concentration solution of ammonium fluorosilicate and ammonium fluoride. The ammonia and water vapor produced by the dissolution reaction are cooled to below 30°C to obtain dilute ammonia water and ammonia gas, which are sent to the phosphate fertilizer plant for fertilizer processing.

[0028] (2) Filtration: Filtrate the solution i...

Embodiment 2

[0035] A method for preparing ammonium fluorosilicate by utilizing fluorine-containing silicon slag in the production of anhydrous hydrogen fluoride, comprising the steps of:

[0036] (1) Dissolution reaction: In a dissolution reaction kettle with a stirrer and a heating device, according to SiO 2 The calculated ammonium fluoride and fluorine-containing silicon slag molar ratio is 9, adding fluorine-containing silicon slag and the mixed mother liquor obtained in step (5) and (6) of embodiment 1 and the ammonium fluoride solution with a mass concentration of 45% added, The dissolution reaction takes place under the conditions of temperature 95-105°C and pressure -12-8kpa until all the silicon slag is dissolved to obtain a mixed solution of high-concentration ammonium fluorosilicate and ammonium fluoride. The ammonia and water vapor produced by the dissolution reaction are cooled to below 30°C to obtain dilute ammonia water and ammonia gas, which are sent to the phosphate fertil...

Embodiment 3

[0044] A method for preparing ammonium fluorosilicate by utilizing fluorine-containing silicon slag in the production of anhydrous hydrogen fluoride, comprising the steps of:

[0045] (1) Dissolution reaction: the method is the same as step (1) in Example 2. Wherein, the dissolution reaction conditions are: temperature 100-108° C., pressure -5-0 kpa. The proportion of fluorine-containing silicon slag and ammonium fluoride is: SiO 2 The calculated molar ratio of ammonium fluoride to fluorine-containing silicon slag is 15.

[0046] (2) Filtration: the method is the same as step (2) of Example 1;

[0047] (3) Heat exchange: the method is the same as step (3) of embodiment 1. Among them, the hot mixed solution of ammonium fluorosilicate and ammonium fluoride is heated to 70°C through indirect heat exchange;

[0048](4) Crystallization by cooling: the method is the same as step (4) of Example 1. Among them, the cooling medium is circulating cooling water, and the mixed solutio...

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Abstract

The invention discloses a method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production. The method comprises the following steps of: under the condition that the mol ratio of ammonium fluoride calculated based on SiO2 to the fluorine-containing white slime is 9-15, adding the fluorine-containing white slime, a mixed mother liquid and a supplementary ammonium fluoride solution under the conditions that the temperature is 90-108 DEG C and the pressure is minus 15 to 0Kpa, performing a dissolution reaction until the white slime is completely dissolved, so as to obtain a dissolved solution; while the dissolved solution is hot, filtering the dissolved solution to remove undissolved SiO2 and mechanical impurities, so as to obtain a mixed solution; performing heat exchange on the mixed solution until the temperature is 60-70 DEG C; cooling to 12-30 DEG C, separating out ammonium fluorosilicate crystal and performing liquid solid separation, so as to obtain a crystallization mother liquid and crystal ammonium fluorosilicate; washing and filtering to obtain the crystal ammonium fluorosilicate; and drying the crystal ammonium fluorosilicate, so as to obtain the product ammonium fluorosilicate. The method disclosed by the invention has the advantages of simple technical process, less equipment, simplicity and convenience in operation and low production cost.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and specifically relates to a method for preparing ammonium fluorosilicate by utilizing fluorine-containing silicon slag, a by-product produced in the production of anhydrous hydrogen fluoride. [0002] Background technique [0003] A large amount of fluorosilicic acid is by-produced in the production process of phosphate fertilizer industry. When anhydrous hydrogen fluoride (AHF) is produced by the one-step method of contacting concentrated sulfuric acid with fluorosilicic acid as raw material, a large amount of fluorine-containing silicon slag is produced by-product. Silicic acid exists in the form of free fluorine and lattice fluorine. How to make good use of fluorine and silicon resources in fluorine-containing silicon slag is a major issue in clean production and comprehensive utilization of resources. [0004] Ammonium fluorosilicate [(NH 4 ) 2 SiF 6 ] Also known as ammonium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/10B09B3/00
Inventor 何浩明骆吉林刘松林汤仁恒何勇岗李白玉
Owner WENGFU (GRP) CO LTD
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