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Method for preparing hydrogen fluoride by using phosphorus fertilizer by-product fluosilicic acid

A fluorosilicic acid and by-product technology, applied in fluorine/hydrogen fluoride, silicon oxide, etc., can solve the problems of fluorine pollution, waste of fluorite resources, etc., and achieve the effect of increasing investment, good economic benefits, and increasing the added value of raw materials

Inactive Publication Date: 2014-04-30
SHANDONG BOFENG LIZHONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the by-product fluosilicic acid cannot be recycled, it will not only cause serious fluorine pollution, but also seriously waste the dwindling fluorite resources.

Method used

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  • Method for preparing hydrogen fluoride by using phosphorus fertilizer by-product fluosilicic acid

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Experimental program
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Effect test

Embodiment 1

[0023] Add 260g, 14% fluosilicic acid solution to the reactor with stirrer, the temperature is 20-25°C, then slowly drop 55g, 31% concentrated ammonia water into the fluosilicic acid solution, after the reaction is completed, The temperature is 55-60°C, aged for 40 minutes, and then the first step of filtration is carried out. The filter cake obtained by filtration is washed several times to recover the fluorine mother liquor, and 33g of 31% concentrated ammonia water is slowly dripped into the filtrate obtained by the first step of filtration. After the reaction is completed, the temperature is 50-56 ° C, aged for 40 minutes, and then the second step of filtration is carried out, and the filtered cake is washed several times to recover the fluorine mother liquor; the solution obtained in the second step is evaporated, concentrated and crystallized to obtain ammonia hydrogen fluoride Solid and ammonia gas, the collected ammonia gas can be made into ammonia water, which can be d...

Embodiment 2

[0031] Operation is with embodiment 1. Add 175g, 20% fluosilicic acid solution to the reactor with stirrer, the temperature is 20-25°C, then slowly drop 48g, 35% concentrated ammonia water into the fluosilicic acid solution, after the reaction is completed, The temperature is 71-76°C, aged for 40 minutes, and then the first step of filtration is carried out. The filter cake obtained by filtration is washed several times to recover the fluorine mother liquor, and 28g of 35% concentrated ammonia water is slowly added to the filtrate obtained by the first step of filtration. After the reaction is completed, the temperature is 65-70°C, aged for 40 minutes, and then the second step of filtration is carried out, and the filtered cake is washed several times to recover the fluorine mother liquor; Ammonia gas, the collected ammonia gas can be directly used in the subsequent ammoniation reaction to make ammonia water; the ammonia hydrogen fluoride obtained in the third step is dissolve...

Embodiment 3

[0033] Operation is with embodiment 1. Add 175g, 20% fluosilicic acid solution to the reactor with stirrer, the temperature is 20-25°C, then slowly drop 42g, 40% concentrated ammonia water into the fluosilicic acid solution, after the reaction is completed, The temperature is 87-92°C, age for 40 minutes, and then perform the first step of filtration. The filter cake obtained by filtration is washed several times to recover the fluorine mother liquor, and slowly drop 24.5g of 40% concentrated ammonia water into the filtrate obtained by the first step of filtration. , after the reaction is completed, the temperature is 81-86 ° C, aged for 40 minutes, and then the second step of filtration is carried out, and the filtered cake is washed several times to recover the fluorine mother liquor; the solution obtained in the second step is evaporated, concentrated and crystallized, and ammonia hydrogen fluoride is solid and ammonia gas, the collected ammonia gas can be made into ammonia ...

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Abstract

The present invention discloses a method for preparing hydrogen fluoride by using a phosphorus fertilizer by-product fluosilicic acid. The method comprises that: fluosilicic acid is subjected to ammonification to produce a fluorinated ammonia solution; ammonification conditions of every step are controlled to adjust the morphology and the specific surface area of white carbon black aggregate, such that the produced white carbon black filter cake has characteristics of easy filtration, easy washing and high activity structure; and the filtered filter cake is washed a plurality of times with a dilute fluorinated ammonia solution and clear water, the entrained fluorine mother liquor is recovered, and the fluorinated ammonia solution is adopted to further produce hydrofluoric acid, such that fluorine and silicon in the fluosilicic acid are completely converted into the fluorine product and the silicon product so as to be utilized. According to the present invention, fluosilicic acid, sulfuric acid, liquid ammonia and other raw materials are processed into the useful products so as to protect fluorite and the fluorine resources, substantially increase the raw material added value, and provide good economic benefits; the intermediate product ammonium hydrogen difluoride can be adopted as the product so as to be directly sold; and the fluorinated ammonia product can be produced if the investment is slightly increased, such that the product variety can be conveniently adjusted so as to adapt to market demands.

Description

technical field [0001] The invention relates to a method for preparing hydrogen fluoride, in particular to a method for preparing hydrogen fluoride by using fluorosilicic acid, a by-product of phosphate fertilizer. Background technique [0002] In nature, the minerals that can be used as fluorine resources are limited to fluorite, natural cryolite and phosphate rock. The fluorine content in fluorite is high, but its reserves are limited. In recent years, the global fluorspar powder price has shown an increasing trend. In addition, the reserves of natural cryolite are also very small, which is far from meeting the needs of the electrolytic aluminum industry. Phosphate rock has a large reserve and is an important fluorine resource. When phosphate rock is used as raw material to produce wet-process phosphoric acid and phosphate fertilizer, a large amount of fluorine-containing gas will be emitted, which can be absorbed and treated by water to obtain fluorosilicic acid. Acco...

Claims

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Application Information

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IPC IPC(8): C01B7/19C01B33/113
Inventor 刘涛高艳红韩玉莲袁勇
Owner SHANDONG BOFENG LIZHONG CHEM
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