Preparation method of fluoride

A technology of fluoride and silicon tetrafluoride, applied in the direction of fluorine/hydrogen fluoride, silicon oxide, silicon dioxide, etc., can solve the problem that the downstream products of sodium fluorosilicate cannot achieve high-efficiency and high-efficiency comprehensive utilization and comprehensive silicon resources. Utilize the problems of low added value and low economic benefits to achieve the effect of avoiding waste water and slag, efficient utilization and less environmental load

Active Publication Date: 2013-04-17
KUNMING DAOERSEN TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The above is the traditional process and product status of the downstream product development of sodium fluorosilicate by phosphate fertilizer enterprises. No matter what process route is adopted, there are the following disadvantages: low added value for the comprehensive utilization of silicon resources and low economic benefits; various processes The route will produce "three wastes" pollution, which cannot be recycled
All in all, at present, the development of downstream products of sodium fluorosilicate by phosphate fertilizer enterprises has failed to achieve high efficiency and high benefit comprehensive utilization

Method used

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  • Preparation method of fluoride

Examples

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Embodiment 1

[0026] At 80°C, add 1000g of sodium fluorosilicate and an equal amount of concentrated sulfuric acid into the reactor for reaction to obtain hydrogen fluoride and silicon tetrafluoride gas, and sodium sulfate as a by-product. The two gases are dehydrated, dust-removed, condensed and separated to obtain anhydrous hydrogen fluoride product. Silicon tetrafluoride gas is passed into water, the molar ratio of silicon tetrafluoride and water is controlled at 3:2, the pressure of silicon tetrafluoride gas is controlled at 400mbar, the hydrolysis temperature is controlled at 20°C, and the hydrolysis time is controlled at 40min to obtain active white Carbon black and fluosilicic acid solution, after suction filtration, the vacuum degree is controlled at 0.02MPa, the amount of washing and washing water is controlled at 10% of the filter cake, drying, and the drying temperature is controlled at 100°C, and dried for 2 hours to obtain the activated white carbon black product. The fluorosil...

Embodiment 2

[0028] Under the temperature condition of 120°C, add 1000g of sodium fluorosilicate and an equal amount of concentrated sulfuric acid into the reactor for reaction to obtain hydrogen fluoride and silicon tetrafluoride gas, and sodium sulfate as a by-product. The anhydrous hydrogen fluoride product is obtained after dehydration, dust removal and membrane separation of the two gases. Silicon tetrafluoride gas is passed into water, the molar ratio of silicon tetrafluoride and water is controlled at 3:3, the pressure of silicon tetrafluoride gas is controlled at 600mbar, the hydrolysis temperature is controlled at 40°C, and the hydrolysis time is controlled at 60min to obtain active white Carbon black and fluosilicic acid solution, after suction filtration, the vacuum degree is controlled at 0.06MPa, the amount of washing and washing water is controlled at 15% of the filter cake, drying, and the drying temperature is controlled at 110°C, and the activated white carbon black product...

Embodiment 3

[0030] Under the temperature condition of 160°C, add 1000g of sodium fluorosilicate and an equal amount of concentrated sulfuric acid into the reactor for reaction to obtain hydrogen fluoride and silicon tetrafluoride gas, and sodium sulfate by-product. The anhydrous hydrogen fluoride product is obtained after dehydration, dust removal and pressure swing adsorption separation of the two gases. Silicon tetrafluoride gas is passed into water, the molar ratio of silicon tetrafluoride and water is controlled at 3:4, the pressure of silicon tetrafluoride gas is controlled at 900mbar, the hydrolysis temperature is controlled at 60°C, and the hydrolysis time is controlled at 120min to obtain active white Carbon black and fluosilicic acid solution, after suction filtration, the vacuum degree is controlled at 0.1MPa, the amount of washing and washing water is controlled at 20% of the filter cake, drying, and the drying temperature is controlled at 110°C, and dried for 2 hours to obtain ...

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Abstract

The invention relates to a preparation method of fluoride, which comprises the following steps: reacting sodium fluosilicate and concentrated sulfuric acid at 80-300 DEG C to obtain the product gases of silicon tetrafluoride and hydrogen fluoride and the byproduct sodium sulfate, and carrying out dehydration, dust removal, purification and separation on the two gases to obtain an anhydrous hydrogen fluoride product; introducing the silicon tetrafluoride gas into water, and controlling the hydrolysis reaction conditions to obtain active white carbon black and a fluosilicic acid solution; and reacting the fluosilicic acid solution with the byproduct sodium sulfate to obtain sodium fluosilicate and sulfuric acid, thereby implementing cyclic utilization. The reaction between the sodium fluosilicate and concentrated sulfuric acid and the hydrolysis reaction of the silicon tetrafluoride are carried out to finally obtain the products anhydrous hydrogen fluoride and active white carbon black. The low-value byproduct sodium fluosilicate in phosphate fertilizer enterprises is utilized to prepare the high-added-value products anhydrous hydrogen fluoride and active white carbon black; the byproduct sodium fluosilicate in the phosphate fertilizer enterprises is subjected to high-efficiency high-benefit comprehensive utilization of fluorine and silicon resources; and no unmanageable waste can be generated in the preparation process.

Description

technical field [0001] The invention relates to a preparation method of fluoride. The reaction of sodium fluorosilicate and concentrated sulfuric acid is used to generate silicon tetrafluoride and hydrogen fluoride gas, which are separated to obtain anhydrous hydrogen fluoride, and then the silicon tetrafluoride is hydrolyzed to obtain activated white carbon black. Background technique [0002] At present, the development of downstream products of sodium fluorosilicate by phosphate fertilizer enterprises mainly focuses on the use of sodium fluorosilicate to produce traditional products such as artificial cryolite, sodium fluoride and white carbon black. There are three ways to produce artificial cryolite: 1) aluminum sulfate-salt method; 2) sodium aluminate method; 3) carbonation method. The first step of these three methods is to use ammonia water or soda ash to separate the fluorine and silicon in sodium fluorosilicate, and the silicon is converted into silica gel, which c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/19C01B33/12
Inventor 裴文俊
Owner KUNMING DAOERSEN TECH
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