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Preparation method of anhydrous hydrofluoric acid

A technology of anhydrous hydrofluoric acid and anhydrous hydrogen fluoride, applied in the preparation of sulfate/bisulfate, fluorosilicic acid, hydrogen fluoride, etc., can solve the problems of excessive sulfuric acid, complicated process, no industrial application, etc., to reduce consumption , the process is simple, the effect of low energy consumption

Inactive Publication Date: 2018-08-24
SHANDONG LUBEI ENTERPRISE GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has two disadvantages, one is two-stage heating, the process is more complicated, and the other is excessive sulfuric acid, it is difficult to obtain hydrogen fluoride with high purity
Huangpu Chemical Technology Co., Ltd. patented "Sodium Fluosilicate to Produce Dry Process Aluminum Fluoride and Anhydrous Hydrogen Fluoride", which cannot completely convert the fluorine in sodium fluosilicate into anhydrous hydrogen fluoride
Moreover, the current research and patents have not realized industrial application, and have relatively large limitations.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) First, sodium fluorosilicate with a content greater than 99% and concentrated sulfuric acid with a content of 98%, according to the molar ratio Na 2 SiF 6 :H 2 SO 4 =1:1.05 Mix evenly, react at 320°C for 3 hours to obtain solid sodium sulfate.

[0024] (2) The purity of solid sodium sulfate is 98.6%. After grinding, it is a sodium sulfate product, part of which is used for sales, and part of which is reacted with fluorosilicic acid to obtain sodium fluorosilicate.

[0025] (3) Freeze the gas generated during the reaction to 12°C to obtain liquid hydrogen fluoride, and obtain anhydrous hydrogen fluoride product after rectification, with a purity of 99.6%.

[0026] (4) Absorb the remaining gas with water to generate fluosilicic acid and silicon dioxide. h 2 SiF 6 After the concentration reaches 12%, liquid-solid separation is carried out, the solid is washed and dried to obtain industrial white carbon black, and the liquid is fluosilicic acid solution.

[0027]...

Embodiment 2

[0029] (1) First, sodium fluorosilicate with a content greater than 99% and concentrated sulfuric acid with a content of 98%, according to the molar ratio Na 2 SiF 6 :H 2 SO 4 =1:1.1 Mix well, react at 330°C for 2.5h to obtain solid sodium sulfate.

[0030] (2) The purity of solid sodium sulfate is 98.2%. After grinding, it is a sodium sulfate product, part of which is used for sales, and part of which is reacted with fluorosilicic acid to produce sodium fluorosilicate.

[0031] (3) Freeze the gas generated during the reaction to 8°C to obtain liquid hydrogen fluoride, and obtain anhydrous hydrogen fluoride product after rectification, with a purity of 99.5%.

[0032] (4) Absorb the remaining gas with water to generate fluosilicic acid and silicon dioxide. h 2 SiF 6 After the concentration reaches 14%, liquid-solid separation is carried out, the solid is washed and dried to obtain industrial white carbon black, and the liquid is fluosilicic acid solution.

[0033] (5) F...

Embodiment 3

[0035] (1) First, sodium fluorosilicate with a content greater than 99% and concentrated sulfuric acid with a content of 98%, according to the molar ratio Na 2 SiF 6 :H 2 SO 4 =1:1.2 Mix well, react at 290°C for 2.5h to obtain solid sodium sulfate.

[0036] (2) The purity of solid sodium sulfate is 98.1%. After grinding, it is a sodium sulfate product, part of which is used for sales, and part of which is reacted with fluorosilicic acid to produce sodium fluorosilicate.

[0037] (3) Freeze the gas generated during the reaction to 14°C to obtain liquid hydrogen fluoride, and obtain anhydrous hydrogen fluoride product after rectification with a purity of 99.7%.

[0038] (4) Absorb the remaining gas with water to generate fluosilicic acid and silicon dioxide. h 2 SiF 6 After the concentration reaches 11%, liquid-solid separation is carried out, the solid is washed and dried to obtain industrial white carbon black, and the liquid is fluosilicic acid solution.

[0039] (5) F...

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Abstract

The invention discloses a preparation method of anhydrous hydrofluoric acid. The preparation method comprises the following steps of: adopting a sulfuric-acid method to mix sodium fluorosilicate and concentrated sulfuric acid uniformly, after reaction, obtaining sodium sulfate for reaction with fluosilicic acid to prepare sodium fluorosilicate; freezing to obtain liquid hydrofluoric acid, and after distillation, obtaining an anhydrous hydrogen fluoride product; absorbing the remaining gas by water to obtain fluosilicic acid solution and silicon dioxide, adding solid sodium sulfate into the fluosilicic acid solution, and separating to obtain anhydrous hydrofluoric acid. The preparation method disclosed by the invention has the beneficial effects that the fluorine utilization rate in sodiumfluorosilicate is high, so that not only can the technical process be simplified, but also the production cost can be reduced; the new method is simple in operation and high in safety, and is especially suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of anhydrous hydrogen fluoride, in particular to a preparation method of decomposing sodium fluorosilicate to produce anhydrous hydrogen fluoride by adopting a sulfuric acid method. Background technique [0002] The fluorine chemical industry is a sub-industry of the chemical industry. Due to the variety of products, excellent performance and wide application fields, this industry has become an important industry with rapid development. Fluorine chemical products are divided into inorganic fluorides and organic fluorides. Inorganic fluorides refer to non-hydrocarbon compounds containing fluorine in fluorine chemical products, which are the basis of the entire fluorine chemical industry. Other products in the fluorine chemical industry are processed on the basis of inorganic fluorides; organic fluorides are Refers to hydrocarbons containing fluorine in fluorine chemical products, mainly including fluorine-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/19C01D5/02C01B33/12C01B33/10C01F11/46
CPCC01B7/193C01B33/103C01B33/12C01D5/02C01F11/46
Inventor 冯祥义冯怡利马荣刚卢实凯
Owner SHANDONG LUBEI ENTERPRISE GROUP
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