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Circulating production process for preparing hydrogen fluoride by utilizing fluorosilicic acid

A production process, fluosilicic acid technology, applied in the direction of fluorine/hydrogen fluoride, hydrogen fluoride, silicon oxide, etc., can solve the problems of high yield, low value of by-products, low cost, etc., and achieve the effect of high yield and low process cost

Active Publication Date: 2017-06-20
张旭
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Aiming at the problems of high consumption of raw materials, high cost and low value of by-products in the existing process of producing hydrogen fluoride by using fluorosilicic acid, the purpose of the present invention is to provide a new method for producing hydrogen fluoride with fluorosilicic acid with low cost and high yield

Method used

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  • Circulating production process for preparing hydrogen fluoride by utilizing fluorosilicic acid

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Experimental program
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Effect test

Embodiment 1

[0040] 1. The first production cycle

[0041] 1) 10 kg of fluorosilicate with a mass fraction of 20% and 0.73 kg of lithium fluoride solid are placed in a distillation still to react to obtain a mixed solution of hydrogen fluoride and lithium fluorosilicate;

[0042] 2) Vacuum distillation in the reaction kettle at 95 degrees Celsius for 1.5h, distilling hydrogen fluoride gas to obtain lithium fluorosilicate solid;

[0043] 3) Take out the solid in step 2) and heat to 450 degrees centigrade, heat for 1.5h to obtain lithium fluoride solid and silicon tetrafluoride gas; use 3.3kg mass fraction of 20% fluosilicic acid solution to absorb, so that the concentration of fluosilicic acid solution Elevate, and generate silica gel, filter the silica gel, and keep the fluorosilicic acid solution for later use;

[0044] 2. The second production cycle

[0045] 1) Fluosilicic acid obtained after absorbing silicon tetrafluoride in step 3) of the first production cycle and lithium fluoride ...

Embodiment 2

[0052] 1. The first production cycle

[0053] 1) Take 10 kg of fluorosilicate with a mass fraction of 15% and 1.27 kg of lithium fluoride solids and place them in a distillation pot for reaction to obtain a suspension mixture of hydrogen fluoride, lithium fluorosilicate and the remaining excess lithium fluoride;

[0054] 2) Distill at 180 degrees Celsius for 1 hour in a reaction kettle to distill hydrogen fluoride gas to obtain lithium fluorosilicate and lithium fluoride solids;

[0055] 3) Take out the solid in step 2) and heat it to 550 degrees centigrade, and heat for 1h to obtain lithium fluoride solid and silicon tetrafluoride gas; use 3.3kg of 15% fluosilicic acid solution to absorb it, so that the concentration of the fluosilicic acid solution rises High, and produce silica gel, fluosilicic acid solution is reserved for later use.

[0056] 2. The second production cycle

[0057] 1) Fluorosilicic acid obtained after absorbing silicon tetrafluoride in step 3) of the fir...

Embodiment 3

[0064] 1. The first production cycle

[0065] 1) Take 10 kg of fluorosilicate with a mass fraction of 10% and 1.08 kg of lithium fluoride solid and place them in a distillation still to react to obtain a suspension mixture of hydrogen fluoride, lithium fluorosilicate and the remaining excess lithium fluoride;

[0066] 2) Distill at 150 degrees Celsius for 2 hours in a reaction kettle to distill hydrogen fluoride gas to obtain a solid mixture of lithium fluorosilicate and lithium fluoride;

[0067] 3) Take out the solid in step 2) and heat to 300 degrees centigrade, heat for 3 hours to obtain lithium fluoride solid and silicon tetrafluoride gas; use 3.3 kg of 10% fluorosilicic acid solution to absorb, so that the concentration of fluorosilicic acid solution rises High, and produce silica gel, fluosilicic acid solution is reserved for later use.

[0068] 2. The second production cycle

[0069] 1) Fluorosilicic acid obtained after absorbing silicon tetrafluoride in step 3) of t...

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Abstract

The invention discloses a circulating production process for preparing hydrogen fluoride by utilizing fluorosilicic acid. The circulating production process comprises the following steps: 1) mixing the fluorosilicic acid with alkaline-earth metal fluoride or alkaline metal fluoride to react to obtain a mixed solution of the fluorosilicic acid and fluorosilicate; 2) distilling the mixed solution obtained by the step 1) and collecting hydrogen fluoride gas to obtain a fluorosilicate solid; 3) heating and decomposing the fluorosilicate solid to obtain a fluoride solid and silicon tetrafluoride gas; absorbing the silicon tetrafluoride gas with a fluorosilicic acid solution and filtering to obtain the fluorosilicic acid solution with increased concentration and silica gel sediment, so that one production period is finished; 4) taking the fluorosilicic acid solution obtained by the step 3) and the fluoride solid to react according to step 1) to step 3). According to the process disclosed by the invention, metal fluoride is actually not consumed, and only needs to be added at the initial stage of the process; the fluoride can be circularly utilized and only the fluorosilicic acid raw material and water are consumed; the process has low cost, a byproduct only contains silica gel and the yield of the hydrogen fluoride reaches 98.8 percent or more.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry, and in particular relates to a cyclic production process for preparing hydrogen fluoride with fluorosilicic acid. Background technique [0002] Fluosilicic acid is a by-product obtained from the production of phosphate fertilizers, which contains useful elements fluorine and silicon. my country is a large producer of phosphate fertilizers, and the production is accompanied by a large amount of fluorosilicic acid. At present, fluosilicic acid is mainly used to produce sodium fluosilicate, which has low product value, excess production capacity, and poor economic benefits. Therefore, rational development and utilization of fluosilicic acid resources can create great economic and social benefits. Hydrogen fluoride is the most important source of fluorine in fluorine chemical industry. It is used to synthesize organic fluorine and inorganic fluoride, and occupies an irreplaceable position i...

Claims

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Application Information

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IPC IPC(8): C01B7/19C01B33/14
CPCC01B7/193C01B33/14
Inventor 张旭张文清李新娥张松
Owner 张旭
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