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Method for production of high-purity potassium fluoride by using hydrofluoric acid residual liquid

A technology of hydrofluoric acid raffinate and potassium fluoride, which is applied in the direction of preparation/separation of alkali metal fluoride and ammonia, etc. It can solve the problem of raffinate utilization or harmless treatment for enterprises that do not meet clean production and circular economy, High production equipment requirements and other issues, to achieve the effect of stable crystal form, low production cost, and low requirements for reaction conditions

Active Publication Date: 2014-05-28
ZHEJIANG DAYANG BIOTECH GROUP
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  • Claims
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Problems solved by technology

However, there are still several problems in this invention: (1) The organic waste contained in potassium chloride or the mixture of potassium chloride and potassium fluoride is treated at high temperature, which requires high production equipment, and at the same time, the removal of organic waste by high temperature method will pollute the environment Serious; (2) In addition to the target product potassium fluorosilicate, the reaction product of the mixture of fluorosilicic acid and potassium chloride or potassium chloride and potassium fluoride will also produce a large amount of mixture of hydrochloric acid and hydrofluoric acid, which needs to be treated to Discharge;
When using this method for disposal, the utilization rate of fluorine resources is low, resulting in waste of resources, and the processing cost is high, which does not meet the requirements of clean production and circular economy
Due to many problems in treatment technology and cost, the utilization or harmless treatment of the residual liquid has always troubled enterprises.

Method used

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  • Method for production of high-purity potassium fluoride by using hydrofluoric acid residual liquid

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Effect test

Embodiment 1-1

[0050] Embodiment 1-1, a kind of method that utilizes the hydrofluoric acid raffinate containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurity to produce high-purity potassium fluoride, carry out the following steps successively:

[0051] 1) Add 330 kg of 92% solid potassium hydroxide to 170 kg of water, and stir until the potassium hydroxide is completely dissolved; obtain potassium hydroxide solution I, and the final concentration of potassium hydroxide in the potassium hydroxide solution I is 60.7 %(quality%);

[0052] 2) Slowly add the potassium hydroxide solution I obtained in step 1) dropwise into 280 kg of hydrofluoric acid raffinate containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurities under stirring, until the pH reaches 6.8, stop dripping Add potassium hydroxide solution I;

[0053] 3) The material obtained from the reaction in step 2) was filtered while it was hot (90-95°C) to obtain potassium fluoride ...

Embodiment 1-2

[0062] Embodiment 1-2, a kind of method that utilizes the hydrofluoric acid raffinate containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurity to produce high-purity potassium fluoride, carry out the following steps successively:

[0063] 1) Add 330 kg of 92% solid potassium hydroxide to 186 kg of the sodium fluoride washing solution I obtained in step 4) of Example 1-1, and stir until the potassium hydroxide is completely dissolved; to obtain potassium hydroxide solution I , the final concentration of potassium hydroxide in the potassium hydroxide solution I is 60% (mass %);

[0064] 2) Slowly add potassium hydroxide solution I obtained in step 1) dropwise to 280 kg of hydrofluoric acid residue containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurities under stirring, and control the pH of the reaction solution to 7.0 , stop dripping potassium hydroxide solution I;

[0065] 3) The material obtained from the reaction i...

Embodiment 2

[0075] Embodiment 2, a kind of method that utilizes the hydrofluoric acid raffinate containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurity to produce high-purity potassium fluoride, carries out following steps successively:

[0076] 1) Add 300 kg of solid potassium hydroxide with a content of 92% to 160 kg of the sodium fluoride washing solution I obtained in step 4) of Example 1-2, and stir until the potassium hydroxide is completely dissolved; to obtain potassium hydroxide solution I , the final concentration of potassium hydroxide in the potassium hydroxide solution I is 60% (mass %);

[0077] 2) Slowly add potassium hydroxide solution I obtained in step 1) dropwise to 280 kg of hydrofluoric acid residue containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurities under stirring, and control the pH of the reaction solution to 6.5 , stop dripping potassium hydroxide solution I;

[0078] 3) The material obtained from ...

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Abstract

The technical problem to be solved is that a method for production of high-purity potassium fluoride by using a hydrofluoric acid residual liquid is provided. The method makes full use of the hydrofluoric acid residual liquid produced in a 2-chloro-6-fluorotoluene production process and containing hydrogen fluoride, ammonium fluoride, sodium fluoride and other organic impurities. According to the method, the hydrofluoric acid residual liquid and potassium hydroxide are used as basal raw materials, the high-purity potassium fluoride is prepared through the steps of carrying out a neutralization reaction, adding a strong alkali and dispersing ammonia, carrying out neutralization, decolorization and filtration, carrying out evaporative crystallization and carrying out air flow drying, and at the same time, by-products are sodium fluoride and aqua ammonia. With adopting of the method, the recovery rate of the fluorine resource reaches above 99.9%, and the quality of the prepared potassium fluoride is superior to a standard of a national potassium fluoride superior product.

Description

technical field [0001] The invention belongs to the fields of fine chemical industry and environmental protection, and relates to the synthesis technology of fine pharmaceutical intermediates, in particular to a method for producing high-purity potassium fluoride by using hydrofluoric acid raffinate containing hydrogen fluoride, ammonium fluoride, sodium fluoride and organic impurities method. Background technique [0002] Potassium fluoride is the potassium salt of hydrofluoric acid. It is the main source of fluoride ions except hydrogen fluoride. It belongs to alkali metal halides. Its aqueous solution will corrode glass and form soluble fluorosilicate. It can also be used as a mixture of hydrogen fluoride and water. Absorbent is also the raw material for the preparation of potassium hydrogen fluoride. Potassium fluoride is stable and decomposes when heated to the sublimation temperature. [0003] Due to the advantages of small volume, large electronegativity and high el...

Claims

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Application Information

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IPC IPC(8): C01D3/02C01C1/02
Inventor 王国平翁甜徐旭辉刘思鹏关卫军汪贤高仇建龙周转忠兰金林鲁高明仇旭辉鲍志娟
Owner ZHEJIANG DAYANG BIOTECH GROUP
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