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Preparation method of potassium hexafluorophosphate

A technology of potassium hexafluorophosphate and potassium hydrogen fluoride, which is applied in chemical instruments and methods, sodium/potassium compounds, alkali metal compounds, etc., can solve the problems of easily causing danger and increasing the difficulty of control, so as to reduce the risk and be easy to control , the effect of peaceful response

Active Publication Date: 2018-03-06
JIANGXI DONGYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] When potassium chloride, anhydrous hydrogen fluoride, and phosphorus pentachloride are used to prepare potassium hexafluorophosphate, the phosphorus pentachloride solid needs to be added in small amounts to the mixture of potassium chloride and anhydrous hydrogen fluoride several times. Overwhelming the difficulty of control, it is easy to cause danger

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0035] A preparation method of potassium hexafluorophosphate, comprising the following steps:

[0036] (1) Add 150 g of anhydrous hydrogen fluoride to 78 g of dried potassium hydrogen fluoride solid at 0-8°C;

[0037] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum degree to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 160g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;

[0038] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.7Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;

[0039] (4) Slowly add 50% potassium hydroxide solution to the reaction to adjust the pH value to 7;

[0040] (5) The reacted material is cooled to room temperature, and 181g of pota...

Embodiment 2

[0045] A preparation method of potassium hexafluorophosphate, comprising the following steps:

[0046] (1) Add 160 g of anhydrous hydrogen fluoride to 78 g of dried potassium hydrogen fluoride solid at 0-8°C;

[0047] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum degree to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 163g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;

[0048] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.7Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;

[0049] (4) Slowly add 50% potassium hydroxide solution to the reaction to adjust the pH value to 7;

[0050] (5) The reacted material is cooled to room temperature, and the 182g pot...

Embodiment 3

[0055] (1) Add 167g of anhydrous hydrogen fluoride to 78g of dry potassium hydrogen fluoride solid at 0-8°C;

[0056] (2) Adjust the temperature to -5°C, turn on the vacuum pump and adjust the vacuum to 0.5Pa, make the reaction condition a slight negative pressure, slowly add 165g of phosphorus oxychloride dropwise, and control the dropping rate so that the temperature does not exceed -2°C After the dropwise addition is completed, continue to stir and react for 30 minutes;

[0057] (3) Adjust the temperature to 80°C and keep it warm for 30 minutes; adjust the vacuum to 0.8Pa, extract the residual hydrogen fluoride gas and the generated hydrochloric acid gas, and neutralize it with the lye;

[0058](4) Slowly add 50% potassium hydroxide solution to the reaction to adjust the pH value to 7;

[0059] (5) The reacted material was cooled to room temperature, and 183.7g of potassium hexafluorophosphate crude product was obtained after centrifugation;

[0060] (6) Add 300ml of wate...

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Abstract

The invention relates to the field of synthesis of an inorganic compound, and particularly relates to a preparation method of potassium hexafluorophosphate. The preparation method of the potassium hexafluorophosphate comprises the following steps: performing an initial reaction under a certain condition by taking potassium bifluoride (or potassium chloride), anhydrous hydrogen fluoride and phosphorus oxychloride as reaction raw materials to obtain a potassium hexafluorophosphate crude product, adjusting the acidity by using potassium hydroxide, eliminating iron ions, adsorbing and decoloring by activated carbon, performing evaporation and concentration on the crude product after removing impurities, and performing recrystallization to obtain the potassium hexafluorophosphate finished product. Compared with the traditional preparation method, the preparation method of the potassium hexafluorophosphate has the following advantages: the preparation method is simple in operation, mild in reaction and easy to control, and the use of a large amount of unstable, corrosive and toxic raw materials is avoided, so that the operation dangerousness is reduced; by adopting the potassium hexafluorophosphate produced by the method, the yield is up to 88 percent and the purity exceeds 99 percent.

Description

technical field [0001] The invention relates to the field of synthesis of inorganic compounds, in particular to a preparation method of potassium hexafluorophosphate. Background technique [0002] Hexafluorophosphate series is a very important class of inorganic fluorine salts, among which potassium hexafluorophosphate is an important one among hexafluorophosphates. Potassium hexafluorophosphate can be used to prepare other hexafluorophosphates, and can also be used as an organic fluorine substitution agent, such as a photopolymerization catalyst. The preparation method of hexafluorophosphate has been greatly developed due to the application of lithium hexafluorophosphate. In the late 20th century, chemists in some western countries such as the United States and Germany proposed the idea of ​​preparing lithium hexafluorophosphate from potassium hexafluorophosphate, which made the production of potassium hexafluorophosphate The workmanship has been greatly improved. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D13/00
CPCC01D13/00C01P2006/80
Inventor 段晓军孙燕
Owner JIANGXI DONGYAN PHARMA
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