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Preparation method of potassium hexafluorophosphate

A technology of potassium hexafluorophosphate and hydrofluoric acid, applied in chemical instruments and methods, phosphorus compounds, sodium/potassium compounds, etc., can solve the problem that phosphorus pentachloride is easy to decompose and sublime, the reaction control is difficult, and phosphorus pentafluoride is difficult. Purification and other problems, to achieve the effect of high degree of automation, good product quality, and no three waste emissions

Pending Publication Date: 2022-04-08
DO FLUORIDE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, potassium hexafluorophosphate is mostly prepared from phosphorus pentachloride / phosphorus pentafluoride / phosphorus oxychloride and potassium chloride / potassium fluoride through a one-step or two-step method, which is difficult to control the reaction and the raw materials Phosphorus pentachloride is easy to decompose and sublimate, the intermediate product phosphorus pentafluoride is difficult to purify, and the product yield is low.

Method used

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Examples

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preparation example Construction

[0020] The invention provides a kind of preparation method of potassium hexafluorophosphate, comprising:

[0021] Carrying out the first reaction with hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution;

[0022] The reaction solution and the potassium salt solution are subjected to a second reaction to obtain potassium hexafluorophosphate.

[0023] In the present invention, it is preferable to add hexafluorophosphoric acid solution for priming during the first reaction; the method for the first reaction preferably includes:

[0024] After mixing the hexafluorophosphoric acid solution and hydrofluoric acid, the first reaction is carried out with phosphorus pentoxide to obtain a reaction solution.

[0025] In the present invention, the hexafluorophosphoric acid solution used in the first reaction process is preferably an aqueous solution of hexafluorophosphoric acid; the mass concentration of the hexafluorophosphoric acid solution is preferably 70-76%, mor...

Embodiment 1

[0050] Use hexafluorophosphoric acid solution as a primer, add 169g of anhydrous hydrofluoric acid and stir to mix evenly, add 100g of phosphorus pentoxide in batches for reaction, after the addition is complete, control the reaction temperature at -5°C, and the reaction time for 2 hours. After the reaction, get 266 g of hexafluorophosphoric acid solution (reaction solution).

[0051] Weigh 96g of potassium carbonate and put it into the mother liquor of potassium hexafluorophosphate and stir to form a solution with a mass concentration of 20%, then add the above-mentioned hexafluorophosphoric acid solution (reaction solution) into a plug-flow reactor at room temperature and mix evenly, then immediately react, and react Finally, the obtained slurry was filtered, washed, and dried to obtain 242 g of potassium hexafluorophosphate; the filtrate was the mother liquor of potassium hexafluorophosphate, which was used to prepare a saturated solution of potassium carbonate.

[0052] Ca...

Embodiment 2

[0057] Use hexafluorophosphoric acid solution as a primer, add 338g of anhydrous hydrofluoric acid and stir to mix evenly, add 200g of phosphorus pentoxide in batches for reaction, after the addition is complete, control the reaction temperature at 0°C, and the reaction time for 1.5h. After the reaction, you can get 535 g of hexafluorophosphoric acid solution (reaction solution).

[0058] Weigh 150g of potassium hydroxide and put it into the potassium hexafluorophosphate mother liquor and stir to configure a solution with a mass concentration of 50%, then add the hexafluorophosphoric acid solution (reaction solution) to a static mixer at room temperature and mix uniformly, then react immediately. The slurry was filtered, washed, and dried to obtain 478.5 g of potassium hexafluorophosphate; the filtrate was the mother liquor of potassium hexafluorophosphate, which was used to prepare a saturated solution of potassium hydroxide.

[0059] According to the method of Example 1, the y...

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Abstract

The invention provides a potassium hexafluorophosphate preparation method, which comprises: carrying out a first reaction on hydrofluoric acid and phosphorus pentoxide to obtain a reaction solution; and carrying out a second reaction on the reaction solution and a potassium salt solution to obtain potassium hexafluorophosphate. Compared with the prior art, the preparation method of the potassium hexafluorophosphate provided by the invention has the advantages that water generated by reaction is used as a solvent, the potassium hexafluorophosphate is prepared by liquid-liquid reaction, and the problems of product impurity wrapping and low reaction conversion rate in the traditional process are solved; meanwhile, the microreactor device is adopted, so that the automation degree is high, the reaction is more sufficient, the time is shorter, the control is more accurate, and continuous production can be realized. The preparation method of potassium hexafluorophosphate provided by the invention has the advantages of simple process, controllable reaction, good product quality, no emission of three wastes and the like, and is easy to industrially implement and popularize.

Description

technical field [0001] The invention belongs to the technical field of potassium hexafluorophosphate, and in particular relates to a preparation method of potassium hexafluorophosphate. Background technique [0002] Potassium hexafluorophosphate, white square crystal, melting point 575°C, relative density 2.55, solubility 8.35g / 100g water (25°C), is an important inorganic fluoride salt. Potassium hexafluorophosphate can be dissolved in acetonitrile solution, and can be used as an organic fluorine substitute, and used to prepare other hexafluorophosphate and fluorinating agents; potassium hexafluorophosphate is also a new development in the late 1990s when the world's UV coating industry emerged. It is an important chemical raw material, mainly used for UV photoinitiator (that is, UV curing agent) in the coating industry; it can also be used as a catalyst for polymer synthesis, etc. With the continuous advancement of science and technology, some large foreign pharmaceutical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455C01B25/30C01D13/00
Inventor 李云峰杨华春薛旭金耿梦湍尚钟声刘海庆刘海霞张照坡张永明
Owner DO FLUORIDE CHEM CO LTD
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