Method for separating potassium chloride and potassium fluoride

A separation method, potassium chloride technology, applied in the direction of purification of boron halide compounds, alkali metal halides, etc., can solve the problems of secondary waste water or waste gas pollution, high cost, large cost and environmental protection problems, and achieve low cost and reduced The effect of simple production cost and process

Active Publication Date: 2014-01-22
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The above methods all have the disadvantages of high cost, serious secondary wastewater or waste gas pollution, etc., and there are relatively large cost and environmental protection problems in industrialization

Method used

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  • Method for separating potassium chloride and potassium fluoride
  • Method for separating potassium chloride and potassium fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 75.0 g of fluorination reaction by-product KCl-KF mixed salt (9.2% potassium fluoride mass fraction) dried at 300°C for 1 hour to 200.2 g of 5% boron trifluoride acetonitrile solution, and reflux for 5 hours under stirring. Filter to obtain 65.8g of potassium chloride, heat and evaporate the acetonitrile solution containing potassium tetrafluoroborate to recover acetonitrile and excess boron trifluoride acetonitrile, cool and crystallize, filter to obtain potassium tetrafluoroborate, and dry to obtain 14.6g of potassium tetrafluoroborate , through the solid moisture detection instrument (Mitsubishi Chemical CA-200 / VA200), the moisture is 785ppm, and the yield is 97.4%.

Embodiment 2

[0026] Add 100.0 g of fluorination reaction by-product KCl-KF mixed salt (12% potassium fluoride mass fraction) dried at 400°C for 3 hours to 85.1 g of 20% boron trifluoride acetonitrile solution, and reflux for 24 hours under stirring. 86g of potassium chloride was obtained by filtration, and the acetonitrile solution containing potassium tetrafluoroborate was directly spray-dried to obtain 25.3g of potassium tetrafluoroborate, which passed the solid moisture detection instrument (Mitsubishi Chemical CA-200 / VA200) with a moisture content of 687ppm and a yield of 97.0%.

Embodiment 3

[0028] Add 100.0g of fluorination reaction by-product KCl-KF mixed salt (20% potassium fluoride mass fraction) dried at 500°C for 5 hours to 260.5g of 10% boron trifluoride acetonitrile solution, and reflux for 24 hours under stirring. 78.2g of potassium chloride was obtained by filtration, and the clear liquid of the acetonitrile solution containing potassium tetrafluoroborate was directly spray-dried to obtain 42.3g of potassium tetrafluoroborate, and the moisture content was 693ppm through the solid moisture detection instrument (Mitsubishi Chemical CA-200 / VA200). The rate is 97.3%.

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Abstract

The invention discloses a method for separating mixture of potassium chloride and potassium fluoride, which comprises the steps of: carrying out heat treatment on the mixture of the potassium chloride and the potassium fluoride at the temperature of 300-500 DEG C for 1-5h to remove organic waste in the mixture; then reacting with acetonitrile solution of boron trifluoride with the mass percent of 5-20wt% for 5-24h under the condition of refluxing to obtain mixed acetonitrile solution containing potassium fluoroborate and potassium chloride; filtering to remove potassium chloride; and concentrating, crystallizing, drying or spray-drying the filtrate containing potassium fluoroborate until the water content is lower than 1000ppm to finally obtain potassium fluoroborate. After the technical scheme disclosed by the invention is adopted, potassium chloride can be separated out, and potassium fluoroborate is obtained at the same time; and the separation method is simple in technology and low in cost, and the problems of safety, environmental protection and the like are basically solved.

Description

technical field [0001] The invention relates to a method for separating a mixture of potassium chloride and potassium fluoride, in particular to a method for converting potassium fluoride produced by a fluorination reaction into potassium tetrafluoroborate so as to realize the separation. Background technique [0002] Potassium fluoride is a widely used fluorinating agent in organic synthesis. It can also be used for glass engraving, food preservation, electroplating, insecticide, catalyst, absorbent and fluorine-containing table salt. The by-product potassium chloride and potassium fluoride mixture produced in organic synthesis as a fluorinating agent is generally dissolved in water and then enters the sewage treatment system, which is a waste of limited fluorine resources and causes great pollution to the environment. . [0003] At present, the most commonly used separation method in China: ① The mixture of potassium fluoride and potassium chloride is neutralized with flu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06C01D3/18
Inventor 张先林杨志勇陆海媛吴国栋
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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