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Separation method of industrial mixed sylvite

A separation method and potassium salt technology are applied in the direction of alkali metal fluoride, alkali metal halide purification, alkali metal chloride and other directions, which can solve the problems of difficult application in industrialized production, difficulty in solvent recovery, large solvent consumption, etc., and achieve recycling and utilization. High efficiency, strong operability, and the effect of reducing production costs

Pending Publication Date: 2021-03-05
LIANHE CHEM TECH YANCHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the need for two different types of solvent systems in the prior art for the separation and treatment of industrial mixed potassium salts, the existence of conditions requiring high temperature and high pressure, unfriendly to the environment, and difficulty in solvent recovery , Difficult to apply to industrial production, or there are defects such as large solvent consumption, large environmental pollution and high cost, thus providing a separation method for industrial mixed potassium salts

Method used

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  • Separation method of industrial mixed sylvite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Add 150 g of by-product mixed potassium salts and 300 g of sulfolane to a 500 mL four-necked bottle, incubate at 90° C. for 2 hours, and filter to obtain 151.0 g of crude mixed potassium salts (dry weight 135.9 g). After testing: Wt(KCl)%=88.19%, Wt (KF)%=10.89%, Wt (water)%=0.21%, then it is dissolved with 231.6g 90 ℃ of hot water, after dissolving completely, cool down to 60 ℃, then slowly add 271.8g methanol, crystallize (terminal temperature 15 ℃), suction filtration, the filter cake is rinsed with a small amount of methanol, and dried to obtain 104.1g of potassium chloride dry product, appearance: white crystal, after testing: Wt(KCl)%=99.30%, Wt(KF)%=0.23 %, Wt (water)%=0.15%; 535.8g filtrate after the above-mentioned crystallization is concentrated under reduced pressure, after being concentrated to the content of initial mixed potassium salt is 90%, add 31.8g methyl alcohol, crystallization (terminal temperature 15 ℃), Suction filtration, the filter cake is rins...

Embodiment 2

[0064] Add 150 g of by-product mixed potassium salts and 300 g of dichloromethane into a 500 mL four-necked bottle, incubate at 40° C. for 2 hours, and filter to obtain 150.1 g of crude mixed potassium salts (dry weight 135.1 g). After testing: Wt(K Cl)%=88.78 %, Wt(KF)%=10.88%, Wt(water)%=0.15%, then it is dissolved with 232.3g 90 ℃ of hot water, after dissolving completely, cool down to 60 ℃, slowly add 270.2g methyl alcohol afterwards, crystallization ( End point temperature 15°C), suction filtration, filter cake rinsed with a small amount of methanol, dried to obtain 103.3g potassium chloride dry product, appearance: white crystal, after testing: Wt(KCl)%=99.36%, Wt(KF) %=0.06%, Wt (water)%=0.06%; 534.3g filtrate after above-mentioned crystallization is concentrated under reduced pressure, after being concentrated to the content of initial mixed potassium salt is 90%, add 31.8g methyl alcohol, crystallization (terminal temperature 15°C), suction filtration, the filter cake...

Embodiment 3

[0066] Add 150 g of by-product mixed potassium salts and 300 g of toluene to a 500 mL four-necked bottle, incubate at 90° C. for 2 hours, and filter to obtain 154.0 g of mixed potassium salt crude product (dry weight 135.5 g). After testing: Wt(KCl)%=88.56%, Wt (KF)%=10.98%, Wt (water)%=0.31%, then it is dissolved with 232.6g 90 ℃ hot water, after dissolving completely, cool down to 60 ℃, then slowly add 271.0g methanol, crystallize (terminal temperature 15 ℃), suction filtration, the filter cake is rinsed with a small amount of methanol, and dried to obtain 103.7g potassium chloride dry product, appearance: white crystal, after testing: Wt(KCl)%=99.34%, Wt(KF)%=0.06 %, Wt (water)%=0.06%; 535.4g filtrate after above-mentioned crystallization is concentrated under reduced pressure, after being concentrated to the content of initial mixed potassium salt is 90%, add 31.8g methanol, crystallization (terminal temperature 15 ℃) , suction filtration, the filter cake is rinsed with a ...

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Abstract

The invention discloses a separation method of industrial mixed sylvite. The separation method of the mixed sylvite comprises the following steps: step (1) recrystallizing the mixed sylvite in water and methanol to obtain potassium chloride and mother liquor A; and step (2) concentrating the mother liquor A obtained in the step (1) to obtain mother liquor A', recrystallizing the obtained mother liquor A' in methanol to obtain a potassium chloride enriched product, collecting mother liquor B, and performing concentrating to obtain potassium fluoride.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for separating industrial mixed potassium salts. Background technique [0002] Potassium chloride and potassium fluoride are widely used, among which potassium chloride is mainly used in the inorganic industry, and is the basic raw material for the manufacture of various potassium salts, such as potassium hydroxide, potassium sulfate, potassium nitrate, potassium chlorate, potassium red alum, etc. It is used as potassium fertilizer; while potassium fluoride is mainly used as fluorinating agent in organic synthesis, and can also be used as glass engraving, catalyst, insecticide, etc. [0003] Usually, in the waste residue (also known as "industrial mixed potassium salt") produced by organic fluorination reaction, potassium chloride accounts for about 80%, potassium fluoride accounts for about 10%, and others are tar, sulfolane, etc. Because the above-mentioned waste resi...

Claims

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Application Information

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IPC IPC(8): C01D3/04C01D3/14C01D3/02
CPCC01D3/04C01D3/14C01D3/02C01P2006/80
Inventor 梁海峰郝佳佳叶朝辉李高峰徐其林周小渊
Owner LIANHE CHEM TECH YANCHENG
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