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Method for treating potassium chloride residues in organic fluorination reaction

A treatment method, potassium chloride technology, applied in the chemical field, can solve problems such as limited application fields and increased fluorination costs, achieve considerable economic benefits, and eliminate the risk of environmental pollution

Active Publication Date: 2015-04-01
JIANGSU HENGAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since fluoride is an important hazardous chemical, the country has very strict control over the use of fluoride, so the application of potassium chloride containing potassium fluoride is limited
The expensive organic solvent sulfolane is also burned together during incineration, which increases the cost of fluorination

Method used

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  • Method for treating potassium chloride residues in organic fluorination reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: In a 1000ml beaker, add 600ml water and 300g potassium chloride residue, stir and leach for 50min at room temperature, suction filter, transfer the leaching solution into a 1000ml beaker, wash the filter residue twice with 50ml hot water, and dry to obtain a dry filter residue 21g, washed with water for next leaching; the leaching solution was extracted twice with 500ml toluene, and after the oil phase was detoluene, 9g of sulfolane was obtained, and the toluene was recycled; 126ml of calcium chloride solution with a mass concentration of 30% was added to the water phase at room temperature , stirred to complete the precipitation reaction, separated the precipitate, washed with hot water, and dried to obtain 24g of white powdery calcium fluoride, with a content of 97%; evaporated and concentrated the separated liquid to nearly dryness, filtered, and dried to obtain 224g of white crystal potassium chloride, with a content of 98%.

Embodiment 2

[0013] Example 2: In a 1000ml beaker, add 400ml of water and 300g of potassium chloride residue, heat up to 50°C, stir and leach for 10 minutes, filter with suction, transfer the leaching solution into a 1000ml beaker, wash the filter residue twice with 50ml of hot water, and dry Obtain 23g of dry filter residue, and wash with water for the next leaching; the leaching solution is extracted twice with 200ml chloroform, and after the oil phase is removed from chloroform, 8g of sulfolane is obtained, and the chloroform is recycled; ℃, add 15g of calcium oxide powder, stir to complete the precipitation conversion reaction, separate the precipitate, wash with hot water, and dry to obtain 22g of white powdery calcium fluoride, with a content of 96%; evaporate and concentrate the separated liquid to nearly dryness, filter and dry to obtain White crystalline potassium chloride 221g, content 98.5%.

Embodiment 3

[0014] Example 3: In a 1000ml beaker, add 600ml of water and 300g of potassium chloride residue, heat up to 40°C, stir and leach for 20 minutes, filter with suction, transfer the leaching solution into a 1000ml beaker, wash the filter residue twice with 50ml of hot water, and dry Obtain 21g of dry filter residue, wash with water for the next leaching; the leaching solution is extracted twice with 300ml carbon tetrachloride, and after the oil phase removes carbon tetrachloride, 7g of sulfolane is obtained, and the carbon tetrachloride is recycled; Add 18g of calcium hydroxide at 40°C, stir to complete the precipitation transformation reaction, separate the precipitate, wash with hot water, and dry to obtain 22g of white powdery calcium fluoride, with a content of 96%; evaporate and concentrate the separated liquid to nearly dryness, filter and dry to obtain White crystalline potassium chloride 223g, content 98%.

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Abstract

The invention discloses a method for treating potassium chloride residues in an organic fluorination reaction. The potassium chloride residues are soaked with water in a soaking kettle, potassium chloride, potassium fluoride and sulfolane are dissolved in the water, carbide and water-insoluble organic impurities of tar are filtered and separated, the impurities are washed in hot water and then sent to a qualified solid waste treatment plant, and the washing water is used for soaking of the residues; soaking solutions enter an extraction kettle, sulfolane dissolved in water is extracted with an organic solvent and stands still for layering, an oil phase is desolventized, the organic solvent is recycled and returned for extraction, and the remainder is sulfolane; a water phase enters a settlement kettle, and precipitants are added into the settlement kettle and stirred until a precipitation reaction is sufficient; sediments are separated, washed and dried to obtain calcium fluoride, and the washing water is used for soaking of the residues; separating media enter an evaporator and are condensed to crystalize and dried centrifugally, and potassium chloride is obtained. According to the method, sulfolane, potassium chloride and potassium fluoride in the residues are all converted into qualified chemical materials except the organic impurities, so that the risk of environmental pollution is eliminated and considerable economic benefits are achieved.

Description

technical field [0001] The invention relates to a treatment method in the field of chemistry, in particular to a treatment method for potassium chloride residues in organic fluorination reactions. Background technique [0002] In the organic fluorination reaction, sulfolane is often used as the solvent, and potassium fluoride is used as the fluorinating agent. In the organic chloride molecule, the fluorine and the chlorine atom undergo a substitution reaction to obtain an organic fluoride, and at the same time, the potassium fluoride is converted into potassium chloride. into the residue. In addition to a large amount of potassium chloride, the residue also contains unreacted potassium fluoride, sulfolane, organic carbon and tar. The recycling of this residue not only affects the production cost of fluorinated products, but is also related to the safe disposal of hazardous solid waste and the prevention of environmental pollution. [0003] The current treatment method for ...

Claims

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Application Information

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IPC IPC(8): C01D3/14C01F11/22
Inventor 刘秉贤
Owner JIANGSU HENGAN CHEM
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