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Method for recycling halogenated short chain quaternary ammonium salt waste

A quaternary ammonium salt, short-chain technology, applied in organic chemistry, alkali metal bromide, alkali metal chloride, etc., can solve the problems of high production cost, poor environmental protection, and large waste discharge, so as to improve environmental protection and reduce Effects of waste discharge and waste reduction

Inactive Publication Date: 2018-02-09
KENTE CATALYSTS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But even through the recycling of halogenated short-chain quaternary ammonium salt waste by the above-mentioned patented method, the production of halogenated short-chain quaternary ammonium salt still has the disadvantages of poor environmental protection, large waste discharge and high production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Tetraethylammonium bromide waste 500KG, dissolve in 500KG water, add sodium hydroxide, adjust the pH value to more than 12, stir and mix, let stand for more than 3 hours, release the lower water layer to be treated, release the upper organic layer, pass through normal About 100KG of triethylamine is recovered by pressure distillation, with a content of more than 98%, which is used for the production of tetraethylammonium bromide. Add 300KG chloroform to 850KG of the lower water layer, stir and mix, let it stand for more than 3 hours, release the lower organic layer to be processed, release the upper water layer, remove water and concentrate by vacuum distillation, cool and crystallize the concentrated solution, and centrifuge to obtain sodium bromide The solid is 100KG, and the mother liquor is used for the next concentration to extract sodium bromide. The lower organic layer is distilled to recover chloroform, which is used for the next treatment. The concentrated solu...

Embodiment 2

[0016] Tetrapropylammonium bromide waste 500KG, be dissolved in 500KG water, add potassium hydroxide, adjust the pH value to more than 12, stir and mix, let stand for more than 3 hours, release the lower water layer to be treated, release the upper organic layer, by reducing Pressure distillation recovers about 110KG of tripropylamine with a content of more than 98%, which is used for the production of tetrapropylammonium bromide. Add 300KG chloroform to 850KG of the lower water layer, stir and mix, let it stand for more than 3 hours, release the lower organic layer to be processed, release the upper water layer, remove water and concentrate by vacuum distillation, cool and crystallize the concentrate, and centrifuge to obtain potassium bromide The solid is 120KG, and the mother liquor is used for the next concentration to extract potassium bromide. The lower organic layer is distilled to recover chloroform, which is used for the next treatment. The concentrated solution is ad...

Embodiment 3

[0018] Tetrabutylammonium bromide waste material 500KG, be dissolved in 500KG water, add calcium hydroxide, adjust pH value to more than 12, stir and mix, let stand for more than 3 hours, release the lower water layer to be treated, release the upper organic layer, by reducing About 100KG of tributylamine is recovered by pressure distillation, with a content of more than 97%, which is used for the production of tetrabutylammonium bromide. Add 300KG chloroform to 850KG of the lower water layer, stir and mix, let it stand for more than 3 hours, release the lower organic layer to be processed, release the upper water layer, remove water and concentrate by vacuum distillation, cool and crystallize the concentrate, and centrifuge to obtain calcium bromide The solid is 130KG, and the mother liquor is used for the next concentration to extract calcium bromide. The lower organic layer is distilled to recover chloroform, which is used for the next treatment. The concentrated solution i...

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PUM

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Abstract

The invention discloses a method for recycling halogenated short chain quaternary ammonium salt waste. The method comprises the following process steps: the halogenated short chain quaternary ammoniumsalt waste is dissolved in water and decomposed under the action of inorganic base, a tertiary amine organic layer is produced and separated from a water layer, and raw material tertiary amine is recovered from the tertiary amine organic layer through distillation and applied to production of halogenated short chain quaternary ammonium salt; the water layer is subjected to extraction through trichloromethane, an extracted organic layer and an extracted water layer are produced, trichloromethane is recovered from the extracted organic layer through distillation for recycling, halogenated shortchain quaternary ammonium salt after recovery of trichloromethane is recrystallized, and qualified halogenated short chain quaternary ammonium salt is obtained; distilling concentration, crystallization and centrifugation are performed on the extracted water layer, and an inorganic bromide byproduct is obtained for recycling. The efficient, economical and environment-friendly method for recyclinghalogenated short chain quaternary ammonium salt waste is provided, so that the environment-friendliness of production of halogenated short chain quaternary ammonium salt is improved, waste dischargeis reduced, and production cost is reduced.

Description

technical field [0001] The invention relates to a method for recycling halogenated short-chain quaternary ammonium salt waste. Background technique [0002] Halogenated short-chain quaternary ammonium salts, as phase transfer catalysts, have been widely used in the synthesis of fine chemicals, pharmaceuticals, pesticide intermediates, and dye intermediates since the 1970s. Accelerator, used as clay stabilizer in petrochemical industry. [0003] Halogenated short-chain quaternary ammonium salts include tetraethylammonium bromide, tetrapropylammonium bromide, tetrabutylammonium bromide, benzyltriethylammonium chloride, benzyltripropylammonium chloride, benzyltributylammonium Ammonium chloride, etc., currently mainly use short-chain tertiary amines such as triethylamine, tripropylamine, tributylamine and haloalkanes such as bromoethane, bromopropane, bromobutane, benzyl chloride, etc. as raw materials, through quaternization reaction Prepare synthetically. In the synthesis a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/84C07C209/86C01D3/10C01D3/04
CPCC01D3/04C01D3/10C07C209/84C07C209/86C07C211/63
Inventor 项飞勇吴尖平王新伟
Owner KENTE CATALYSTS INC
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