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Method for reclaiming halogen acid salt of triethylamine in residue of synthesized vinylene carbonate

A technology of vinylene carbonate and ethylene carbonate, which is applied in the field of hydrohalide recovery, can solve environmental pollution and other problems, and achieve the effect of improving purity

Active Publication Date: 2013-01-30
BYD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, abandonment will undoubtedly bring environmental pollution. The use of the above-mentioned method to produce 1 ton of vinylene carbonate will produce about 7 tons of filter residue and consume 20 kilograms of activated carbon. The remaining residue is processed and recovered to obtain triethylamine hydrohalide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0016]The decolorization method can be various decolorization methods, so as to reduce the chromaticity of the mixed solution for removing solid matter to below 100 degrees under the condition of decolorization, for example, it can be a mixture of removing solid matter The method of fully contacting the liquid with the decolorizing agent, the method of fully contacting the mixed liquid for removing solid matter with the decolorizing agent may be a method of immersing the decolorizing agent in the mixed liquid for removing solid matter, or making the mixed liquid for removing solid matter The method in which the mixed solution of solid matter is passed through a chromatographic column with a decolorizing agent as a stationary phase. According to a preferred embodiment of the present invention, the method for decoloring includes immersing a decolorizing agent in the mixed solution for removing solid matter under decolorizing conditions, and making the mixed solution for removing ...

reference example 1

[0027] This reference example is used to obtain the residue containing triethylamine hydrochloride produced by the synthesis of vinylene carbonate.

[0028] Under nitrogen protection, under stirring conditions, 250 grams of chloroethylene carbonate, 400 grams of dimethyl carbonate, 2 grams of activated carbon, 2 grams of 2,6-di-tert-butyl-p-cresol (BHT) were added to 1000 ml In the three-necked round-bottomed flask, heat the temperature of the material in the three-necked round-bottomed flask to 55°C, then add 247 grams of triethylamine dropwise into the three-necked round-bottomed flask, and drop it in 100 minutes. The temperature of the material in the bottom flask was kept constant at 55°C, and then continued to react at this temperature for 24 hours and then filtered to obtain 350 grams of filter cake, which was the residue produced by the synthesis of vinylene carbonate containing triethylamine hydrochloride .

Embodiment 1

[0030] This embodiment is used to illustrate the recovery method of the hydrohalide salt of triethylamine in the residue of the synthetic vinylene carbonate provided by the present invention.

[0031] (1) 1100 grams of water and 1000 grams of the residue produced by the synthesis of vinylene carbonate containing triethylamine hydrochloride obtained according to the method of above-mentioned Reference Example 1 were fully mixed under stirring conditions at 25 ° C, and then decompressed Filtrate to obtain 1850 g of filtrate, which is the mixed solution for removing solid matter, and the mixed solution for removing solid matter is brown and opaque.

[0032] (2) Add 30 grams of activated carbon with a specific surface area of ​​1000 square meters per gram as a decolorizing agent to the above-mentioned mixed solution for removing solid matter, stir at 80°C for 30 minutes for adsorption and decolorization, and obtain a yellow opaque solution after filtration, using Shanghai Precision...

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Abstract

The invention discloses a method for reclaiming halogen acid salt of triethylamine in residue of synthesized vinylene carbonate. The method comprises the following steps: mixing the residue and a solvent to obtain mixed solution, and dissolving the halogen acid salt of the triethylamine in the residue by the category and dosage of the solvent; and then, removing solid substances in the mixed solution, contacting the mixed solution in which the solid substances are removed and a decolorizing agent to obtain the mixed solution with reduced chromaticity, crystallizing the mixed solution with reduced chromaticity, and contacting the crystallized solid and an extracting agent, wherein the extracting agent is a solvent used for a reaction capable of dissolving the vinylene carbonate, the triethylamine and the synthesized vinylene carbonate and a solvent for dissolving monohalogenated ethylene carbonate but not dissolving the halogen acid salt of the triethylamine. The purity of the halogen acid salt of the triethylamine obtained by the method is as high as 98 percent, and the halogen acid salt of the triethylamine can be used as a basic raw material for quaternary ammonium salt, medicine, pesticide, dye and organic synthesis. The method saves resources, and reduces environment pollution.

Description

technical field [0001] The present invention relates to the recovery method of the hydrohalide salt of triethylamine in the residue of synthesizing vinylene carbonate. Background technique [0002] As a new type of monomer and dienophile, vinylene carbonate has a wide range of uses. It can be used as a solvent in the electrolyte of lithium-ion batteries, and can also be used as a component of the surface coating of battery pole pieces. When vinylene carbonate is used as a highly reactive additive in lithium-ion secondary batteries, it can inhibit various undesirable reactions in the electrolyte, such as the decomposition of lithium hexafluorophosphate into LiF. When vinylene carbonate is used as a surface coating, for example, an SEI film with excellent performance can be formed on the surface of the negative electrode of the lithium-ion secondary battery, which can improve the charge-discharge efficiency and cycle characteristics of the lithium-ion secondary battery, so it ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/05C07C209/82C07D317/40
Inventor 袁园陈明先雪峰周雪永王艳峰
Owner BYD CO LTD