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Decoloring method of 1,3,6-hexane trinitrile

A technology of hexanetrinitrile and hexanetrinitrile ethanol, which is applied to the purification/separation of carboxylic acid nitriles, organic chemistry, etc., can solve the problems of high chroma, prolonged storage time, and increased chroma, and achieve simple processing steps, The effect of improving quality stability

Inactive Publication Date: 2018-05-15
HUIZHOU CAPCHEM CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the invention is that the chroma of 1,3,6-hexanetrinitrile prepared in the prior art is relatively high, and the chroma increases significantly after prolonged storage, which is not conducive to using it in lithium battery electrolyte According to the situation of production, a simple and easy to obtain qualified electronic grade 1,3,6-hexanetrinitrile additive quickly and effectively

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] S1, 1,3,6-hexanetrinitrile pretreatment: add absolute ethanol to 1,3,6-hexanetrinitrile, the addition of said absolute ethanol is 1,3,6-hexanetrinitrile weight 10%, configured as 1,3,6-hexanetrinitrile ethanol solution;

[0024] S2, Activated carbon pretreatment: Pack granular activated carbon into a column, add 5% sodium hydroxide solution to soak, let it stand for 3 hours, then wash with water until the pH value of the effluent is 8, then rinse with ethanol until the effluent The water content is 0.5%, and the activated carbon column is obtained;

[0025] S3, decolorization treatment: put the 1,3,6-hexanetrinitrile ethanol solution described in step S1 on the column for decolorization, and control the outflow rate to 10 L / h to obtain the 1,3,6-hexanetrinitrile decolorization solution;

[0026] S4, concentration and drying: the 1,3,6-hexanetrinitrile decolorization solution described in step S3 is concentrated under reduced pressure at a temperature of 50°C and a vacu...

Embodiment 2

[0028] S1, 1,3,6-hexanetrinitrile pretreatment: add absolute ethanol to 1,3,6-hexanetrinitrile, the addition of said absolute ethanol is 1,3,6-hexanetrinitrile weight 30%, configured as 1,3,6-hexanetrinitrile ethanol solution;

[0029] S2, Activated carbon pretreatment: Pack granular activated carbon into a column, add potassium hydroxide solution with a concentration of 15% to soak, let stand for 2 hours, then wash with water until the pH value of the effluent is 9, then rinse with ethanol until the effluent The water content is 1%, and the activated carbon column is obtained;

[0030] S3, decolorization treatment: put the 1,3,6-hexanetrinitrile ethanol solution described in step S1 on the column for decolorization, and control the outflow rate to 25 L / h to obtain the 1,3,6-hexanetrinitrile decolorization solution;

[0031] S4, concentration and drying: the 1,3,6-hexanetrinitrile decolorization solution described in step S3 is concentrated under reduced pressure at a tempera...

Embodiment 3

[0033] S1, 1,3,6-hexanetrinitrile pretreatment: add absolute ethanol to 1,3,6-hexanetrinitrile, the addition of said absolute ethanol is 1,3,6-hexanetrinitrile weight 50%, configured as 1,3,6-hexanetrinitrile ethanol solution;

[0034] S2, Activated carbon pretreatment: Pack granular activated carbon into a column, add 25% sodium hydroxide solution to soak, let it stand for 2.5 hours, then wash with water until the pH value of the effluent is 9.5, and then rinse with ethanol until the effluent The water content is 0.4%, and the activated carbon column is obtained;

[0035] S3, decolorization treatment: put the 1,3,6-hexanetrinitrile ethanol solution described in step S1 on the column for decolorization, and control the outflow rate to 50 L / h to obtain the 1,3,6-hexanetrinitrile decolorization solution;

[0036] S4, concentration and drying: the 1,3,6-hexanetrinitrile decolorization solution described in step S3 is concentrated under reduced pressure at a temperature of 70°C a...

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PUM

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Abstract

The invention discloses a decoloring method of 1,3,6-hexane trinitrile. The decoloring method comprises the following steps: S1, pretreatment of the 1,3,6-hexane trinitrile; S2, pretreatment of activated carbon; S3, decoloring treatment; and S4, concentration and drying, so that 1,3,6-hexane trinitrile with low colourity and low free acid content is obtained. The invention provides a high-efficiency 1,3,6-hexane trinitrile decoloring method capable of reducing the free acid content; and the decoloring method has simple processing steps, and has popularization and application values.

Description

technical field [0001] The invention relates to the field of decolorization of electrolyte additives for lithium ion batteries, in particular to a decolorization method for 1,3,6-hexanetrinitrile. Background technique [0002] 1,3,6-Hexanetrinitrile has excellent properties such as wide electrochemical window, high anode stability, low viscosity and high boiling point, and has been widely used as an electrolyte additive for lithium-ion batteries. 1,3,6-Hexanetrinitrile as an electrolyte additive must meet the requirements of high purity and low chroma. [0003] The preparation of electronic grade 1,3,6-hexanetrinitrile in the prior art is first processed by vacuum distillation to obtain an orange-yellow liquid, which is dissolved in ethyl acetate, then a strong oxidant is added, and stirred for 6 to 24 hours; then Filtrate, wash the filter cake with ethyl acetate, collect the filtrate, and separate the filtrate to obtain an aqueous phase and an organic phase. Wash the organ...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C255/05
CPCC07C253/34C07C255/05
Inventor 曹英杰陈群杨婷元周建新程萌
Owner HUIZHOU CAPCHEM CHEM CO LTD
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