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The preparation method of 2-hexyl adipic acid

A technology based on adipic acid and hexyl, applied in the field of chemical synthesis, can solve the problems of poor high temperature resistance of capacitors, large amount of solvent used, and long reaction time, etc.

Active Publication Date: 2021-03-19
武汉海斯普林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of electrolyte has low conductivity, and the water produced by the esterification reaction during cooking makes the capacitor's high temperature resistance extremely poor.
In recent years, dicarboxylic acids or ammonium salts of linear chains (azelaic acid, sebacic acid) or branched chains (alkyl sebacic acid, butyl suberic acid) have been used as the main solute. This type of electrolyte is stable at high temperatures. There are more or less defects in performance, solubility, low temperature performance, conductivity and other properties
[0003] 2-Hexyl adipic acid, as a new type of branched dicarboxylic acid, has high thermal stability, but its preparation method is rarely reported
The problems of this method are: the amount of solvent used is large, the potential safety hazard is large, the reaction time is long, the equipment is corroded, the waste liquid is difficult to handle, and there are many condensation by-products, etc.
Because carbonyl cyclopentanone is easy to open the ring under alkaline conditions and alcohol solution, there are many by-products, and the yield is as low as 50% or less

Method used

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  • The preparation method of 2-hexyl adipic acid
  • The preparation method of 2-hexyl adipic acid
  • The preparation method of 2-hexyl adipic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 126g cyclopentanone, 567g dimethyl carbonate and 12.6g solid base catalyst KF / Al in the 1000ml there-necked flask that has stirrer, condensing tube and thermometer 2 o 3 , wherein, the solid base catalyst loading is 10 (w / w)%, and the reflux reaction is carried out for 3h. After cooling, the catalyst was filtered off, the filtrate was distilled off the solvent under reduced pressure and rectified, and 167 g of fractions were collected under a pressure of 11 mmHg and 102 ° C to 104 ° C to obtain a colorless and transparent liquid 2-methoxycarbonyl cyclopentanone. The yield of this step was 78.4 %. The recovered solvent is collected, rectified, and recycled again, which reduces costs on the one hand and is beneficial to environmental protection on the other.

[0032] Add 110g of ethylene glycol dimethyl ether, 28.4g of 2-methoxycarbonylcyclopentanone, and 66g of n-bromohexane into a 500ml three-necked flask equipped with a stirrer, condenser and thermometer, slowly ...

Embodiment 2

[0035] Add 126g cyclopentanone, 567g dimethyl carbonate and 12.6g solid base catalyst KF / Al in the 1000ml there-necked flask that has stirrer, condensing tube and thermometer 2 o 3, wherein, the solid base catalyst loading is 40 (w / w)%, and the reflux reaction is 8h. After cooling, the catalyst was filtered off, the filtrate was distilled off the solvent under reduced pressure and rectified, and 167 g of fractions were collected under a pressure of 11 mmHg and 102°C to 104°C to obtain a colorless and transparent liquid 2-methoxycarbonylcyclopentanone. The yield of this step was 78.4 %. The recovered solvent is collected, rectified, and recycled again, which reduces costs on the one hand and is beneficial to environmental protection on the other.

[0036] Add 170g of ethylene glycol dimethyl ether, 42.6g of 2-methoxycarbonylcyclopentanone, 99g of n-bromohexane, slowly add 124g of potassium carbonate in batches, and phase Transfer catalyst tetrabutylammonium bromide and 0.426...

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Abstract

The invention provides a 2-hexyl adipic acid preparation method. The method comprises the following steps: 1) reacting cyclopentanone and dimethyl carbonate in existence of a solid base catalyst; 2) performing substitution on an intermediate methyl 2-cyclopentanonecarboxylate obtained in the step 1) and n-hexyl bromide under the effect of phase transfer catalysis to form methyl 2-hexyl cyclopentanone; 3) performing a ring-opening reaction on the product obtained in the step 2) under basic condition to obtain methyl 2-hexyl-methyl adipate; and 4) performing saponification and acidifying on theproduct obtained in the step 3) to obtain 2-hexyl adipic acid. The preparation method of the invention has low cost and high yield; the post-treatment is simple, and a solvent can be recycled after being simply processed.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of 2-hexyl adipic acid. Background technique [0002] The traditional middle and high voltage aluminum electrolytic capacitor capacitor electrolyte mainly uses ethylene glycol as the main solvent, and inorganic compounds such as boric acid or ammonium pentaborate as the main solute. This type of electrolyte has low conductivity, and the water produced by the esterification reaction during cooking makes the capacitor's high temperature resistance extremely poor. In recent years, dicarboxylic acids or ammonium salts of linear chains (azelaic acid, sebacic acid) or branched chains (alkyl sebacic acid, butyl suberic acid) have been used as the main solute. This type of electrolyte is stable at high temperatures. Performance, solubility, low temperature performance, electrical conductivity and other properties have more or less certain defects. [0003] 2-Hexyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00C07C67/343C07C69/757C07C67/333C07C69/34C07C51/09C07C51/02C07C55/21
CPCC07C51/02C07C51/09C07C67/00C07C67/333C07C67/343C07C2601/08C07C2601/14C07C69/757C07C69/34C07C55/21
Inventor 郭春花周宜海王文刘司齐
Owner 武汉海斯普林科技发展有限公司