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Preparation method of 6-hydroxyhexanoate

A technology of hydroxycaproic acid ester and hydroxycaproic acid is applied in the field of preparation of 6-hydroxycaproic acid ester, which can solve the problems of high price, difficult to crystallize, and reduce viscosity, and achieves low production cost, high product quality and simple steps. Effect

Inactive Publication Date: 2020-12-01
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN109796420A uses trishydroxyethyl isocyanurate and caprolactone as raw materials to generate trishydroxyethyl isocyanurate 3(6-hydroxyl-1-hexanoate) under the action of a nitrogen atmosphere and a catalyst at 100-180°C. Its essence is to modify trihydroxyethyl isocyanurate to improve its water resistance, curing speed and pigment dispersion performance, so as to facilitate the synthesis of trihydroxyethyl isocyanurate and acrylate. Ethylisocyanurate triacrylate reduces viscosity at room temperature, and makes it difficult to crystallize at low temperature, so as to facilitate its use. The domestic production of ε-caprolactone used in it is relatively low, and most of it needs to be imported from abroad, which makes it high prices

Method used

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  • Preparation method of 6-hydroxyhexanoate
  • Preparation method of 6-hydroxyhexanoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix 30g of 6-hydroxycaproic acid and 20g of glycerol in a 250ml round-bottomed flask, add 0.5g of cation exchange resin at 50°C, place it in a collector-type constant temperature heating magnetic stirrer, and undergo an esterification reaction for 2 hours to obtain poly 6-hydroxycaproic acid ester, then add 20ml cyclohexane in the obtained poly 6-hydroxycaproic acid ester, remove water to obtain poly 6-hydroxycaproic acid ester 28.3g, poly 6-hydroxycaproic acid ester yield 94.3% .

Embodiment 2-5

[0020] The quality of 6-hydroxycaproic acid is the same as in Example 1, and others are different from Example 1, see Table 1 for details.

Embodiment 6-10

[0022] The quality of 6-hydroxycaproic acid is 40g, and others are different from Example 1, see Table 1 for details.

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Abstract

The invention provides a preparation method of 6-hydroxyhexanoate, which comprises the following steps: mixing 6-hydroxyhexanoic acid, a catalyst and alcohol, carrying out esterification reaction at 40-300 DEG C for 1-5 hours, adding a water-carrying agent after the reaction is finished, and removing water to obtain the poly-6-hydroxyhexanoate. The method has the beneficial effects that (1) the technical steps are simple, the production cost is low, and the economic benefit is high, (2) no intermediate product is produced in the technology, other product water is easy to separate and has no influence on the environment, and the process safety coefficient is high, and (3) the yield of the 6-hydroxyhexanoate is 90% or above, the production effect is good, and the product quality is high.

Description

technical field [0001] The invention belongs to the chemical industry, and in particular relates to a preparation method of 6-hydroxycaproic acid ester. Background technique [0002] 6-Hydroxycaproate is a very useful organic chemical intermediate. Poly6-Hydroxycaproate can be synthesized by polymerization of 6-Hydroxycaproate, and can further generate polycaprolactone or polycaprolactone polyol , Polycaprolactone has a wide range of uses in medical materials, drug carriers, plastic modifiers and plasticizers. [0003] Currently in the production data about 6-hydroxyhexanoate, the patent CN101945847A produces 6-hydroxy from the by-product mixture of the process of oxidizing cyclohexane into cyclohexanone and cyclohexanol using oxygen or an oxygen-containing gas mixture. Hexanoic acid esters, which are 6-hydroperoxycaproic acid, 6-hydroxycaproic acid, 5-formylvaleric acid, and α, ω- Dicarboxylic acid is used as a raw material, and 6-hydroxycaproic acid is prepared by hydrog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/675
CPCC07C67/08C07C69/675
Inventor 谢传欣
Owner QINGDAO UNIV OF SCI & TECH
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