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Preparation method of 1,12-dihydroxydodecane

A technology of dodecanediol and dodecanedioic acid, applied in the field of medicine and chemical industry, can solve the problems of difficult separation and purification, low added value of market application, etc., achieve low hydrogenation pressure, increase added value of market application, low hydrogen The effect of ester ratio

Active Publication Date: 2019-12-13
ZHEJIANG BOJU NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is difficult to separate and purify n-hexanol and methylcyclopentanol in mixed monohydric alcohols through general rectification process, and the added value of market application is low

Method used

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  • Preparation method of 1,12-dihydroxydodecane
  • Preparation method of 1,12-dihydroxydodecane
  • Preparation method of 1,12-dihydroxydodecane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: 575 g of dodecanedioic acid and 2875 g of n-hexanol mixture were put into the reaction flask, stirred and heated up. The reaction was refluxed, and the water produced by the reaction was separated. Finally, the temperature was raised to 150°C for reflux reaction, and the reflux water separation reaction lasted for 8 hours. The acid value of the measured sample was 36.1mgKOH / g. After the reaction was completed, the heat preservation and reflux was stopped, and the material was cooled for standby.

Embodiment 2

[0040] Example 2: 575 g of dodecanedioic acid and 2300 g of n-hexanol mixture were put into the reaction flask, stirred and heated up. The reaction was refluxed, and the water produced by the reaction was separated. Finally, the temperature was raised to 170°C for reflux reaction, and the reflux water separation reaction lasted for 9 hours. The acid value of the measured sample was 32.1mgKOH / g. After the reaction was completed, the heat preservation and reflux was stopped, and the material was cooled for standby.

Embodiment 3

[0041] Example 3: 575 g of dodecanedioic acid and 2012.5 g of n-hexanol mixture were put into the reaction flask, stirred and heated up. The reaction was refluxed, and the water produced by the reaction was separated. Finally, the temperature was raised to 185°C, and the reflux and water separation reaction was carried out for a total of 10 hours. The acid value of the measured sample was 30.3 mgKOH / g. After the reaction was completed, the heat preservation and reflux was stopped, and the material was cooled for later use.

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Abstract

The invention relates to the technical field of pharmaceutical and chemical industry, in particular to a preparation method of 1,12-dihydroxydodecane. The preparation method of 1,12-dihydroxydodecanecomprises the steps that dodecanedioic acid is adopted to be subjected to an esterification reaction with n-hexanol, dihexyl dodecanedioate is obtained, and the target product 1,12-dihydroxydodecane is prepared through hydrogenation reduction. The method can be implemented without a catalyst, the separation step of the catalyst is reduced, so that esterification can be realized, the production steps are reduced, and the production cost is reduced.

Description

technical field [0001] The present application relates to the technical field of medicine and chemical industry, in particular to a preparation method of 1,12-dodecanediol. Background technique [0002] 1,12-Dodecanediol is used in the synthesis of pharmaceuticals, advanced coatings, advanced inks, advanced resins, synthetic fiber rubber, surfactants, etc. It is a white solid at room temperature, environmentally friendly and has good chemical stability. At present, the application for the production of high-carbon diols adopted by researchers at home and abroad is to generate high-carbon dibasic esters through the esterification of high-carbon dibasic acids with methanol, and then hydrogenate to prepare high-carbon dibasic alcohols, which are finally purified by rectification. Pure high-carbon diols can effectively improve the purity of the product and reduce the generation of by-products, with less waste and easy access to raw materials. [0003] Chinese invention patent a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/149C07C31/20C07C31/125C07C29/80
CPCC07C29/149C07C29/80C07C31/20C07C31/125
Inventor 周明和周兆昌周俊
Owner ZHEJIANG BOJU NEW MATERIALS CO LTD
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