Method for preparing linalool

A technology of linalool and dehydrolinalool, which is applied in hydrogenation preparation, chemical instruments and methods, preparation of hydroxyl compounds, etc., and can solve problems affecting the aroma of the final product linalool, etc.

Active Publication Date: 2020-04-17
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the post-processing process, it is found that if it is not handled properly, impurities will be produced, which will seriously affect the aroma of the final product linalool

Method used

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  • Method for preparing linalool

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Experimental program
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Effect test

Embodiment 1

[0031] First, after replacing the ammonia gas in the autoclave, add liquid ammonia (481g, 28.3mol), start stirring at a set speed, feed acetylene (112L, 5.0mol) and 50wt% potassium hydroxide aqueous solution (substrate 3mol%), add 6 -Methyl-5-hepten-2-one (126.1g, 1.0mol), control the temperature at 30°C, and react for 2 hours after the feeding of 6-methyl-5-hepten-2-one is completed, then release the pressure Acetylene gas and ammonia gas. Add 60g of pure water to the reaction solution for extraction, keep the water phase, add 60g of pure water to the organic phase for extraction, and sample the organic phase.

[0032] GC detection reaction. Composition of organic phase reaction liquid: dehydrolinalool 98.43%, 6-methyl-5-hepten-2-one 1.36%, 6-methyl-5-hepten-2-one acetylenic diol 0.03%, others 1.31%. The conversion rate is 98.64%, and the selectivity is 98.79%.

[0033] The composition of the rectification raw material methyl heptenone ynylation reaction liquid: water con...

Embodiment 2

[0040]Firstly, after replacing the ammonia in the autoclave, add liquid ammonia (481g, 28.3mol), start stirring at a set speed, feed acetylene (67.2L, 3.0mol) and 50wt% potassium hydroxide aqueous solution (substrate 1mol%), add 6-Methyl-5-hepten-2-one (126.1g, 1.0mol), control the temperature at 50°C, after the 6-methyl-5-hepten-2-one feed is completed, react for 6h, and release the pressure Release acetylene gas and ammonia gas. Add 60g of pure water to the reaction solution for extraction, keep the water phase, add 60g of pure water to the organic phase for extraction, and sample the organic phase.

[0041] GC detection reaction. Composition of organic phase reaction liquid: dehydrolinalool 97.09%, 6-methyl-5-hepten-2-one 1.57%, 6-methyl-5-hepten-2-one acetylenic diol 0.01%, others 1.33%. The conversion rate is 98.43%, and the selectivity is 98.64%.

[0042] The composition of the rectification raw material methyl heptenone ynylation reaction liquid: water content 4.52%...

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Abstract

The invention provides a method for preparing linalool. The method specifically comprises the following steps: taking 6-methyl-5-heptene-2 one as a raw material, carrying out ethynylation reaction toprepare dehydrolinalool, removing water in a reaction system, carrying out conventional distillation or rectification for separating dehydrolinalool, and carrying out selective hydrogenation to synthesize linalool. Impurities with the molecular weight of 170 (M = 170) can be generated in the treatment process of the 6-methyl-5-heptene-2 one ethynylation reaction liquid, and the content of the impurities should be strictly controlled to be 0.01% or below in order to regulate and control the final product linalool aroma. In order to control the content of the impurity, the generation of the impurity can be optimized and inhibited in the aspect of a post-treatment mode of a 6-methyl-5-heptene-2 one acetylation reaction solution, or the impurity is removed by adopting an efficient rectification mode.

Description

technical field [0001] The invention relates to a method for preparing linalool. Background technique [0002] Linalool is an important fragrance product and can synthesize vitamin E and dozens of fragrances, such as linalyl acetate, linalyl propionate, Erinthal, dihydrolinalool and its esters, tetrahydrolinalyl Alcohols and their esters, etc. One of the synthetic methods of linalool is to use 6-methyl-5-hepten-2-ketone as raw material to prepare dehydrolinalool through acetylenization reaction, and then synthesize linalool through selective hydrogenation. [0003] [0004] Linalool is an important spice species, the purity of its aroma is the most important indicator of its quality, and trace impurities may affect its aroma. [0005] One of the synthetic methods of linalool is to use 6-methyl-5-hepten-2-ketone as raw material to prepare dehydrolinalool through acetylenization reaction, and then synthesize linalool through selective hydrogenation. 6-Methyl-5-hepten-2 k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C29/80C07C33/02
CPCC07C29/17C07C29/44C07C29/80C07C33/02C07C33/048
Inventor 鲍元野陈帅张永振黎源
Owner WANHUA CHEM GRP CO LTD
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