Method for continuously preparing linalool from allylic alcohol by isomerization process

A technology of allyl alcohol and isomerization, which is applied in the field of continuous preparation of linalool from allyl alcohol by isomerization method, can solve the problems of high waste rate, low reaction conversion rate and high reaction temperature, and achieves low price. , high yield and high selectivity

Active Publication Date: 2016-01-06
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the price of vanadium-based catalysts is low, which is conducive to reducing costs. The disadvantages are that the reaction conversion rate is low and the reaction temperature is high (above 160 ° C), resulting in a high waste rate.

Method used

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  • Method for continuously preparing linalool from allylic alcohol by isomerization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1 A kind of method that allyl alcohol continuously prepares linalool through isomerization method

[0038] (1) Preparation of vanadium amine complex catalyst

[0039] Add 500.0g of xylene to a 1000ml three-necked flask equipped with a thermometer, condenser and mechanical stirring, add 5.0g (0.0274mol) of vanadium pentoxide and 5g (0.0494mol) of triethylamine, turn on the mechanical stirring to raise the temperature, at 140 ℃ for 1 hour, lower the temperature, and then filter through a sand core funnel, and the filter cake is washed twice with ether to obtain a vanadium amine complex catalyst, about 5.9 g.

[0040] (2) Add reactants and catalysts

[0041] In the 1000ml there-necked flask that is furnished with thermometer, 60cm rectifying column and magnetic force stirrer, add 500.0g geraniol content and be 35.6% geraniol / nerol mixture with geraniol content, add vanadium amine Complex catalyst 5.9g.

[0042] (3) Control of isomerization reaction conditions...

Embodiment 2

[0049] Embodiment 2 A kind of method that allyl alcohol continuously prepares linalool through isomerization

[0050] (1) Preparation of catalyst vanadium amine complexes

[0051]Add 500.0g of xylene, 20g (0.133mol) of vanadium trioxide and 8.5g (0.144mol) of n-propylamine into a 1000ml three-neck flask equipped with a thermometer, condenser and mechanical stirring, and turn on mechanical stirring to raise the temperature. Keep warm for 2 hours, lower the temperature, and then filter through a sand core funnel. The filter cake is washed twice with ether to obtain about 25.2 g of vanadium amine complex catalyst.

[0052] (2) Add reactants and catalysts

[0053] Add 500.0 g of geraniol with a content of 98.7% to a 1000 ml three-necked flask equipped with a thermometer, a 60 cm rectifying tower and a magnetic stirrer, and 25.2 g of a vanadium amine complex catalyst.

[0054] (3) Control of isomerization reaction conditions

[0055] Stir and heat up, turn on the vacuum pump to ...

Embodiment 3

[0061] Embodiment 3 A kind of method that allyl alcohol continuously prepares linalool through isomerization method

[0062] (1) Preparation of vanadium amine complex catalyst

[0063] Add 500.0g xylene, 30g (0.256mol) ammonium metavanadate and 10.5g (0.172mol) ethanolamine to a 1000ml three-neck flask equipped with a thermometer, condenser and mechanical stirring, turn on the mechanical stirring to raise the temperature, and keep it warm at 140°C After 2 hours, the temperature was lowered, and then filtered through a sand core funnel, and the filter cake was washed twice with ether to obtain about 33.6 g of vanadium amine complex catalyst.

[0064] (2) Add reactants and catalysts

[0065] In a 1000ml three-neck flask equipped with a thermometer, a 60cm rectifying tower and a magnetic stirrer, 500.0g of nerolidol with a content of 98.0% was added, and 33.6g of a vanadium amine complex catalyst was added.

[0066] (3) Control of isomerization reaction conditions

[0067] Sti...

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Abstract

The invention provides a method for continuously preparing linalool from allylic alcohol by an isomerization process. The method comprises the following steps: preparing a vanadium-amine complex catalyst, adding a reacting product and a catalyst, controlling isomerization reaction conditions, constantly adding the reacting product, and constantly rectifying, wherein the vanadium-amine complex catalyst is prepared by adding 1 part by weight of xylene, 0.01-0.1 part by weight of a vanadium compound and 0.01-0.1 part by weight of nitrogen base, starting to stir and heat, insulating for 1-3 hours at 140 DEG C, cooling to below 50 DEG C, and filtering to reclaim the catalyst. According to the method, the catalyst system has high reaction selectivity, the selectivity of linalool is 93.2-96.2 percent, the yield of linalool is 92.7-94.5 percent, the scrap rate is 2.7-4.0 percent, and the linalool content is 98.5-98.7 percent. The catalyst has low unit consumption.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for continuously preparing linalool from allyl alcohol through an isomerization method. Background technique [0002] Linalool (Linaloo1) has another name called linalool, linalool. The scientific name is 3,7-dimethyl-1,6-octadien-3-ol. Most of linalool and its esters have a beautiful and pleasant floral aroma. It occupies an important position in many fragrance-type flavor formulas. It can be used to blend various flavors such as lily, clove, and orange blossom, or to synthesize vitamin E, An important raw material for A. [0003] The isomerization reaction of allyl alcohol is the 1,3-migration of the corresponding hydroxyl group and the movement of the corresponding double bond. The isomerization reaction equation of geraniol / nerol is as follows: [0004] [0005] The catalysts currently available for the isomerization of allyl alcohol mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/56C07C29/80C07C33/02
CPCC07C29/56C07C29/80C07C33/02
Inventor 马啸赵文乐张相如周剑平鲁光银陈为超马书召
Owner SHANDONG NHU PHARMA
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