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Technology for preparing vanillyl alcohol ether by using one step method

A kind of technology, vanilla technology, applied in the field of vanillyl alcohol ether production technology, can solve the problems of non-reusable, low yield, high price, etc., and achieve the effect of no waste discharge, simple process route and mild reaction conditions

Active Publication Date: 2016-06-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the acid-catalyzed dehydration system generally has a low yield and needs to be added to a water outlet, and it is easy to produce vanillyl alcohol ether and butyl ether as by-products. Secondly, the price of vanillyl alcohol as a raw material is relatively expensive, which increases the production cost.
It is a good method to use vanillin as a raw material to reduce vanillyl alcohol through sodium borohydride, and then to synthesize vanillyl butyl ether with n-butanol. However, this method is carried out in two steps, which increases the complexity of the process. Using sodium borohydride as a reducing agent is not only expensive, but also cannot be reused

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Preparation of nano-ruthenium metal catalyst A: Dissolve 10 g of ruthenium trichloride in ethanol, add 200 g of silicon dioxide, stir for 24 hours, evaporate the ethanol to dryness to obtain a solid, and reduce the solid under hydrogen at 180° C. for 3 hours to obtain catalyst A.

Embodiment 2

[0014] Preparation of nano-ruthenium metal catalyst B: Dissolve 10 g of ruthenium trichloride in ethanol, add 400 g of aluminum oxide, stir for 24 hours, evaporate the ethanol to dryness to obtain a solid, and reduce the solid under hydrogen at 220°C for 2 hours to obtain catalyst B.

Embodiment 3

[0016] Preparation of nano-ruthenium metal catalyst C: Dissolve 10 g of ruthenium trichloride in ethanol, add 300 g of titanium dioxide, stir for 24 hours, evaporate the ethanol to dryness to obtain a solid, and reduce the solid under hydrogen at 200° C. for 4 hours to obtain catalyst C.

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PUM

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Abstract

The invention relates to a technology for preparing vanillyl alcohol ether by using a one step method. The technology combines co-catalysis of a nano ruthenium metal catalyst and an immobilized tin phosphotungstate catalyst, and vanillin is subjected to a reaction for 18-24 hours under hydrogen pressure of 1-2 MPa and an alcohols solvent in a reaction vessel at the temperature of 20-60 DEG C to obtain vanillyl alcohol ether by using the one step method. The technology can be carried out under mild condition, has the advantages of environmental protection and high product yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a production process of vanillyl alcohol ether, in particular to a one-step preparation method using vanillin as a raw material, n-butanol as a solvent, hydrogen as a reducing agent, and catalyzed by a nanometer ruthenium metal catalyst and an immobilized tin phosphotungstate catalyst Process of vanillyl ether. Background technique [0002] Vanillyl ether, also known as capsicum ether, has a strong curry aroma and is widely used as a food flavoring agent. And because of the remarkable heating effect, it has the effect of accelerating the blood circulation of the human body and causing a local heating sensation. As a heating agent in cosmetics, it is especially suitable for women's cleansing in cold winter, and as a heating agent in plasters, it has the effect of dispelling wind and cold. Among them, vanillyl butyl ether is most widely used in food and cosmetics. In the traditional synthesis method, it is obtained by reacting ...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/09C07C41/18
Inventor 黄军常俊
Owner NANJING UNIV OF TECH
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