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Method for preparing alpha-phenethyl alcohol by using supported zirconium oxide as catalyst

A technology of zirconium oxide and phenethyl alcohol, which is applied in the field of preparing α-phenethyl alcohol by using supported zirconium oxide as a catalyst, can solve the problems of unfavorable industrial application, increased catalyst difficulty and production cost, active site poisoning and deactivation, etc. The effect of reducing reaction energy consumption, easy separation and high selectivity

Inactive Publication Date: 2011-09-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the patent (publication number: CN 101792368A), a method for preparing α-phenylethanol with activated carbon supported alkaline earth metals has been disclosed, which has higher catalyst activity, shorter reaction time and higher selectivity, but there is also the need for activated carbon to The disadvantage of roasting at higher temperature and under the protection of nitrogen, and the active component is alkaline earth metal, which is harmful to moisture and CO in the air 2 More sensitive, easy to cause active site poisoning and inactivation
These disadvantages have increased the difficulty and production cost of catalyst preparation, which is not conducive to industrial application.

Method used

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  • Method for preparing alpha-phenethyl alcohol by using supported zirconium oxide as catalyst
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  • Method for preparing alpha-phenethyl alcohol by using supported zirconium oxide as catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: Preparation of MCM-41 mesoporous molecular sieve carrier

[0030] Fully dissolve 14.00g (0.038mol) cetyltrimethylammonium bromide in 400mL deionized water, add it to a 1000mL round bottom flask, and slowly add 41.00g (0.20mol) orthosilicic acid dropwise under stirring Ethyl ester, while using 4M sodium hydroxide solution to adjust the pH value to 11.0. After the dropwise addition, the reaction solution was aged at room temperature (25°C) for 2 hours, and then the reaction solution was poured into a crystallization kettle and crystallized at 110°C. After 24 hours of crystallization, the crystal was washed with about 5.0L deionized water for several times until neutral, and dried to obtain the semi-finished product of MCM-41 mesoporous molecular sieve. Calcined for 6 hours to obtain about 9.00 g of the MCM-41 mesoporous molecular sieve carrier.

Embodiment 2Z

[0031] Example 2ZrO 2 Preparation and Catalytic Performance of / MCM-41 Mesoporous Molecular Sieve Catalyst

[0032] 0.14gZr(NO 3 ) 4 ·5H 2 After O is completely dissolved in 60 mL of deionized water, pour it into a 250 mL three-necked flask, add 4 g of the MCM-41 type mesoporous molecular sieve carrier prepared by the method in Example 1, place the flask in a 60°C oil bath, and keep stirring until Evaporate to dryness, then dry in an oven at 100°C for 24h, and finally bake in a muffle furnace at 550°C for 4h to obtain ZrO with a loading of 1wt%. 2 / MCM-41 mesoporous molecular sieve catalyst is about 4.04g.

[0033]In a 50mL single-necked flask, add the ZrO prepared above with a loading of 1wt%. 2 / MCM-41 type mesoporous molecular sieve catalyst 0.5g, isopropanol 3.6g (30mmol), acetophenone 0.24g (1mmol), then the flask was reacted at a constant temperature in an 82°C oil bath while stirring continuously, after 8 hours of reaction, Finish the reaction, filter and separate...

Embodiment 3～8

[0034] Embodiment 3~8: different load ZrO 2 Preparation and Catalytic Performance of / MCM-41 Mesoporous Molecular Sieve Catalyst

[0035] 0.28g, 0.7g, 1.4g, 2.8g, 4.2g and 7.0g Zr(NO 3 ) 4 ·5H 2 After O was completely dissolved in 60 mL of deionized water, pour them into 250 mL three-necked flasks respectively, then add 4 g of MCM-41 type mesoporous molecular sieve carriers prepared according to the method in Example 1, and place the flasks in an oil bath at 60° C. Stir continuously until evaporated to dryness, then dry in an oven at 100°C for 24h, and finally bake in a muffle furnace at 550°C for 4h to obtain loadings (based on carrier mass) of 2wt%, 5wt%, 10wt%, 20wt%, 30wt% and 50wt% ZrO 2 / MCM-41 type mesoporous molecular sieve catalyst, the quality of each catalyst obtained after the roasting is completed: 2wt%ZrO 2 / The mass of MCM-41 is about 4.08g, 5wt% ZrO 2 / The mass of MCM-41 is about 4.2g, 10wt% ZrO 2 / The mass of MCM-41 is about 4.4g, 20wt% ZrO 2 / The ...

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Abstract

The invention discloses a method for preparing alpha-phenethyl alcohol by using supported zirconium oxide as a catalyst, which comprises the following steps of: reacting acetophenone serving as a raw material at the temperature of between 50 and 120DEG C and normal pressure for 2 to 12 hours by taking alcohol as a hydrogen source and the supported zirconium oxide as the catalyst, and performing posttreatment on reaction liquid obtained through the reaction to obtain the alpha-phenethyl alcohol, wherein the alcohol is C1-C7 fatty alcohol or C3-C7 alicyclic alcohol; the molar ratio of the acetophenone to the alcohol is 1:(1-40); and the supported zirconium oxide consists of a carrier and an active ingredient of zirconium oxide supported on the carrier, the carrier is an MCM-41 mesoporous molecular sieve, and the capacity of the zirconium oxide is 0.2 to 50 weight percent. The reaction is carried out at normal pressure, reaction conditions are mild, the energy consumption of the reaction is reduced, and the requirement of reaction equipment is reduced; and the catalyst has high selectivity, activity and water resistance, is a multi-phase catalyst, and is easy to separate from a product.

Description

(1) Technical field [0001] The invention relates to a method for preparing alcohol, in particular to a method for preparing α-phenethyl alcohol by using supported zirconium oxide as a catalyst. (2) Background technology [0002] α-Phenylethyl alcohol is a more important compound in aromatic compounds. It is widely used in the synthesis of food flavors and various rose oils and essential oils because of its pleasant and long-lasting rose aroma. In the synthesis of many drugs, α-phenylethanol is also an important drug intermediate. [0003] Currently known synthetic methods for producing α-phenylethanol mainly include: microbial fermentation, organic synthesis and other main methods. [0004] For example, Huabao Aroma Technology Development (Shanghai) Co., Ltd. (authorized announcement number CN1159447C) uses tobacco as the precursor of biotransformation, selects suitable strains, and carries out fermentation and cultivation under certain fermentation process conditions to co...

Claims

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Application Information

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IPC IPC(8): C07C33/22C07C29/143B01J29/70
Inventor 袁剑张波徐春雷汤明慧葛忠华
Owner ZHEJIANG UNIV OF TECH