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Method of preparing dibenzyl ether from benzyl alcohol under catalysis of graphene oxide

A technology of graphene catalyzing benzyl alcohol and dibenzyl ether, which is applied in the directions of dehydration of hydroxyl-containing compounds to prepare ether, chemical instruments and methods, catalysts for physical/chemical processes, etc. problem, to achieve the effect of high selectivity, environmental friendliness and high catalytic activity

Active Publication Date: 2012-10-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses microwave radiation, which is expensive, consumes a lot of energy, and is difficult to realize industrial application.

Method used

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  • Method of preparing dibenzyl ether from benzyl alcohol under catalysis of graphene oxide
  • Method of preparing dibenzyl ether from benzyl alcohol under catalysis of graphene oxide
  • Method of preparing dibenzyl ether from benzyl alcohol under catalysis of graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 0.5g of graphene oxide and 5g of benzyl alcohol in a 50ml three-necked flask, stir while heating, keep the temperature at about 90°C, and react for 24h. The reacted product was filtered under reduced pressure, and the filtrate was collected, which was a mixture of dibenzyl ether. Then the collected mixture containing dibenzyl ether was treated with CH 2 Cl 2 Diluted, and measured by Fuli GC9790 gas chromatography, the conversion rate of benzyl alcohol was 64.5%, and the selectivity of dibenzyl ether was 86.5%.

Embodiment 2

[0028] Mix 0.3g of graphene oxide and 6g of benzyl alcohol in a 50ml three-necked flask, stir while heating, keep the temperature at about 90°C, and react for 24h. The product after the reaction was suction filtered under reduced pressure, and the filtrate was collected, which was a mixture of dibenzyl ether. A 6 μL mixed sample was extracted with a gas chromatographic injection needle and the conversion rate of benzyl alcohol was 84.6% as measured by Fuli GC9790 gas chromatography. Dibenzyl ether The selectivity of ether is 84.8%, and the GC-MS test chart is attached figure 2 . Then the dibenzyl ether mixture was distilled at 220-240°C under normal pressure for 1 hour to obtain the remaining liquid which was dibenzyl ether, with a yield of 3.9 g and a yield of 70.9%.

Embodiment 3

[0030] Mix 0.3g of graphene oxide and 18g of benzyl alcohol in a 50ml three-necked flask, stir while heating, keep the temperature at about 90°C, and react for 24h. The reacted product was filtered under reduced pressure, and the filtrate was collected, which was a mixture of dibenzyl ether. Then the collected mixture containing dibenzyl ether was treated with CH 2 Cl 2 Diluted, and measured by Fuli GC9790 gas chromatography, the conversion rate of benzyl alcohol was 39.2%, and the selectivity of dibenzyl ether was 88.3%.

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Abstract

The invention discloses a method of preparing dibenzyl ether from benzyl alcohol under the catalysis of graphene oxide. The method is as follows: graphene oxide is used as a catalyst, benzyl alcohol is used as a raw material, then a reaction is carried out at a temperature of 70 to 170 DEG C and a normal pressure for 12 to 36 h under an insulation condition, and a reaction solution is subjected to post-treatment after the reaction is finished so as to prepare dibenzyl ether. According to the invention, graphene oxide is used as the catalyst to catalyze dehydration of benzyl alcohol so as to produce dibenzyl ether, and the catalyst has high catalytic activity, high selectivity and no pollution, is green and environment friendly and can selectively catalyze dehydration of benzyl alcohol to produce dibenzyl ether; no solvent is used in the reaction, no metal participates in the reaction, reaction conditions are mild, and environment friendliness of a resultant is obtained on the premise that the conversion rate of benzyl alcohol and high selectivity of dibenzyl ether are guaranteed.

Description

technical field [0001] The invention relates to a method for preparing dibenzyl ether by catalyzing benzyl alcohol with graphene oxide. Background technique [0002] Dibenzyl ether can be used in daily chemical flavor formulations, and is identified as GRAS (FEMANo.2371), approved by the FDA for use in food flavor formulations; used as plasticizers for nitrocellulose and cellulose acetate, resins, rubber, Solvent for wax, artificial musk, etc.; the mixture of dibenzyl ether and zinc oxide is a repellent for mosquitoes, flies, and fleas; it is used as a fixed liquid for gas chromatography; it is also used as a medium-level anti-aging agent, mainly for the manufacture of sponge rubber products . [0003] At present, dibenzyl ether can be produced industrially by co-heating benzyl alcohol and dilute sulfuric acid, but the separation of the product is difficult, it will corrode equipment, and there is also a hidden danger of environmental pollution. But because it is also a by...

Claims

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Application Information

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IPC IPC(8): C07C43/164C07C41/09B01J21/18C01B31/04C01B32/198
Inventor 王建国祝远帅庄桂林潘西
Owner ZHEJIANG UNIV OF TECH
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