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Method for preparing ethylene glycol by photocatalytic methanol dehydrogenation coupling

A dehydrocoupling and ethylene glycol technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, organic compounds, etc., can solve problems such as poor selectivity of ethylene glycol, easy deactivation of catalysts, ZnS photocorrosion, etc. Achieve the effects of promoting performance, high product selectivity, and mild reaction conditions

Active Publication Date: 2020-02-04
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction activity is low, the selectivity of ethylene glycol is poor, and the photocorrosion of ZnS is serious under the condition of ultraviolet light, and the catalyst is easily deactivated.

Method used

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  • Method for preparing ethylene glycol by photocatalytic methanol dehydrogenation coupling
  • Method for preparing ethylene glycol by photocatalytic methanol dehydrogenation coupling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 20mmol of CdCl2 2.5H 2 O and 60 mmol of CH 4 N 2 S was added to 60 mL of anhydrous ethylenediamine, stirred thoroughly for 30 min, and then the solution was transferred to a 200 mL autoclave and kept at 150 °C for 12 h to obtain CdS nanorods. CdS nanorods were centrifuged and washed 3 times, placed in an oven at 60°C for 12 hours, dried for later use, dried and ground to obtain CdS solid powder, and 1% Co was photodeposited onto CdS nanorods to obtain a photocatalyst. Take 10 mg of the above photocatalyst and 300 mg of (trifluoromethyl)benzene, add them into 5 mL of methanol solvent, turn on a 300 W xenon lamp, and carry out photocatalytic reaction under visible light conditions for 12 h. After the reaction solution was filtered, liquid chromatography analysis showed that the generation rate of ethylene glycol was 23.3mmol g cat -1 h -1 , the selectivity of ethylene glycol is 90%.

[0035] Such as figure 1 Shown is the transmission electron microscope image of th...

Embodiment 2

[0037] 10mmol of Cd(CH 3 COO) 2 and 10mmol of Zn(CH 3 COO) 2 Add to 40mL deionized water, add ethylenediamine and thioacetamide, then add water to 60mL, transfer the above solution into a 100mL autoclave, heat to 230°C for 12h to obtain Zn 0.5 Cd 0.5 S nanorods, washed by centrifugation several times after cooling, dried for 12 h, and photodeposited 1% Mn to Zn 0.5 Cd 0.5 S, that is, the photocatalyst is prepared. Take 10 mg of the above photocatalyst and add it to 5 mL of methanol aqueous solution, add 100 mg of benzene, turn on a 300 W mercury lamp, and carry out photocatalytic reaction under visible light conditions for 4 hours. After the reaction solution was filtered, liquid chromatography analysis showed that the generation rate of ethylene glycol was 32mmol g cat -1 h -1 , the selectivity of ethylene glycol is 90%.

Embodiment 3

[0039] 3mmol Zn(CH 3 COO) 2 and 3mmol InCl 3 Add to 250mL deionized water respectively, then add thioacetamide, heat the above solution to 95°C and keep stirring for 5h to obtain Zn 2 In 2 S 5 . Ultrasonic washing and centrifugal drying, photodeposition of 1% Co to Zn 2 In 2 S 5 On, the photocatalyst is prepared. Take 10 mg of the above photocatalyst and add it to 5 mL of methanol solvent, add 100 mg of toluene, turn on a 300 W xenon lamp, and carry out photocatalytic reaction under ultraviolet light for 12 hours. After the reaction solution was filtered, liquid chromatography analysis showed that the generation rate of ethylene glycol was 15mmol g cat -1 h -1 , the selectivity of ethylene glycol is 85%.

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Abstract

The invention relates to a method for preparing ethylene glycol by photocatalytic methanol dehydrogenation coupling, belonging to the chemical field, which comprises the following steps: adding additive and photocatalyst into a solvent, uniformly dispersing, removing oxygen in the system, and then carrying out photocatalytic reaction to prepare ethylene glycol, wherein the solvent is methanol or methanol-water system, wherein the additive comprises at least one of an aromatic organic substance, a fluorine-containing organic compound and a fluorinated salt, and the photocatalyst is a semiconductor catalyst or a modified semiconductor catalyst. Using a small amount of additives can significantly promote methanol photocatalytisis to prepare ethylene glycol. The reaction is carried out in an inert atmosphere and has the characteristics of high catalytic activity, high product selectivity, mild reaction conditions and the like.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing ethylene glycol through photocatalytic methanol dehydrogenation coupling. Background technique [0002] Ethylene glycol is an important basic chemical product. In addition to being used as an antifreeze agent, it is also an important monomer for the synthesis of polyester polymers, mainly used in the production of polyester. The global annual consumption of ethylene glycol is as high as 34 million tons, of which my country accounts for about 50%. In recent years, the demand for ethylene glycol in my country has been increasing year by year, exceeding 15 million tons in 2018, more than half of which is dependent on imports. The traditional production methods of ethylene glycol can be divided into petroleum route and non-petroleum route according to different raw material sources. Among them, the petroleum route uses ethylene refined from petroleum to obtai...

Claims

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Application Information

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IPC IPC(8): C07C29/34C07C31/20B01J27/043B01J27/04B01J27/045B01J27/051
CPCC07C29/34B01J27/043B01J27/04B01J27/045B01J27/051B01J35/39C07C31/202Y02P20/52
Inventor 谢顺吉李径张海坤张庆红王野
Owner XIAMEN UNIV
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