Method for preparing ethylene glycol through photocatalytic conversion of methanol

A technology for preparing methanol and ethylene glycol, applied in the field of ethylene glycol, can solve problems such as unreported reports, and achieve the effects of broad application prospects, improved utilization, and low raw material prices

Active Publication Date: 2017-06-13
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, the above reports on the photocatalytic conversion of methanol to ethylene glycol all require the reaction of

Method used

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  • Method for preparing ethylene glycol through photocatalytic conversion of methanol
  • Method for preparing ethylene glycol through photocatalytic conversion of methanol
  • Method for preparing ethylene glycol through photocatalytic conversion of methanol

Examples

Experimental program
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Embodiment 1

[0041] 5mmol of Cd(NO 3 ) and 5mmol of Na 2 S was added to 80mL water respectively, and stirred thoroughly for 30min. The solution was transferred to a 100mL autoclave, the temperature was raised at a rate of 5°C / min, and the temperature was kept at 180°C for 24h to obtain hydrothermally synthesized CdS nanoparticles. After washing by centrifugation for 3 times, place it in an oven at 60°C for 12 hours, and dry it for later use. 20 mg of the prepared CdS nanoparticles were taken and added to 5 mL of a methanol-water solution with a mass percentage of methanol of 20%. Evacuate or feed inert gas under stirring to remove oxygen in the system, turn on a 300W xenon lamp, and carry out photocatalytic reaction under visible light conditions for 100h. After the reaction solution was filtered, liquid chromatography analysis showed that the conversion rate of methanol was 8.5%, the selectivity of ethylene glycol was 80%, and the yield of ethylene glycol was 6.8%.

Embodiment 2

[0043] Add 5 mmol of Cd(NO 3 ) 2 and 10mmol of (NH 3 ) 2 CS, magnetically stirred evenly, transferred to a 100mL autoclave, heated at a rate of 5°C / min, and kept at 160°C for 48h to obtain CdS nanorods. After washing by centrifugation for 3 times, place it in an oven at 60°C for 12 hours, and dry it for later use. CdS solid powder can be obtained after drying and grinding. 10 mg of the prepared CdS was added to 5 mL of methanol-water solution with a mass percentage of methanol of 80%. Evacuate or pass inert gas under stirring to remove the oxygen in the system, turn on the 500W xenon lamp, and carry out the photocatalytic reaction under the condition of visible light for 90h. After the reaction solution was filtered, liquid chromatography analysis showed that the conversion rate of methanol was 13%, the selectivity of ethylene glycol was 85%, and the yield of ethylene glycol was 11%.

Embodiment 3

[0045] Add 5 mmol of Cd(NO 3 ) 2 and 10mmol of (NH 3 ) 2 CS, magnetically stirred evenly, transferred to a 100ml autoclave, heated at a rate of 5°C / min, and kept at 150°C for 24h to obtain CdS nanorods. After centrifugal washing for 3 times, place in an oven at 60°C for 12 hours, dry and grind to obtain CdS solid powder. Take 0.5 g of the prepared CdS and disperse it into 100 mL of methanol-water solution with a methanol volume fraction of 20%, add 5 μL of chloroplatinic acid solution (0.1 g / ml) according to the loading capacity of 0.1%, stir and pump air. Reduction with a 300W xenon lamp for 1 h yielded CdS loaded with noble metal Pt nanoparticles, ie 0.1% Pt-CdS. Centrifugal washing, drying and grinding for later use. 5 mg of 0.1% Pt-CdS was added to 5 mL of methanol-water solution with a mass percentage of methanol of 95%. Evacuate or pass inert gas under stirring to remove the oxygen in the system, turn on the 300W xenon lamp, and carry out the photocatalytic reactio...

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Abstract

The invention provides a method for preparing ethylene glycol through photocatalytic conversion of methanol, and relates to ethylene glycol. The method for preparing ethylene glycol through photocatalytic conversion of methanol has the characteristics of greenness, environment friendliness, mild reaction conditions, high product selectivity and the like. The method comprises the following steps: adding a sulphide semiconductor catalyst or modified sulphide semiconductor catalyst into solvent, wherein the solvent is methanol or a methanol-water solution; removing oxygen gas in the system; and turning on a lamp source to perform photocatalytic reaction so as to obtain ethylene glycol. The ethylene glycol can be generated through conversion of methanol after performing photocatalytic reaction under the condition of visible light irradiation for some time by taking the sulphide semiconductor or modified sulphide semiconductor as a photocatalyst, thereby having the characteristics of greenness, environment friendliness, mild reaction conditions, high product selectivity and the like.

Description

technical field [0001] The invention relates to ethylene glycol, in particular to a method for photocatalytically converting methanol to prepare ethylene glycol. Background technique [0002] Ethylene glycol is an important basic chemical raw material, mainly used in the manufacture of resins, polyester fibers, cosmetics and explosives, etc. It can also be used as a solvent and antifreeze, and has a wide range of uses. my country is the largest ethylene glycol consumer in the world, and it is not self-sufficient at present, and the import volume of ethylene glycol is increasing year by year. According to the source of raw materials, the production methods of ethylene glycol can be divided into petroleum route and non-petroleum route. At present, the production method of ethylene glycol in the industry mainly adopts the petroleum route. The ethylene obtained from petroleum refining is oxidized in the gas phase to obtain ethylene oxide, and the ethylene oxide is then subjecte...

Claims

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Application Information

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IPC IPC(8): C07C29/32C07C31/20
Inventor 王野沈泽斌谢顺吉邓德会张庆红
Owner XIAMEN UNIV
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