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Copper and silicon catalyst for preparing ethanediol by hydrogenating dimethyl oxalate and preparation method thereof

A technology of dimethyl oxalate and catalyst is applied in the field of copper-silicon catalyst and preparation, and achieves the effects of being beneficial to industrial application, easy to operate, and high ethylene glycol selectivity

Active Publication Date: 2010-02-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using orthosilicate as a silicon source and using alcohol as a co-solvent to prepare a copper-silicon catalyst through a one-pot method, and using it for the gas-phase hydrogenation of dimethyl oxalate to produce ethylene glycol has not been proposed.

Method used

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  • Copper and silicon catalyst for preparing ethanediol by hydrogenating dimethyl oxalate and preparation method thereof
  • Copper and silicon catalyst for preparing ethanediol by hydrogenating dimethyl oxalate and preparation method thereof
  • Copper and silicon catalyst for preparing ethanediol by hydrogenating dimethyl oxalate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: Tetraethyl orthosilicate is the Cu that silicon source ethanol is co-solvent 0.3 Si-TEOS-E catalyst

[0020] Under stirring, 8.5g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 75 mL of water, and 25 mL of ethanol was added as a co-solvent. Then add ammonia water dropwise to the above solution until the pH value reaches 12-13, and continue stirring for 0.5 h after the dropwise addition to obtain a water-alcohol mixed solution of the copper ammonia complex. Then, 24.43 g of ethyl orthosilicate was added dropwise to the above mixed solution, and after stirring for 6 hours, it was aged at room temperature for 12 hours. The resulting mixture was heated and evaporated to remove most of the water, alcohol and ammonia, and then filtered, and the obtained solid was washed 5 times with water, dried at 120°C for 15 hours, and calcined at 450°C for 4 hours to obtain the catalyst precursor. The catalyst precursor was treated with 50 mL / min of H in a fixed-bed reactor 2 Af...

Embodiment 2

[0021] Embodiment 2: Ethyl orthosilicate is Cu that silicon source ethanol is co-solvent 0.05 Si-TEOS-E catalyst

[0022] Under stirring, 4.5g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 25 mL of water, and 125 mL of ethanol was added as a co-solvent. Then add ammonia water dropwise to the above solution until the pH value reaches 12-13, and continue stirring for 0.5 h after the dropwise addition to obtain a water-alcohol mixed solution of the copper ammonia complex. Then, 77.61 g of ethyl orthosilicate was added dropwise to the above mixed solution, and after stirring for several 6 hours, it was aged at room temperature for 6 hours. Other preparation conditions are the same as in Example 1, and the test results of the hydrogenation reaction activity of dimethyl oxalate are shown in Table 2.

Embodiment 3

[0023] Embodiment 3: Ethyl orthosilicate is silicon source methanol is the Cu of co-solvent 0.2 Si-TEOS-M catalyst

[0024] Under stirring, 8.5g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 150 mL of water, and 25 mL of methanol was added as a co-solvent. Then add ammonia water dropwise to the above solution until the pH value reaches 12-13, and continue stirring for 0.5 h after the dropwise addition to obtain a water-alcohol mixed solution of the copper ammonia complex. Add 36.65 g of ethyl orthosilicate dropwise to the above mixed solution, continue stirring for 6 hours, and then age at room temperature for 16 hours. Other preparation conditions are the same as in Example 1, and the test results of the hydrogenation reaction activity of dimethyl oxalate are shown in Table 3.

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Abstract

The invention discloses a copper and silicon catalyst for preparing ethanediol by hydrogenating dimethyl oxalate and a preparation method thereof. The copper and silicon catalyst is prepared by a one-pot method under conditions of taking ester orthosilicate as a silicon source and taking alcohol as a cosolvent and is concretely prepared in such a way that the ester orthosilicate is hydrolyzed andaged in a water-alcohol mixing solution of a copper ammonia complex, and then moisture, alcohol and ammonia are evaporated to enable copper components inside a copper ammonia solution to be uniformlysubsided, and finally washing, drying, roasting and reducing are carried out. The copper and silicon catalyst comprises copper and silicon dioxide, wherein the mol ratio of the copper to the silicon dioxide is 0.05-0.4 to 1. The copper and silicon catalyst shows very high reaction activity and selectivity in the reaction for preparing the ethanediol by hydrogenating the dimethyl oxalate and withina wider temperature range, is easy to operate and beneficial to industrial application.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a copper-silicon catalyst for hydrogenating dimethyl oxalate to prepare ethylene glycol and a preparation method thereof. Background technique [0002] Ethylene glycol, also known as glycol, is a colorless, odorless, sweet liquid that can be miscible with water in any proportion. Ethylene glycol is widely used and is an important chemical raw material. It reacts with terephthalic acid or dimethyl terephthalate to form polyethylene terephthalate, which can be used as polyester fiber and polyester plastic raw materials. Ethylene glycol can also be used as raw materials for films, rubber, plasticizers, lubricants, desiccants, brake fluids, and explosives. The freezing point of 60% ethylene glycol aqueous solution is -40°C, so it can also be used as an antifreeze for car radiators in winter. [0003] At present, ethylene glycol is mainly produced by ethylene oxide hydrat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J21/08B01J37/03B01J37/08B01J37/18C07C31/20C07C29/149
Inventor 王树荣骆仲泱岑可法方梦祥王勤辉朱玲君
Owner ZHEJIANG UNIV
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