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Catalyst for preparing methyl glycolate through hydrogenation of dimethyl oxalate and synthesis method and application of catalyst

A technology of dimethyl oxalate and methyl glycolate, which is applied in the preparation of carboxylate, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problem that the preparation cost of silver-based catalysts is high, which is unsuitable for industrial device application and the price of catalysts. Expensive, stability is yet to be investigated and other issues, to achieve the effect of improving activity and stability, high selectivity and low cost

Active Publication Date: 2020-11-13
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the copper-based catalyst has high hydrogenation activity and is the main catalyst for the preparation of ethylene glycol and ethanol; although the silver-based catalyst has a high selectivity for methyl glycolate, it has poor activity and poor stability, and the high preparation cost of the silver-based catalyst is not suitable for industrial applications.
Chinese patent CN 103785408A reports that a variety of metal-modified copper-silicon catalysts prepared by co-precipitation method have excellent selectivity in the hydrogenation of dimethyl oxalate to methyl glycolate, but the stability has yet to be investigated
However, the use of noble metal Ag as the main active component of the catalyst makes the catalyst expensive

Method used

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  • Catalyst for preparing methyl glycolate through hydrogenation of dimethyl oxalate and synthesis method and application of catalyst
  • Catalyst for preparing methyl glycolate through hydrogenation of dimethyl oxalate and synthesis method and application of catalyst
  • Catalyst for preparing methyl glycolate through hydrogenation of dimethyl oxalate and synthesis method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Weigh 7.6g of nickel nitrate hexahydrate and dissolve it in 75mL of deionized water, then take 10.0g of aluminum sesquioxide and put it in the above solution, add dropwise with 0.3mol / L sodium carbonate solution until the pH of the above solution is 12, at 80°C Stir for 5 hours, filter and wash with deionized water until the pH of the filtrate is about 7, dry at 100°C for 5 hours, and roast at 500°C for 5 hours. Weigh 2.0 g of sodium dihydrogen phosphate and dissolve it in 12 mL of deionized water, soak and age the calcined sample at room temperature for 24 h, dry at 100°C for 5 h, and calcinate at 500°C for 5 h to obtain the catalyst.

[0050] The above-mentioned catalyst is packed in a continuous fixed-bed reactor for reduction and activation treatment. The reduction temperature rises from room temperature to 600°C at 2°C / min, the reduction pressure is 0.2MPa, and the hydrogen volume space velocity is 150h -1 , the reduction time is 6h. The temperature is lowered to...

Embodiment 2

[0052] Weigh 7.6g of nickel nitrate hexahydrate and dissolve it in 75mL of deionized water, then take 10.0g of activated carbon and place it in the above solution, add dropwise 0.3mol / L sodium carbonate solution until the pH of the above solution is 12, stir at 80°C for 5h, After filtering, wash with deionized water until the pH of the filtrate is about 7, dry at 100°C for 5 hours, and roast at 500°C for 5 hours. Weigh 2.0 g of sodium dihydrogen phosphate and dissolve it in 12 mL of deionized water, soak and age the calcined sample at room temperature for 24 h, dry at 100°C for 5 h, and calcinate at 500°C for 5 h to obtain the catalyst.

[0053]The above-mentioned catalyst is packed in a continuous fixed-bed reactor for reduction and activation treatment. The reduction temperature rises from room temperature to 600°C at 2°C / min, the reduction pressure is 0.2MPa, and the hydrogen volume space velocity is 150h -1 , the reduction time is 6h. The temperature is lowered to 200°C,...

Embodiment 3

[0055] Weigh 7.6g of nickel nitrate hexahydrate and dissolve it in 75mL of deionized water, then take 10.0g of silicon dioxide and place it in the above solution, add dropwise 0.3mol / L sodium carbonate solution until the pH of the above solution is 12, and stir at 80°C After filtering for 5 hours, wash with deionized water until the pH of the filtrate is about 7, dry at 100°C for 5 hours, and roast at 500°C for 5 hours. Weigh 2.0 g of sodium dihydrogen phosphate and dissolve it in 12 mL of deionized water, soak and age the calcined sample at room temperature for 24 h, dry at 100°C for 5 h, and calcinate at 500°C for 5 h to obtain the catalyst.

[0056] The above-mentioned catalyst is packed in a continuous fixed-bed reactor for reduction and activation treatment. The reduction temperature rises from room temperature to 600°C at 2°C / min, the reduction pressure is 0.2MPa, and the hydrogen volume space velocity is 150h -1 , the reduction time is 6h. The temperature is lowered t...

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Abstract

The invention discloses a catalyst for preparing methyl glycolate through hydrogenation of dimethyl oxalate. The catalyst can be synthesized by two methods, the first method is that nickel salt and phosphate are simultaneously loaded directly through a co-deposition precipitation method to synthesize the catalyst containing different components of Ni and NiP at the same time; according to the second method, a catalyst intermediate containing Ni is synthesized through a deposition and precipitation method, and then the catalyst containing different components of Ni and NiP at the same time is synthesized through a secondary impregnation or programmed heating phosphate decomposition method. The catalyst is a non-noble metal catalyst, is low in cost and simple in synthesis method, and has thecharacteristics of good activity, high conversion rate, high selectivity, good stability and environmental friendliness in the reaction of selectively preparing methyl glycolate by hydrogenating dimethyl oxalate.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a catalyst for preparing methyl glycolate by hydrogenation of dimethyl oxalate and its synthesis method and application. Background technique [0002] Methyl glycolate (HOCH 2 COOCH 3 , MG) is the simplest alkyd ester, which is an important chemical product and intermediate, widely used in many fields such as chemical industry, medicine, pesticide, feed, dye and spice. Because its molecular structure contains α-H, hydroxyl and ester groups at the same time and has both the chemical properties of alcohol and ester, methyl glycolate can undergo catalytic hydrogenation to synthesize ethylene glycol, hydrolyze to form glycolic acid, and oxidize to form acetaldehyde Acid methyl ester, carbonylation reaction to prepare dimethyl malonate, ammonia solution to prepare glycine. Among them, methyl glycolate is hydrolyzed to prepare glycolic acid, and then biodegradable aliphat...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J35/10C07C69/675C07C67/31
CPCB01J27/185C07C67/31B01J35/61C07C69/675
Inventor 陈兴坤丁云杰林荣和王雪鹏
Owner ZHEJIANG NORMAL UNIVERSITY
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