Method for preparing catalyst for hydrogenation reaction of dimethyl oxalate and product

A technology of dimethyl oxalate and hydrogenation reaction, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of unutilization, low conversion rate of dissociation and fermentation, etc. The conditions are simple and are conducive to the effect of industrial application

Active Publication Date: 2011-07-20
ZHEJIANG UNIV
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  • Description
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  • Application Information

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Problems solved by technology

However, the current fermentation ethanol mainly comes from the fermentation of grains and grains, and can only use 6-carbon sugars in biomass, but cannot use 5-carbon sugars and lignin in biomass
In addition, the raw materials of ethanol in the current fermentation method mainly come from grain grains (the conversion rate of straw cellulose dissociation and fermentation is still too low), and grain grain fermentation produces ethanol and people compete for grain, and grain prices rise accordingly. At present, the state strictly restricts grain grain production. Fermentation to produce ethanol

Method used

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  • Method for preparing catalyst for hydrogenation reaction of dimethyl oxalate and product
  • Method for preparing catalyst for hydrogenation reaction of dimethyl oxalate and product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 3g copper nitrate (Cu(NO 3 ) 2 ·3H 2 O) solid, dissolved in 300ml deionized water, then add 7.47g urea, after dissolving, add dropwise 60g of silica sol with a silicon dioxide weight percentage content of 25%, stir for 4h, move the above mixture into a hydrothermal kettle, and heat at 60°C Keep the conditions for 24h, then keep at 120°C for 24h, then filter, wash with water, dry at 120°C, and roast at 450°C for 4h to obtain the catalyst precursor; use the catalyst precursor in a fixed-bed reactor 50mL / min H 2 After reduction at 350° C. for 3 h, a copper catalyst with a loading of 5% was obtained.

[0028] In the reaction of hydrogenation of dimethyl oxalate to produce methyl glycolate, at a temperature of 200°C and a pressure of 2 MPa, the ratio of hydrogen to dimethyl oxalate is 200, and the liquid volume space velocity is 0.8h -1 Under the above conditions, the conversion rate of dimethyl oxalate is 82%, and the selectivity of methyl glycolate is 92%.

Embodiment 2

[0030] Weigh 6.34g copper nitrate (Cu(NO 3 ) 2 ·3H 2 O) solid, be dissolved in 300ml deionized water, then add 7.87g urea. After dissolving, add 60g of silica sol with a weight percentage of 25% silica dropwise, and stir for 4 hours; transfer the above mixture into a hydrothermal kettle, keep it at 60°C for 48h, and then keep it at 90°C for 24h; other conditions are the same In Example 1, a copper catalyst with a loading of 10% was obtained.

[0031]In the reaction of hydrogenating dimethyl oxalate to produce methyl glycolate, at a temperature of 195°C and a pressure of 2 MPa, the ratio of the amount of hydrogen to dimethyl oxalate is 200, and the liquid volume space velocity is 1.0h -1 Under the above conditions, the conversion rate of dimethyl oxalate is 90%, and the selectivity of methyl glycolate is 87%.

Embodiment 3

[0033] Weigh 9.51g copper nitrate (Cu(NO 3 ) 2 ·3H 2 (0) Solid, dissolved in 200ml deionized water, then add 7.1g urea, after dissolving, add dropwise 40g silica sol with a silicon dioxide weight percentage content of 25%, and stir for 4h; The conditions were maintained for 36 hours; other conditions were the same as in Example 1, and a copper catalyst with a loading capacity of 20% was obtained.

[0034] In the reaction of hydrogenation of dimethyl oxalate to ethylene glycol, at a temperature of 200°C and a pressure of 2 MPa, the ratio of hydrogen to dimethyl oxalate is 200, and the liquid volume space velocity is 1.0h -1 Under the conditions, the conversion rate of dimethyl oxalate is 100%, and the selectivity of ethylene glycol is 99%.

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Abstract

The invention discloses a method for preparing a catalyst for a hydrogenation reaction of dimethyl oxalate, which comprises the following steps of: dissolving copper nitrate in water at room temperature to prepare aqueous solution of copper nitrate, wherein the concentration of the aqueous solution is between 0.04 and 1.0 mol / L; adding urea to dissolve a solid completely, adding silica sol with stirring, and continuing to stir for over 4 hours; adding a reaction mixture into a hydrothermal kettle, and keeping the temperature between 50 and 250 DEG C until the pH value is between 6 and 7; and filtering, and washing, drying, roasting and reducing the obtained solid to obtain a catalyst with 0.5 to 50 percent of the capacity of copper, wherein a ratio of the amount of substance of the coppernitrate to the urea is 1: (2-10). The invention also discloses a catalyst prepared by the method. In the preparation method, the catalyst is prepared from the low-cost silica sol serving as a siliconsource and the urea serving as a precipitant by a method of uniform precipitation, so the method has a simple process condition and is favorable for industrial production.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a method for preparing a multifunctional catalyst used for the hydrogenation reaction of dimethyl oxalate and a product prepared therefrom. Background technique [0002] Methyl glycolate is a colorless liquid with a pleasant odour. It has both the chemical properties of alcohol and ester, and is an important chemical raw material and pharmaceutical synthesis intermediate. It is widely used in many fields such as chemical industry, medicine, pesticide, feed, essence and fuel. Methyl glycolate is also an excellent solvent for cellulose, resin and rubber. Methyl glycolate is an important intermediate in the synthesis of isotricapine and its analogs with anticancer activity, and it is also a raw material for the synthesis of some anti-pressure carrier additives that improve the pressure resistance and wear resistance of lubricating oils. Methyl glycolate is hydrogenat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C31/20C07C29/149
Inventor 骆仲泱王树荣倪明江岑可法方梦祥朱玲君
Owner ZHEJIANG UNIV
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