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Ethylene glycol catalyst prepared by dimethyl oxalate plus hydrogen and preparation method and application thereof

A technology of dimethyl oxalate and catalyst, which is applied in the field of copper-hydrotalcite catalyst and its preparation, can solve the problems of unsatisfactory batch preparation repeatability, insufficient research on ethylene glycol, and poor dispersion of active metals, etc., and achieve easy industrialization The effect of production, low cost and easy operation

Inactive Publication Date: 2009-06-03
SHANGHAI UNIV OF ENG SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the research on the hydrogenation of oxalate to ethylene glycol is not thorough enough. They use Cu / SiO 2 Catalyst, for 200-2500℃, below 3.0MPa, hydrogen-ester ratio 30-100, liquid space velocity 0.1875-1.875h -1 Research within the scope, the best result is the conversion rate of diethyl oxalate is 95%, and the yield of ethylene glycol is about 80%.
[0009] The above-mentioned patents or the technology reported in the literature have an obvious defect that the surface of the catalyst is non-alkaline, the dispersion of the active metal is poor, the catalyst preparation cost is high and the steps are cumbersome, the repeatability of batch preparation is not ideal, and it is not suitable for industrial production.

Method used

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  • Ethylene glycol catalyst prepared by dimethyl oxalate plus hydrogen and preparation method and application thereof
  • Ethylene glycol catalyst prepared by dimethyl oxalate plus hydrogen and preparation method and application thereof
  • Ethylene glycol catalyst prepared by dimethyl oxalate plus hydrogen and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Synthesis of Cu-Al hydrotalcite (Cu 20w%):

[0052] Al(NO 3 ) 3 9H 2 O 7.5026g (0.02mol) and Cu(NO 3 ) 2 ·3H 2 O 1.9256g (0.00797mol) was dissolved in 100mL of distilled water to prepare 100ml of salt solution.

[0053] NaOH 0.8g (0.02mol) and NaCO 3 4. Put 2396g (0.04mol) in a 100ml beaker, add deionized water to make up to 100ml, and prepare 100ml lye.

[0054] Another NaOH 0.8g (0.02mol), NaOH 2 CO 3 4.24g (0.04mol)

[0055] Put the two solutions into two separating funnels respectively, add them dropwise into a beaker containing 300ml of distilled water under the vigorous stirring of a magnetic constant temperature heating stirrer, control the dropping rate at about 1 drop / s, and ensure the pH of the reaction system The value is 8.5. After the dropwise addition, stir and crystallize in a constant temperature water bath at 65±1°C for 12 hours. Filtrate, wash until neutral, dry the product at 80°C for 6 hours to obtain the Cu-Al binary hydrotalcite compo...

Embodiment 2

[0060] Synthesis of Cu-Mg-Al hydrotalcite (Cu 20w%):

[0061] 0.1molCu(Cu(NO 3 ) 2 ·3H 2 O 32.17g), 0.05molMg (Mg(NO 3 ) 2 ·6H 2 O 12.8g) and 0.1molAl (Al(NO 3 ) 3 9H 2 O 29.07g) was dissolved in 100mL of distilled water to prepare 100ml of salt solution.

[0062] NaOH 4g (0.1mol) and NaCO 3 16.96g (0.2mol) was placed in a 100ml beaker, and deionized water was added to make the volume to 100ml, and 100ml of lye was prepared.

[0063] Put the two solutions into two separating funnels respectively, add them dropwise into a beaker containing 300ml of distilled water under the vigorous stirring of a magnetic constant temperature heating stirrer, control the dropping rate at about 1 drop / s, and ensure the pH of the reaction system The value is 10. After the dropwise addition, stir and crystallize in a constant temperature water bath at 65±1°C for 12 hours. Filter, wash until neutral, dry the product at 80°C for 6 hours, then heat up to 450°C at a rate of 5°C / min and ro...

Embodiment 3

[0066] Synthesis of Cu-Co-Al hydrotalcite (Cu 15w%, Co 5w%):

[0067] Al(NO 3 ) 3 9H 2 O 7.5026g (0.02mol), Cu(NO 3 ) 2 ·3H 2 O 0.722g (0.00299mol) and Co (NO 3 ) 2 ·6H 2 O 0.314g (0.00108mol) was dissolved in some distilled water to prepare 100ml salt solution.

[0068] NaOH 0.8g (0.02mol) and NaCO 3 4.2396g (0.04mol) was dissolved in some distilled water to obtain 100mol alkali solution.

[0069] Put the two solutions into two separating funnels respectively, add them dropwise into a beaker containing 300ml of distilled water under the vigorous stirring of a magnetic constant temperature heating stirrer, control the dropping rate at about 1 drop / s, and ensure the pH of the reaction system The value is 8.5-10. After the dropwise addition, stir and crystallize in a constant temperature water bath at 40°C (tested, 80°C water bath will decompose the reaction product into brown-black powder particles, suspected to be CuO) for 12h. Filtrate, wash until neutral, and dr...

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Abstract

The invention discloses an ethylene glycol catalyst prepared by dimethyl oxalate plus hydrogen, a preparation method and application thereof. According to weight percentage, the catalyst comprises the following components: 70 to 84 percent of metal oxide, 1 to 5 percent of transitional metal additives, and 15 to 25 percent of copper. The catalyst belongs to an anion clay type hydrotalcite catalyst; and under the conditions that a reaction temperature is 160 to 230 DEG C, pressure is 1.0 to 5Mpa, a hydrogen ester molar ratio equals to 20-100:1, and a volume space velocity equals to 0.5 to 3h<-1>, the catalyst can be used in a reaction of preparing ethylene glycol by dimethyl oxalate plus hydrogen. The catalyst has the advantages of low reaction temperature, high activity, good selectivity, simple catalyst preparation process, easy operation and low cost, and is easy for conducting industrial production.

Description

technical field [0001] The invention relates to a method for preparing ethylene glycol by hydrogenation of dimethyl oxalate, in particular to a copper-hydrotalcite catalyst for the hydrogenation reaction of dimethyl oxalate and a preparation method thereof. Background technique [0002] Ethylene glycol is the simplest and most important aliphatic dihydric alcohol. It is an important basic raw material in organic chemical production, especially widely used in the production of polyester fiber and polyester plastic. It is an important component of antifreeze in the cooling system of automobile, aviation and instrument industry. It also has various uses in the production of solvents, lubricants, softeners, plasticizers and explosives. [0003] The main method of industrial synthesis of ethylene glycol is to first synthesize ethylene through the petroleum route, then oxidize ethylene to produce ethylene oxide, and finally obtain ethylene glycol by non-catalytic hydration of eth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/78B01J23/70B01J23/80C07C31/20C07C29/149
Inventor 徐菁利唐博合金谢庆华曹俭赵家昌孙彦刚陈艳青郑静李洪森
Owner SHANGHAI UNIV OF ENG SCI
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