Effective catalyst used in hydrogenation of dimethyl oxalate to synthesizing ethylene glycol and production method thereof

A technology of dimethyl oxalate and ethylene glycol, applied in the field of chemical industry, can solve problems such as unindustrialized reports, and achieve the effects of excellent hydrogenation activity and ethylene glycol selectivity, high pore structure, and improved selectivity and stability

Inactive Publication Date: 2009-06-17
SHANGHAI HUAYI ENERGY CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the process of preparing oxalate by CO gas-phase oxidation coupling is mature at home and abroad, but there are still problems in the preparation of ethylene glycol catalyst by catalytic hydrogenation of oxalate, and no industrial reports have been made.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Carrier HMS is synthesized

[0026] Add 5.04g of dodecylamine to a solution consisting of 100ml of water and 70ml of ethanol and stir vigorously for 30min, add 90ml of ethanol solution containing 30ml tetraethyl orthosilicate, stir vigorously at 30°C for 4h, let it stand for 24h, and wash it in Dry at 100°C for 12h, then calcined at 650°C for 4h, and finally obtain carrier HMS with regular hexagonal mesoporous structure.

Embodiment 2

[0027] Embodiment 2: Cu:Mn / HMS-1# catalyst

[0028] The first step: 15.25g Cu(NO 3 ) 2 ·3H 2 O and 10.04g Mn(NO 3 ) 2 4H 2 O dissolved in 100ml H 2 Form a metal ion solution in O;

[0029] The second step: in a water bath at 50°C, under stirring, slowly and uniformly drop into an aqueous solution containing 8g of HMS for adsorption;

[0030] The third step: after the dropwise addition, continue to stir at a constant temperature for 4 hours to obtain the precursor;

[0031] Step 4: The precursor is filtered and washed, and dried at 120°C for 12 hours;

[0032] Step 5: Gradually raise the temperature to 650° C. in the muffle furnace at 10° C. / minute, and bake at this temperature for 2 hours at a constant temperature.

[0033] Granulate the catalyst powder into 40-60 mesh, 2 / N 2 The activity evaluation was carried out after the mixed gas was reduced, and it was used to selectively prepare ethylene glycol by the hydrogenation reaction of dimethyl oxalate. The results o...

Embodiment 3

[0034] Embodiment 3: Cu:Mn / HMS-2# catalyst

[0035] The first step: 19.36g Cu(NO 3 ) 2 ·3H 2 O and 4.72g Mn(NO 3 ) 2 4H 2 O dissolved in 100ml H 2 Form a metal ion solution in O;

[0036] The second step: 50 ℃ water bath, under stirring, slowly and uniformly drop into the aqueous solution containing 10g HMS for adsorption;

[0037] The third step: after the dropwise addition, continue to stir at a constant temperature for 4 hours to obtain the precursor;

[0038] Step 4: The precursor is filtered and washed, and dried at 120°C for 12 hours;

[0039] Step 5: Gradually raise the temperature to 650° C. in a muffle furnace at 10° C. / minute, and bake at this temperature for 4 hours at a constant temperature.

[0040] Granulate the catalyst powder into 40-60 mesh, 2 / N 2 The activity evaluation was carried out after the mixed gas was reduced, and it was used to selectively prepare ethylene glycol by the hydrogenation reaction of dimethyl oxalate. The results of the select...

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Abstract

The invention provides an efficient catalyst used in glycol synthesis through dimethyl oxalate hydrogenation, and a preparation method thereof. A hexagonal mesoporous silicon molecular sieve is taken as a carrier which carries copper and additive metal, and the mass ratio of the copper to the additive metal to the hexagonal mesoporous silicon molecular sieve is 0.25-0.6:0.04-0.4:1. The preparation method comprises the following steps: soluble nitrates of the copper and the additive metal are compounded to be a metal ion solution with the total concentration between 0.5 and 2 M in water; the metal ion solution is slowly dripped into an aqueous solution containing the hexagonal mesoporous silicon molecular sieve; the adsorption temperature is between 20 and 90 DEG C; the solutions continue to be stirred at a constant temperature, so as to prepare a precursor; and the precursor is washed, dried, progressively heated to 250 to 950 DEG C and roasted, so as to obtain the powdered efficient catalyst. The catalyst has the advantages that the catalyst has a regular pore structure and high specific surface area, and can be better dispersed after an active copper species is stabilized by the additive metal and dispersed by the hexagonal mesoporous silicon molecular sieve, and the catalyst shows excellent hydrogenation activity and glycol selectivity in the reaction of synthesizing glycol through the catalytic hydrogenation of dimethyl oxalate.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a high-efficiency catalyst used in the hydrogenation of dimethyl oxalate to synthesize ethylene glycol and a preparation method thereof. Background technique [0002] Ethylene glycol, commonly known as glycol, is an important organic chemical raw material. It is not only an important raw material for the production of polyethylene terephthalate (PET, polyester resin), alkyd resin, polyester fiber and polyester plastic, but also a commonly used high boiling point solvent. Its 60% aqueous solution Its freezing point is -40°C, and it can be used as an antifreeze for car radiators in winter and as a refrigerant for aircraft engines. In addition, the dinitrate of ethylene glycol can also be used as explosives, and the steam generated after heating can be used as a stage smoke screen, and it is also an indispensable ingredient in the production of plasticizers, p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C07C31/20C07C29/149
Inventor 周亚明吴良泉李永刚戴维林尹安远范康年
Owner SHANGHAI HUAYI ENERGY CHEM
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