Method for synthesizing methyl glycollate and ethylene glycol by dimethyl oxalate hydrogenation

A technology of dimethyl oxalate and methyl glycolate, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low dispersion of active components, low-temperature activity to be improved, catalyst ratio Low surface area and other issues, to achieve the effect of low payload, high activity at low temperature, and increase conversion rate

Active Publication Date: 2012-02-01
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, although the silver-based catalyst has obtained relatively high methyl glycolate selectivity, its low-temperature activity still needs to be improved, and further promotes the improvement of its reaction performance at high space velocity
Though traditional dimethyl oxalate hydrogenation catalyst adopts silicon dioxide as carrier more, mostly use silic

Method used

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  • Method for synthesizing methyl glycollate and ethylene glycol by dimethyl oxalate hydrogenation
  • Method for synthesizing methyl glycollate and ethylene glycol by dimethyl oxalate hydrogenation
  • Method for synthesizing methyl glycollate and ethylene glycol by dimethyl oxalate hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1 Preparation of silver-containing SBA-15 mesoporous molecular sieve catalyst S1

[0025] Weigh 3.0 grams of SBA-15 molecular sieve after pretreatment at 200°C for 2 hours, impregnate it in equal volume in an aqueous solution containing 0.23 grams of silver nitrate for 12 hours, and then dry it at 80°C. The dried silver-containing SBA-15 is baked in a muffle furnace at 500°C for 5 hours, then pressed into tablets, and then reduced for reaction. The reduction temperature is 350°C, the reduction pressure is 2.5Mpa, and the hydrogen space velocity is 1000h -1 , the reduction time is 6 hours. The obtained catalyst is numbered S1.

Embodiment 2

[0026] Embodiment 2 Preparation of silver-containing SBA-15 mesoporous molecular sieve catalyst S2

[0027] Using orthoethyl silicate (TEOS) as silicon source, silver lactate (C 3 h 5 AgO 3 ) is the silver source, and the three-stage copolymer P123 is the template agent, and the silver-containing SBA-15 is synthesized under acidic (hydrochloric acid) conditions, and the static synthesis temperature in the autoclave is 100 ° C, and the corresponding raw material molar ratio is: P123: HCl: TEOS : C 3 h 5 AgO 3 :H 2 O=0.017:5.88:1:0.03:197. After 3 days of crystallization in the kettle, the synthesized silver-containing SBA-15 was washed with water, washed with alcohol, and dried. After drying, bake the silver-containing SBA-15 in a muffle furnace at 500°C for 5 hours, then press it into tablets, and reduce it for reaction. The reduction temperature is 350°C, the reduction hydrogen pressure is 2.5MPa, and the hydrogen space velocity is 1200h -1 , the reduction time is 7 ...

Embodiment 3

[0028] Example 3 Preparation of silver-containing MCM-41 mesoporous molecular sieve catalyst M1

[0029] The preparation method is the same as that of Example 1, except that the mesoporous molecular sieve used is MCM-41. The obtained mesoporous molecular sieve catalyst is coded as M1.

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Abstract

The invention discloses a method for synthesizing methyl glycollate and ethylene glycol by dimethyl oxalate hydrogenation. The method comprises the following steps of: performing hydrogenation reaction on dimethyl oxalate serving as a raw material under the action of a catalyst at the temperature of between 120 and 300 DEG C under the hydrogen pressure of 0.2 to 10.0MPa, performing fixed bed continuous reaction, and thus obtaining target products, namely the methyl glycollate and the ethylene glycol. The method is mild in reaction conditions and environmentally-friendly, the conversion rate of the dimethyl oxalate reaches over 99 percent, the total selectivity of the methyl glycollate and the ethylene glycol reaches over 98 percent, the selectivity of the methyl glycollate serving as a main product reaches 95 percent, and a new effective path is provided for preparing the methyl glycollate and the ethylene glycol by dimethyl oxalate hydrogenation.

Description

technical field [0001] The invention relates to a preparation method for synthesizing methyl glycolate and ethylene glycol by hydrogenating dimethyl oxalate. Background technique [0002] With the increasing shortage of petroleum resources, it is of great practical significance to develop C1 chemical industry mainly based on natural gas and coal-based raw materials. Related technologies have also achieved rapid development in the 1990s. Among them, the gas-phase catalytic synthesis of dimethyl oxalate (DMO) by CO and nitrite is an important breakthrough in the synthesis of chemicals by the C1 route, and thus opens up a non-petroleum route from hydrogenation of DMO to ethylene glycol (EG). In recent years, under the condition that the upstream process technology for producing DMO is mature and stable, the further development of the downstream product chain of DMO has become a research focus and focus in the field of catalysis. [0003] Both ethylene glycol and methyl glycol...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C31/20B01J35/10B01J29/03B01J29/89C07C29/149B01J29/74C07C67/31
CPCY02P20/52
Inventor 廖湘洲宁春利卢磊张春雷
Owner SHANGHAI HUAYI GRP CO
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