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Method for preparing catalyst used in method for preparing ethanediol by dimethyl oxalate hydrogenation

A dimethyl oxalate and catalyst technology, applied in the chemical industry, can solve the problems of production cost dependence, cost increase, unsuitability, etc., and achieve the effects of easy control, long life and stable reaction performance

Inactive Publication Date: 2009-04-22
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material ethylene oxide used in this route is obtained from the oxidation of ethylene, and ethylene is obtained from petroleum cracking, so the production cost of the ethylene oxide hydrolysis route is heavily dependent on the price of petroleum and its downstream products, making the current cost of this route also greatly improved
Especially in our country, there is a lot of coal and little oil, and the import of oil is increasing year by year, so the hydrolysis route of ethylene oxide is not suitable for the national conditions of our country.

Method used

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  • Method for preparing catalyst used in method for preparing ethanediol by dimethyl oxalate hydrogenation
  • Method for preparing catalyst used in method for preparing ethanediol by dimethyl oxalate hydrogenation
  • Method for preparing catalyst used in method for preparing ethanediol by dimethyl oxalate hydrogenation

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Effect test

Embodiment 1

[0028] The present invention is further described by the following examples, but the present invention is not limited thereto. Embodiment 1: Mesoporous silica molecular sieve SBA-15 supported catalyst:

[0029] The catalyst preparation method used in the hydrogenation of dimethyl oxalate to prepare ethylene glycol method may further comprise the steps:

[0030] The first step: at room temperature, 7.56g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 200ml of distilled water, 25wt% concentrated ammonia water was added dropwise to pH = 9.0±0.2, and stirred for 50 minutes to form a copper ammonia complex;

[0031] Step 2: Add 10g of mesoporous silica molecular sieve SBA-15 to the copper ammonium complex, stir at room temperature for 50min, then continue to stir in an ice-water bath, and at the same time add 5000ml of distilled water dropwise at a speed of 10ml / min, dropwise Continue to stir for 60 minutes after completion; filter, wash with distilled water and ethanol three times respe...

Embodiment 2

[0033] Embodiment 2: The catalyst preparation method used in the method for preparing ethylene glycol by hydrogenation of dimethyl oxalate supported by mesoporous silica molecular sieve MCM-41 comprises the following steps:

[0034] The first step: with embodiment 1;

[0035] Step 2: Add 10g of mesoporous silica molecular sieve MCM-41 to the copper ammonium complex, stir at room temperature for 50min, then continue to stir in an ice-water bath, and at the same time add 5000ml of distilled water dropwise at a speed of 10ml / min, dropwise Continue to stir for 60 minutes after completion; filter, wash with distilled water and ethanol three times respectively, then dry at 100°C for 10h, and then roast at 450°C for 4h to make a catalyst precursor;

[0036] The third step: the same as in Example 1, the catalyst Cu / MCM-41 was obtained, and the copper content in the catalyst was determined by ICP to be 16.8 wt%.

Embodiment 3

[0037] Example 3: Catalyst supported by mesoporous silica molecular sieve MCF

[0038] The catalyst preparation method used in the hydrogenation of dimethyl oxalate to prepare ethylene glycol method may further comprise the steps:

[0039] The first step: with embodiment 1;

[0040] Step 2: Add 10g of mesoporous silica molecular sieve MCF to the copper ammonium complex, stir at room temperature for 50min, then continue to stir in the ice-water bath, and at the same time add 5000ml of distilled water dropwise at a speed of 10ml / min, after the dropwise addition Continue to stir for 60 minutes; filter, wash with distilled water and ethanol three times respectively, then dry at 100°C for 10h, and then roast at 450°C for 4h to make a catalyst precursor;

[0041] The third step: the same as in Example 1, the catalyst Cu / MCF was obtained, and the copper content in the catalyst was determined by ICP to be 16.2 wt%.

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Abstract

The invention relates to the field of chemical technology, in particular to a method for preparing a catalyst for hydrogenating dimethyl oxalate to prepare glycol. The method comprises the following steps: step one, copper nitrate is used to prepare a cuprammonium complex compound; step two, the cuprammonium complex compound is added with a mesoporous silica molecular sieve, is dripped with distilled water, and is filtered, washed, dried and roasted to prepare a catalyst precursor; and step three, the catalyst precursor is reduced in a hydrogen-nitrogen mixed atmosphere to prepare the catalyst. In the catalyst, according to mass percentage, the content of copper is between 5 and 40 percent; and the content of the mesoporous silica molecular sieve is between 60 and 95 percent. The method has the advantages that a silicon copper catalyst prepared through the new method has high catalytic activity and glycol selectivity in the reaction of hydrogenating the dimethyl oxalate to prepare the glycol, has long service life, smooth reaction performance and easy control.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing a catalyst, in particular to a method for preparing a catalyst used in the method for hydrogenating dimethyl oxalate to prepare ethylene glycol and a product obtained by the method. Background technique [0002] Ethylene glycol is an important basic organic raw material in petrochemical industry. It can be mixed with water in any proportion. It has a high boiling point and a low freezing point. It reacts with terephthalic acid to form polyethylene terephthalate, which can be used as polyester Fiber and polyester plastic raw materials are also widely used in the production of lubricants, plasticizers, paints, adhesives, surfactants, explosives and other industrial fields, and can also be used to prepare antifreeze or directly as organic solvents. In addition, it can also be used in industries such as paint, photographic developer, brake fluid and ink....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J29/072C07C31/20C07C29/149
Inventor 陈梁锋乔明华沈伟徐华龙范康年
Owner FUDAN UNIV
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