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A kind of preparation method of copper-based catalyst for selective hydrogenation of dimethyl oxalate

A technology of dimethyl oxalate and copper-based catalyst is applied in the field of catalysis to achieve the effects of directional synthesis of products, reduction of volatilization, reduction of waste water treatment volume and treatment difficulty

Active Publication Date: 2017-10-17
商丘国龙新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102989490A, CN103566949A and CN104492445A disclose the selective hydrogenation of dimethyl oxalate by changing the catalyst preparation conditions and reaction conditions by using the ammonia distillation method or combustion method, and the selective hydrogenation of dimethyl oxalate by changing the solvent type by using the sol-gel solvothermal method The method of hydrogenation has not been reported yet

Method used

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  • A kind of preparation method of copper-based catalyst for selective hydrogenation of dimethyl oxalate

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Effect test

Embodiment 1

[0024] The preparation method of the copper-based catalyst for the selective hydrogenation of dimethyl oxalate of the present embodiment, the steps are as follows:

[0025] 12.3gCu(NO 3 ) 2 ·3H 2 O and 4.22gNi (NO 3 ) 2 ·6H 2 O was dissolved in 25.0g of distilled water, fully dissolved and then added to the mixed solution formed by 42.0g of ethanol and 46.5g of ethyl orthosilicate, mechanically stirred the above mixed solution and placed in a water bath at 60°C for 1 hour to form a sol-gel. After aging the gel at room temperature for 24 hours, cut it into thin slices, add an aqueous solution of methylamine with pH = 10, place the mixture in a hydrothermal kettle, seal it and put it in an oven at 80 °C for 48 hours. After the reaction, take the reactants out of the reaction kettle and place Treat it in a water bath at 90°C for 24 hours, then move it into an oven and dry it at 140°C for 12 hours, roast and dry the solid particles in a muffle furnace at 350°C for 5 hours, pr...

Embodiment 2

[0028] The preparation method of the copper-based catalyst for the selective hydrogenation of dimethyl oxalate of the present embodiment, the steps are as follows:

[0029] 16.4gCu (NO 3 ) 2 ·3H 2 O and 0.09gCo (NO 3 ) 2 ·6H 2 O was dissolved in 50.0g of distilled water, fully dissolved and then added to a mixed solution formed by 42.0g of ethanol and 46.5g of tetraethyl orthosilicate, mechanically stirred the above mixed solution and placed in a water bath at 80°C for 0.5h to form a sol-gel. After aging the gel at room temperature for 48 hours, cut it into thin slices, add a mixed solution of methylamine and ethylenediamine with pH = 11, the solvent is a mixture of water and methanol, put the mixture in a hydrothermal kettle and put it into React in an oven at 140°C for 8 hours. After the reaction, take the reactant out of the reactor and place it in a water bath at 80°C for 36 hours, then move it into an oven and dry it at 100°C for 24 hours, and roast and dry it in a m...

Embodiment 3

[0032] The preparation method of the copper-based catalyst for the selective hydrogenation of dimethyl oxalate of the present embodiment, the steps are as follows:

[0033] 32.2gCu (NO 3 ) 2 ·3H 2 O and 1.24gH 3 BO 3 and 0.69gLa (NO 3 ) 2 ·6H 2 O was dissolved in 100.0g distilled water, fully dissolved and then added to the mixed solution formed by 75.0g ethanol and 46.5g tetraethyl orthosilicate, the above mixed solution was mechanically stirred and placed in a water bath at 40°C for 1 hour to form a sol-gel. After aging the gel at room temperature for 48 hours, cut it into thin slices, add ethylenediamine solution with pH = 13, the solvent is ethanol solution, put the mixture in a hydrothermal kettle and put it in an oven for 12 hours at 140 °C to react for 12 hours. Take the reactants out of the reactor and place them in a water bath at 90°C for 30 hours, then move them into an oven and dry them at 120°C for 24 hours, then roast and dry the solid particles in a muffle ...

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Abstract

The invention discloses a preparation method of a copper-based catalyst for the selective hydrogenation of synthetic dimethyl oxalate. The catalyst is composed of active components, additives and carriers. The catalyst uses metal copper as the active component, orthosilicate as the silicon source, and under the condition of using alcohol as a co-solvent, the additives prepared by the sol-gel method The modified copper-silicon catalyst is subjected to solvothermal post-treatment, and by changing the type of solvent, the selective hydrogenation of oxalate is realized, and the directional synthesis of methyl glycolate, ethylene glycol or ethanol is achieved. Compared with the sol-gel ammonia distillation method, at a lower reaction temperature (180°C), the conversion rate of dimethyl oxalate is 100%, the selectivity of ethylene glycol is greater than 98%, and the consumption of ammonia source is reduced. Compared with the conventional precipitation method, there is no need to wash the catalyst precursor, which saves a lot of water resources, reduces the amount and difficulty of wastewater treatment, and improves the environmental friendliness of the whole process.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a preparation method of a copper-based catalyst for selective hydrogenation of dimethyl oxalate synthesized by a sol-gel-solvothermal method. Background technique [0002] Coal-based syngas has entered the stage of industrialization through the development of dimethyl oxalate to ethylene glycol technology. This technology mainly includes CO dehydrogenation, CO oxidative coupling to dimethyl oxalate (DMO) and dimethyl oxalate hydrogenation to ethylene glycol. Alcohol (EG) three main processes. The hydrogenation of dimethyl oxalate to ethylene glycol is a key step in the coal-to-ethylene glycol technical route. By adjusting the catalyst composition and reaction conditions, dimethyl oxalate can be selectively hydrogenated to methyl glycolate (MG) and ethanol . Methyl glycolate is the simplest alkyd ester, also known as methyl glycolate or methyl glycolate, which can ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/75B01J23/83B01J23/80B01J23/72B01J37/08B01J37/03C07C31/20C07C29/149
CPCY02P20/52
Inventor 穆仕芳尚如静宋军超宋灿李丰闫捷魏灵朝蒋元力张秀全陈涛
Owner 商丘国龙新材料有限公司
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