A kind of CO gas-phase coupling synthesis dimethyl oxalate catalyst and preparation method thereof

A technology of dimethyl oxalate and catalyst, which is applied in the field of CO gas-phase coupling synthesis of dimethyl oxalate and its preparation, and can solve the problems of not considering the utilization rate of methyl nitrite

Active Publication Date: 2018-04-10
XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD +1
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  • Abstract
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  • Application Information

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Problems solved by technology

For example, the Chinese patent CN102219680A improves the utilization rate of nitrogen oxides by using a rotating bed high-gravity reactor. Specifically, after the coupling reaction, the gas-phase effluent containing NO enters the rotating-bed high-gravity reactor with methanol and oxygen, and reacts to form methyl nitrite. effluent, but with the addition of a rotating bed hypergravity reactor, no consideration was given to improving methyl nitrite utilization from the catalyst itself

Method used

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  • A kind of CO gas-phase coupling synthesis dimethyl oxalate catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] carrier modification

[0024] Zirconium tetrachloride (ZrCl 4 ) 0.1025g, add 1mL 1:1 (volume ratio) hydrochloric acid solution and 9mL deionized water to make auxiliary agent solution, impregnate α-Al in this solution 2 o 3 20g, after natural drying, baked at 800°C for 12h to obtain 0.2% ZrO 2 / α-Al 2 o 3 .

[0025] Catalyst preparation

[0026] After adding 0.0851 g of palladium acetate into 10 mL of acetone, ultrasonic treatment was performed for 1 h, followed by light irradiation for 72 h to prepare a palladium acetate / acetone impregnation solution. Then, the solution was impregnated with Zr-modified α-Al 2 o 3 20g, acetone was distilled off after soaking for 6h. Finally, put it into a blast drying oven and dry it at 120°C for 4h, and then reduce it at 300°C for 2h under a hydrogen atmosphere to obtain 0.2% Pd / α-Al 2 o 3 -ZrO 2 catalyst.

[0027] Response Performance Evaluation

[0028] In a fixed-bed reactor with an internal diameter of 12mm and a le...

Embodiment 2

[0030] ZrCl 4 Add 1 mL of 1:1 (volume ratio) hydrochloric acid solution and 9 mL of deionized water to 0.1025 g to make an auxiliary agent solution, impregnate 20 g of alumina in the solution, dry it naturally, and roast at 1100 ° C for 8 hours to obtain 0.2% ZrO 2 / α-Al 2 o 3 .

[0031] Catalyst preparation and reaction performance evaluation are the same as in Example 1.

Embodiment 3

[0033] ZrCl 4 Add 1mL 1:1 (volume ratio) hydrochloric acid solution and 9mL deionized water to 0.1025g to make an auxiliary agent solution, impregnate 20g of alumina in the solution, dry it naturally, and roast at 1300°C for 4h to obtain 0.2% ZrO 2 / α-Al 2 o 3 .

[0034] Catalyst preparation and reaction performance evaluation are the same as in Example 1.

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Abstract

The invention relates to a catalyst for synthesizing dimethyl oxalate through CO gas phase coupling and a preparation method thereof. Alumina is first modified with additives to prepare modified α-Al2O3, and then impregnated with palladium acetate / acetone solution that has been treated with ultrasonic waves and light irradiation to prepare a catalyst with modified α-Al2O3 as the carrier and noble metal Pd as the active component. The Pd / α-Al2O3 catalyst prepared by modifying the α-Al2O3 carrier in the present invention not only has a low palladium load, but also can improve the utilization rate of methyl nitrite, efficiently synthesize dimethyl oxalate and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry catalysis, and in particular relates to a catalyst for synthesizing dimethyl oxalate through CO gas phase coupling and a preparation method thereof. Background technique [0002] As an important organic chemical raw material, oxalic acid diester can be used in the fine chemical industry to produce various dyes, medicines, important solvents, extractants and other intermediates, and is widely used in the synthesis of various chemical products. A particularly important application is the hydrogenation of oxalic acid diesters to produce ethylene glycol. Ethylene glycol is an important organic chemical raw material. It is mainly used to react with terephthalic acid to produce ethylene terephthalate (PET). [0003] Compared with the traditional production method of oxalic acid diester and the liquid phase method of carbon monoxide coupling to synthesize oxalic acid diester, the process of carbon mono...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C69/36C07C67/36
Inventor 潘振栋田志坚夏锐夏伦超曲炜王从新周佳王伟王炳春韩健强
Owner XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD
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