Copper-based catalyst for dimethyl oxalate hydrogenation as well as preparation method and application of copper-based catalyst

A copper-based catalyst, dimethyl oxalate technology, applied in the preparation of hydroxyl compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of low ethylene glycol selectivity and catalyst reaction temperature. and high pressure, catalyst deactivation and other problems

Active Publication Date: 2019-03-08
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature and pressure of the above-mentioned catalysts are high, and the selectivity of ethylene glycol is low, which leads to high heat and power consumption and increased by-products. In addition, the copper-based catalysts are prone to grain agglomeration and deactivation, which makes the life of the catalyst difficult to meet the requirements of industrialization.

Method used

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  • Copper-based catalyst for dimethyl oxalate hydrogenation as well as preparation method and application of copper-based catalyst
  • Copper-based catalyst for dimethyl oxalate hydrogenation as well as preparation method and application of copper-based catalyst
  • Copper-based catalyst for dimethyl oxalate hydrogenation as well as preparation method and application of copper-based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A copper-based catalyst for the hydrogenation of dimethyl oxalate is prepared by the following method:

[0036] (1) Preparation of mesoporous silica nanospheres with central radial channels:

[0037] ① Fully dissolve 20.0g ethyl silicate (TEOS) in 187.20g cyclohexane and 9.84g pentanol solution;

[0038] ②Stir 8.0g of cetylpyridinium bromide (CTPB) and 4.8g of urea in 240ml of water evenly, then add to the solution of ①, stir the mixed solution for 30 minutes at room temperature, and then place it in a Teflon sealed reaction In the container, heat the reaction at 120°C for 4 hours;

[0039] ③After the reaction is completed, take out the reaction mixture in ② to quench, then centrifuge, wash with distilled water until the pH value is close to neutral, dry at 105°C for 12 hours, and then increase the temperature at a rate of 2°C / min from room temperature to 550°C for roasting After 6 hours, mesoporous silica nanospheres (DMSNs) with central radial channels were obtained...

Embodiment 2

[0043] A copper-based catalyst for the hydrogenation of dimethyl oxalate is prepared by the following method:

[0044] (1) Preparation of mesoporous silica nanospheres with central radial channels:

[0045] ①Dissolve 20g of methyl silicate (TMOS) in 430.50g of decalin and 11.05g of isopropanol.

[0046] ②Stir 14.37g of cetyltrimethylammonium bromide (CTAB) and 14.32g of trishydroxymethylaminomethane in 236.50ml of water and then add to the solution of ①. Stir the mixed solution for 30 minutes at room temperature, then Place it in a Teflon sealed reactor and heat it at 115°C for 6 hours;

[0047] ③After the reaction is completed, take out the reaction mixture in 2), quench it, and perform centrifugation, wash with distilled water until the pH value is close to neutral, dry at 105°C for 12 hours, and then increase the temperature at a rate of 1°C / min from room temperature to 550°C Calcined for 4 hours to obtain mesoporous silica nanospheres (DMSNs) with central radial channels...

Embodiment 3

[0051] A copper-based catalyst for the hydrogenation of dimethyl oxalate is prepared by the following method:

[0052] (1) Preparation of mesoporous silica nanospheres with central radial channels:

[0053] ①Dissolve 20g of propyl silicate in 301.72g of 1-octadecene and 6.96g of hexanol solution;

[0054] ②Stir 4.84g of cetyltrimethylammonium chloride (CTAC) and 8.85g of lysine in 204ml of water, then add to the solution of ①, stir the mixed solution for 30 minutes at room temperature, and then place it in In a Teflon sealed reactor, heat the reaction at 120°C for 6 hours;

[0055] ③ After the reaction is completed, take out the reaction mixture in ② to quench, and perform centrifugation, wash with distilled water until the pH value is close to neutral, dry at 105°C for 12 hours, and then increase the temperature at a rate of 5°C / min from room temperature to 550°C for roasting After 4 hours, mesoporous silica nanospheres (DMSNs) with central radial channels were obtained.

...

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Abstract

The invention discloses a copper-based catalyst for dimethyl oxalate hydrogenation as well as a preparation method and an application of the copper-based catalyst. Soluble copper salt is supported tomesoporous silica nanospheres with central radial pore channels with a deposition-precipitation method; copper in the prepared catalyst accounts for 10%-45% of total weight of the catalyst, and monovalent copper accounts for 10-60mol% of total active copper; the catalyst has the specific surface area larger than 500 m<2>/g, the pore volume higher than 1.0 ml/g and the average mesoporous size being2.8-10 nm. With the adoption of the preparation method of the catalyst, size and dispersity of copper in the final catalyst can be regulated, the synergistic effect of monovalent copper and zero-valent copper is improved, and the high-dispersity supported nano-copper metal catalyst is obtained; when the catalyst is used for dimethyl oxalate hydrogenation for synthesizing ethylene glycol, conversion rate of dimethyl oxalate is higher than 99%, selectivity of ethylene glycol is higher than 96%, the preparation process of the catalyst is simple, the cost is low, and industrial application can berealized.

Description

technical field [0001] The present invention relates to a hydrogenation catalyst and its preparation method and application, in particular to a Cu / SiO catalyst for hydrogenation of dimethyl oxalate 2 Catalyst and its preparation method and application. Background technique [0002] The hydrogenation reaction of dimethyl oxalate (DMO) is the most critical step in the process of CO coupling synthesis of ethylene glycol. At the same time, in addition to the production of ethylene glycol, the hydrogenation reaction of dimethyl oxalate can also be used to produce methyl glycolate (MG) and ethanol, which are important components of the coal chemical industry chain. In 1985, UCC Corporation of the United States applied for two patents on the hydrogenation of dimethyl oxalate. The US4677234 technology mainly uses copper carbonate and ammonium carbonate as raw materials to prepare Cu-Si catalysts; US4628128 introduces a Cu-Si catalyst prepared by impregnation. catalyst. US4112245 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C29/149C07C31/20
CPCB01J23/72C07C29/149C07C31/202Y02P20/52
Inventor 王志光王建青王炳春李进
Owner CHINA CATALYST HLDG CO LTD
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