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Copper-based catalyst for preparing methyl glycolate and preparation and application thereof

A technology of methyl glycolate and copper-based catalysts, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve problems such as limitations and unavoidable, and achieve The effect of simple composition, increased binding capacity, energy saving and time saving

Active Publication Date: 2020-03-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. Add noble metal Au, Ag, Pt, Ru and other auxiliary agents in the Cu-based catalyst to improve the selectivity of methyl glycolate (such as Chinese patents CN101954288A, CN101700496A, CN10233666A, CN102463122A, CN101700496A, etc.), but this method still cannot avoid Use expensive precious metals
[0007] 2. Add Mn, Zn, Zr, Mo, Co, Ni, La and other additives to the Cu catalyst to improve the selectivity of methyl glycolate (such as Chinese patents CN103785408A, CN 108325532A, etc.), but due to the limitation of the preparation method , only with SiO 2 as a carrier, with certain limitations

Method used

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  • Copper-based catalyst for preparing methyl glycolate and preparation and application thereof
  • Copper-based catalyst for preparing methyl glycolate and preparation and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The high-purity copper (99.9%) target was pre-bombarded with Ar ions generated by a plasma generator for 30 minutes, and then the SiO 2 Carrier (specific surface area 267m 2 / g) As for the multi-angle rotating barrel, vacuumize the barrel until the pressure reaches 9.9×10 -4 Below Pa, put high-purity Ar gas into the barrel until the pressure reaches 2.0Pa, adjust the voltage of the Ar ion generator to 450V, and increase the barrel speed to 3.5rpm, so that the nano-metal copper particles produced by the Ar ion bombardment of the copper target are evenly deposited on the On the surface of the carrier, sputter for 4 hours. After the sputtering is over, the barrel is filled with 1% O by volume 2 / Ar mixture until the pressure reaches normal pressure. After testing, Cu / SiO with a mass loading of Cu of 15% was obtained 2 Catalyst, denoted as SP-15Cu / SiO 2 .

[0021] Fill the reactor with 0.5g of prepared SP-15Cu / SiO 2 Catalyst, without pre-reduction treatment, feed the ...

Embodiment 2

[0023] In the reactor, fill the SP-15Cu / SiO prepared by 0.5g embodiment 1 2 Catalyst, without pre-reduction treatment, feed the reaction raw material, H 2 / Dimethyl oxalate (DMO) molar ratio is 80, reaction temperature is 250°C, pressure is 3.0MPa, liquid hourly space velocity is 0.5h -1 , the conversion rate of dimethyl oxalate is 38.8%, the selectivity of methyl glycolate is 86.5%, the selectivity of ethylene glycol is 12.2%, the selectivity of ethanol is 0.4%, and the selectivity of C3-C4 alcohols is 0%. The yield of methyl glycolate was 33.6%.

Embodiment 3

[0025] In the reactor, fill the SP-15Cu / SiO prepared by 0.5g embodiment 1 2 Catalyst, without pre-reduction treatment, feed the reaction raw material, H 2 / Dimethyl oxalate (DMO) molar ratio is 80, reaction temperature is 260°C, pressure is 3.0MPa, liquid hourly space velocity is 0.5h -1 , the conversion rate of dimethyl oxalate is 53.8%, the selectivity of methyl glycolate is 80.4%, the selectivity of ethylene glycol is 18.6%, the selectivity of ethanol is 0.8%, and the selectivity of C3-C4 alcohols is 0.2%. The yield of methyl glycolate was 43.3%.

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Abstract

The invention provides a copper-based catalyst for preparing methyl glycolate at high selectivity, wherein the catalyst is prepared with a high-specific surface area material as a supporter and copperas an active component through a physical sputtering method in one step. The catalyst is used for a reaction for preparing the methyl glycolate through hydrogenation by catalyzing dimethyl oxalate, wherein the mass content of copper in the catalyst is 5-30% and the balanced being the supporter. The catalyst has the following advantages: (1) the copper is subjected to bombarding of Ar ion, so thatelectron structure of copper is varied, and the copper shows a noble metal-like property, wherein the copper on the catalyst is zero-valent stable copper, which is not liable to be oxidized, so thatthe copper can replace noble metals such as Au and Ag in the ester hydrogenation reaction; (2) the active metal, copper, has high selectivity on the methyl glycolate, so that the catalyst is free of any other additives.

Description

technical field [0001] The invention relates to a catalyst for ester hydrogenation and its application field, in particular to a copper-based catalyst for hydrogenating dimethyl oxalate to prepare methyl glycolate and its application. Background technique [0002] Methyl glycolate (HOCH 2 COOCH 3 , MG), because it contains both hydroxyl and ester groups in its molecular structure, and has both the chemical properties of alcohols and esters. Methyl glycolate is a high value-added organic chemical intermediate, and is an excellent solvent for many cellulose, resins, and rubbers. It is widely used in various fields such as chemical industry, medicine, pesticide, feed, spices and dyes. The downstream product branches centered on esters, such as hydrolysis of methyl glycolate to glycolic acid, oxidation to methyl glyoxylate, carbonylation to dimethyl malonate, and ammonia solution to glycine, have broad application prospects. [0003] There are many traditional production meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/78B01J23/80B01J23/83B01J23/745C07C67/03C07C69/675
CPCB01J23/72B01J23/78B01J23/80B01J23/83B01J23/745C07C67/03C07C69/675
Inventor 孙剑俞佳枫孟繁琼椿范立徐恒泳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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