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Method for preparing ethylene glycol from oxalic ester

A technology of ethylene glycol and oxalate, which is applied in the field of hydrogenation of dimethyl oxalate or hydrogenation of diethyl oxalate to produce ethylene glycol, which can solve the problems of short life and poor catalyst stability

Active Publication Date: 2009-07-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that the catalysts in the methods of the previous documents have poor stability and short life, and a new method for the production of ethylene glycol from oxalic acid esters is provided

Method used

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  • Method for preparing ethylene glycol from oxalic ester

Examples

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Embodiment 1

[0018] Weigh 100 grams of silicon oxide carrier whose specific surface area is 200 square meters per gram, according to 25% CuO / SiO 2 Content configuration catalyst, the steps are as follows: select copper nitrate, prepare an impregnation solution according to the Cu loading capacity, impregnate the silicon oxide carrier in the solution for 20 hours, and dry it in vacuum at room temperature for 8 hours to obtain a solid. The solid was then dried at 120°C for 10 hours and calcined at 500°C for 6 hours to obtain the desired CuO / SiO2 catalyst precursor.

[0019] Weigh the prepared CuO / SiO 2 The catalyst precursor is loaded into the tube reactor with a diameter of 18 mm according to the required amount. The pre-reaction catalyst is at 100 ml / min, the hydrogen molar content is 20%, and the nitrogen molar content is 80%. Minutes to 450 ° C, constant temperature for 4 hours for activation to obtain catalyst I and catalyst II with the same composition.

[0020] Using hydrogen and di...

Embodiment 2

[0022] According to the various steps and conditions of Example 1, 35%Cu+10%Cu was produced 2 O+5%Zn / SiO 2 Cu-Cu 2 O-Zn / SiO 2 Catalyst I and 20% Cu+5% Cu 2 O / Al 2 o 3 Cu-Cu 2 O / Al 2 o 3 Catalyst II.

[0023] Using hydrogen and dimethyl oxalate as raw materials, the dimethyl oxalate raw material is divided into the first raw material and the second raw material, the molar ratio of the first raw material and the second raw material is 1:1, hydrogen and the first raw material and The total molar ratio of the sum of the second raw materials is 60:1, and both the first raw material and the second raw material are selected from dimethyl oxalate. Hydrogen and the first stream of raw material first enter the first reactor to contact with catalyst I to generate the first reaction effluent containing ethylene glycol; the first reaction effluent and the second raw material enter the second reactor to be contacted with Catalyst II is contacted to generate a second reaction efflu...

Embodiment 3

[0025] Prepare 48%Cu+2%Cu according to the various steps and conditions of Example 1 2 O+5%Fe 2 o 3 / SiO 2 Cu-Cu 2 O-Fe 2 o 3 / SiO 2 Catalyst I and 40% Cu+20% Cu 2 O / Al 2 o 3 Cu-Cu 2 O / Al 2 o 3 Catalyst II.

[0026] Hydrogen and oxalate are used as raw materials. The oxalate is a mixture of dimethyl oxalate and diethyl oxalate with a molar ratio of 1:1. The raw material of oxalate is divided into the first raw material and the second raw material. The molar ratio of the raw material to the second raw material is 3:1, and the total molar ratio of hydrogen to the sum of the first raw material and the second raw material is 160:1, and the first raw material and the second raw material are all selected from dioxalic acid A mixture of methyl ester and diethyl oxalate with a molar ratio of 1:1. Hydrogen and the first stream of raw material first enter the first reactor to contact with catalyst I to generate the first reaction effluent containing ethylene glycol; the fi...

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Abstract

The invention relates to a method for producing glycol from oxalate, which mainly solves the problem that the prior art is low in the selectivity of target products and short in the regeneration period of catalysts. The method adopts oxalate as raw material, and comprises the following steps that: (a) hydrogen and a first stream of raw material enter a first reaction zone to be in contact with a copper-bearing catalyst I so as to form a first stream of glycol-containing reaction effluent; and (b) the first stream of reaction effluent and a second stream of raw material enter at least one second reaction zone to be in contact with a copper-bearing catalyst II so as to form a second stream of glycol-containing reaction effluent, wherein the molar ratio of the first stream of raw material to the second stream of raw material is 0.1-10:1; the molar ratio of the hydrogen to the sum of the first and second streams of raw material is 20-300:1; the first stream of raw material is selected from dimethyl oxalate, diethyl oxalate or a mixture thereof; and the second stream of raw material is selected from dimethyl oxalate, diethyl oxalate or a mixture thereof. The technical proposal well solves the problem, and the method can be used in the industrial production for increasing the yield of glycol.

Description

technical field [0001] The invention relates to a method for producing ethylene glycol from oxalate, in particular to a method for hydrogenating dimethyl oxalate or diethyl oxalate to produce ethylene glycol. Background technique [0002] Ethylene glycol (EG) is an important organic chemical raw material, mainly used in the production of polyester fiber, antifreeze, unsaturated polyester resin, lubricant, plasticizer, nonionic surfactant and explosives, etc. It can be used in industries such as paint, photographic developer, brake fluid and ink, as a solvent and medium for ammonium perborate, and for the production of special solvents such as glycol ether, etc., and has a wide range of uses. [0003] At present, large-scale ethylene glycol production at home and abroad adopts the process route of direct hydration or pressurized hydration. This process is to prepare a mixed aqueous solution of ethylene oxide and water at a ratio of 1:20 to 22 (molar ratio) in a fixed bed. Re...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/149
CPCY02P20/52Y02P20/584
Inventor 刘俊涛孙凤侠钟思青
Owner CHINA PETROLEUM & CHEM CORP
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