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Method for preparing glycol by using oxalic ester

A technology for ethylene glycol and oxalate, which is applied in the field of ethylene glycol production by hydrogenation of dimethyl oxalate or hydrogenation of diethyl oxalate, and can solve the problems of low selectivity of target products and low utilization rate of hydrogen.

Inactive Publication Date: 2011-03-30
SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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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 the low selectivity of the target product existing in the prior art, the technical problem that the hydrogen utilization rate is low, and a kind of new method for producing ethylene glycol from oxalic acid ester is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 200 grams of a silicon oxide carrier with a specific surface area of ​​300 square meters per gram, and configure the catalyst according to the content of 35 parts of active metal copper. After soaking in the solution for 24 hours, vacuum-dry at room temperature for 12 hours to obtain a solid. The solid was then dried at 120°C for 12 hours and calcined at 450°C for 4 hours to obtain the desired CuO / SiO 2 catalyst precursor.

[0022] Weigh the CuO / SiO to be prepared 230 grams of catalyst precursors are loaded into a tube reactor with a diameter of 18 mm. The pre-reaction catalyst is at 200 ml / min, hydrogen molar content is 20%, and nitrogen molar content is 80% from room temperature to 3°C / min. 450° C. and constant temperature for 6 hours to activate to obtain the desired catalyst.

[0023] Using dimethyl oxalate as raw material, fresh hydrogen, recycle gas I, recycle gas II are mixed with dimethyl oxalate raw materials, and then first enter the reactor to contac...

Embodiment 2

[0025] 48%Cu+8%Zn+0.2%K / SiO obtained according to the various steps and conditions of Example 1 2 catalyst.

[0026] Taking by weighing 30 grams of the prepared catalyst and packing it into a tube reactor with a diameter of 18 millimeters, the pre-reaction catalyst is at 200 ml / min, hydrogen molar content 20%, nitrogen molar content 80% conditions, from room temperature to 3 ℃ / Minutes to 450 ° C, constant temperature for 6 hours to activate the reaction.

[0027] Using dimethyl oxalate as raw material, fresh hydrogen, recycle gas I, recycle gas II are mixed with dimethyl oxalate raw materials, and then first enter the reactor to contact with copper-containing catalyst to generate reaction effluent I containing ethylene glycol; After the reaction effluent I of glycol is separated by gas and liquid, the liquid phase effluent enters the separation system and is separated to obtain ethylene glycol products. The gas phase effluent is divided into gas phase effluent I and gas pha...

Embodiment 3

[0029] 25%Cu+5%Zn+1%Fe / SiO obtained according to the various steps and conditions of Example 1 2 catalyst.

[0030] Take by weighing 30 grams of the prepared catalyst and pack it into a tube reactor with a diameter of 18 millimeters. The pre-reaction catalyst is at 200 ml / min, hydrogen molar content 20%, nitrogen molar content 80% conditions, from room temperature to 3 ℃ Rise to 450°C per minute, keep the temperature for 6 hours for activation and then react.

[0031] Diethyl oxalate is used as raw material, fresh hydrogen, cycle gas I, cycle gas II are mixed with diethyl oxalate raw material, and firstly enter the reactor to contact with copper-containing catalyst to generate reaction effluent I containing ethylene glycol; After the reaction effluent I of glycol is separated by gas and liquid, the liquid phase effluent enters the separation system and is separated to obtain ethylene glycol products. The gas phase effluent is divided into gas phase effluent I and gas phase ef...

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Abstract

The invention relates to a method for preparing glycol by using oxalic ester, which mainly solves the technical problems of low target product selectivity and low hydrogen utilization in the prior art. The method uses the oxalic ester as a raw material, and comprises the following steps: a) raw materials of fresh hydrogen, circulating gas I, circulating gas II and dimethyl oxalate first is fed in a reactor to be contacted with copper-containing catalyst to generate glycol-containing reactor effluent I; b) the reactor effluent I is subject to gas-liquid separation, the liquid-phase effluent is separated to obtain a glycol product, and the gas-phase effluent is separated into a gaseous phase effluent I which is used as circulating gas I and a gaseous phase effluent II; and c) the gaseous phase effluent II is fed to a hydrogen recycle system to obtain circulating gas II and analytic gas, and the circulating gas II is mixed with the fresh hydrogen for continuous recycling, wherein the molar ratio of the gaseous phase effluent I to the fresh hydrogen is 0.5-100:1, and the molar ratio of the gaseous phase effluent II to the gaseous phase effluent I is 0.01-5:1. In the invention, the technical problem is well solved, and the method can be used in the industrial production of increasing production of the 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): C07C31/20C07C29/149B01J23/72B01J23/80B01J23/889B01J23/78B01J23/888B01J23/847
CPCY02P20/52
Inventor 李斯琴刘俊涛朱志焱张琳娜
Owner SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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