Method for preparing glycol from oxalate

A technology of oxalate and ethylene glycol, which is applied in chemical instruments and methods, chemical/physical processes, and the preparation of organic compounds. question

Active Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is that there is a large temperature difference in the reactor in the prior art, which easily causes the problems of catalyst overheating, deactivation and low selectivity of the targ

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  • Method for preparing glycol from oxalate
  • Method for preparing glycol from oxalate

Examples

Experimental program
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Effect test

Embodiment 1

[0018] according to figure 1 , Hydrogenation of dimethyl oxalate to produce ethylene glycol. The inner diameter of the tubular fixed-bed reactor is 2 meters. The copper-containing catalyst is Cu-Zn / SiO 2 The catalyst is based on the weight of elemental copper, and the amount of oxides selected from copper is 35% by weight, and based on the weight of elemental zinc, the amount of oxides selected from zinc is 5% by weight. The cooling medium is dimethyl oxalate. The molar ratio of hydrogen to dimethyl oxalate is 120: 1, and the dimethyl oxalate weight percentage content is 25% dimethyl oxalate and methanol mixture and hydrogen enters in the reactor through raw material inlet, is 220 ℃ at reaction temperature, with The weight of the mixture of dimethyl oxalate and methanol is based on the weight space velocity of 1.2h -1 , the molar ratio of hydrogen / ester is 120:1, and the reaction pressure is 3.2MPa, the contact reaction with the copper-containing catalyst outside the tube, ...

Embodiment 2

[0020] according to figure 1 , The hydrogenation of dimethyl oxalate to produce ethylene glycol has a tubular fixed-bed reactor with an inner diameter of 2.5 meters. The copper-containing catalyst is Cu-Cr / SiO 2 The catalyst is based on the weight of copper, and the amount of oxides selected from copper is 25% by weight, and based on the weight of elemental chromium, the amount of oxides selected from chromium is 10% by weight. The cooling medium is boiler water. The molar ratio of hydrogen to dimethyl oxalate is 110: 1, and the dimethyl oxalate weight percent content is 50% dimethyl oxalate and methanol mixture and hydrogen enters in the reactor through raw material inlet, is 230 ℃ at reaction temperature, with The weight space velocity based on the weight of the mixture of dimethyl oxalate and methanol is 0.7hr -1 , the molar ratio of hydrogen / ester is 110:1, and the reaction pressure is 3.8MPa, the contact reaction with the copper-containing catalyst outside the tube, th...

Embodiment 3

[0022] according to figure 1 , Hydrogenation of diethyl oxalate to produce ethylene glycol. The inner diameter of the tubular fixed-bed reactor is 2.5 meters. The copper-containing catalyst is Cu-Mg / SiO 2 The catalyst is selected from metal copper and copper oxides in an amount of 40% by weight based on the weight of elemental copper, and the amount selected from magnesium oxides is 0.1% by weight based on the weight of elemental magnesium. The cooling medium is hydrogen. The molar ratio of hydrogen to diethyl oxalate is 60: 1, and the diethyl oxalate and ethanol mixture and hydrogen enter the reactor through the raw material inlet with the weight percentage of diethyl oxalate being 60%, and the reaction temperature is 260 ° C. The weight of the mixture of diethyl oxalate and ethanol is based on the weight space velocity of 0.8hr -1 , with a hydrogen / ester molar ratio of 60:1 and a reaction pressure of 6.0 MPa, it contacts and reacts with the copper-containing catalyst outs...

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Abstract

The invention relates to a method for preparing glycol from oxalate, which mainly solves the problems of easy catalyst deactivation and low selectivity of glycol serving as a target product caused by large temperature difference in a reactor in the prior art. The technical scheme of the invention is that: oxalate and hydrogen are used as raw materials, a molar ratio of the hydrogen to the oxalateis 40-200:1, fatty alcohol having 1 to 4 carbon atoms is used as a solvent, the weight ratio of the solvent to the oxalate in the raw materials is 0-0.9:1, and at least one of the oxalate, hydrogen, solvent and water is used as a cooling medium; and the cooling medium passes through a tube nest in a shell and tube fixed bed reactor at the temperature of 160 and 280 DEG C, under the pressure of between 1.0 and 6.0 MPa and under the conditions that the weight space velocity is between 0.1 and 10 hours<-1> on the basis of the weight of a mixture of the oxalate and the solvent and the molar ratioof the hydrogen to the oxalate is 40-200:1, a catalyst bed is positioned outside the tube nest, and after entering the reactor, the mixture of the raw materials and the solvent contacts a copper-containing catalyst outside the tube nest for reacting to form the glycol, wherein the flow direction of the cooling medium is the same or opposite to that of the mixture of the raw materials and the solvent, and the oxalate accounts for more than or equal to 10 weight percent of the mixture. By adopting the technical scheme, the problems are solved better. The method can be used for the industrial production of the glycol.

Description

technical field [0001] The present invention relates to a kind of method of producing ethylene glycol by oxalic acid ester, more specifically, relate to a kind of dimethyl oxalate or diethyl oxalate hydrogenation in the shell-and-tube fixed-bed reactor of internal shell-and-tube heat exchange Process for producing ethylene glycol. Background technique [0002] Ethylene glycol (EG) is an important basic organic raw material in petrochemical industry. It can be mixed with water in any proportion, and has a high boiling point and a low freezing point. Mainly used in the production of polyester fibers, antifreeze, unsaturated polyester resins, lubricants, plasticizers, non-ionic surfactants and explosives, etc., in addition to coatings, photographic developers, brake fluids and inks and other industries, It is used as a solvent and medium for ammonium perborate, used in the production of special solvents such as glycol ether, etc., and has a wide range of uses. [0003] At pre...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/149B01J8/02
Inventor 孙凤侠王万民蒯骏李蕾
Owner CHINA PETROLEUM & CHEM CORP
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