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Method for generating glycol through two-step catalytic hydrogenation reaction of oxalate

A technology for catalytic hydrogenation and oxalate ester, applied in chemical instruments and methods, production of bulk chemicals, preparation of organic compounds, etc. The effect of magnifying the problem

Inactive Publication Date: 2012-05-09
PUJING CHEM IND SHA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although great research progress has been made in the research on the hydrogenation of oxalate to ethylene glycol, there are still some problems in the stability of the hydrogenation catalyst, and because the hydrogen ester molar ratio is as high as 40 during the reaction ~200:1, far exceeding the 4:1 required by the stoichiometric ratio. Therefore, in the process of large-scale production of ethylene glycol, the requirements for the hydrogen cycle compressor are relatively high. Therefore, how to effectively improve the process conditions and prolong the The service life of the catalyst and the reduction of the compressor load have become important factors affecting the production cost in the process of industrial scale-up

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  • Method for generating glycol through two-step catalytic hydrogenation reaction of oxalate

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Embodiment 1

[0032] Such as figure 1 Shown, adopt technological process of the present invention to test.

[0033] First prepare Cu-Zn / SiO 2 The catalyst, wherein the weight content of Cu is 20%, and the weight content of Zn is 5%. Cu with (Cu+CuO+Cu 2 O) form exists in the catalyst, and Zn exists in the catalyst in the form of (Zn+ZnO). Catalyst preparation method is as follows: first weigh specific surface area 215m 2 / g of 200g of silica carrier, weigh a certain amount of copper nitrate and zinc nitrate to prepare a solution, impregnate and stir the silica carrier in the solution for 24 hours, vacuum dry at room temperature for 12 hours, and then dry at 120C 24 hours, followed by calcination at 400 °C for 6 hours to prepare the catalyst precursor. Before use, it was reduced with pure hydrogen at a volumetric space velocity of 2000 / h, raised from room temperature to 350 °C at a rate of 2 °C / min, and reduced at normal pressure for 8 hours to obtain an active catalyst.

[0034] Secon...

Embodiment 2

[0047] Adopt the Cu-Zn / SiO that embodiment 1 is used simultaneously 2 Catalysts and Cu-Co / SiO 2 catalyst.

[0048] According to attached figure 1 The process flow shown is that two glycolate synthesis reactors are filled with the same weight of Cu-Zn / SiO 2 Catalyst, the same weight of Cu-Co / SiO was loaded in two ethylene glycol synthesis reactors 2 catalyst. The feed was dimethyl oxalate and hydrogen with a purity of 99.8%. The reaction temperature in the first glycolate synthesis reactor is 180°C, the reaction pressure is 3.0MPa, the reaction weight space velocity is 1.5 / h, and the molar ratio of hydrogen to dimethyl oxalate is 40:1; the first ethylene glycol synthesis reactor The reaction temperature is 210° C., the reaction pressure is 2.8 MPa, the reaction weight space velocity is 1.5 / h, and the molar ratio of hydrogen to glycolate is 60:1. In the second glycolate synthesis reactor, the reaction temperature is 180°C, the reaction pressure is 2.6MPa, the reaction weig...

Embodiment 3

[0060] Adopt the Cu-Zn / SiO that embodiment 1 is used simultaneously 2 Catalysts and Cu-Co / SiO 2 catalyst.

[0061] According to the process flow shown in the accompanying drawing, the same weight of Cu-Zn / SiO is filled in two glycolate synthesis reactors 2 Catalyst, the same weight of Cu-Co / SiO was loaded in two ethylene glycol synthesis reactors 2 catalyst. The feed was dimethyl oxalate and hydrogen with a purity of 99.8%. The reaction temperature in the first glycolate synthesis reactor is 160°C, the reaction pressure is 3.0MPa, the reaction weight space velocity is 4.0 / h, and the molar ratio of hydrogen to dimethyl oxalate is 80:1; the first ethylene glycol synthesis reactor The reaction temperature is 230° C., the reaction pressure is 2.8 MPa, the reaction weight space velocity is 4.0 / h, and the molar ratio of hydrogen to glycolate is 120:1. In the second glycolate synthesis reactor, the reaction temperature is 160°C, the reaction pressure is 2.6MPa, the reaction weig...

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Abstract

The invention relates to a method for generating glycol through a two-step catalytic hydrogenation reaction of oxalate. The method is realized by adopting oxalate and hydrogen as raw materials, utilizing the coupling of the series connection and the parallel connection of a plurality of reactors and arranging a circulating hydrogen compressor. The hydrogenation reaction depth can be well controlled through the series connection, so the service life of a catalyst is prolonged; and the hydrogen: ester ratio of a whole technological system can be greatly reduced on condition that hydrogen: ester ratios of all reactors are not reduced through the parallel connection. Compared with the prior art, the method of the invention well solves the catalyst service life problem when glycol is produced through the hydrogenation of oxalate in non-petrochemical engineering routes and engineering amplification problems of the overlarge compressor load during the large scale production of glycol, so the method can be widely applied to the industrial production of glycol.

Description

technical field [0001] The invention relates to a two-step catalytic hydrogenation reaction method of oxalate, in particular to a new process technology for producing ethylene glycol by hydrogenation of oxalate in a non-petrochemical route. Background technique [0002] Coal-based synthesis gas to ethylene glycol technology is an important coal chemical industry route, that is, oxalate is prepared from CO through carbonylation coupling reaction, and then ethylene glycol is produced through catalytic hydrogenation. Aiming at this process route, some domestic research institutes such as Fujian Institute of Physical Structure, Chinese Academy of Sciences, Tianjin University, East China University of Science and Technology, etc. have made in-depth research. The chemical reaction equation for the hydrogenation of dimethyl oxalate to produce ethylene glycol is CH 3 OCOCOOCH 3 +2H 2 =CH 3 OCOCH 2 OH+CH 3 OH, CH 3 OCOCH 2 OH+2H 2 =CH 2 OHCH 2 OH+CH 3 Oh. The commonly us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/149B01J23/75
CPCY02P20/52
Inventor 骆念军计扬
Owner PUJING CHEM IND SHA
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