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Method for synthesizing glycol by hydrogenation of dimethyl oxalate

A technology of dimethyl oxalate and ethylene glycol, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of poor thermal stability, accelerated catalyst deactivation, poor stability, etc.

Active Publication Date: 2011-10-12
PUJING CHEM IND SHA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current public reports, most of these hydrogenation catalysts have high initial activity, but poor stability, and short life. According to reports, the reason for the deactivation of this type of Cu-Si catalyst is the poor thermal stability of Cu. On the other hand, if there is excessive hydrogenation of ethylene glycol in the reaction area, a small amount of water will be generated, which will cause the raw material oxalate water to form oxalic acid, thereby accelerating the deactivation of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh the specific surface area as 210m 2 / g of silicon oxide carrier 100g, according to 30%CuO+4%ZnO+66%SiO 2 The content of the catalyst is prepared as follows: select copper nitrate and zinc nitrate, prepare a solution according to the loading capacity, immerse the silicon oxide carrier in the solution and stir for 24 hours, dry it in vacuum at room temperature for 12 hours, and then dry it under infrared rays The solid was obtained in 12 hours, and then the solid was dried at 120°C for 8 hours, and then calcined at 450°C for 5 hours to obtain Cu-Zn / SiO 2 catalyst.

[0019] Weigh the specific surface area as 210m 2 / g of silica carrier 100g, according to 30%CuO+4%CoO+66%SiO 2 The content of the catalyst is prepared as follows: Weigh copper nitrate and cobalt nitrate to prepare a solution according to the load, immerse the silica carrier in the solution for 24 hours, dry it in vacuum at room temperature for 12 hours, and then dry it under infrared rays for 12 hours...

Embodiment 2

[0023] The same Cu-Zn catalyst as in Example 1 is used in the first reactor, and the Cu-Co catalyst as in Example 1 is used in the second reactor, and the catalysis and reduction methods are the same as in Example 1. The raw material is dimethyl oxalate solution with a mass fraction of 100%, the mass space velocity is 0.2 / h, the reaction temperature of the first reactor is 180C, the reaction pressure is 2.0MPa, and the ratio of hydrogen to ester is 80:1; the reaction in the second reactor The temperature is 240C, the reaction pressure is 1.8MPa, and the ratio of hydrogen to ester is 140:1. The final reaction result is: the conversion rate of dimethyl oxalate is 96.8%, the selectivity of ethylene glycol is 90.3%, and the selectivity of ethanol is 5.7%. The catalyst in the first stage reactor was evaluated for 2500 hours and no obvious deactivation was found, and the catalyst in the second stage reactor was evaluated for 3000 hours and no obvious deactivation was found.

Embodiment 3

[0025] The same Cu-Zn catalyst as in Example 1 is used in the first reactor, and the Cu-Co catalyst as in Example 1 is used in the second reactor, and the catalysis and reduction methods are the same as in Example 1. The raw material is an oxalate ester solution with a mass fraction of 5%, the reaction temperature of the first reactor is 215C, the reaction pressure is 1.5MPa, and the ratio of hydrogen to ester is 60:1; the reaction temperature in the second reactor is 180C, and the reaction pressure is 2.0MPa , the ratio of hydrogen to ester is 100:1. The final reaction result is: the conversion rate of dimethyl oxalate is 100%, and the selectivity of ethylene glycol is 92.7%. The catalyst in the first stage reactor was evaluated for 3500 hours and no obvious deactivation was found, and the catalyst in the second stage reactor was evaluated for 4000 hours and no obvious deactivation was found.

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Abstract

The invention relates to a method for synthesizing glycol by hydrogenation of dimethyl oxalate. The method comprises the following steps: I) based on dimethyl oxalate and hydrogen serving as raw materials, firstly, enabling a methanol solution of dimethyl oxalate serving as a first strand of liquid phase raw material and a first strand of hydrogen to enter into a first reactor so as to generate a first strand of reaction products in which methyl glycolate is used as a main product; and II) enabling the first strand of reaction products and a second strand of hydrogen to enter into a second reactor so as to generate a second strand of reaction products in which glycol is a main product. The stability of a catalyst can be improved by using the method.

Description

technical field [0001] The invention relates to a method for producing ethylene glycol by hydrogenation of dimethyl oxalate, in particular, the invention relates to a method for synthesizing ethylene glycol by hydrogenation of dimethyl oxalate in a two-step process. Background technique [0002] Ethylene glycol is an important organic chemical raw material. In recent years, the domestic demand for ethylene glycol has been increasing year by year, but the domestic production is far from meeting the demand. At present, the production of large-scale ethylene glycol at home and abroad mainly comes from petroleum routes. The technical scheme of direct hydration of ethylene oxide or pressurized hydration is adopted, and the mixed aqueous solution with a molar ratio of ethylene oxide: water of 1:20 is used as the The raw materials are reacted in a fixed bed at 130-180°C and 1.0-2.5 MPa to generate an aqueous solution of ethylene glycol containing about 10 wt%, and then separated to...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/149
Inventor 计扬骆念军毛彦鹏张博
Owner PUJING CHEM IND SHA
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