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Glycol catalyst synthesized by hydrogenating oxalic ester and preparation method and application thereof

A technology of oxalate ester and ethylene glycol, which is applied in the field of oxalate ester hydrogenation synthesis ethylene glycol catalyst and its preparation, which can solve the problem of unsatisfactory conversion rate and selectivity, high catalyst reaction temperature, high heat and power consumption and other problems, to achieve the effect of stable reaction, low reaction temperature and reduced investment cost

Inactive Publication Date: 2009-09-09
DANYANG DANHUA COAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the 1980s, countries around the world have applied for a series of patents on oxalate ester hydrogenation to ethylene glycol catalysts. The disadvantages are that the catalyst has high reaction temperature, high pressure, high heat and power consumption, and the conversion rate and selectivity of the reaction are not very good. Ideal, not suitable for industrial production, and the catalyst is not easy to separate from the product, the space-time yield is not high, and the service life of the catalyst is short

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Pour 97g of urea into a three-necked flask, add 2000g of distilled water, stir to make it completely dissolved, and 121.5g of Cu(NO 3 ) 2 .3H 2 O, 146.2g Zn(NO 3 ) 2 .6H 2 O and 147g Al(NO 3 ) 3 .9H 2 O was placed in a beaker, and 1500g of distilled water was added to dissolve it completely. Add the prepared mixed metal salt solution into the urea solution, stir and raise the temperature to 95°C, control the pH value at the end point of the reflux reaction to 7.2, and then bubble for 2 hours after the reaction is completed, the catalyst is washed and filtered and dried at 90°C for 10 pieces Hours, it was ground into fine powder, calcined at 350°C for 2 hours, and then pressed into tablets to form 3×5mm particles. The catalyst specific surface area of ​​above-mentioned preparation is 80m 2 / g, the pore volume is 0.3cm 3 / g, the average pore radius is 3nm.

[0028] Catalyst application: put the catalyst prepared above in a fixed-bed reactor, gradually raise the...

Embodiment 2

[0030] Pour 130g of urea into a three-necked flask, add 2000g of distilled water, stir to make it completely dissolved, and 190.2g of Cu(NO 3 ) 2 .3H 2 O, 94.7g Cr(NO 3 ) 2 .9H 2 O, 9.2g Mn(NO 3 ) 3 .9H 2 O and 220.6gAl(NO 3 ) 3 .9H 2 O was placed in a beaker, and 2000g of distilled water was added to dissolve it completely. Add the prepared mixed metal salt solution into the urea solution, stir and raise the temperature to 93°C, control the pH value at the end point of the reflux reaction to 7.6, and bubble for another 2 hours after the reaction is completed, and dry the catalyst at 95°C for 14 hours after washing and filtering , grind it into fine powder, bake it at 500°C for 2 hours, and then press it to form 3×5mm particles. The catalyst specific surface area of ​​above-mentioned preparation is 450m 2 / g, the pore volume is 1.1cm 3 / g, the average pore radius is 10nm. Catalyst application: put the catalyst prepared above in a fixed-bed reactor, gradually raise...

Embodiment 3

[0032] Pour 86g of urea into a three-necked flask, add 2000g of distilled water, stir to dissolve it completely, and mix 220g of Cu(NO 3 ) 2 .3H 2 O, 36.6g Zn(NO 3 ) 2 .6H 2 O, 31.8g Mg(NO 3 ) 2 .6H 2 O and 36.8g Al(NO 3 ) 3 .9H 2 O was placed in a beaker, and 1500g of distilled water was added to dissolve it completely. Add the prepared mixed metal salt solution into the urea solution, stir and raise the temperature to 90°C, control the end point pH value of the reflux reaction to be 8.0, and then bubble for 2 hours after the reaction is completed. After the catalyst is washed and filtered, it is dried at 100°C for 16 Hours, it was ground into fine powder, calcined at 600°C for 3 hours, and then compressed to form 3×5mm particles. The catalyst specific surface area of ​​above-mentioned preparation is 150m 2 / g, the pore volume is 0.6cm 3 / g, the average pore radius is 15nm.

[0033] Catalyst application: put the catalyst prepared above in a fixed-bed reactor, gr...

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Abstract

The invention discloses a glycol catalyst synthesized by hydrogenating oxalic ester and a preparation method and an application thereof. The catalyst has the chemical formula of CuO-AOx / Al2O3, wherein A is one or more than one metallic element of Zn, Mn, Mg and Cr, x is half of the valence number of A, the content of CuO accounts for 40 percent to 80 percent of the catalyst mass, the content of AOx accounts for 5 percent to 40 percent of the catalyst mass and the content of Al2O3 accounts for 5 percent to 30 percent of the catalyst mass. The catalyst has high activity and selectivity at low temperature and under low pressure, the energy and power consumption in production can be reduced greatly and the catalyst has good stability and long service life. The preparation method of the catalyst is simple and raw materials as industrial products are easily obtained and have low price.

Description

technical field [0001] The invention belongs to the field of catalyst chemistry, in particular to a catalyst for oxalate hydrogenation to synthesize ethylene glycol, a preparation method and application thereof. Background technique [0002] Ethylene glycol is an important organic chemical raw material, mainly used in the production of polyester fiber, antifreeze, unsaturated polyester resin, lubricant, plasticizer, non-ionic surfactant and explosives, etc. In industries such as developer, brake fluid and ink, it is used as a solvent and medium for ammonium perborate, and is used for the production of special solvents such as glycol ether, etc., and has a wide range of uses. [0003] The industrial production of ethylene glycol in my country began in the 1960s. At the beginning, the traditional chlorohydrin hydrolysis method was adopted, that is, the reaction of chlorohydrin and alkali to generate ethylene oxide, and then hydrolysis of ethylene oxide to produce ethylene glyc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/889C07C29/149C07C31/20
Inventor 吴晓金刘志刚胡晓鸣许叶飞
Owner DANYANG DANHUA COAL CHEM
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