Catalyst for hydrogenation of oxalate to ethylene glycol and preparation method thereof

A technology of catalyst and oxalate, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, and preparation of organic compounds, etc., can solve the problems of uneven distribution of catalyst particles and low activity, and achieve difficult aggregation and sintering, high catalytic activity, The effect of catalyst performance improvement

Active Publication Date: 2017-02-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of uneven distribution of catalyst particles and low activity in the prior art, and to provide a catalyst for the hydrogenation of oxalate ester to ethylene glycol with simple preparation, high activity and good stability

Method used

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  • Catalyst for hydrogenation of oxalate to ethylene glycol and preparation method thereof
  • Catalyst for hydrogenation of oxalate to ethylene glycol and preparation method thereof
  • Catalyst for hydrogenation of oxalate to ethylene glycol and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0050] To 600ml copper nitrate solution (molar concentration is 0.39mol / L), add 150g alkaline silica sol (silicon dioxide content is 30wt%), stir evenly, directly add 25% ammonia water until the pH value of the solution is 11.5, stir After 5 hours, heat to 80°C for reflux reaction until the pH of the solution is 6.0, then filter, wash with water until neutral, and wash with ethanol, then dry the obtained filter cake at 120°C, and roast at 450°C for 5 hours to obtain the catalyst.

[0051] After the catalyst precursor is pretreated by reduction in a hydrogen-containing atmosphere, the oxalate ester solution (mass fraction 15%) was vaporized and then contacted with a copper-containing catalyst to generate an effluent containing ethylene glycol. The hydrogenation data are shown in Table 1. The reaction result is: the conversion rate of oxalate is 100%, and the selectivity of ethylene glycol is 89%.

Embodiment 2

[0053] The preparation of the catalyst was the same as in Example 1, except that the pH value of the solution was adjusted to 12.

[0054] Catalyst evaluation is the same as in Example 1, except that the reaction temperature is 195° C., and the hydrogenation data are shown in Table 1. The reaction result is: the conversion rate of oxalate is 100%, and the ethanol selectivity is 92%.

Embodiment 3

[0056] To 600ml copper nitrate and magnesium nitrate solution (molar concentration is 0.39mol / L and 0.22mol / L respectively), add 150g alkaline silica sol (silicon dioxide content is 30wt%), stir evenly, slowly add 25% Ammonia water until the pH value of the solution reaches 12, after stirring for 5 hours, heat to 80°C for reflux reaction until the pH value of the solution is 6.0, then filter, wash with water until neutral, and wash with ethanol, and then bake the obtained filter cake at 120°C Dry, and calcined at 450°C for 5h to obtain a hydrogenation catalyst.

[0057] The catalyst evaluation was the same as in Example 1, except that the reaction temperature was 195° C., the mass space velocity was 0.9 g / gcat / h, and the hydrogenation data were shown in Table 1. The reaction result is: the conversion rate of oxalate is 100%, and the selectivity of ethylene glycol is 97%.

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Abstract

The invention discloses a catalyst for preparation of glycol by oxalate hydrogenation; the catalyst comprises a) a carrier and b) copper or a copper compound, the carrier is selected from the group consisting of silica, alumina, zirconia and titania, the carrier accounts for 65 to 85% of the total weight of the catalyst, the copper or the copper compound accounts for 15-29% of the total weight of the catalyst on the basis of copper element, the catalyst BET specific surface area is 350-650m<2> / g, the pore volume is 0.5-1.3ml / g, and the most probable pore diameter is 5-11nm. The catalyst has high catalytic activity, selectivity and stability of the synthesis of preparation of the glycol by oxalate hydrogenation, after 2000h of stable operation of the catalyst, catalytic performance decline is not found. The present invention provides a preparation method of the catalyst, and the method is simple, easy in operation and good in repeatability.

Description

technical field [0001] The invention relates to a hydrogenation catalyst, in particular to a catalyst for oxalate hydrogenation to prepare ethylene glycol. The present invention also relates to a method for preparing the above-mentioned catalyst. Background technique [0002] Ethylene glycol is mainly used in the production of polyester monomers, antifreeze agents, solvents, unsaturated polyester resins, lubricants, plasticizers, nonionic surfactants, glycol ethers, and explosives. In addition, ethylene glycol can also be used in industries such as paint, photographic developer, brake fluid and ink. Therefore, ethylene glycol is widely used and is an important petrochemical organic raw material. At present, my country has surpassed the United States to become the world's largest consumer of ethylene glycol. The amount of ethylene glycol produced cannot meet the demand and needs to be imported in large quantities. [0003] At present, the large-scale industrial production ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72C07C31/20C07C29/149
CPCY02P20/52
Inventor 王瑞璞曾佳谢伦嘉马京生何海龙
Owner CHINA PETROLEUM & CHEM CORP
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