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Composite carrier catalyst used for glycol and synthesized from hydrogenation of alkyl oxalate, and preparation method thereof

A technology of alkyl oxalate and composite carrier, which is used in catalyst activation/preparation, hydroxyl compound preparation, chemical instruments and methods, etc., to achieve the effects of ensuring thermal stability, improving dispersibility and poor thermal stability

Active Publication Date: 2011-10-26
PUJING CHEM IND SHA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The American ARCO company proposed in the patent US 54112245 that copper-chromium catalysts have high hydrogenation activity and selectivity, and the catalysts supported on Al 2 o 3 , SiO 2 Or copper-chromium catalyst on glass beads, the temperature is 200-230°C, but the yield of ethylene glycol is only 11.7-18.9%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of composite carrier catalyst for hydrogenation of alkyl oxalate to synthesize ethylene glycol, comprises the following steps:

[0025] In the first step, take 22.80g of 25wt% silica sol, dilute it to 200ml with deionized water, adjust the pH value to 3.0, and make solution I;

[0026] In the second step, 4.29g of cerium nitrate was dissolved in 100ml of deionized water, and the pH value was adjusted to 3.0 to form solution II;

[0027] The third step is to dissolve 12.00g urea in 100ml deionized water to form solution III;

[0028] The fourth step is to dissolve 12.08g copper nitrate in 200ml deionized water, adjust the pH value to 3.0, and make solution IV;

[0029] The fifth step is to add solution I, solution II, and solution III together dropwise and mix them, stir vigorously, and age at 90°C for 3 hours, then slowly add solution IV to the mixed solution dropwise, continue to age for 16 hours, and filter and wash to obtain a filter cak...

Embodiment 2

[0035] According to the steps and conditions of Example 1, only the catalyst composition is 25%CuO / 65%SiO 2 -10%B 2 o 3 . Using dimethyl oxalate as raw material, methanol as solvent, at a reaction temperature of 240°C, a reaction pressure of 3.0MPa, and a liquid hourly space velocity of 2.0h -1 , under the condition of hydrogen ester ratio of 200, the conversion rate of dimethyl oxalate is greater than 99.9%, and the selectivity of ethylene glycol is greater than 95%.

Embodiment 3

[0037] According to the steps and conditions of Example 1, only the catalyst composition is 35%CuO / 55%TiO 2 -10% ZrO 2 . Using dimethyl oxalate as raw material, methanol as solvent, at a reaction temperature of 240°C, a reaction pressure of 5.0MPa, and a liquid hourly space velocity of 1.0h -1 , under the condition of hydrogen ester ratio of 160, the conversion rate of dimethyl oxalate is greater than 99.9%, and the selectivity of ethylene glycol is greater than 95%.

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Abstract

The invention relates to a composite carrier catalyst used for glycol and synthesized from hydrogenation of alkyl oxalate, and a preparation method thereof. The chemical formula of the composite carrier catalyst is CuO / ROx-Moy. Wherein, CuO accounts for 5-60 mass percent, ROx accounts for 10-90 mass percent, and Moy accounts for 0.1-60 mass percent, x as 1 / 2 of the highest valency of R, y is 1 / 2 of the highest valency of M, R is one of Si, Al, Zr and Ti, and M is one of Si, Al, Cr, Zr, Ti, B, Zn, Mo, Ce, Bi, La. Compared with the prior art, in the invention a composite carrier is employed in the catalyst used for glycol and synthesized from hydrogenation of alkyl oxalate. The carrier can effectively disperse the active component copper so as to make the sintering of copper grains hard andextend the service life of the catalyst. Meanwhile, the composite carrier can effectively adjust the surface acidity and basicity, reduce the generation of by-products, and improve the selectivity ofglycol. The total conversion rate of oxalate can reach over 99.9%, while the selectivity of glycol is above 95%. Thus, the catalyst of the invention can be used in the industrial production of glycol.

Description

technical field [0001] The invention relates to a catalyst in the field of organic synthesis, in particular to a composite carrier catalyst for hydrogenating alkyl oxalate to synthesize ethylene glycol and a preparation method thereof. Background technique [0002] Ethylene glycol is an important organic chemical raw material, which can react with terephthalic acid (PTA) to produce polyethylene terephthalate (PET), that is, polyester resin, which can be used as polyester fiber and polyester Plastic raw material, which is currently the most important use of ethylene glycol. Ethylene glycol can also react with polybasic acids such as phthalic acid, maleic acid, and fumaric acid to form corresponding polymers, which are collectively referred to as alkyd resins. Secondly, ethylene glycol can also be directly used as antifreeze and formulated Engine coolant, ethylene glycol dinitrate can be used as explosives, and it is also an indispensable substance for the production of plast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J23/72B01J23/843B01J23/86C07C31/20C07C29/149
CPCC07C29/149B01J23/72B01J23/80B01J23/83B01J23/8437B01J23/868B01J23/885B01J37/031Y02P20/52
Inventor 张博计扬骆念军毛彦鹏
Owner PUJING CHEM IND SHA
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