Preparation method of catalyst for preparation of glycol by oxalate hydrogenation

A technology of oxalate and ethylene glycol is applied in the field of preparation of oxalate hydrogenation to ethylene glycol catalyst, which can solve the problems of low ethylene glycol selectivity and poor catalyst activity, and achieves improved selectivity and activity. Effect

Inactive Publication Date: 2014-09-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is the technical problem of poor catalyst activity and low ethylene glycol selectivity in the prior art, and a new preparation method of oxalate hydrogenation catalyst for ethylene glycol is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1 liter of a solution containing 0.5 mol / liter copper nitrate, 0.05 mol / liter nickel nitrate and 0.05 mol / liter barium nitrate was used as solution I, and 80 grams of silicon dioxide was added to solution I under stirring to obtain slurry II, and then 3 mol / liter of ammonium bicarbonate was added to the slurry II as a precipitant, the pH at the end point was controlled to be 6.5, aged at 90°C for 4 hours, then the slurry was filtered and washed, and the obtained filter cake was dried at 80-120°C for 10 hour, 400 DEG C for 5 hours, and the calcined catalyst is pressed into pellets to form a catalyst. The catalyst composition is: 30%CuO+5%NiO+3.5%BaO+61.5%SiO 2 .

[0024]

Embodiment 2

[0026] 1 liter of a solution containing 0.3 mol / L copper nitrate, 0.03 mol / L ammonium molybdate and 0.1 mol / L nickel nitrate was used as solution I, and 80 grams of alumina was added to solution I under stirring to obtain slurry II, and then 2 Add mole / liter sodium bicarbonate as a precipitant to the slurry II, control the end point pH to 7, age at 80°C for 4 hours, then filter and wash the slurry, and dry the obtained filter cake at 80-120°C for 10 hours , and then calcined at 400°C for 5 hours, and the calcined catalyst is pressed into tablets to form a catalyst. The catalyst composition is: 11.4% CuO+5%Cu +5%NiO+2.6%MoO 3 +76%Al 2 o 3.

[0027]

Embodiment 3

[0029] Take 1 liter of a solution containing 0.15 mol / L copper nitrate, 0.01 mol / L magnesium nitrate and 0.1 mol / L zinc nitrate as solution I, and add 80 grams of ZSM-5 molecular sieve into solution I under stirring to obtain slurry II, and then Add 1.5 mol / liter of sodium carbonate as a precipitating agent into the slurry II, control the end point pH to 9, age at 70°C for 4 hours, filter and wash the slurry, and dry the obtained filter cake at 80-120°C for 10 hours. Calcined at 450°C for 5 hours, the calcined catalyst was pressed into pellets to form the catalyst. The catalyst composition is: 10% CuO+1%Cu+14%MgO+15%ZnO+61%ZSM-5.

[0030]

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Abstract

The invention relates to a preparation method of a catalyst for preparation of glycol by oxalate hydrogenation, and mainly solves the problems of poor catalyst activity and low glycol selectivity in the prior art. The method comprises the following steps: a) mixing a soluble salt of an active component copper and a soluble salt of an additive to prepare a mixed solution I; b) under the condition of stirring, adding a carrier into the solution I to obtain slurry II; c) preparing at least one substance selected from the group consisting of carbonate, bicarbonate, alkali metal hydroxide or inorganic ammonia into a solution III as a precipitating agent; d) mixing the solution III and the slurry II, controlling the precipitation reaction end point pH value to be 5.6-12 to obtain slurry IV; e) aging the slurry IV at 50-95 DEG C for 0.5-10 hours, then filtering and washing; and f) drying a filter cake at 60-120 DEG C, and then roasting at 300-600 DEG C; the technical scheme of the method can well solve the problems of poor catalyst activity and low glycol selectivity in the prior art, and the method can be used for the industrial production of preparation of the glycol by oxalate hydrogenation.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for hydrogenation of oxalate to ethylene glycol, in particular to a preparation method for a catalyst for the catalytic hydrogenation of dimethyl oxalate or diethyl oxalate to produce ethylene glycol. Background technique [0002] Ethylene glycol (EG) is an important organic chemical raw material, mainly used in the production of polyester fibers, antifreeze agents, unsaturated polyester resins, lubricants, plasticizers, nonionic surfactants and explosives, etc. It can be used in industries such as paint, photographic developer, brake fluid and ink, as a solvent and medium for ammonium perborate, and can also be used in the production of special solvents such as glycol ether, etc., and has a wide range of uses. [0003] In the past 10 years, due to the strong demand of the polyester industry, the demand for ethylene glycol in the domestic market has maintained a rapid growth trend. In 1995, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78B01J23/885B01J29/46B01J23/755B01J23/89C07C31/20C07C29/149
Inventor 龚海燕刘俊涛刘国强
Owner CHINA PETROLEUM & CHEM CORP
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