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A kind of preparation method of copper-based hydrogenation catalyst without reduction activation

A hydrogenation catalyst, copper-based technology, applied in the preparation of organic compounds, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the inconvenience of catalyst energy consumption and take a long time, etc. problem, achieve the effect of saving in-situ reduction and activation steps and improving catalyst performance

Active Publication Date: 2016-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In summary, the reduction and activation process of the copper-based hydrogenation catalyst before use requires the consumption of H 2 , and often takes a long time, bringing extra energy consumption and inconvenience to the catalyst use process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 48.32g Cu(NO 3 ) 2 ∙3H 2 O, 297.5g Zn(NO 3 ) 2 ∙6H 2 O and 300.1g Al(NO 3 ) 3 ∙9H 2 O is dissolved in water to form a solution with a total salt concentration of 1mol / L, and the mixed nitrate solution and 1mol / L Na 2 CO 3 After the solution was preheated to 60°C, it was poured into 60°C deionized water to maintain the pH of the solution at 7~8; after aging for 30 minutes, the precipitate was washed with deionized water and filtered to obtain a filter cake; weigh 19.3 g citric acid, and uniformly dispersed in 3L ethanol together with the filter cake, after stirring at room temperature for 30min, the temperature rose to 60°C to recover the ethanol by distillation, and the obtained solid A was roasted at 500°C for 4h under a nitrogen atmosphere, and then the temperature was lowered to At 40°C, switch the nitrogen gas to oxygen / nitrogen with an oxygen volume percentage of 1% and maintain it for 30 minutes, then cool down to room temperature, shape and crush t...

Embodiment 2

[0032] Weigh 120.8g Cu(NO 3 ) 2 ∙3H 2 O, 178.5g Zn(NO 3 ) 2 ∙6H 2 O, 337.6g Al(NO 3 ) 3 ∙9H 2 O and 52.2g Ba(NO 3 ) 2 Dissolve in water to form a solution with a total salt concentration of 1mol / L, mix the nitrate solution and 1mol / L K 2 CO 3After the solution was preheated to 60°C, it was poured into 60°C deionized water to maintain the pH of the solution at 7~8; after aging for 30 minutes, the precipitate was washed with deionized water and filtered to obtain a filter cake; weigh 75.05 g of tartaric acid, and evenly dispersed in 3L of acetone together with the filter cake, stirred at room temperature for 30min, then the temperature was raised to 60°C to recover ethanol by distillation, and the obtained solid A was roasted at 600°C for 2h in a nitrogen atmosphere, and then the temperature was lowered to 30°C ℃, switch the nitrogen gas to oxygen / nitrogen with an oxygen volume percentage of 1% and maintain it for 30 minutes, then cool down to room temperature, shape ...

Embodiment 3

[0038] Weigh 241.6g Cu(NO 3 ) 2 ∙3H 2 O, 267.7g Zn(NO 3 ) 2 ∙6H 2 O, 37.5g Al(NO 3 ) 3 ∙9H 2 O and 43.4gCe(NO 3 ) 3 ∙6H 2 O is dissolved in water to form a solution with a total salt concentration of 1mol / L, and the mixed nitrate solution and 1mol / L Na 2 CO 3 After the solution was preheated to 60°C, it was poured into 60°C deionized water to maintain the pH of the solution at 7~8; after aging for 30 minutes, the precipitate was washed with deionized water and filtered to obtain a filter cake; weigh 120.1 g tartaric acid, and evenly dispersed in 3L ether together with the filter cake, after stirring at room temperature for 30min, the temperature was raised to 60°C to recover ethanol by distillation, and the obtained solid formazan was roasted at 600°C for 2h under a nitrogen atmosphere, and then the temperature was lowered to 25°C °C, switch nitrogen to oxygen / nitrogen with 1% oxygen by volume and keep it for 30 minutes. The obtained solid B is shaped and crushed i...

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Abstract

The invention relates to a method for preparing a copper-based hydrogenation catalyst without reduction and activation, and belongs to the technical field of catalyst preparation. Catalyst composition contains Cu, CuO, ZnO and Al 2 o 3 , can also contain other additives, such as MgO, BaO, La 2 o 3 , CeO 2 , Ga 2 o 3 and ZrO 2 One or more of them, the Cu 2+ , Zn 2+ and Al 3+ And the mixed nitrate solution of the auxiliary agent and the alkaline precipitant are added to the water in parallel, and the pH of the solution is maintained at 7~8; after the neutralization process is completed, after aging, washing, and filtration, the obtained filter cake is mixed with The acid is evenly dispersed in a volatile organic solvent, and then the organic solvent is removed, and the remaining solid is roasted in an inert atmosphere, and the roasted solid is passivated in an oxidizing atmosphere, and finally shaped into tablets. On the basis of improving the performance of the catalyst, the invention saves the in-situ reduction and activation step when the catalyst is used.

Description

technical field [0001] The invention relates to a method for preparing a copper-based hydrogenation catalyst that does not require reduction and activation. Specifically, citric acid is introduced in the preparation process, roasted under an inert atmosphere, and the gas and solid C generated by thermal decomposition of citric acid, Pores are made to the catalyst and the CuO is reduced to metallic Cu. The invention belongs to the technical field of catalyst preparation. Background technique [0002] Hydrogenation reaction is the most common and one of the most important reaction types in the chemical process, such as carbon monoxide and / or carbon dioxide hydrogenation to methanol, maleic anhydride gas-phase hydrogenation to γ-butyrolactone, etc. In order to enable the reaction to proceed quickly and obtain more target products, the use of hydrogenation catalysts is essential, such as the heterogeneous hydrogenation reaction catalyst CuO-ZnO-Al commonly used in industry 2 o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80C07D307/33C07C31/04C07C29/154
CPCY02P20/52
Inventor 于杨陈海波贺健毛春鹏曹建平魏士新殷玉圣
Owner CHINA PETROLEUM & CHEM CORP
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