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Catalyst for synthesizing diethyl oxalate with carbon monoxide, preparation method and application thereof

A technology of diethyl oxalate and carbon monoxide, applied in the directions of carbon monoxide or formate reaction preparation, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of poor catalytic performance, oxalate space-time Problems such as low yield, to achieve obvious effect

Active Publication Date: 2010-02-24
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the reported catalysts for the synthesis of oxalates, SiO 2 And active carbon is that the catalyzer of carrier all shows poor catalytic performance (USP 4229591,1980); Take metal palladium (Pd) as the catalyst of the synthetic oxalate of active component to show better catalytic performance, but with palladium catalyst For the synthesis of oxalate, there is a problem of low space-time yield of oxalate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 20gα-Al 2 o 3 , by 0.5wt%Pd+0.5wt%Ni / α-Al 2 o 3 content preparation catalyst, the steps are as follows: select Ni(NO 3 ) 2 ·6H 2 O, according to the Ni load, prepare a solution containing nickel ions with a concentration of 0.05M, and then select PdCl according to the Pd load 2 , adding it to the above solution to prepare an impregnation solution, the content of palladium ions in the impregnation solution is 0.03M, and then the carrier α-Al 2 o 3 Immerse in the impregnating solution for 10 hours, and after fully absorbed, stir and evaporate to dryness in a 70°C water bath. The obtained solid is roasted in an air atmosphere at 300°C for 3 hours, and then reduced with hydrogen at a temperature of 300°C for 3 hours. for 2000h -1 , and finally cooled to room temperature in a hydrogen atmosphere to obtain the desired catalyst (catalyst A).

[0025] The catalyst A of this embodiment is used in the reaction of carbon monoxide and ethyl nitrite to synthesize diet...

Embodiment 2

[0029] Weigh 20gα-Al 2 o 3 , according to 0.5wt%Pd+0.5wt%Ni / α-Al 2 o 3 content preparation catalyst, the steps are as follows: select Ni(NO 3 ) 2 ·6H 2 O, according to the Ni loading, prepare a solution containing nickel ions with a concentration of 0.009M, and then select Pd(NO 3 ) 2 , adding it to the above solution to prepare an impregnation solution, the palladium ion content in the impregnation solution is 0.005M, and then the carrier αAl 2 o 3 Immerse in the impregnation solution for 24 hours, and after fully absorbed, stir and evaporate to dryness in a water bath at 80°C. The solid obtained is roasted in an air atmosphere at 500°C for 6 hours, and then reduced with hydrogen at a temperature of 500°C for 6 hours. 800h -1 , and finally cooled to room temperature in a hydrogen atmosphere to obtain the desired catalyst (catalyst B).

[0030]Catalyst B of this embodiment is used in the reaction of carbon monoxide and ethyl nitrite synthetic diethyl oxalate, carbon ...

Embodiment 3

[0032] Weigh 20gα-Al 2 o 3 , according to 0.5wt%Pd+0.1wt%Ni / α-Al 2 o 3 content preparation catalyst, the steps are as follows: choose NiCl 2 ·6H 2 O, prepare a solution with a nickel ion concentration of 0.002M according to the Ni loading amount, and then select PdCl according to the Pd loading amount 2 , adding it to the above solution to prepare an impregnation solution, the palladium ion content in the impregnation solution is 0.005M, and then the carrier α-Al 2 o 3 Immerse in the impregnating solution for 24 hours, and after fully absorbed, stir and evaporate to dryness in a water bath at 80°C. The solid obtained is roasted in an air atmosphere at 300°C for 6 hours, and then reduced with hydrogen at a temperature of 300°C for 3 hours. 3000h -1 , and finally cooled to room temperature in a hydrogen atmosphere to obtain the desired catalyst (catalyst C).

[0033] Catalyst C of the present embodiment is used in the reaction of carbon monoxide and ethyl nitrite synthet...

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Abstract

The invention discloses a catalyst for synthesizing diethyl oxalate and a preparation method thereof, belonging to the oxalate preparation technical field. The catalyst includes the main active components of Pd, a carrier of alpha-Al2O3 and the auxiliary agent of the transition metal Ni. The catalyst is prepared by an immersion method. Test proves that Pd-Ni / alpha-Al2O3 catalyst has good reactionactivity and high selectivity. The diethyl oxalate space-time yield reaches more than 1000l[-1]h[-1] at the highest level.

Description

[0001] Catalyst for synthesizing diethyl oxalate from carbon monoxide and its preparation method and application technical field [0002] The invention belongs to the technical field of oxalate preparation, and further relates to a catalyst for synthesizing diethyl oxalate from carbon monoxide, a preparation method and application thereof. Background technique [0003] Diethyl Oxalate (Diethyl Oxalate), the molecular formula is C 6 h 10 o 4 , is an important chemical raw material, which can be used to prepare important chemical raw materials such as ethylene glycol, oxalic acid and high-quality fertilizer oxamide, and is widely used in the preparation of various dyes, pharmaceutical intermediates, extractants, plastic accelerators and solvents. [0004] The traditional production of diethyl oxalate is to use oxalic acid and ethanol as raw materials, toluene as dehydrating agent, and adopt the method of esterification and dehydration to prepare. The production process has ...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/18C07C69/36C07C67/36
Inventor 胡玉容李扬王科范鑫袁小金许红云
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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