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Binary metal nano Pd/aluminum oxide catalyst, preparation method thereof and method for preparing dimethyl oxalate through CO coupling oxidation

A technology of binary metal and catalyst, applied in the field of preparation of dimethyl oxalate, can solve problems such as uneconomical and complicated catalyst modification methods, and achieve the effects of reducing energy consumption and improving catalyst performance

Pending Publication Date: 2020-11-17
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst has certain defects in the space-time yield and stability of dimethyl oxalate, and the catalyst modification method is very cumbersome and uneconomical

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0019] The invention provides a binary metal nano Pd / Al 2 o 3 The preparation method of catalyst comprises:

[0020] 1) the carrier Al 2 o 3 , metal salt and water for impregnation and drying to obtain metal salt modified Al 2 o 3 ;

[0021] 2) modifying Al with the second modifier and metal salt 2 o 3 Coupling modification in water and drying to obtain coupling modified Al 2 o 3 ;

[0022] 3) Carbonate, water and coupling modified Al 2 o 3 Mixing, crystallization, washing and drying are performed to obtain crystallized Al 2 o 3 ;

[0023] 4) The palladium-containing compound, solvent, reducing agent and crystallized Al 2 o 3 Contact reaction, washing and drying to produce binary metal nano Pd / Al 2 o 3 catalyst;

[0024] Wherein, the metal salt is selected from at least one of magnesium salt, ferrous salt, cobalt salt, nickel salt and zinc salt; the second modifying agent is selected from at least one of cellulose, glucose, sorbitol and xylitol.

[0025] In...

Embodiment 1

[0054] 1) Weigh Al 2 o 3 (0.28mol, 100-200 mesh) and 28.5g of water are fully stirred and mixed and placed in a reaction kettle, then 3.7g of cobalt chloride (0.028mol) is added, fully stirred and impregnated for 3-6 hours, and then placed in a vacuum oven at 80°C Dry for 6 hours to obtain a metal salt-modified carrier, which is taken out for later use.

[0055] 2) Fully mix 11g of metal salt modified carrier and 20g of water, add 0.22g of cellulose (second modifier), stir and mix thoroughly for 3 hours, and dry in a vacuum oven at 80°C for 6 hours to obtain coupling modification carrier.

[0056] 3) Fully mix 10g of coupling modified carrier 10 with water, gradually add 100mL sodium carbonate solution (0.5mol / L), stir well, crystallize at 80°C for 15h, then wash with water until neutral, dry at 110°C, crystallized Al 2 o 3 ,spare.

[0057] 4) 2g crystallized Al 2 o 3 Immersed in 3.5mL palladium chloride solution (1% by weight Pd), added 0.004mol sodium borohydride, st...

Embodiment 2

[0059] Proceed according to the method of embodiment 1, make catalyst A2, only difference is, the glucose of equal weight is replaced by cellulose.

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Abstract

The invention discloses a binary metal nano Pd / Al2O3 catalyst and a preparation method thereof, and a method for preparing dimethyl oxalate through CO coupling oxidation, the preparation method comprises the following steps: 1) dipping and drying a carrier Al2O3, a metal salt and water to prepare metal salt modified Al2O3; 2) carrying out coupling modification on a second modifier and the metal salt modified Al2O3 in water, and conducting drying to obtain coupled modified Al2O3; 3) mixing a carbonate, water and the coupling modified Al2O3, and condcuting crystallizing, washing and drying to obtain crystallized Al2O3; and 4) carrying out contact reaction on the palladium-containing compound, a solvent, a reducing agent and the crystallized Al2O3, and conducting washing and drying to obtainthe binary metal nano Pd / Al2O3 catalyst. The binary metal nano Pd / Al2O3 catalyst has excellent space-time yield and stability in a CO gas phase catalytic coupling method.

Description

technical field [0001] The present invention relates to the preparation of dimethyl oxalate, specifically, relate to a kind of binary metal nano Pd / Al 2 o 3 Catalyst and its preparation method and method for preparing dimethyl oxalate by CO coupling oxidation. Background technique [0002] Dimethyl oxalate is an important chemical raw material, which can be widely used in solvents, plasticizers and other fields, and its main use is to prepare ethylene glycol. The technology of preparing ethylene glycol from dimethyl oxalate has become one of the current research hotspots. [0003] Dimethyl oxalate can be obtained by the esterification reaction between oxalic acid and methanol, and can also be obtained by CO catalyzed coupling reaction. Since the utilization and elimination of CO has important research significance for the utilization of resources, the technical process of producing dimethyl oxalate by CO catalytic method has attracted much attention, especially the CO gas...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/58B01J23/60B01J37/02B01J37/03B01J37/16C07C67/36C07C69/36
CPCB01J23/8913B01J23/58B01J23/8906B01J23/892B01J23/60B01J37/0207B01J37/035B01J37/16C07C67/36
Inventor 章青刘化良朱加明李兵
Owner ANHUI NORMAL UNIV
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