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Au-Pd bimetallic catalyst for preparing methyl formate by selective oxidation of methanol as well as preparation method and application thereof

A technology of bimetallic catalysts and methyl formate, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low conversion rate and high reaction temperature, Achieve the effect of high selectivity, good catalytic activity and long life

Inactive Publication Date: 2013-07-10
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yang et al. used the Ag catalyst reduced by sodium borohydride for the selective oxidation of methanol and found that the catalyst achieved a conversion rate of 23% and a selectivity of 90% at 300°C [Catal.Lett., 2005, 100:205-211], but such The problem with the catalyst is that the reaction temperature is high and the conversion rate is low
However, there are still relatively few research reports on using graphene as a catalyst support, and there are no relevant literature and patent reports on the use of graphene support-supported Au-Pd bimetallic catalysts for methanol selective oxidation reactions.

Method used

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  • Au-Pd bimetallic catalyst for preparing methyl formate by selective oxidation of methanol as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) 1g of graphene carrier (specific surface area 120m 2 / g, C / O molar ratio 6, conductivity 15S / cm) into 20ml of water, heated to 60oC and stirred evenly. Add 2g of NaOH therein, the pH must be controlled at 14, and continue to stir for 0.5h.

[0042] (2) Add 5ml HAuCl containing Au0.0025g 4 solution and 20ml PdCl containing Pd0.01g 2 Mix the solution and stir well.

[0043] (3) Add the prepared solution in (2) to (1) drop by drop under constant stirring, and continue to stir for 2 hours after the dropwise addition is completed.

[0044] (4) Pump and wash the precipitate of (3) with deionized water until there is no Cl - , dried at 110°C for 15h, and calcined at 200°C for 5h in a nitrogen atmosphere to prepare the catalyst Au 0.25 PD 1.0 / Graphene.

[0045] After the catalyst was activated on-line at 150°C in a fixed bed for 1 hour in an air atmosphere, CH 3 OH / O 2 Molar ratio 1:5, reaction space velocity 3000ml·g -1 h -1 , 50 ° C reaction. The conversion r...

Embodiment 2

[0047] (1) 1g of graphene carrier (specific surface area 100m 2 / g, C / O molar ratio 8, conductivity 30S / cm) was added to 20ml of water, heated to 70°C and stirred evenly. After adding 1g of KOH therein, the pH must be controlled at 13, and the stirring was continued for 1h.

[0048] (2) Add 15ml HAuCl containing Au0.01g 4 solution and 20ml PdCl containing Pd0.01g 2 Mix the solution and stir well.

[0049] (3) Add the prepared solution in (2) to (1) drop by drop under constant stirring, and continue to stir for 1 hour after the dropwise addition is completed.

[0050] (4) Pump and wash the precipitate of (3) with deionized water until there is no Cl - , dried at 110°C for 13h, and calcined at 200°C for 4h in a nitrogen atmosphere to prepare the catalyst Au 1.0 PD 1.0 / Graphene.

[0051] After the catalyst was activated online at 160°C in a fixed bed for 1.5h in an air atmosphere, CH 3 OH / O 2 Molar ratio 1:3, reaction space velocity 10000ml·g -1 h -1 , 90 ° C reaction...

Embodiment 3

[0053] (1) 1g of graphene carrier (specific surface area 150m 2 / g, C / O molar ratio 8, conductivity 10S / cm) was added to 20ml of water, heated to 60°C and stirred evenly. After adding 2g KOH therein, the pH must be controlled at 13, and the stirring was continued for 2h.

[0054] (2) Add 15ml HAuCl containing Au0.01g 4 solution and 40ml Pd(NO 3 ) 2 Mix the solution and stir well.

[0055] (3) Add the solution prepared in (2) to (1) drop by drop under continuous stirring. After the dropwise addition, the pH value needs to be controlled at 12, and continue to stir for 1 hour.

[0056] (4) Pump and wash the precipitate of (3) with deionized water until there is no Cl - , Dry at 110°C for 20h, and bake at 250°C for 4h in a nitrogen atmosphere. Catalyst Au 1.0 PD 2.0 / Graphene.

[0057] After the catalyst was activated on-line at 180°C in a fixed bed for 1.0 h in an air atmosphere, CH 3 OH / O 2 Molar ratio 1:5, reaction space velocity 15000ml·g -1 h -1 , 70 ° C reaction...

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Abstract

The invention discloses an Au-Pd bimetallic catalyst for preparing methyl formate by selective oxidation of methanol. The Au-Pd bimetallic catalyst comprises a carrier and active components, namely Au oxide and Pd oxide, wherein the loading amount of Au is 0.25-5.0wt%, the loading amount of Pd is 0.25-5.0wt%, and the balance is the graphene carrier. The Au-Pd bimetallic catalyst disclosed by the invention has the advantages of low reaction temperature, high catalytic activity and good stability.

Description

technical field [0001] The invention belongs to a catalyst and its preparation method and application, in particular to an Au-Pd bimetallic catalyst used for the selective oxidation of methanol to produce methyl formate, as well as its preparation method and application. technical background [0002] Methyl Formate (MF for short), the molecular formula is C 2 h 4 o 2 , the structural formula is HCOOCH 3 , molecular weight 60.5, is a colorless liquid with aromatic odor. Its melting point is -99.38°C, boiling point is 32°C, relative density is 0.98, heat of combustion is 978.7kJ / mol, critical temperature is 214°C, flash point is -32°C, and ignition temperature is 449°C. It is soluble in water, ethanol, methanol, and ether. As a versatile chemical intermediate, many chemical products can be synthesized. For example, formic acid can be prepared by hydrolysis of MF; MF can be used for the synthesis of amides; MF can also be used for the synthesis of esters; MF can also be us...

Claims

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Application Information

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IPC IPC(8): B01J23/52C07C69/06C07C67/40
Inventor 王建国吴志伟秦张峰朱华青王瑞义王国富樊卫斌
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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