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

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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 temperatur

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0040] Example 1

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

[0042] (2) 5ml HAuCl containing Au0.0025g 4 Solution and 20ml PdCl containing Pd0.01g 2 The solution is mixed and stirred well.

[0043] (3) The solution prepared in (2) was added dropwise to (1) under constant stirring, and the stirring was continued for 2 hours after the dropwise addition was completed.

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

[0045] After the catalyst was activated online at 150 °C in a fixed bed for 1 h, CH under normal pressure 3 OH / O 2 Molar ratio 1:5, reaction space velocity 3000ml·g -1 ·h...

Example Embodiment

[0046] Example 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 well. 1 g of KOH was added to it, the pH must be controlled at 13, and stirring was continued for 1 h.

[0048] (2) 15ml HAuCl containing Au0.01g 4 Solution and 20ml PdCl containing Pd0.01g 2 The solution is mixed and stirred well.

[0049] (3) The solution prepared in (2) was added dropwise to (1) under constant stirring, and the stirring was continued for 1 h after the dropwise addition was completed.

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

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

Example Embodiment

[0052] Example 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. 2g KOH was added to it, the pH must be controlled at 13, and stirring was continued for 2h.

[0054] (2) 15ml HAuCl containing Au0.01g 4 solution and 40ml Pd(NO) containing Pd0.02g 3 ) 2 The solution is mixed and stirred well.

[0055] (3) The solution prepared in (2) was added dropwise to (1) under constant stirring. After the dropwise addition, the pH value should be controlled at 12, and stirring was continued for 1 hour.

[0056] (4) Pump and wash the precipitate of (3) with deionized water until no Cl - , dried at 110°C for 20h, and calcined at 250°C for 4h in a nitrogen atmosphere. Preparation of catalyst Au 1.0 Pd 2.0 / Graphene.

[0057] After the catalyst was activated online at 180 °C in a fixed bed for 1.0 h, CH under normal pressure 3 OH / O 2 Molar ratio 1:5, 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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