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Catalyst Au-Pd/PDDA-GO for glyoxal air oxidation synthesis of glyoxylic acid and preparation method of catalyst Au-Pd/PDDA-GO

A technology of air oxidation and catalyst, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. It can solve the problems of difficult dispersion, easy aggregation, and influence on Au and Pd dispersion, etc. question

Inactive Publication Date: 2017-04-26
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a strong van der Waals force between graphene sheets, which is easy to aggregate and difficult to disperse in water and common organic solvents. However, graphene oxide GO has excellent dispersibility in water because of its rich oxygen-containing functional groups.
Although GO has good dispersion in solvents, there are still big problems when it is directly used as a catalyst carrier. The main reason is that there are a large number of defects on the surface of GO. When used as a carrier of Au and Pd nanoparticles, these nanoparticles tend to be in the The accumulation of surface defects affects the dispersion of Au and Pd on GO, and it is difficult to prepare a catalyst with high noble metal loading and good dispersion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Graphene oxide (GO) was dispersed in 50 times the mass of water with the assistance of ultrasound, and a PDDA aqueous solution with a mass of 20% of GO was added dropwise under stirring. The molecular weight of PDDA was 8000±500, and the concentration of PDDA aqueous solution was 10%. Continue stirring for 12 hours to obtain sample A-1;

[0018] (2) Mix sample A-1 with 1.5 times the mass of ethylene glycol, and add HAuCl dropwise under stirring 4 and H 2 PdCl 4 The mixed ethylene glycol solution, the total mass of Au and Pd is 5% of the total mass of GO and PDDA, the atomic ratio of Au to Pd is 1:5, and the prepared HAuCl 4 and H 2 PdCl 4 In the mixed ethylene glycol solution, the total number of moles of Au and Pd per liter of solution is 0.01. Continue stirring for 24 hours to obtain sample B-1;

[0019] (3) Adjust the pH of sample B-1 to 10 with NaOH, treat it at 130°C for 2 hours under the protection of nitrogen, and filter it with suction after cooling to...

Embodiment 2

[0022] (1) Graphene oxide (GO) was dispersed in 70 times the mass of water with the assistance of ultrasound, and a PDDA aqueous solution with a mass of 20% of GO was added dropwise under stirring. The molecular weight of PDDA was 8000±500, and the concentration of PDDA aqueous solution was 15%. Continue stirring for 24 hours to obtain sample A-2;

[0023] (2) Mix sample A-2 with 1.3 times the mass of ethylene glycol, and add HAuCl dropwise under stirring 4 and H 2 PdCl 4 The mixed ethylene glycol solution, the total mass of Au and Pd is 8% of the total mass of GO and PDDA, the atomic ratio of Au to Pd is 5:1, and the prepared HAuCl 4 and H 2 PdCl 4 In the mixed ethylene glycol solution, the total number of moles of Au and Pd per liter of solution is 0.02. Continue stirring for 36 hours to obtain sample B-2;

[0024] (3) The pH of sample B was adjusted to 11 with NaOH, treated at 140 °C for 1 hour under the protection of nitrogen, cooled and filtered to obtain 8% Au5-Pd1...

Embodiment 3

[0027](1) Graphene oxide (GO) was dispersed in 80 times the mass of water with the assistance of ultrasound, and a PDDA aqueous solution with a mass of 30% of GO was added dropwise under stirring. The molecular weight of PDDA was 8000±500, and the concentration of PDDA aqueous solution was 20%. Continue stirring for 36 hours to obtain sample A-3;

[0028] (2) Mix sample A-3 with 1.2 times the mass of ethylene glycol, and add HAuCl dropwise under stirring 4 and H 2 PdCl 4 The mixed ethylene glycol solution, the total mass of Au and Pd is 9% of the total mass of GO and PDDA, the atomic ratio of Au and Pd is 1:1, and the prepared HAuCl 4 and H 2 PdCl 4 In the mixed ethylene glycol solution, the total number of moles of Au and Pd per liter of solution is 0.03. Continue stirring for 30 hours to obtain sample B-3;

[0029] (3) The pH of sample B was adjusted to 12 with NaOH, treated at 130 °C for 1 hour under the protection of nitrogen, cooled and filtered to obtain 9% Au1-Pd1...

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PUM

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Abstract

The invention belongs to the technical field of chemical engineering catalysts, and particularly relates to a catalyst Au-Pd / PDDA-GO for glyoxal air oxidation synthesis of glyoxylic acid and a preparation method of the catalyst Au-Pd / PDDA-GO. The catalyst is composed of Au, Pd, PDDA and GO, wherein GO serves as a carrier, PDDA molecules carrying positive charges are adsorbed to GO with the surface carrying negative charges under the electrostatic interaction, then Au and Pd precursors are electrostatically assembled on PDDA to make metal Au and Pd highly dispersed on the surface of GO, and after ethylene glycol reduction, the catalyst Au-Pd / PDDA-GO is obtained; the total mass of Au and Pd is 5-10% that of GO and PDDA, and the atomic ratio of Au to Pd is 1:5-5:1. The catalyst Au-Pd / PDDA-GO shows excellent activity in the reaction of glyoxal liquid-phase air oxidation synthesis of glyoxylic acid.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, in particular to a catalyst for glyoxal liquid-phase air oxidation to synthesize glyoxylic acid and a preparation method thereof. Background technique [0002] Glyoxylic acid is an important organic chemical and pharmaceutical intermediate, widely used in the production of spices, cosmetics, food additives, pharmaceutical and pesticide intermediates and other chemicals. At present, there are three main methods for the production of glyoxylic acid in industry, namely glyoxal nitric acid oxidation method; oxalic acid electrolytic reduction method; maleic anhydride ozone oxidation method. Domestic glyoxylic acid mainly adopts glyoxal nitric acid oxidation method. These three methods are not environmentally friendly enough, especially the domestic mainstream nitric acid oxidation method has the problems of severe equipment corrosion and high environmental pressure, which restricts the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C51/235C07C59/147
CPCB01J31/06B01J2231/70C07C51/235C07C59/147
Inventor 徐华龙沈伟秦枫邓支华付义发周拥军
Owner FUDAN UNIV