Nano Pd catalyst used for preparing oxalic ester by CO gas phase oxidation coupling and its preparation method

An oxidative coupling and catalyst technology, applied in the fields of carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve serious pollution and cannot precisely control Pd particles , Unreasonable utilization of raw materials, etc.

Active Publication Date: 2012-06-27
贵州鑫醇科技发展有限公司
View PDF9 Cites 25 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has high production process cost, high energy consumption, serious pollution and unreasonable utilization of raw materials
In the 1960s, Fenton in the United States reported a method of directly coupling CO and alcohols into oxalate esters, which opened up a new way for C1 to chemically synthesize ox

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Nano Pd catalyst used for preparing oxalic ester by CO gas phase oxidation coupling and its preparation method
  • Nano Pd catalyst used for preparing oxalic ester by CO gas phase oxidation coupling and its preparation method
  • Nano Pd catalyst used for preparing oxalic ester by CO gas phase oxidation coupling and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 1g of α-alumina and add to the solution containing Pd(OAc) 2 0.010 g, 0.016 g of ascorbic acid, 0.054 g of sodium oxalate, and 0.111 g of polyvinylpyrrolidone (PVP) in 20 mL of aqueous solution, stirred at 100°C for 0.5 hours, washed three times with acetone, water, and ethanol, and dried in vacuum at 60°C for 2 hours. The transmission electron microscope photos of the obtained samples are shown in figure 1 , It can be observed from the figure that Pd is uniformly dispersed on the surface of the carrier, and the particles are non-spherical polyhedrons with an average size of 2-3nm. The high-resolution transmission electron microscope photograph of the sample is shown in Figure 5-Figure 8, it can be seen from the figure that the lattice spacing of the non-spherical polyhedral particles is 0.226nm, which is consistent with the lattice spacing of the face-centered cubic (111) plane of Pd, and it can be seen that the exposed crystal plane is the (111) plane. Accord...

Embodiment 2

[0040] Weigh 1g of α-alumina and add to the 2 PdCl 4 0.015g, 0.084g citric acid, and 0.111g polyvinylpyrrolidone (PVP) in 20mL aqueous solution, when heated to 60°C, add 1mL formaldehyde, stir for 3 hours, wash with acetone, water, and ethanol three times, and dry at 60°C for 2 hours in vacuum . TEM photo see image 3 , It can be seen from the figure that Pd is highly dispersed on the surface of the carrier, and the particles are octahedral, with an average size of 20-22nm. High-resolution transmission electron microscope photos see Figure 11-Figure 14 , it can be seen from the figure that the lattice spacing of the octahedral particles is 0.226nm, which is consistent with the lattice spacing of the face-centered cubic (111) plane of Pd. It can be seen that the exposed crystal plane is the (111) plane. According to the statistics of the analysis results of multiple high-resolution transmission electron microscope photos, it can be known that more than 50% of the exposed ...

Embodiment 3

[0042] Weigh 1g of α-alumina and add to the solution containing Pd(OAc) 2 0.004g, 0.007g of sodium formate, 0.084g of citric acid, and 0.111g of polyvinylpyrrolidone (PVP) in a 20mL aqueous solution, stirred at 100°C for 0.5 hours, washed three times with acetone, water, and ethanol, and dried in vacuum at 60°C for 2 hours. TEM photo see Figure 4 , It can be seen from the figure that Pd is highly dispersed on the surface of the carrier, and the particles appear as non-spherical polyhedrons with an average size of 2-3nm. High-resolution transmission electron microscope photos see Figure 15-Figure 18 , it can be seen from the figure that the lattice spacing of the non-spherical polyhedral particles is 0.226nm, which is consistent with the lattice spacing of the face-centered cubic (111) plane of Pd, and it can be seen that the exposed crystal plane is the (111) plane. According to the statistics of the analysis results of multiple high-resolution transmission electron micro...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention belongs to the oxalic ester preparation technical field, and provides a nano Pd catalyst used for preparing oxalic ester by CO gas phase oxidation coupling in coal glycol, its preparation method and its purpose. According to the invention, the catalyst takes alpha-alumina as a carrier, precious metal Pd nano particles are taken as an active component, by referring the weight of the catalyst carrier, the weight percentage content of the active ingredient Pd is 0.05-2%. The catalyst is prepared by using a nano metal in-situ loading method. The preparation method has the advantages of simple process and low energy consumption, and enables accurate regulation and control on the size and bare crystal face of the Pd nano particles. The catalyst with the bare crystal face of (lll) surface has the advantages of high Pd dispersiveness of active components, small size and narrow distribution, and can catalyze CO gas phase oxidation coupling to oxalic ester with high efficiency under low precious metal load capacity.

Description

technical field [0001] The invention relates to the synthesis of oxalate, in particular to a nano-Pd catalyst for preparing oxalate by CO gas-phase oxidation coupling in coal-based ethylene glycol, as well as its preparation method and application. Background technique [0002] Coal-based ethylene glycol is mainly divided into three steps. The first step: CO dehydrogenation and purification of coal-based syngas after pressure swing adsorption separation; the second step: CO gas-phase oxidation coupling to oxalate; the third step: oxalate hydrogenation to ethylene glycol. Among them, CO gas-phase oxidative coupling to oxalate is a key step in the conversion of inorganic CO to organic chemical oxalate in coal-to-ethylene glycol. Oxalate is an important organic chemical raw material, which can be used to prepare intermediates of ethylene glycol, oxalic acid, oxalyl chloride, oxalamide, certain drugs, dyes and solvents. At present, the method of esterification and dehydration ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J23/44B01J35/10C07C69/36C07C67/36
Inventor 徐忠宁郭国聪王明盛姚元根
Owner 贵州鑫醇科技发展有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap