High-dispersion polyoxometallate magnetic microsphere catalyst, and preparation method and application thereof

A technology of polyoxometalates and magnetic microspheres, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve difficult recovery, difficult separation, active Limited space and other issues

Inactive Publication Date: 2019-12-20
ZHONGBEI UNIV
View PDF8 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polyacids have disadvantages such as small specific surface area, limited active sites, easily solu

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
  • High-dispersion polyoxometallate magnetic microsphere catalyst, and preparation method and application thereof
  • High-dispersion polyoxometallate magnetic microsphere catalyst, and preparation method and application thereof
  • High-dispersion polyoxometallate magnetic microsphere catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the Fc of chitosan modification 3 o 4 Covalent loading of P on magnetic microspheres 2 W 17 Composite catalyst P 2 W 17 -CS@Fe 3 o 4 -1 preparation: the steps are as follows: 156 mg KH-560 and 1.0 g P 2 W 17 Add it to a mixed solution of 30 mL of acetonitrile and water ((V / V)=1:2), adjust the pH of the solution to 2, react at room temperature for 6 h, and then pour the reaction solution into a beaker. Then containing 0.84 gNBu 4 Add 5 mL of Br aqueous solution to the above reaction solution, the solution turns white, and viscous precipitates form at the bottom, filter, wash with ethanol and water in sequence, and dry with ether to obtain a white solid powder, which is epoxy-modified tungsten phospholipid Salt P 2 W 17 -EPO; then 0.3 g CS@Fe 3 o 4 Microspheres were added to 30 mL of DMF, N 2 Under protection, add 0.1 g NaOH solid and 0.3 gP 2 W 17 -EPO,N 2 Under protection, raise the temperature to 60 °C, react for 24 h, cool to room temper...

Embodiment 2

[0024] Embodiment 2: the Fc of chitosan modification 3 o 4 Covalent loading of P on magnetic microspheres 2 W 17 Composite catalyst P 2 W 17 -CS@Fe 3 o 4 -1 preparation: the steps are as follows: 256 mg KH-560 and 2.0 g P 2 W 17 Add it to a mixed solution of 40 mL of acetonitrile and water ((V / V)=2:2), adjust the pH of the solution to 3, react at room temperature for 8 h, and then pour the reaction solution into a beaker. Then containing 0.84 gNBu 4 Add 7 mL of Br aqueous solution to the above reaction solution, the solution turns white, and a viscous precipitate forms at the bottom. Then, filter, wash with ethanol and water in sequence, and dry with ether to obtain a white solid powder, which is epoxy-modified Phosphotungstate P 2 W 17 -EPO; then 0.4 g CS@Fe 3 o 4 Microspheres were added to 40 mL of DMF, N 2 Under protection, add 0.2 g Na 2 CO 3 solid and 0.4 g P 2 W 17 -EPO,N 2 Under protection, the temperature was raised to 70 °C, reacted for 25 h, cooled...

Embodiment 3

[0025] Embodiment 3: the Fc of chitosan modification 3o 4 Covalent loading of P on magnetic microspheres 2 W 17 Composite catalyst P 2 W 17 -CS@Fe 3 o 4 -1 preparation: the steps are as follows: 356 mg KH-560 and 3.0 g P 2 W 17 Add it to a mixed solution of 50 mL of acetonitrile and water ((V / V)=2:3), adjust the pH of the solution to 4, react at room temperature for 9 h, and then pour the reaction solution into a beaker. Then containing 0.84 gNBu 4 9 mL of aqueous solution of Br was added to the above reaction solution, the solution turned white, and a viscous precipitate formed at the bottom. Then, it was filtered, washed with ethanol and water in sequence, and dried with ether to obtain a white solid powder, which was epoxy-modified Phosphotungstate P 2 W 17 -EPO. Then 0.5 g CS@Fe 3 o 4 Microspheres were added to 50 mL of DMF, N 2 Under protection, add 0.3 g NaHCO 3 Solid and 0.5 g epoxy-modified phosphotungstate P 2 W 17 -EPO,N 2 Under protection, raise t...

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 technical field of loaded polyoxometallate catalysts, and provides a high-dispersion polyoxometallate magnetic microsphere catalyst, and a preparation method and application thereof so as to overcome the defects that polyoxometallate used as a catalyst is small in specific surface area, few in reaction activity sites, prone to aggregation, soluble in water, difficult to separate and recycle and the like. Dawson type phosphotungstate is loaded onto a CS@Fe3O4 microsphere by a covalent bonding method, and a covalent loaded Dawson type phosphotungstate magnetic microsphere P2W17-CS@Fe3O4-1 is obtained; or, Keggin type phosphotungstate and the Dawson type phosphotungstate are respectively loaded to an organic modified magnetic Fe3O4 microsphere by an electrostaticbonding method, and loaded Keggin type phosphotungstate and loaded Dawson type phosphotungstate are obtained. The dispersity and the specific surface area of the polyoxometallate are improved, the catalytic oxidation activity of the polyoxometallate and the oxidation efficiency of tetrahydrothiophene are improved, and a magnetic carrier provides favorable conditions for catalyst separation and recycling.

Description

technical field [0001] The invention belongs to the technical field of supported polyoxometalate catalysts, and in particular relates to a highly dispersed polyoxometalate magnetic microsphere catalyst and its preparation method and application. The Dawson type polyacid is combined with an electrostatic combination method by covalent bonding. Keggin-type and Dawson-type polyacids were respectively loaded on the organically modified magnetic microsphere carrier. Background technique [0002] Polyoxometalates (POMs) are composed of early transition metals MO x Polyoxometallic coordination clusters are assembled by sharing corners, planes and edges, and have rich topological structures and compositions, which determine their chemical and physical properties, the most prominent of which are catalytic properties, which are widely used in catalysis , medicine, materials chemistry and other fields. As a homogeneous catalyst, it is used in the desulfurization of hydrogen peroxide ...

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): B01J31/18B01J31/06B01J35/08C07D333/48
CPCB01J31/069B01J31/06B01J35/0033B01J27/188B01J35/08C07D333/48Y02P20/584
Inventor 王蕊欣刘叶峰左鹏陈南王飞焦纬洲
Owner ZHONGBEI UNIV
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