Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method of TEMPO load adjustable magnetic nanometer interface catalyst

A magnetic nanometer, loading technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. Difficult to control, complex catalyst synthesis methods, etc., to achieve the effect of simple operation

Active Publication Date: 2017-06-30
ZHEJIANG UNIV OF TECH
View PDF5 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst synthesis method is complicated, and the TEMPO loading is limited by the content of chloromethyl active groups on the surface of the nanoparticles, which is difficult to control.

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
  • Preparation method of TEMPO load adjustable magnetic nanometer interface catalyst
  • Preparation method of TEMPO load adjustable magnetic nanometer interface catalyst
  • Preparation method of TEMPO load adjustable magnetic nanometer interface catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the preparation of nano magnetic microsphere (Ⅱ)

[0027] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 90 mL of xylene to obtain a clear and transparent solution. FeCl 2 4H 2 O (1.2g, 6mmol) and Fe (NO 3 ) 3 9H 2 O (4.85g, 12mmol) was dissolved in 5.4mL deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecylbenzenesulfonate under stirring, and stirred overnight after passing nitrogen gas for 1h , forming a uniform and stable inverse micellar emulsion. Then the temperature of the reverse micellar emulsion was raised to 70° C. and kept for 3 hours. After adding 6 mL of 34 wt % hydrazine hydrate solution, it was reacted for 1 hour, and the emulsion system turned black. Cool down to 30°C, add tetraethyl silicate (6 mL) and methacryloxypropyltrimethoxysilane (15 mL) for hydrolysis for 24 h. After the reaction, the emulsion was first demulsified with absolute etha...

Embodiment 2

[0029] Embodiment 2: the preparation of nano magnetic microsphere (II)

[0030] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 90 mL of xylene to obtain a clear and transparent solution. FeCl 2 4H 2 O (1.2g, 6mmol) and Fe (NO 3 ) 3 9H 2 O (4.85g, 12mmol) was dissolved in 5.4mL deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecylbenzenesulfonate under stirring, and stirred overnight after passing nitrogen gas for 1h , forming a uniform and stable inverse micellar emulsion. Then the temperature of the reverse micellar emulsion was raised to 90° C. and kept for 1 hour. After adding 6 mL of 34 wt % hydrazine hydrate solution, it was reacted for 3 hours, and the emulsion system turned black. Cool down to 40°C, add tetraethyl silicate (6 mL) and methacryloxypropyltrimethoxysilane (15 mL) for hydrolysis for 24 h. After the reaction, the emulsion was first demulsified with absolute eth...

Embodiment 3

[0032] Embodiment 3: the preparation of nano magnetic microsphere (II)

[0033] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 111.5 mL of xylene to obtain a clear and transparent solution. FeCl 2 4H 2 O (2.4g, 12mmol) and Fe(NO 3 ) 3 9H 2 O (9.7g, 24mmol) was dissolved in 5.4mL deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecylbenzenesulfonate under stirring, and stirred overnight after 1h of nitrogen gas , forming a uniform and stable inverse micellar emulsion. Then the temperature of the reverse micellar emulsion was raised to 90° C. and kept for 1 hour. After adding 6 mL of 34 wt % hydrazine hydrate solution, it was reacted for 3 hours, and the emulsion system turned black. Cool down to 40°C, add tetraethyl silicate (16 mL) and methacryloxypropyltrimethoxysilane (43 mL) for hydrolysis for 48 h. After the reaction, the emulsion was first demulsified with absolute ethanol, ...

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 discloses a TEMPO load adjustable magnetic nanometer interface catalyst (I). A preparation method of the TEMPO load adjustable magnetic nanometer interface catalyst (I) comprises the following steps: (1) adding a nano-magnetic microsphere (II), 2-methyl-2-crylic acid-2,2,6,6-tetramethyl-4-piperidyl ester (III), divinyl benzene and a solvent acetonitrile into a reaction container, reacting at the temperature of 90-100 DEG C for 2-4 hours under the protection of nitrogen gas, post-processing a reaction liquid after the reaction to obtain a nano-magnetic microsphere (IV) with the surface coated with the 2-methyl-2-crylic acid-2,2,6,6-tetramethyl-4-piperidyl ester; oxidizing the nano-magnetic microsphere (IV) into the target catalyst (I) through two methods: (2) adding the nano-magnetic microsphere (IV) with the surface coated with the 2-methyl-2-crylic acid-2,2,6,6-tetramethyl-4-piperidyl ester, sodium tungstate, ethylenediamine tetraacetic acid and a solvent tetrahydrofuran into the reaction container, adding hydrogen peroxide, reacting at the temperature of 50-60 DEG C for 12-24 hours, magnetically separating a reaction liquid after the reaction to obtain a solid, washing, and drying the solid to obtain the target catalyst (I) (Refer to Specification).

Description

technical field [0001] The invention belongs to the technical field of catalysts and their preparation, and in particular relates to a preparation method of a magnetic nano-interface catalyst whose loading capacity of TEMPO can be adjusted. Background technique [0002] In basic research and industrial production, the selective oxidation of alcohols to corresponding aldehydes and ketones is one of the very important functional group conversion reactions (ACS Catalysis, 2015, 5(3):1556–1559.). In the traditional production process, most alcohol oxidation processes involve expensive and highly toxic oxidants, such as chromium reagents, manganese reagents and other transition metal oxides, etc., and the products are easily over-oxidized into acids, resulting in reduced selectivity . Therefore, the development of green and efficient alcohol oxidation methods has important economic and social value. [0003] In recent years, the application of 2,2,6,6-tetramethylpiperidine nitr...

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): B01J31/06B01J35/08
CPCB01J31/06B01J35/33B01J35/51
Inventor 王建黎汤骏张祺
Owner ZHEJIANG UNIV OF TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com