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Preparation method of a magnetic nano-interface catalyst with adjustable tempo loading

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: 2019-10-29
ZHEJIANG UNIV OF TECH
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  • 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

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  • Preparation method of a magnetic nano-interface catalyst with adjustable tempo loading
  • Preparation method of a magnetic nano-interface catalyst with adjustable tempo loading
  • Preparation method of a magnetic nano-interface catalyst with adjustable tempo loading

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Preparation of Nanomagnetic Microspheres (II)

[0027] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 90 mL of xylene to give a clear and transparent solution. FeCl 2 ·4H 2 O (1.2 g, 6 mmol) and Fe (NO 3 ) 3 ·9H 2 O (4.85 g, 12 mmol) was dissolved in 5.4 mL of deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecyl benzene sulfonate under stirring, and stirred overnight with nitrogen for 1 h. , forming a homogeneous and stable inverse micellar emulsion. Then, the reverse micelle emulsion was heated to 70°C and kept for 3 hours. After adding 6mL of 34wt% hydrazine hydrate solution and reacting for 1 hour, the emulsion system turned black. The temperature was lowered to 30°C, and tetraethyl silicate (6 mL) and methacryloyloxypropyltrimethoxysilane (15 mL) were added for hydrolysis for 24 h. After the reaction, the emulsion was first broken with anhydrous ethanol, t...

Embodiment 2

[0029] Example 2: Preparation of Nanomagnetic Microspheres (II)

[0030] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 90 mL of xylene to give a clear and transparent solution. FeCl 2 ·4H 2 O (1.2 g, 6 mmol) and Fe (NO 3 ) 3 ·9H 2 O (4.85 g, 12 mmol) was dissolved in 5.4 mL of deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecyl benzene sulfonate under stirring, and stirred overnight with nitrogen for 1 h. , forming a homogeneous and stable inverse micellar emulsion. Then the reverse micelle emulsion was heated to 90° C. and kept for 1 hour. After adding 6 mL of 34 wt % hydrazine hydrate solution and reacting for 3 hours, the emulsion system turned black. The temperature was lowered to 40° C., and tetraethyl silicate (6 mL) and methacryloyloxypropyltrimethoxysilane (15 mL) were added for hydrolysis for 24 h. After the reaction, the emulsion was first broken with anhydrous etha...

Embodiment 3

[0032] Example 3: Preparation of Nanomagnetic Microspheres (II)

[0033] Sodium dodecylbenzenesulfonate (10.5 g, 30 mmol) was ultrasonically dispersed in 111.5 mL of xylene to give a clear and transparent solution. FeCl 2 ·4H 2 O (2.4 g, 12 mmol) and Fe (NO 3 ) 3 ·9H 2 O (9.7 g, 24 mmol) was dissolved in 5.4 mL of deionized water to form an iron salt solution, which was added dropwise to the xylene solution of sodium dodecyl benzene sulfonate under stirring, and stirred overnight with nitrogen for 1 h. , forming a homogeneous and stable inverse micellar emulsion. Then the reverse micelle emulsion was heated to 90° C. and kept for 1 h. After adding 6 mL of 34 wt% hydrazine hydrate solution, the reaction was performed for 3 h, and the emulsion system turned black. The temperature was lowered to 40° C., and tetraethyl silicate (16 mL) and methacryloyloxypropyltrimethoxysilane (43 mL) were added for hydrolysis for 48 h. After the reaction, the emulsion was first broken with...

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Abstract

The invention discloses a magnetic nano-interface catalyst (Ⅰ) with adjustable TEMPO loading capacity. Its preparation method is: (1) adding nano-magnetic microspheres (Ⅱ) and 2-methyl-2-acrylic acid- 2,2,6,6-tetramethyl-4-piperidinyl ester (III), divinylbenzene and solvent acetonitrile were reacted at 90-100°C for 2-4 hours under nitrogen protection. After the reaction, the reaction solution was After post-processing, nanomagnetic microspheres (IV) coated with poly-2-methyl-2-acrylate-2,2,6,6-tetramethyl-4-piperidinyl ester were obtained; the nanomagnetic microspheres (IV) were ) is oxidized to the target catalyst (Ⅰ) by two methods: (2) adding surface-coated poly-2-methyl-2-acrylic acid-2,2,6,6-tetramethyl-4-piper in the reaction vessel Nanomagnetic microspheres of pyridyl ester (IV), sodium tungstate, ethylenediaminetetraacetic acid and solvent tetrahydrofuran, then add hydrogen peroxide, react at 50-60°C for 12-24 hours, after the reaction is completed, the reaction solution is magnetically separated to obtain a solid After washing and drying, the target catalyst (I) was obtained.

Description

technical field [0001] The invention belongs to the technical field of catalysts and preparations thereof, and in particular relates to a preparation method of a magnetic nano-interface catalyst with adjustable TEMPO loading. Background technique [0002] The selective oxidation of alcohols to corresponding aldehydes and ketones is one of the most important functional group conversion reactions in basic research and industrial production (ACS Catalysis, 2015, 5(3): 1556–1559.). In traditional production processes, most alcohol oxidation processes involve expensive and highly toxic oxidants, such as chromium reagents, manganese reagents and other transition metal oxides, 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 nitroxide radical (TEMPO) i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J35/08
CPCB01J31/06B01J35/33B01J35/51
Inventor 王建黎汤骏张祺
Owner ZHEJIANG UNIV OF TECH
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