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Preparation method of polymer brush supported 2,2,6,6-tetramethylpiperidine-n-oxygen free radical catalyst system

A technology of tetramethylpiperidine and polymer brush, which is applied in the field of preparation of polymer brush-loaded TEMPO catalytic system

Active Publication Date: 2016-04-13
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the study of loading organic small molecule catalyst TEMPO on polymer brushes in the form of covalent bonds has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 1. Surface triggering ARGETATRP to prepare TMPM homopolymer brush.

[0018] 1) Under the protection of nitrogen, put 27g styrene, 8g divinylbenzene, 540g deionized water, 0.0545gNaOH, 0.0545gNaHCO into a 1000ml glass reactor with condenser, thermometer and mechanical stirrer 3 . Under nitrogen protection, after the temperature of the system reaches 70°C, 0.54 g of initiator potassium persulfate is added to react for 2 hours. Then add 2.7g HEMA and react for 3 hours, take out the reaction solution, centrifuge and dry to obtain 21.2g hydroxylated cross-linked PS balls.

[0019] 2) Under nitrogen protection, add 10.8 g of the above-mentioned hydroxylated cross-linked PS microspheres and 50 ml of solvent DMF to a 100 ml three-neck flask equipped with a thermometer, a constant pressure separating funnel and a magnetic stirring rotor, and dissolve 3.3 ml of 2-bromoisobutyl The acid bromide was dissolved in 10ml of DMF and added to an isobaric separatory funnel, an...

Embodiment 2

[0024] Example 2 1. Surface-initiated ARGETATRP to prepare MMA-TMPM random copolymer brushes.

[0025] 1) Under nitrogen protection, put 36g styrene, 4g divinylbenzene, 540g deionized water, 0.0545gNaOH, 0.0545gNaHCO into a 1000ml glass reactor with condenser, thermometer and mechanical stirrer 3 . After the temperature of the system reached 70°C, 0.54 g of potassium persulfate as an initiator was added to react for 2 hours. Then add 3.6g HEMA and react for 5 hours, take out the reaction solution, centrifuge and dry to obtain 28.6g hydroxylated cross-linked PS balls.

[0026] 2) Under nitrogen protection, add 10.8 g of the above-mentioned hydroxylated cross-linked PS microspheres and 50 ml of solvent DMF to a 100 ml three-neck flask equipped with a thermometer, a constant pressure separating funnel and a magnetic stirring rotor, and dissolve 3.3 ml of 2-bromoisobutyl The acid bromide was dissolved in 10ml of DMF and added to an isobaric separatory funnel, and the addition wa...

Embodiment 3

[0031] Example 3 1. Surface-initiated ARGETATRP to prepare MMA-TMPM block copolymer brushes.

[0032] 1) Under the protection of nitrogen, put 27g styrene, 8g divinylbenzene, 540g deionized water, 0.0545gNaOH, 0.0545gNaHCO into a 1000ml glass reactor with condenser, thermometer and mechanical stirrer 3 . After the system temperature reached 80°C, 0.27 g of potassium persulfate as an initiator was added to react for 5 hours. After adding 3.6g HEMA to react for 3 hours, the reaction solution was taken out, centrifuged and dried to obtain 20.3g hydroxylated cross-linked PS balls.

[0033] 2) Under the protection of nitrogen, add 10.8 g of the above-mentioned hydroxylated cross-linked PS microspheres and 50 ml of solvent DMF to a 100 ml three-necked flask equipped with a thermometer, a constant pressure separating funnel and a magnetic stirring rotor, feed N2, and dissolve 3.3 ml2 -Bromoisobutyryl bromide was dissolved in 10ml of DMF and added to an isobaric separatory funnel, a...

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PUM

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Abstract

The invention relates to a preparation method for a polymer brush supported TEMPO catalyst system. Specifically, the method includes the steps of: 1) conducting soap-free emulsion polymerization to prepare a surface hydroxylated crosslinked polystyrene (PS) microsphere; 2) loading an ATRP initiator to the PS microsphere surface through O-acylation reaction of 2-bromoisobutyryl bromide and hydroxyl; 3) taking the PS microsphere as a macroinitiator, grafting a structure controllable polymer brush containing methacrylic acid-2, 2, 6, 6-tetramethyl-4-piperidyl ester (TMPM) to the microsphere surface through an ARGETATRP technology; and 4) oxidizing the piperidyl of TMPM into free radical of nitroxide by m-chloroperoxybenzoic acid (mCPBA) so as to load the TEMPO to the polymer brush in the form of a covalent bond. The polymer brush supported TEMPO catalyst system can employ O2 as the oxidizing agent to efficiently catalyze the selective oxidation reaction of alcohol, is convenient to recycle, and can maintain catalytic performance basically unchanged after 5 times of recycling.

Description

technical field [0001] The invention relates to a method for preparing a polymer brush-loaded TEMPO catalytic system, specifically, a polymer brush with a controllable structure is prepared by surface-initiated ARGETATRP, and TEMPO is loaded on it to prepare a load with controllable quantity and position of TEMPO loads catalytic system. Background technique [0002] 2,2,6,6-Tetramethylpiperidine-N-oxyl radical (TEMPO) is a stable N-oxyl radical, which catalyzes the oxidation reaction of alcohols under mild conditions, simple operation, and cheap and easy-to-obtain oxidants. The reaction is fast, and the selectivity of aldehydes or ketones is close to quantitative, and has been successfully applied in industrial production. However, the price of TEMPO is high, and it is difficult to recover after the reaction, which is the bottleneck of the wide application of TEMPO catalytic alcohol oxidation reaction. [0003] It has been an important direction in this field to load TEMPO...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J31/30C08F257/02C08F293/00C07C45/38C07C47/54
Inventor 刘少杰李配欣赵风清张志国
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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