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Atom transition free radical polymerization initiation system and application of the same for preparing macromolecular compound

A high molecular compound, polymerization initiation technology, applied in the application of the preparation of high molecular compounds, AGETATRP atom transfer radical polymerization initiation system field, can solve the problems of amine ligand toxicity, affect active polymerization, large amount of catalyst, etc., to avoid The effect of toxicity, overcoming high temperature polymerization, and low synthesis cost

Inactive Publication Date: 2007-09-12
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the ATRP system of ionic liquid and reverse polymerization has been adopted, it also has defects: because the polymerization rate is related to the amount of catalyst and ligand, in order to reach a suitable polymerization rate, the amount of catalyst used in the polymerization system is relatively large (1: 100 ); the amine ligands added to the polymerization system are toxic; the PF in the currently used ionic liquid 6 - The price is more expensive; in reverse ATRP, the free radical generated by the azo free radical initiator itself is an active group, which affects the conditions of active polymerization

Method used

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  • Atom transition free radical polymerization initiation system and application of the same for preparing macromolecular compound
  • Atom transition free radical polymerization initiation system and application of the same for preparing macromolecular compound

Examples

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Effect test

Embodiment 1

[0034] Embodiment 1: Methylimidazole acetate ionic liquid ([Hmim][CH 3 AGET Atom Transfer Radical Polymerization of Methyl Methacrylate (MMA) in COO])

[0035] Weigh the catalyst CuBr 2 (copper bromide) 1 part, 0.5 part of reducing agent hydroquinone in 600 parts of [Hmim][CH 3 COO] (methylimidazolium formate) dissolved in the ionic liquid, nitrogen in addition to oxygen. Weigh 600 parts of MMA (methyl methacrylate) monomer, pass nitrogen to remove oxygen, add to ionic liquid, continue to pass nitrogen to remove oxygen, seal, keep the temperature at 60°C for 20 minutes, inject 1 part of 2-bromo Ethyl isobutyrate initiator, constant temperature reaction at 60°C. After three hours, the polymerization liquid was treated with methanol to obtain PMMA (polymethyl methacrylate), Mn=36700, PDI=1.30.

Embodiment 2

[0036] Embodiment 2: Methylimidazole acetate ([Hmim][CH 3 AGET Atom Transfer Radical Polymerization of Methyl Methacrylate (MMA) in COO]) Ionic Liquid

[0037] Weigh the catalyst CuBr 2 1 part, reducing agent hydroquinone 0.5 part in 100 parts of [Hmim][CH 3 COO] dissolved in the ionic liquid, nitrogen in addition to oxygen. Take by weighing 100 parts of MMA monomer, after passing nitrogen to remove oxygen, add in the ionic liquid, continue to pass nitrogen to remove oxygen, seal, keep the temperature at 60 ℃ for 20 minutes, inject 3 parts of initiator 2-bromoisobutyrate ethyl ( (CH 3 ) 2 CBrCOOC 2 h 5 ), react at a constant temperature of 60°C. Two hours later, the reaction conversion rate was 92%. The polymerization solution was treated with aqueous methanol to obtain PMMA with Mn=7200 and PDI=1.17.

Embodiment 3

[0038] Embodiment 3: Methylimidazole acetate ([Hmim][CH 3 COO]) AGET Atom Transfer Radical Polymerization of Methyl Methacrylate (MMA) in Ionic Liquid

[0039] Weigh 1 part of catalyst CuBr 2 , 0.5 parts of reducing agent hydroquinone in 100 parts of [Hmim][CH 3 Dissolve in COO] ionic liquid, take by weighing 100 parts of MMA monomer, add in the ionic liquid, keep the temperature at 60 ℃ for 20 minutes, inject 3 parts of initiator 2-bromoisobutyric acid ethyl ester ((CH 3 ) 2 CBrCOOC 2 h 5 ), constant temperature reaction at 60°C. Two hours later, the reaction conversion rate was 87.4%, and the polymerization solution was treated with aqueous methanol, resulting in PMMA with Mn=7500 and PDI=1.16, and oxygen had no effect on the polymerization.

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Abstract

This invention relates to an atom transfer radical polymerization initiating system and its application in the preparation of polymers. The technical problem it needs to solve is to provide an initiating system with less catalyst, cost and environmental pollution. The method is characterized with the general formula [Hmim][RCOO] / PX / hydroquinone / MX1n, in which, [Hmim][RCOO] is methylimidazol organic acid salt ion liquid and R is alkyl, PX is a initiator with R1 of alkyl and X of halogen, catalyst MX1n is tall-price transition metal mineral salt, hydroquinone is a reductor, and oxygen has no effect on the polymerization system. The polymerization polymer of a monomer prepared from reaction of the above system and the monomers can react with different shapes of initiator obtaining linear, stellate and other polymers.

Description

technical field [0001] The present invention relates to the field of polymer compounds, in particular to an AGET (activator generated by electron transfer) ATRP atom transfer radical polymerization initiation system using novel ionic liquids and hydroquinone as reducing agents and its application in the preparation of polymer compounds . Background technique [0002] In 1995, Wang Jinshan first reported in J.Am.chem.Soc., 1995,117,5614 in the atomic group transfer radical polymerization (abbreviated ATRP) initiation system, as initiator is alkyl halide hydrocarbon R-X, wherein X is Cl and Br, and R is an organic group with conjugation inducing effect. In the first-generation ATRP initiation system, CuX and organic ligands are mainly used as catalysts. Anbo and Granel (Macromolecules, 1996, 29: 8576, 1074) used Ru and Ni complexes such as RuCl 2 (pph 3 ) / Al(OR) 3 , Ni(NCN)Br, Ni[O, 0'(CH 2 NMe 2 ) 2 C 6 H] Br, as the catalyst and the alkyl halide hydrocarbon initiator...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/00C08F4/50C08F4/80C08F297/00
Inventor 来国桥胡自强邱化玉李文清齐帆许文东
Owner HANGZHOU NORMAL UNIVERSITY
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