Controllable free-radical polymerization method by using organic-inorganic composite material as photoinitiator

A photoinitiator and initiator technology, applied in the field of polymer chemistry, can solve problems such as corrosion, achieve the effect of reducing the dosage and increasing the polymerization reaction rate

Inactive Publication Date: 2015-09-16
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, strong acid and strong alkali have certain corrosion on zinc oxide / titanium dioxide composite materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Weigh 1.5 g (150 mmol) of methyl methacrylate, 0.027 g (1 mmol) of ferric chloride hexahydrate, 0.0787 g (3 mmol) of triphenylphosphine, and 20 mg of polyaniline / zinc oxide / titanium dioxide into 30 ml PEG-400 three-necked flask, ultrasonically disperse at room temperature for a period of time, add 0.0195 g (1 mmol) ethyl 2-bromoisobutyrate, fill with nitrogen to replace the oxygen in the three-necked flask, and plug the bottle tightly with a stopper. Then place it in a constant temperature water bath, irradiate with a 500 W high-pressure mercury lamp, and react for 1.5 hours. After the reaction was completed, the reaction mixture solution was poured into methanol, suction filtered, vacuum-dried, and repeated three times to obtain pure polymethyl methacrylate. Adopt gravimetric method to measure its conversion rate to be 52.4%, analyze its molecular weight with gel permeation chromatography to be M n,GPC =9300 g / mol, polymerization dispersion PDI=1.33.

Embodiment 2

[0011] Weigh 1.5 g (150 mmol) of methyl methacrylate, 0.027 g (1 mmol) of ferric chloride hexahydrate, and 0.0787 g (3 mmol) of triphenylphosphine into a three-necked flask containing 30 ml of PEG-400. After ultrasonic dispersion for a period of time, add 0.0195 g (1 mmol) ethyl 2-bromoisobutyrate, fill with nitrogen to replace the oxygen in the three-necked bottle, and seal the bottle with a stopper. Then place it in a constant temperature water bath, irradiate with a 500 W high-pressure mercury lamp, and react for 1.5 hours. Adopt gravimetric method to measure its conversion rate to be 0.

Embodiment 3

[0013] Weigh 1.5 g (150 mmol) of methyl methacrylate, 0.027 g (1 mmol) of ferric chloride hexahydrate, 0.0787 g (3 mmol) of triphenylphosphine, and 30 mg of polyaniline / zinc oxide / titanium dioxide into 30 ml PEG-400 three-necked flask, ultrasonically disperse at room temperature for a period of time, add 0.0195 g (1 mmol) ethyl 2-bromoisobutyrate, fill with nitrogen to replace the oxygen in the three-necked flask, and plug the bottle tightly with a stopper. Then place it in a constant temperature water bath, irradiate with a 500 W high-pressure mercury lamp, and react for 1.5 hours. After the reaction was completed, the reaction mixture solution was poured into methanol, suction filtered, vacuum-dried, and repeated three times to obtain pure polymethyl methacrylate. Measure its conversion rate by gravimetric method to be 61.6%, analyze its molecular weight with gel permeation chromatography to be M n,GPC =11100 g / mol, polymerization dispersion PDI=1.31.

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PUM

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Abstract

The invention relates to an initiator for atom transfer free-radical polymerization and application thereof. The initiator uses an organic-inorganic composite material as the atom transfer free-radical polymerization photoinitiator. The photoinitiator performs photo-control atom transfer free-radical polymerization on monomers for atom transfer free-radical polymerization, an atom free-radical initiator, a catalyst and a ligand at room temperature. The reaction has the characteristic of active polymerization. The method can perform atom transfer free-radical reaction under ultraviolet irradiation, and can also perform atom transfer free-radical reaction under visible light irradiation. The method obviously lowers the catalyst consumption. The photoinitiator is recyclable, and has the advantages of simple technique, environment friendliness and the like.

Description

technical field [0001] The invention belongs to the field of macromolecular chemistry, and in particular relates to a method for preparing a polymer by using an organic-inorganic composite material as a photoinitiator by a controllable radical polymerization method. Background technique [0002] Atom transfer radical polymerization (ATRP) is achieved by using the reversible redox effect of transition metals. ATRP is one of the most effective "living" free radical polymerization methods for the synthesis of high molecular compounds with well-defined chemical composition and structure. In 1995, Matyjaszewski [Controlled / living radical polymerization. atom transfer radical polymerization in the presence of transition-metal complexes, J Am Chem Soc, 1995, 117, 5614-5615.] and Sawamoto [Polymerization of methyl methacrylate with the carbon tetrachloride dichlorotris (triphenylphosphine)ruthenium(II) / Methylaluminum Bis (2, 6-di-tert-butylphenoxide) initiating system: possibili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F112/08C08F2/46
Inventor 王国祥
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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