Ferric bromide-catalyzed ligand-free photoinduced controllable free radical polymerization method

A light-induced and free radical technology, applied in the field of polymer chemistry, can solve the problems of high temperature and high price of controllable polymerization ligands, and achieve the effects of mild conditions, reduced reaction system components, and simple process

Inactive Publication Date: 2014-07-23
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved in the present invention is that the price of the controllable polymerization ligand is high and the temperature is high, and the serious limitation is to provide a technology using iron bromide as a catalyst to induce controllable free radical polymerization under the premise of no ligand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh 10 g (100 mmol) of methyl methacrylate, 0.5911 g (2 mmol) of ferric bromide, and 0.2642 g of vitamin C (1.5 mmol) into 100 ml of N,N-dimethylformamide In a three-neck flask, magnetically stirred at room temperature, added 0.1538 g (1 mmol) of carbon tetrachloride, filled with nitrogen and exhausted oxygen, and placed in a constant temperature oil bath at 25°C to perform living radical polymerization of methyl methacrylate. After the high-pressure mercury lamp is irradiated for a predetermined time, put the three-neck flask in ice water to cool, then pour the reaction solution into a large amount of methanol, filter to obtain a polymer, then dissolve it in tetrahydrofuran, and pour it into a large amount of methanol again to precipitate , suction filtration, repeated three times, and vacuum drying to obtain the polymer product, polymethyl methacrylate. Its conversion ratio is measured as 68.5% with gravimetric method, and its molecular weight is analyzed by GPC as ...

Embodiment 2

[0016] Weigh 10 g (100 mmol) of methyl methacrylate, 0.5911 g (2 mmol) of ferric bromide, and 0.8806 g of vitamin C (5 mmol) into 100 ml of N,N-dimethylformamide In the three-neck flask, after magnetic stirring at room temperature for a period of time, 0.1538 g (1 mmol) of carbon tetrachloride was added, and placed in a constant temperature oil bath at 25°C to carry out living radical polymerization of methyl methacrylate. After the high-pressure mercury lamp is irradiated for a predetermined time, put the three-neck flask in ice water to cool, then pour the reaction solution into a large amount of methanol, filter to obtain a polymer, then dissolve it in tetrahydrofuran, and pour it into a large amount of methanol again to precipitate , suction filtration, repeated three times, and vacuum drying to obtain the polymer product, polymethyl methacrylate. Its conversion ratio is measured as 62.2% with gravimetric method, and its molecular weight is analyzed by GPC as M n,GPC =115...

Embodiment 3

[0018] Weigh 10 g (100 mmol) of methyl methacrylate, 0.5911 g (2 mmol) of ferric bromide, and 0.2642 g of vitamin C (1.5 mmol) into 100 ml of N,N-dimethylformamide In the three-necked flask, after magnetic stirring at room temperature for a period of time, 0.1538 g (1 mmol) of carbon tetrachloride was added, and placed in a constant temperature oil bath at 25°C for living radical polymerization of methyl methacrylate, nitrogen and oxygen exhausted. After the LED lamp is irradiated for a predetermined time, put the three-necked bottle in ice water to cool, then pour the reaction solution into a large amount of methanol, filter to obtain a polymer, then dissolve it in tetrahydrofuran, and pour it into a large amount of methanol again to precipitate. Suction filtration was repeated three times, and vacuum drying was performed to obtain the polymer product, namely polymethyl methacrylate. Its conversion ratio is measured as 63.4% with gravimetric method, and its molecular weight i...

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Abstract

The invention discloses a photoinduced controllable free radical polymerization method which uses ferric bromide as a catalyst and does not need ligand. The polymerization method comprises the following steps: composing a polymerization system from a monomer, an initiator, ferric bromide, a proper amount of reducing agent and a solvent in a certain mol ratio; and carrying out photoinduced polymerization under an anoxic or aerobic condition at room temperature. A polymer prepared by using the method has controllable activity. The method does not need ligand in the process of polymerization, has reduced polymerization substance components and is a low-cost active polymerization technology.

Description

technical field [0001] The invention relates to the field of macromolecule chemistry, in particular to a method for preparing polymers through ferric bromide catalyzed light-induced controllable free radical polymerization. Suitable for acrylate monomers. Background technique [0002] In 1995, Sawamoto (Polymerization of methyl methacrylate with the carbon tetrachloride / dichlorotris (triphenylphosphine) ruthenium(II) / methylaluminum bis (2, 6-di-tert-butylphenoxide) initiating system: possibility of living radical polymerization, Macromolecules, 2195, , 1721-1723.) and Matyjaszewski (Controlled / “living” radical polymerization in the presence of transition metal cornplexes, J Am Chem Soc, 1995, 117(20): 5614-5615; Controlled / “living” radical polymerization. Halogen atomtransfer radical polymerization promoted by a Cu(I) / Cu(1I) redox process, Macromolecules, 1995, 28(23): 7901-7910) two research groups almost simultaneously reported the use of organic halides as initiators, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F2/48C08F4/40
Inventor 王国祥
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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