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Method for atom transfer radical polymerization by using Fe3O4/BiOI/Cu2O as photoinitiator

A polymerization method and atom transfer technology, applied in the field of photopolymerization, can solve the problems of high energy consumption, high polymerization temperature, difficult removal, etc., and achieve the effects of good reaction controllability, mild reaction temperature and simple process

Inactive Publication Date: 2019-06-04
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the ATRP reaction also has its own shortcomings. First, low-valence metal compounds are easy to oxidize, and most of the complexing agents are expensive; secondly, it is difficult to remove the entire catalytic system after the reaction, and the polymerization temperature is high and energy consumption is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Fe 3 o 4 / BiOI / Cu 2 Synthesis of O

[0030] (1) Fe 3 o 4 preparation of

[0031] Weigh 0.25g ferric chloride (FeCl 3 ·6H 2 O), 1.5g of sodium acetate (NaAC) was added to 15mL of ethylene glycol, and then 6mL of oleic acid was added, stirred in a constant temperature water bath at 50°C for 30min, and the solution was transferred to a reaction kettle for 24h at 180°C. After the product was cooled to room temperature, it was washed several times with absolute ethanol and deionized water, and dried at 70 °C.

[0032] (2) Fe 3 o 4 / Preparation of BiOI

[0033] Weigh 1.925g Bi(NO 3 ) 3 ·5H 2 O and a corresponding amount of Fe 3 o 4 Dissolve it in 20mL of ethylene glycol, and call it solution A, and dissolve 0.662g KI in 30mL of deionized water, and call it solution B. Slowly add solution B to solution A drop by drop, after the addition is complete, adjust the pH to 11, stir for 200 min, transfer to the reaction kettle, and react at 140°C for 24 h. After the ...

Embodiment 2

[0037] Weigh 5g (50mmol) methyl methacrylate monomer, 0.0243g (1mmol) ethyl 2-bromoisobutyrate, 0.0002g (0.01mmol) copper bromide, 0.0052g (0.03mmol) pentamethyldiethylenetri Add the amine into a three-neck flask containing 20ml N,N-dimethylformamide, ultrasonically disperse at room temperature, and add 10mg of Fe 3 o 4 / BiOI / Cu 2 O photocatalyst, filled with nitrogen and exhausted oxygen, placed under visible light irradiation at room temperature for light-induced atom transfer radical polymerization of methyl methacrylate, light irradiation for 48 hours. After the reaction is finished, the target product polymethyl methacrylate is obtained.

[0038] Adopt gravimetric method to measure its conversion rate to be 71.4%, analyze its molecular weight with gel permeation chromatography to be M n,GPC = 10100 g / mol, polymerization dispersity PDI = 1.28.

Embodiment 3

[0040] Weigh 10.6g (200mmol) acrylonitrile monomer, 0.0486g (2mmol) ethyl α-bromophenylacetate, 0.0004g (0.02mmol) copper bromide, 0.0052g (0.03mmol) pentamethyldiethylenetriamine and add In a three-neck flask containing 20ml N,N-dimethylformamide, ultrasonically disperse at room temperature, and add 4mg of Fe 3 o 4 / BiOI / Cu 2 O photocatalyst, filled with nitrogen and exhausted oxygen, and irradiated with LED lamps that can emit visible light for 24 hours at room temperature. Filter, add a poor solvent until the polymer precipitates, and filter to obtain the target product polyacrylonitrile.

[0041] Adopt gravimetric method to measure its conversion rate to be 64.3%, analyze its molecular weight with gel permeation chromatography to be M n,GPC = 7400 g / mol, polymerization dispersity PDI = 1.27.

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PUM

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Abstract

The invention discloses a Fe3O4 / BiOI / Cu2O photoinitiator and an atom transfer radical polymerization method applying the Fe3O4 / BiOI / Cu2O photoinitiator in atom transfer radical polymerization. The Fe3O4 / BiOI / Cu2O has wide-range visible-light responsiveness, and visible light can be effectively utilized for atom transfer radical polymerization; and the Fe3O4 / BiOI / Cu2O has magnetic separability. Byusing the photoinitiator, room-temperature atom transfer radical polymerization can be carried out at irradiation of wide wavelength range. The method has good reaction controllability (polymer molecular weight distribution PDI (1.5)). In addition, the catalyst can be magnetically separated, is simple to operate, and is low-cost.

Description

technical field [0001] The invention belongs to the technical field of photopolymerization, and relates to a Fe / BiOI type photoinitiator atom transfer radical polymerization method under room temperature and visible light irradiation conditions, in particular to a Fe 3 o 4 / BiOI / Cu 2 O photoinitiators and their application in atom transfer radical polymerization. Background technique [0002] Atom Transfer Radical Polymerization (ATRP) uses simple organic halides as initiators and transition metal complexes as halogen atom carriers to establish reversible dynamics between active species and dormant species through redox reactions. Equilibrium, so as to realize the control of the polymerization reaction. Compared with other living polymerizations, ATRP has the advantages of a wide range of applicable monomers, mild polymerization conditions, and easy industrialization. Since the birth of this technology in 1995, it has aroused great interest in academia and industry. As ...

Claims

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Application Information

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IPC IPC(8): C08F2/48C08F120/14C08F120/44C08F120/56C08F220/14C08F220/56
Inventor 王国祥梁恩湘
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY