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Polymerization system for atom transfer radical polymerization (ATRP) using activators generated by electron transfer (AGET)

An electron transfer and atom transfer technology, applied in the field of atom transfer radical polymerization, can solve the problems of large difference between theoretical molecular weight and actual molecular weight of polymerization reaction rate, low catalytic activity, etc., to facilitate industrial production, improve polymerization rate, and reduce toxicity. Effect

Inactive Publication Date: 2010-07-07
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the research process, we found that the overall catalytic activity of AGETATRP catalyzed by the iron salt system to polar monomers such as methacrylates was not high, and the theoretical molecular weight and actual molecular weight of the obtained polymer were quite different, and the polymerization reaction rate was still low. to be further improved

Method used

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  • Polymerization system for atom transfer radical polymerization (ATRP) using activators generated by electron transfer (AGET)
  • Polymerization system for atom transfer radical polymerization (ATRP) using activators generated by electron transfer (AGET)
  • Polymerization system for atom transfer radical polymerization (ATRP) using activators generated by electron transfer (AGET)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Synthesis of polystyrene (PS) with TBABr as a ligand (add alkali)

[0040] According to the ratio n(St): n(PEBr): n(FeCl 3 .6H 2 O):n(TBABr):n(VC):n(NaOH)=250:1:1~3:1~6:2:1~3, add FeCl in turn 3 .6H 2 O, TBABr, NaOH, St (2 mL), PEBr, and VC were placed in a 5 mL ampoule. After nitrogen was introduced for 15 minutes, the tube was sealed under an oxygen-free atmosphere (bulk polymerization). Place the sealed ampoule in an oil bath at a constant temperature (110°C) for a predetermined time to react. After the reaction is over, take out the sealed tube, immediately cool it with cold water, open the sealed tube, dissolve it with 2~5mL of tetrahydrofuran, pour it into 250mL of methanol, leave it overnight, suction filtration, wash with water, and dry to obtain "active" polymer. Styrene.

Embodiment 2

[0041] Example 2: Synthesis of polystyrene (PS) with TBABr as a ligand (no alkali added)

[0042] According to the ratio n(St): n(PEBr): n(FeCl 3 .6H 2 O): n(TBABr): n(VC)=250:1:1~3:1~6∶2, add FeCl in turn 3 .6H 2 O, TBABr, St (2 mL), PEBr, and VC were placed in a 5 mL ampoule, and the tube was sealed under an oxygen-free atmosphere (bulk polymerization) after nitrogen gas was introduced for 15 minutes. Place the sealed ampoule in an oil bath at a constant temperature (110°C) for a predetermined time to react. After the reaction is over, take out the sealed tube, immediately cool it with cold water, open the sealed tube, dissolve it with 2~5mL of tetrahydrofuran, pour it into 250mL of methanol, leave it overnight, suction filtration, wash with water, and dry to obtain "active" polymer. Styrene.

[0043] figure 1 The AGET ATRP reaction kinetics (comparison with or without alkali) of styrene catalyzed by the iron salt of TBABr as the ligand in Example 1 and Example 2.

[0044] Polyme...

Embodiment 3

[0048] Example 3: Synthesis of PS prepared with TBPBr as ligand (add alkali, add THF)

[0049] According to the ratio n(St): n(PEBr): n(FeCl 3 .6H 2 O):n(TBPBr):n(VC):n(NaOH)=250:1:1:2:2:2, add FeCl in turn 3 .6H 2 O, TBABr, NaOH, St (2 mL), PEBr, and VC were placed in a 5 mL ampoule. After nitrogen was introduced for 15 minutes, the tube was sealed under an oxygen-free atmosphere (bulk polymerization). Solution polymerization: Add 2mL THF to the system and vent the oxygen with nitrogen, then seal the tube for solution polymerization. Place the sealed ampoule in an oil bath at a constant temperature (110°C) for a predetermined time to react. After the reaction is over, take out the sealed tube, immediately cool it with cold water, open the sealed tube, dissolve it with 2-5ml of tetrahydrofuran, pour it into 250mL of methanol overnight, and then filter, wash with water and dry to obtain "active" polystyrene Vinyl.

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Abstract

The invention discloses a polymerization system for atom transfer radical polymerization (ATRP) using activators generated by electron transfer (AGET), comprising radical polymerization monomers, initiator, coordination agent, catalyst and reducer. The invention is characterized in that the polymerization system still comprises alkaline; the components are proportioned in mol as that monomers: initiator: alkaline equals to 100-1000: 1: 1-5; the catalyst is selected from Iron(III) chloride hexahydrate or iron bromide; and the alkaline is selected from one of sodium hydroxide (NaOH), sodium bicarbonate and ferric hydroxide (Fe (OH) 3). Because the alkaline with the same dose of the catalyst is added into the AGET ATRP polymerization system, the polymerization reaction rate is improved, a polymer with high percent conversion can be generated in a short time and the control performance of polymerization reaction is improved.

Description

Technical field [0001] The invention relates to an atom transfer radical polymerization method, in particular to an atom transfer radical polymerization (activators generated by electron transfer ATRP, AGET ATRP) polymerization system and application thereof. Background technique [0002] Free radical polymerization was developed in the 1950s and has become an important technology for industrial production of polymer products. However, although ordinary free radical polymerization is simple to operate, it has important defects such as poor molecular design ability and difficult control of polymer molecular weight and distribution, making it impossible to synthesize functional polymers with high performance and complex structure. The atom transfer radical polymerization (ATRP) proposed in 1995 is a new living / controllable free radical polymerization technology that integrates ordinary free radical polymerization and living polymerization. Compared with other living polymerization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/02C08F2/06C08F4/26C08F112/08C08F120/14
Inventor 程振平柏良久朱秀林张丽芬张正彪周年琛朱建张伟
Owner SUZHOU UNIV
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