Method for realizing controllable free radical polymerization in air atmosphere and application thereof

A free radical and polymerization reaction technology, applied in the field of polymer synthesis, can solve the problems of long polymerization induction period, cumbersome experimental operation, limited oxygen tolerance and controllable free radical polymerization application field, and achieve high-throughput optimization of polymerization conditions, High monomer conversion rate, fast and efficient polymerization reaction

Active Publication Date: 2022-03-08
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these oxygen-tolerant controlled free radical polymerizations can be carried out in the presence of air to a certain extent, there are also problems such as the need to react in a closed container, the polymerization induction period is long, and the need to introduce additional chemical Reagents and experimental operations are relatively cumbersome and other shortcomings, limiting the application field of oxygen tolerance controlled free radical polymerization

Method used

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  • Method for realizing controllable free radical polymerization in air atmosphere and application thereof
  • Method for realizing controllable free radical polymerization in air atmosphere and application thereof
  • Method for realizing controllable free radical polymerization in air atmosphere and application thereof

Examples

Experimental program
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preparation example Construction

[0050] (1) Preparation of the mixed solution: dissolving the functional monomer, the reversible addition-fragmentation chain transfer reagent and the alkylboramine complex in a solvent and mixing to obtain the mixed solution;

[0051] (2) Polymerization reaction: heating the mixed liquid obtained in step (1), the alkyl boron amine complex releases the alkyl boron compound, the alkyl boron compound autoxidizes to generate an alkyl radical, and the alkyl free radical initiates functional Monomer polymerization forms growth free radicals, and the growth free radicals undergo degeneration transfer with reversible addition-fragmentation chain transfer reagents to realize controllable free radical polymerization;

[0052] (3) After the polymerization reaction is finished, the temperature is lowered to obtain a polymer with controllable molecular weight, narrow molecular weight distribution and active end groups;

[0053] The whole process is completely exposed to the air.

[0054] ...

Embodiment 1

[0074] This embodiment provides triethylboron-4-dimethylaminopyridine complex (Et 3 B-DMAP) preparation, chemical equation is as follows:

[0075]

[0076] In a 50 mL reaction flask, under N 2 Add triethylboron tetrahydrofuran solution (10 mL, 1 mol / L) under the protection of . The above reaction flask was placed in an ice-water bath, and then 2 Slowly add 1.22 g of 4-dimethylaminopyridine (10 mmol) in batches in the atmosphere, continue to react in the ice-water bath for 10 minutes, then remove the ice-water bath, and react at room temperature for 1 hour. After the reaction was completed, the solvent tetrahydrofuran was removed by rotary evaporation under reduced pressure to obtain 2.02 g of white crystals with a yield of 92%. 1 H-NMR nuclear magnetic spectrum analysis is triethylboron-4-dimethylaminopyridine complex (Et 3 B-DMAP).

Embodiment 2

[0078] This embodiment provides triethylboron-4-methoxypyridine complex (Et 3 B-4MeO-Py) preparation, chemical equation is as follows:

[0079]

[0080] In a 50 mL reaction flask, under N 2 Add triethylboron tetrahydrofuran solution (10 mL, 1 mol / L) under the protection of . The above reaction flask was placed in an ice-water bath, and then 2 In the atmosphere, 1.09 g of 4-methoxypyridine (10 mmol) was slowly added dropwise, and the reaction was continued in the ice-water bath for 10 minutes, then the ice-water bath was removed, and the reaction was carried out at room temperature for 1 hour. After the reaction was completed, the solvent tetrahydrofuran was removed by rotary evaporation under reduced pressure to obtain 1.97 g of a colorless oily liquid with a yield of 95%. 1 H-NMR nuclear magnetic spectrum analysis is triethylboron-4-methoxypyridine complex (Et 3 B-4MeO-Py).

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Abstract

The invention relates to the technical field of polymer synthesis, in particular to a method for realizing controllable free radical polymerization in an air atmosphere and application of the method. In an environment completely exposed to air, under the heating condition of the alkyl boron amine complex, a B-N coordinate bond is broken to release an alkyl boron compound, and the alkyl boron compound is self-oxidized to generate alkyl free radicals to initiate a polymerization reaction. The alkyl boron amine complex is used as an initiator to be applied to reversible addition-fragmentation chain transfer polymerization (RAFT) to realize controllable free radical polymerization in an air atmosphere. The method for realizing controllable free radical polymerization in the air atmosphere is high in polymerization efficiency, short in polymerization reaction time, free of obvious polymerization induction period, wide in reaction temperature application range, simple in reaction condition and equipment requirement and free of a deoxygenization link, and is a controllable free radical polymerization method suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a method for realizing controllable radical polymerization in an air atmosphere and its application. Background technique [0002] Controlled radical polymerization is of great significance in the field of polymer synthesis. The precise design of polymers can be realized through controlled free radical polymerization, and polymers with narrow molecular weight distribution, regular structure and complex morphology can be obtained, so that new polymer materials with multiple uses can be prepared. [0003] Common controllable radical polymerization techniques include oxygen nitrogen stabilized radical method, iniferter method, atom transfer radical polymerization (ATRP) method and reversible addition-fragmentation chain transfer (RAFT) method. In the controllable radical polymerization system, the mechanism is to use the balance between growing free radicals and various d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/54C08F120/14C08F293/00C08F220/28C08F4/12
CPCC08F120/54C08F120/14C08F220/281C08F220/286C08F293/005C08F4/12C08F2438/03
Inventor 潘翔城陈哲
Owner FUDAN UNIV
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