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Synthetic method of triblock polymer

A polymer and triblock technology, applied in the field of polymer material synthesis and preparation, can solve the problems of poor molecular structure controllability, harsh reaction conditions, wide molecular weight distribution, etc., and achieve diversified molecular structure design, mild reaction conditions, The effect of high reaction efficiency

Inactive Publication Date: 2014-06-11
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the shortcomings of low initiation efficiency, wide molecular weight distribution, harsh reaction conditions and poor molecular structure controllability in the process of traditional living free radical polymerization to prepare block polymers. For the first time, stepwise polymerization, living free radical polymerization and click chemistry Combining the reaction, the azide-terminated ATRP polymer and the alkyne-terminated polyurethane prepolymer were used to carry out 1,3-dipolar cycloaddition reaction, and a three-block polymer with a triazole ring in the main chain was synthesized. Under mild reaction conditions, triblock polymers with low molecular weight distribution are efficiently prepared, which provides a convenient and efficient method for the synthesis of block polymers with low molecular weight distribution

Method used

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Examples

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Effect test

Embodiment 1

[0035] (1) Synthesis of PS-Br. Put a stirring bar in a clean Schlenk bottle, and add toluene, styrene, PMDETA, and cuprous bromide sequentially according to the molar ratio of 108:192:1:1. After the reaction system was cooled by liquid nitrogen for three times-vacuumizing-nitrogen filling-thawing cycles, ethyl α-bromoisobutyrate (EBiB) was added with a syringe, and the molar ratio of styrene to ethyl α-bromoisobutyrate was 192:1, sealed under a nitrogen atmosphere, reacted at 90°C for 2 hours, cooled with cold water and added to liquid nitrogen to terminate the reaction. After dilution with tetrahydrofuran, neutral alumina column chromatography was used to remove the colored catalyst, and tetrahydrofuran was concentrated by rotary evaporator, and precipitated in a large amount of cold methanol. The dissolution / precipitation operation was repeated three times to obtain a white powder product which was dried in a vacuum oven at 50° C. for 12 hours.

[0036]1 H NMR (CDCl 3 )d ...

Embodiment 2

[0045] (1) Synthesis of PMMA-Br. Put a stirring bar in a clean Schlenk bottle, and add toluene, MMA, PMDETA, and cuprous bromide sequentially according to the molar ratio of 200:200:2:1. After the reaction system was cooled by liquid nitrogen three times-vacuumizing-nitrogen filling-thawing cycle, α-bromoisobutyrate ethyl was added with a syringe, and the molar ratio of MMA to α-bromoisobutyrate was 200:1. Seal it under a nitrogen atmosphere, react at 70°C for 6h, and add liquid nitrogen to terminate the reaction after cooling down with cold water. Use ethanol as precipitant, filter and dissolve in tetrahydrofuran, go through neutral alumina column chromatography to remove colored catalyst, use rotary evaporator to evaporate THF to dryness, and obtain white powdery product and place it in a vacuum oven for drying.

[0046] (2)PMMA-N 3 The synthetic method is with embodiment 1.

[0047] (3) Add polypropylene glycol 2000 to a three-necked bottle equipped with a stirrer and a ...

Embodiment 3

[0050] (1) adopt p-nitrobenzyl bromoisobutyrate except initiator, catalyzer adopts cuprous bromide, ligand adopts bipyridine, initiator: catalyst: ligand: St=1: 1: 2: 200, toluene and The volume ratio of St is 1: 1, the reaction temperature is 110°C, and the reaction time is 4h, the others are the same as step (1) in Example 1.

[0051] (2) Except that the molar ratio of PS-Br and sodium azide is 1:10, and DMF is 20 wt%, other steps are the same as step (2) in Example 1.

[0052] (3), (4) are all with step (3), (4) in embodiment 1.

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Abstract

The invention belongs to the technical field of synthesis and preparation of polymer materials, and discloses a synthetic method of triblock polymer, wherein stepwise polymerization (SGB), atom transfer radical polymerization (ATRP) and click chemistry method are combined at first; and 1, 3-dipolar cycloaddition reaction is performed to polymer with azido terminal group and polyurethane prepolymer with alkynyl terminal group to successfully synthesize triblock polymer containing triazole ring. The synthesis method provided by the invention overcomes the defects in traditional block polymer synthesis that reaction conditions are strict, molecular weight distribution is controlled difficultly, and selectable classes of monomers are less, and has the advantages of high conversion rate, mild reaction conditions, narrow molecular weight distribution and strong controllability. The triblock polymer provided by the invention has potential application in ways of medicine slow release, solubilizers and surfactants.

Description

[0001] Technical field: the invention belongs to the technical field of polymer material synthesis and preparation, and relates to the preparation of triblock polymers by combining atom transfer radical polymerization, stepwise polymerization and click chemical reaction. Background technique [0002] Block copolymers are currently the most studied and widely used structural polymers. They have unique structures and properties. They are not only used in biomaterials, engineering materials, thermoplastic elastomers, adhesives, additives, coatings, etc. It has a wide range of applications, and is also used to prepare nanomaterials (such as LB films, nanodots or nanotube arrays), photonic crystals, inorganic mesoporous molecular sieves, etc. In recent years, researchers have synthesized many different kinds of triblock polymers and conducted extensive and in-depth studies on their physical and chemical properties. [0003] At present, the synthesis methods of tri-block polymers co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02
Inventor 王贵友王立平陈梦莉邹伟李康
Owner EAST CHINA UNIV OF SCI & TECH
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