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Preparation method of block copolymer

A technology of block copolymers and copolymers, applied in the field of block copolymer preparation, which can solve the problems of large amount of raw materials, difficult control of block length, high requirements for monomer types, etc.

Inactive Publication Date: 2011-06-15
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reaction extrusion process is simple, because the copolymer is prepared on the extruder, the amount of raw materials required is large, the type of monomer is high, and the block length is not easy to control

Method used

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  • Preparation method of block copolymer
  • Preparation method of block copolymer
  • Preparation method of block copolymer

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0025] The first step, the synthesis of prepolymer polystyrene-bromine.

[0026] Dry the three-neck flask, hollow stopper, connecting pipe, spherical condenser, etc. at 120°C for 1 hour, install it while it is hot, and put it into a stirring bar. Heat and bake with an oil bath at 60°C and blow nitrogen, then add 100 parts of styrene, 10 parts of 2-2'-bipyridine and 100 parts of cuprous bromide in sequence, and stir for 30 minutes to form a stable complex. Inject 10 parts of ethyl α-bromoisobutyrate with a syringe, continue to use nitrogen to remove oxygen and raise the temperature to 90°C, continue to pass nitrogen under stirring for 4 hours, and then stop the reaction. Add a small amount of tetrahydrofuran to dissolve, and absorb the catalyst through the aluminum oxide column, absorb the reaction solution with a dropper and slowly add the precipitant to anhydrous methanol for precipitation, and stir while adding dropwise. The resulting precipitate was vacuum-dried at 60° C. ...

Embodiment 2

[0037] The first step, the synthesis of prepolymer polystyrene-bromine.

[0038] Dry the three-necked flask, hollow stopper, connecting pipe, spherical condenser, etc. at 120°C for 1 hour, install it while it is hot, and put it into a stirring bar. Heated and baked with an oil bath at 60°C and ventilated with nitrogen, then sequentially added 150 parts of styrene, 15 parts of 2-2'-bipyridine and 150 parts of cuprous bromide, and stirred for 30 minutes to form a stable complex. Inject 10 parts of ethyl α-bromoisobutyrate with a syringe, continue to use nitrogen to remove oxygen and raise the temperature to 90°C, continue to pass nitrogen under stirring for 4 hours, and then stop the reaction. Add a small amount of tetrahydrofuran to dissolve, and absorb the catalyst through the aluminum oxide column, absorb the reaction solution with a dropper and slowly add the precipitant to anhydrous methanol for precipitation, and stir while adding dropwise. The resulting precipitate was v...

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PUM

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Abstract

Aiming at the drawbacks of the prior art, the invention provides a preparation method for synthesizing a triblock copolymer by atom transfer radical active polymerization, which has the advantages of milder reaction conditions, wide range of applicable monomers and low sensitivity to impurities and can synthesize the block copolymer with controllable blocks.

Description

technical field [0001] The invention relates to a preparation method of a copolymer, in particular to a preparation method of a block copolymer. Background technique [0002] A class of polymers in which polymer chains of different chemical compositions are connected by chemical bonds is called a block polymer. The methods for preparing block copolymers mainly include living ion polymerization, polycondensation and free radical polymerization. Living polymerization technology has obvious advantages in synthesizing block copolymers, and copolymers with predetermined structures can be obtained. Compared with other "living" radical polymerizations (SFRP and RAFT), the reaction conditions of atom transfer radical polymerization (ATRP) are milder, applicable to a wide range of monomers, less sensitive to impurities, and block length controllable. The ATRP reaction system includes monomers, initiators (organic halides RX), catalyst transition metal complexes (composed of metal h...

Claims

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Application Information

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IPC IPC(8): C08F293/00
Inventor 张冰黄碧兰周莹罗超
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH