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Method for synthesizing star block copolymer based on combination of active anionic polymerization and hydrosilylation click reaction

A block copolymer and living anion technology, applied in the field of living anion polymerization, can solve the problems that are not conducive to the precise regulation of polymer composition and distribution, cumbersome synthesis methods, and complicated processing operations.

Active Publication Date: 2022-02-25
辽宁科之镁新材料研究有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The strategy of living anionic polymerization combined with linker chlorosilane chemistry, this synthesis method is not conducive to the precise control of polymer composition and distribution; reactivity is also affected by the molecular weight of the active chain, solvent (polar or non-polar) and temperature
In addition, the synthesis method is cumbersome and time-consuming, and the post-treatment operation of a large number of linking agents is complicated.

Method used

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  • Method for synthesizing star block copolymer based on combination of active anionic polymerization and hydrosilylation click reaction
  • Method for synthesizing star block copolymer based on combination of active anionic polymerization and hydrosilylation click reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Using living anionic polymerization combined with hydrosilylation click reaction, the molecular weight of polystyrene is designed to be 6.0×10 4 The molecular weight of g / mol poly-n-butyl methacrylate is designed to be 3.0×10 4 g / mol. The whole process of polystyrene polymerization in this experiment was completed in a glove box protected by argon atmosphere, and the polymerization of polymethyl methacrylate n-butyl ester was carried out under the condition of isolating water and oxygen at -78 ℃. Before the experiment, a certain amount of monomer DPE-2SiH needs to be mixed Prepare for dilution.

[0040] The first step: at 20°C, add (1g, 9.60mmol) styrene and 9g of solvent benzene into a 20mL polymerization bottle, shake slightly for 2min to make it fully mixed, and then quickly inject sec-BuLi (430μl 0.04651mol / L ) to initiate the polymerization of the monomer and shake to make it evenly initiated, and the reaction solution is orange-yellow. After 6 h, quantitative D...

Embodiment 2

[0044] Using living anionic polymerization combined with hydrosilylation click reaction, the molecular weight of polystyrene is designed to be 6.0×10 4 The molecular weight of g / mol poly(n-butyl methacrylate) is designed to be 6.0×10 4 g / mol. The whole process of polystyrene polymerization in this experiment was completed in a glove box protected by argon atmosphere, and the polymerization of poly-n-butyl methacrylate was carried out under the condition of isolating water and oxygen at -78 °C. Before the experiment, a certain amount of monomer DPE-SiH Prepare for dilution.

[0045] The first step: at 20°C, add (0.5g, 4.81mmol) 18ml of styrene solvent benzene into a 20mL polymerization bottle, shake slightly for 2min to make it well mixed, and then quickly inject sec-BuLi (358μl 0.04651mol / L ) to initiate the polymerization of the monomer and shake to make it evenly initiated, and the reaction solution is orange-yellow. After 3h, quantitative DPE-SiH (1.67×10) was rapidly ad...

Embodiment 3

[0049] Using living anionic polymerization combined with hydrosilylation click reaction, the molecular weight of polystyrene is designed to be 6.0×10 4 The molecular weight of g / mol poly-n-butyl methacrylate is designed to be 3.0×10 4 g / mol. The whole process of polystyrene polymerization in this experiment was completed in a glove box protected by an argon atmosphere, and the polymethacrylic acid polymerization was carried out under the condition of isolating water and oxygen at -78 °C. Before the experiment, a certain amount of monomer DPE-2SiH needs to be diluted for use. .

[0050] The first step: at 25°C, add (1g, 9.60mmol) styrene and 9g of solvent benzene into a 20mL polymerization bottle, shake slightly for 2min to make it fully mixed, and then quickly inject sec-BuLi (430μl 0.04651mol / L ) to initiate the polymerization of the monomer and shake to make it evenly initiated, and the reaction solution is orange-yellow. After 6 h, quantitative DPE-2SiH (1.9×10) was rapi...

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Abstract

The invention provides a method for synthesizing a star block copolymer based on active anion polymerization combined with hydrosilylation click reaction, and belongs to the technical field of active anions. The preparation method comprises the following steps: polymerization of styrene acrylate can be respectively initiated by adopting a silicon-hydrogen functionalized 1, 1 '-stilbene derivative and an alkynyl functionalized 1, 1'-stilbene derivative; wherein two kinds of silicon-hydrogen functionalized polystyrene are respectively designed and synthesized, synthesis and post-treatment are complex due to the fact that anionic polymerization is combined with a connecting agent chlorosilane chemical method and the like, and composition of each block cannot be accurately regulated and controlled; the molecular weight and distribution are accurately regulated and controlled through active anionic polymerization, the composition proportion of the block copolymer can be regulated and controlled, the topological structure of a polymerization system is determined by adopting a method of combining active anionic hydrosilylation and click reaction, and the composition proportion and molecular weight distribution of the polymer can be effectively regulated and controlled.

Description

technical field [0001] The invention belongs to the technical field of active anionic polymerization, and relates to a method for synthesizing star-shaped amphiphilic block copolymers by combining active anionic polymerization with hydrosilylation click reaction, and the anionic polymerization module contains functional groups that can participate in hydrosilylation. Click reaction, so it also has broad prospects in the synthesis of star-shaped block copolymers with complex topological structures. Background technique [0002] Living anionic polymerization (LAP) has unique advantages in synthesizing polymers with clear structure, precise and controllable molecular weight, and functionalized polymers at the end and in the chain. Under the condition of isolating water and oxygen, the active center can remain immortal for a long time, the molecular weight is controllable, and the molecular weight distribution is narrow. Living anionic polymerization has the characteristics of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00
CPCC08F293/005
Inventor 马红卫尹钰韩丽
Owner 辽宁科之镁新材料研究有限公司
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