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Four-branched thermo-sensitive polymer and preparation method thereof

A temperature-sensitive polymer and temperature-sensitive monomer technology, which is applied in the fields of polymer chemistry and material chemistry, can solve problems that affect the performance and application range of polymers, are difficult to control, and the terminal functionality of the chain structure is out of control.

Inactive Publication Date: 2017-03-15
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Because the traditional free radical polymerization is not easy to control, it is easy to cause the molecular weight, molecular weight distribution, chain structure and terminal functionality of the polymer to be out of control, and sometimes even branching, cross-linking and other reactions occur, which seriously affects the performance and application range of the polymer.

Method used

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  • Four-branched thermo-sensitive polymer and preparation method thereof
  • Four-branched thermo-sensitive polymer and preparation method thereof
  • Four-branched thermo-sensitive polymer and preparation method thereof

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preparation example Construction

[0042] The present application also provides a preparation method of the above-mentioned thermosensitive polymer, comprising the following steps:

[0043] A), under inert gas and anhydrous conditions, react pentaerythritol, acid-binding agent, catalyst and the acylating agent with the structure of formula (II) in a solvent to obtain the initiator with the structure of formula (III);

[0044] B), under the protection of an inert gas, react the initiator, temperature-sensitive monomer, catalyst and complexing agent in a solvent to obtain an active temperature-sensitive polymer with a structure of formula (IV); the temperature-sensitive The neutral monomer is selected from N-isopropylacrylamide, N-propylacrylamide, N-cyclopropylacrylamide, N,N-diethylacrylamide, N-vinylisopropanamide, N-vinyl N-propionamide, N-vinylcaprolactam, N-vinylpyrrolidone, N-acryloylpyrrolidine, N-acryloyl-N'-n-propiperazine, N-(2,2-dimethyl-1,3 One or more of -dioxan-5 alcohol)-acrylamide and N-(2-ethox...

Embodiment 1

[0071]Add pentaerythritol (0.952g, 7mmol) into a solution containing triethylamine (3.188g, 31.5mmol) and 75ml of dichloromethane, and stir for 30min under ice-bath conditions. 2-Bromoisobutyryl bromide (7.245 g, 31.5 mmol) was slowly added through a constant pressure dropping funnel over 1 hour, and kept at low temperature for 1-2 hours. Then it was gradually raised to room temperature, and the reaction was continued for 12 hours. After the reaction, the obtained product was washed successively with 5% sodium bicarbonate solution (100ml*3), saturated saline (100ml*3), and deionized water (100ml*3). The washed organic layer was rotary evaporated to remove the solvent, dissolved in dichloromethane, slowly added dropwise into glacial ether, and left standing at 0°C for 12 hours. Filter through a funnel and wash with cold diethyl ether (10ml). Dry in a vacuum oven at room temperature to obtain a white crystal tetrakis-(bromoisobutyryl)-pentaerythritol initiator. figure 1 The i...

Embodiment 2

[0077] Add pentaerythritol (0.952g, 7mmol) into a solution containing triethylamine (2.90g, 28.7mmol) and 75ml of dichloromethane, and stir for 30min under ice-bath conditions. 2-Bromoisobutyryl bromide (6.60 g, 28.7 mmol) was added slowly over 1 hour through a constant pressure dropping funnel, and the temperature was kept low for 1-2 hours. Then it was gradually raised to room temperature, and the reaction was continued for 12 hours. After the reaction, the obtained product was washed successively with 5% sodium bicarbonate solution (100ml*3), saturated saline (100ml*3), and deionized water (100ml*3). The washed organic layer was rotary evaporated to remove the solvent, dissolved in dichloromethane, slowly added dropwise into glacial ether, and left standing at 0°C for 12 hours. Filter through a funnel and wash with cold diethyl ether (10ml). At room temperature, dry in a vacuum oven to obtain 2.25 g of white crystal tetrakis-(bromoisobutyryl)-pentaerythritol initiator.

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Abstract

The invention provides a thermo-sensitive polymer. The structural formula of the thermo-sensitive polymer is as shown in the specification. A preparation method of the thermo-sensitive polymer includes the steps: taking pentaerythritol as a core, reacting the pentaerythritol and acylating agents to obtain initiating agents, and performing atom transfer radical polymerization for the initiating agents and thermo-sensitive monomers to obtain active thermo-sensitive polymers with uniform chain length and controllable molecular weight; performing azidation for tail ends of the polymers to obtain the thermo-sensitive polymer with azido tail ends. Compared with the prior art, the polymer has the advantages of simplicity, convenience and easiness in implementation, branch number and branch length can be controlled, and the polymer is flexible and adjustable in structure, can be conveniently modified and has excellent thermo-sensitivity, use ranges close to environment temperature and excellent application prospects.

Description

technical field [0001] The invention belongs to the fields of polymer chemistry and material chemistry, and in particular relates to a four-arm temperature-sensitive polymer and a preparation method thereof. Background technique [0002] Multi-armed star polymers are a class of polymers with a star-like structure composed of multiple polymer arms connected to the core through covalent bonds and together with the core. Due to its special three-dimensional spherical branched structure and characteristics, star polymers have become one of the research hotspots in the field of polymer materials. Star polymers have more terminal functional groups, which can be modified to obtain polymers with different structures and properties. Temperature-sensitive star polymers are a class of polymers that can respond to slight changes in the external environment temperature, resulting in corresponding changes in physical structure and chemical properties or even mutations. The temperature a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/54C08F126/02C08F126/06C08F8/30
CPCC08F8/30C08F2810/40C08F120/54C08F126/02C08F126/06
Inventor 朱东雨薛延敏陈欣杰郭建维罗涛
Owner GUANGDONG UNIV OF TECH
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