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Method for preparing amphipathy copolymerization network

An amphiphilic and copolymerization technology, which is applied in the field of preparation of amphiphilic copolymer networks, can solve the problems of uncontrollable network structure size, poor mechanical properties of network structure, poor controllability of molecular weight, etc., and achieves good anti-oxidative degradation effect.

Inactive Publication Date: 2014-04-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The relative molecular weight distribution of products obtained by this type of polymerization is wide, and the controllability of molecular weight is poor, resulting in poor mechanical properties of the prepared network structure and uncontrollable size of the network structure.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Dissolve 10 parts of hydroxypolydimethylsilane (Mn=4000g / mol) in 80 parts of THF to obtain a functionalized polydimethylsiloxane solution, add 0.7 parts of triethylamine, drop 0.3 parts of 2-bromo Isobutyryl bromide, reacted in ice-water bath for 1 hour, after removing the ice-water bath, reacted at room temperature for 2 hours, filtered the product to remove white precipitate, removed solvent, then added to n-hexane to dissolve, washed with deionized water for 3 times, and dried for 24 hours , to obtain a polydimethylsiloxane macroinitiator with Br at the end.

[0025] (2) Mix 0.8 parts of 2'2-bipyridine, 5 parts of Br-PDMS-Br, 10 parts of hydroxyethyl methacrylate HEMA, 0.36 parts of cuprous chloride, 70 parts of butanone, and 30 parts of n-propanol, -10 After deoxygenation at 10°C, react at 10°C for 24 hours, pass the mixture through a silica gel chromatography column, remove most of the solvent after distillation of the obtained filtrate, and precipitate with 50...

Embodiment 2

[0030] (1) Dissolve 10 parts of hydroxypolydimethylsilane (Mn=4000g / mol) in 1000 parts of dichloromethane to obtain a functionalized polydimethylsiloxane solution, add 0.6 parts of sodium hydroxide, dropwise add 0.6 parts of 2 -Bromoisobutyryl bromide, reacted in an ice-water bath for 2 hours, removed the ice-water bath, and reacted at room temperature for 6 hours. The product was filtered to remove the white precipitate, and the solvent was removed, then dissolved in n-hexane, washed with deionized water for 3 times, and dried After 24 hours, a polydimethylsiloxane macroinitiator with Br at the end was obtained.

[0031](2) Mix 0.8 parts of 2'2-bipyridine, 10 parts of Br-PDMS-Br, 30 parts of dimethylaminoethyl acrylate DMAEA, 0.5 parts of cuprous chloride, and 100 parts of methyl ethyl ketone, and remove oxygen at -10°C, React at 50°C for 24 hours, pass the mixture through a silica gel chromatography column, and remove most of the solvent after distillation of the obtained fi...

Embodiment 3

[0036] (1) Dissolve 10 parts of hydroxyaminopolydimethylsilane (Mn=4000g / mol) in 100 parts of chloroform to obtain a functionalized polydimethylsiloxane solution, add 0.5 parts of potassium hydroxide, and dropwise add 1.2 parts of 2- Bromoisobutyryl bromide, reacted in an ice-water bath for 8 hours, removed the ice-water bath, and reacted at room temperature for 16 hours. The product was filtered to remove the white precipitate, and the solvent was removed, then dissolved in n-hexane, washed with deionized water for 3 times, and dried for 24 hours. Hours, the polydimethylsiloxane macroinitiator with Br at the end was obtained.

[0037] (2) Mix 1.6 parts of DMAP, 20 parts of Br-PDMS-Br, 50 parts of N-isopropylacrylamide NIPAM, 0.72 parts of cuprous chloride, and 1000 parts of 1,4-dioxane, and remove at -10°C After oxygenation, react at 85°C for 24 hours, pass the mixture through a silica gel chromatography column, remove most of the solvent after distillation of the obtained fi...

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PUM

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Abstract

The invention relates to a method for preparing an amphipathy copolymerization network. The method comprises the following steps: dissolving functionalized polydimethylsiloxane in a solvent, adding an acid-binding agent and a nucleophilic substitution agent, reacting for 3-24 hours at 0-80 DEG C, purifying so as to obtain a PDMS (Polydimethylsiloxane) base macroinitiator, mixing a ligand, the PDMS base macroinitiator, a hydrophilic monomer, a solvent and a first catalyst, reacting for 1-24 hours at 10-140 DEG C under the inert atmosphere, purifying so as to obtain a triblock copolymer, mixing the ligand, the triblock copolymer, a band double-bond monomer, a solvent and a second catalyst, reacting for 1-24 hours at 10-140 DEG C, purifying, dissolving with a hydrosilation cross-linking agent into the solvent, performing hydrosilation reaction for 4-36 hours at 25-150 DEG C so as to obtain the amphipathy copolymerization network. Due to a co-continuous structure, the network can be applied to biologic medical fields such as controllable medicine release systems, artificial pancreas and contact lenses.

Description

technical field [0001] The invention belongs to the field of preparation of copolymerized network materials, in particular to a preparation method of amphiphilic copolymerized network. Background technique [0002] Most of the current literature reports are based on free radical polymerization and group transfer polymerization (GTP) to synthesize amphiphilic copolymer networks, such as "Thermally Responsive Amphiphilic Conetworks and Gels Based on Poly(N-isopropylacrylamide)and Polyisobutylene" (Gergely Kali , Szilvia Vavra, Krisztina Laszlo, Bela Ivan.Macromeolecules.2013,46,5337-5344.) The cross-linked network of polyisobutylene and N-isopropylacrylamide was prepared by free radical polymerization, "Amphiphilic Co-networks with Moisture -Induced Surface Segregation for High-Performance Nonfouling Coatings" (Yapei Wang, John A. Finlay, Douglas E. Betts, Timothy J. Merkel, J. Christopher Luft, Maureen E. Callow, James A. Callow, Joseph M. DeSimone. Langmuir.2011,27,10365–10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08F293/00
Inventor 何春菊邱明
Owner DONGHUA UNIV
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