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Preparation method of amphiphilic copolymer network

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

Active Publication Date: 2016-01-06
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

[0030] (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, and drop 0.3 parts of 2-bromo Isobutyryl bromide was reacted in an ice-water bath for 1 hour. After removing the ice-water bath, reacted at room temperature for 2 hours. The product was filtered to remove the white precipitate, and the solvent was removed by rotary evaporation, 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, 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 removing oxygen at ℃, react at 10℃ for 24 hours under the protection of nitrogen, pass the mixture through a silica gel chromatography column, remove most of ...

Embodiment 2

[0036] (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 by rotary evaporation, then dissolved in n-hexane and washed with deionized water for 3 times , and dried for 24 hours to obtain a polydimethylsiloxane macroinitiator with Br at the end.

[0037] (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, Under nitrogen protection, react at 50°C for 24 hours, pass the mixture through a silica gel chromatography column, remove most of the s...

Embodiment 3

[0042] (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 was reacted in an ice-water bath for 8 hours. After removing the ice-water bath, it was reacted at room temperature for 16 hours. The product was filtered to remove the white precipitate, and the solvent was removed by rotary evaporation. After drying for 24 hours, a polydimethylsiloxane macroinitiator with Br at the end was obtained.

[0043] (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 After oxygen, under the protection of nitrogen, 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 filtrate, and precipit...

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PUM

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Abstract

The invention provides a preparation method for an amphipathic copolymerization network. The preparation method is characterized by comprising the specific steps of mixing a ligand, a PMDS-based macromolecular initiator, a hydrophilic monomer, a solvent and a first catalyst, and performing reaction to obtain an amphipathic triblock copolymer; mixing a ligand, the obtained amphipathic triblock copolymer, a monomer with two bonds, a solvent and a second catalyst, and performing reaction to obtain an amphipathic five-block copolymer; dissolving the obtained amphipathic five-block copolymer and mercaptan in a solvent, adding a photoinitiator, and reacting under ultraviolet to obtain the amphipathic copolymerization network. The amphipathic copolymerization network prepared by the preparation method disclosed by the invention has potential application in the aspects such as a biomedical material, such as contact lenses, artificial visceral organs and controlled release carriers of medicaments.

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 synthesize amphiphilic copolymer networks by free radical polymerization and group transfer polymerization (GTP), such as "ThermallyResponsiveAmphiphilicConetworksandGelsBasedonPoly(N-isopropylacrylamide)andPolyisobutylene" (GergelyKali, SzilviaVavra, KrisztinaLaszlo, BelaIvan.Macromeolecules.2013 , 46,5337-5344.) adopted free radical polymerization to prepare the cross-linked network of polyisobutylene and N-isopropylacrylamide, "AmphiphilicCo-networkswithMoisture-InducedSurfaceSegregationforHigh-PerformanceNonfoulingCoatings" (YapeiWang, JohnA.Finlay, DouglasE.Betts , TimothyJ.Merkel, J.ChristopherLuft, MaureenE.Callow, JamesA.Callow, JosephM.DeSimone.Langmuir.2011, 27, 10365–10369.) used free radical polymerization to prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08J3/28C08J3/24C08L53/00
Inventor 何春菊邱明
Owner DONGHUA UNIV
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