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Method for preparing amphiphilic copolymeric network

An amphiphilic and network technology, which is applied in the field of preparation of amphiphilic copolymer networks, can solve the problems of uncontrollable polymer segment size, poor network mechanical properties, and poor molecular weight controllability, and achieves good resistance to oxidative degradation. Effect

Active Publication Date: 2014-06-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The products obtained by this type of polymerization method have a wide relative molecular weight distribution and poor molecular weight controllability, resulting in uncontrollable polymer segment size and poor network mechanical properties.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) The mass fraction of 100 parts of n-dodecyl mercaptan, 150 parts is 40% NaOH lye, 500 parts of acetone and 0.5 part of methyl trioctanoyl ammonium chloride, mix under the condition of 5 ℃, and then 150 parts of carbon disulfide and 150 parts of chloroform were added in sequence. Under the protection of nitrogen, react at 10°C for 10 h to obtain S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate (RAFT reagent).

[0025] (2) Mix 100 parts of hydroxypropyl polymethylsiloxane (Mn=4000), 10 parts of RAFT reagent, 50 parts of EDCI and 50 parts of DMAP, and dissolve them in 500 parts of dichloromethane. , and reacted for 2 hours to obtain a PDMS-based macromolecular chain transfer reagent.

[0026] (3) Dissolve 100 parts of hydroxyethyl methacrylate in 200 parts of isopropanol to make a 50% solution of hydroxyethyl methacrylate, and put in 1 part of PDMS-based macromolecular chain transfer reagent and 0.01 part of AIBN was reacted at 60°C for 0.5h under the p...

Embodiment 2

[0032] (1) 100 parts of n-dodecyl mercaptan, 30 parts of mass fraction of 50% NaOH lye, 100 parts of acetone and 0.1 part of methyl trioctanoyl ammonium chloride were mixed at -5°C, Then add 30 parts of carbon disulfide and 150 parts of dichloromethane in sequence. Under the protection of argon, react at 0°C for 1 h to obtain S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate (RAFT reagent).

[0033] (2) Mix 100 parts of aminopropyl polymethylsiloxane (Mn=4000), 200 parts of RAFT reagent, 100 parts of EDCI and 10 parts of DMAP, and dissolve them in 1000 parts of n-hexane. , and reacted for 15h to obtain a PDMS-based macromolecular chain transfer reagent.

[0034] (3) Dissolve 100 parts of hydroxyethyl acrylate in 900 parts of THF to make a 10% hydroxyethyl acrylate solution, and put 5 parts of PDMS-based macromolecular chain transfer reagent and 0.05 part of initiator into it , Under the protection of argon, react at 60°C for 2h to obtain an amphiphilic triblock ...

Embodiment 3

[0040] (1) 100 parts of n-dodecyl mercaptan, 300 parts of mass fraction of 60% KaOH lye, 1000 parts of acetone and 1 part of methyl trioctanoyl ammonium chloride are mixed at 10 ° C, and then sequentially Add 300 parts of carbon disulfide and 300 parts of dichloromethane. Under nitrogen protection, react at 15°C for 20 h to obtain S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate (RAFT reagent).

[0041] (2) 100 parts of hydroxypropyl polymethylsiloxane (Mn=4000), 500 parts of RAFT reagent, 200 parts of DCC and 20 parts of DMAP were mixed and dissolved in 5000 parts of 1,4-dioxane, Under the condition of 30° C., react for 24 hours to obtain a PDMS-based macromolecular chain transfer reagent.

[0042] (3) Dissolve 100 parts of hydroxypropyl acrylate in 5000 parts of tetrahydrofuran / isopropanol (v / v=1:1) to make a 10% hydroxypropyl acrylate solution, and put 10 parts of PDMS-based The molecular chain transfer reagent and 0.1 part of ACVA were reacted at 60° C. for...

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Abstract

The present invention provides a method for preparing an amphiphilic copolymeric network, which is characterized in that the method comprises the steps of mixing PDMS-containing macromer chain transfer agent, a hydrophilic monomer, solvent and an initiator and reacting to obtain amphiphilic triblock polymers; mixing the amphiphilic triblock polymer, initiator, micromolecule monomer containing two double bonds with solvent, reacting to obtain drape double bond containing amphiphilic pentablock polymer; reacting the drape double bond containing amphiphilic pentablock polymer with n-alkyl primary amine to obtain terminate-modified amphiphilic pentablock polymer; mixing terminate-modified amphiphilic pentablock polymer, hydrogenous silicone oil or hydrogenous silane, solvent, with catalyst and reacting to obtain the amphiphilic copolymeric network. The amphiphilic copolymeric network prepared by the invention is applied in such biomedical materials fields as controlled drug delivery carriers, artificial pancreas structure, contact lens materials.

Description

technical field [0001] The present invention particularly relates to a preparation method of an amphiphilic copolymerization network. Background technique [0002] Most of the reports in the literature are based on free radical polymerization and group transfer polymerization (GTP) method to synthesize amphiphilic polymer network, such as "Anomalous Swelling Behavior of Poly(N-vinylimidazole)-l-Poly(tetrahydrofuran) Amphiphilic Conetwork in Water Studied by Solid-State NMR and Positron Annihilation Lifetime Spectroscopy” (Domjan, Attila; Fodor, Csaba; Kovacs, Szabolcs. Macromolecules 2012, 45, 18) used free radical polymerization to prepare cross-linked N-vinylimidazole and tetrahydrofuran network. "Thermally Responsive Amphiphilic Conetworks and Gels Based on Poly(N-isopropylacrylamide) and Polyisobutylene" (Kali, Gergely; Vavra, Szilvia; Laszlo, Krisztina Macromolecules2013, 46, 5337-5344), prepared PNiPAAm-I by free radical polymerization - Cross-linked network of PIBs....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/442C08F293/00C08F8/32
Inventor 何春菊彭小权
Owner DONGHUA UNIV