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Preparation method and application method of novel amphipathic copolymerization network

A technology of amphiphilic and amphiphilic blocks, which is applied in the field of preparation of amphiphilic copolymer networks, can solve problems such as poor mechanical properties of network structures, poor controllability of molecular weight, and uncontrollable network structure size.

Active Publication Date: 2013-07-24
浙江海富海洋生物科技有限公司
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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 hydroxypropyl polydimethylsilane (Mn=4000g / mol) in 80 parts of solvent to obtain a functionalized polydimethylsiloxane solution, add 0.6 parts of triethylamine, dropwise add 1.5 parts of 2 -Bromoisobutyryl bromide was reacted in an ice-water bath for 3 hours. After removing the ice-water bath, react 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, and dried for 24 hours. A polydimethylsiloxane macroinitiator with Br at the end is obtained.

[0031] (2) Mix 0.8 parts of 2'2-bipyridine, 10 parts of Br-PDMS-Br, 40 parts of DMAA, 0.72 parts of cuprous bromide, and 100 parts of 1'4-dioxane, and deoxygenate at -10°C, Reacted at 85°C for 24 hours to obtain an amphiphilic block copolymer. After adding 1.6 parts of allyl n-butyltin, the temperature was raised to 100°C and reacted for 3 hours. The mixture was passed through a neu...

Embodiment 2

[0035](1) Dissolve 10 parts of hydroxypropyl polydimethylsilane (Mn=4000g / mol) in 1200 parts of solvent to obtain a functionalized polydimethylsiloxane solution, add 0.6 parts of triethylamine, dropwise add 1.5 parts of 2 -Bromoisobutyryl bromide was reacted in an ice-water bath for 6 hours. After removing the ice-water bath, react at room temperature for 12 hours. The product was filtered to remove the white precipitate, and the solvent was removed, then dissolved in n-hexane, washed with deionized water, and dried for 24 hours. , to obtain a polydimethylsiloxane macroinitiator with Br at the end.

[0036] (2) Mix 0.8 parts of 2'2-bipyridine, 10 parts of Br-PDMS-Br, 40 parts of DMAA, 0.72 parts of cuprous bromide and 1000 parts of 1'4-dioxane, and deoxidize at -10°C, After reacting at 70°C for 24 hours, an amphiphilic block copolymer was obtained. After adding 1.6 parts of allyl n-butyltin, the temperature was raised to 90°C. After reacting for 0.5 hours, the mixture was pass...

Embodiment 3

[0041] (1) Dissolve 10 parts of hydroxypropyl polydimethylsilane (Mn=4000g / mol) in 100 parts of solvent to obtain a functionalized polydimethylsiloxane solution, add 0.6 parts of triethylamine, dropwise add 1.5 parts of 2 -Bromoisobutyryl bromide was reacted in an ice-water bath for 8 hours. After removing the ice-water bath, 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, and dried for 24 hours. , to obtain a polydimethylsiloxane macroinitiator with Br at the end.

[0042] (2) Mix 1.6 parts of 2'2-bipyridine, 10 parts of Br-PDMS-Br, 40 parts of DMAA, 0.72 parts of cuprous bromide and 1000 parts of 1'4-dioxane, and deoxygenate at -10°C, After reacting at 85°C for 24 hours, an amphiphilic block copolymer was obtained. After adding 1.6 parts of allyl n-butyltin, the temperature was raised to 70°C, and the reaction was carried out for 1 hour. T...

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PUM

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Abstract

The invention provides a preparation method of a novel amphipathic copolymerization network. The preparation method is characterized by comprising the specific steps of: dissolving functionalized polydimethylsiloxane in a solvent to obtain a functionalized polydimethylsiloxane solution, adding an acid-binding agent, dropping a nucleophilic substitution reagent, reacting for 3-24 hours at a temperature of -5-40 DEG C, and purifying to obtain a PDMS-based macroinitiator; mixing a ligand, the PDMS-based macroinitiator, a hydrophilic monomer, a solvent and a first catalyst, reacting for 1-24 hours at a temperature of 10-140 DEG C under an inert atmosphere to obtain an amphipathic segmented copolymer, adding a micromolecule with double bond in the terminal, reacting for 1-24 hours at a temperature of 0-150 DEG C, and purifying to obtain an amphipathic segmented copolymer with allyl in the terminal; and dissolving the amphipathic segmented copolymer with allyl in the terminal and a hydrosilation crosslinking agent in the solvent, and carrying out hydrosilation at a temperature of 65-110 DEG C for 1-36 hours to obtain the amphipathic copolymerization network. The amphipathic copolymerization network is applied to the biomedical fields such as a controlled drug delivery system, an artificial pancreas and contact lenses due to the adoption of a co-continuous structure.

Description

technical field [0001] The invention relates to a preparation method and application of a novel amphiphilic copolymer network, in particular to the preparation of a highly oxygen-permeable amphiphilic copolymer network synthesized by the ATRP method. Background technique [0002] Most of the current reports in the literature are based on free radical polymerization and group transfer polymerization (GTP) to synthesize amphiphilic copolymer networks, such as "poly(N-viny(imidazide)-l-poly(tetrahydrof uran) amphiphilic conetworks and gels .synthesis, characterization, Thermeal and, Swelling, Behavior” (Csaba Fordor, Gergely Kali, Bela Ivan, Macromeolecules.2011.44.4496-4502.) used free radical polymerization to prepare the cross-linked network of vinylimidazole and tetrahydrofuran,” Nanophase-Separated Amphiphilic Conetworks as Versatile Matrixes for Optical Chemical and Biochemical Sensors" (Michael Hanko, Nico Bruns, Sara Rentmeister, Jorg C. Tiller, Jurgen Heinze." Analytic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08F293/00C08F220/54C08F220/28C08F226/10C08F8/00A61L27/14A61K47/30
Inventor 何春菊徐剑峰
Owner 浙江海富海洋生物科技有限公司
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