Block copolymer/nano-SiO2 composite material and preparation method thereof

A technology of block copolymer and composite material, which is applied in the field of block copolymer/nano-SiO2 composite material and its preparation, can solve the problems of poor thermal stability and insufficient mechanical properties, and achieve the effect of improving thermal stability

Inactive Publication Date: 2011-08-31
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Block Copolymer Polymethyl Methacrylate- b -Poly-2-hydroxyethyl acrylate (PMMA -b- PHEA) has the good hydrophilicity and physiological compatibility of poly(2-hydroxyethyl acrylate), and also has the excellent light transmittance, chemical stability and good processability of polymethyl methacrylate (PMMA), etc. It has good application prospects in biomedicine, but it has defects such as poor thermal stability and insufficient mechanical properties.

Method used

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  • Block copolymer/nano-SiO2 composite material and preparation method thereof
  • Block copolymer/nano-SiO2 composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Nano-SiO 2 Add the modifying agent γ-methacryloxypropyltrimethylsilane into the solvent toluene, and react at 80°C for 5 hours while stirring. Stand still, suck off the supernatant, vacuum dry at 35°C for 12 hours, and then dry at 120°C for 2 hours to obtain modified nano-SiO 2 . Among them, nano-SiO 2 : The mass ratio of γ-methacryloxypropyltrimethylsilane is 1:0.1, nano-SiO in toluene 2 The concentration is 0.2 g / ml.

[0023] (2) Using methyl methacrylate as a monomer, azobisisobutyronitrile as an initiator, ferric chloride / triphenylphosphine as a catalyst / ligand, and xylene as a solvent, continuously blowing nitrogen for 0.5 hours, in React at 70°C for 4 hours, cool, add tetrahydrofuran until the polymer is completely dissolved, pass through a neutral alumina chromatography column, add methanol to the filtrate until complete precipitation, wash the precipitate with deionized water 3 times, and store at 80°C Vacuum-dried to constant weight to obtain polymethy...

Embodiment 2

[0027] (1) The method is the same as step (1) in Example 1. Among them, the reaction temperature is 100°C, the reaction time is 5 hours, and the nano-SiO 2 : The mass ratio of γ-methacryloxypropyltrimethylsilane is 1:0.2, nano-SiO in toluene 2 The concentration is 0.4 g / ml.

[0028] (2) The method is the same as step (2) of Example 1. The reaction temperature is 90°C, the reaction time is 4 hours, the molar ratio of initiator:catalyst:ligand:monomer is 1:1:3:150, and the concentration of monomer methyl methacrylate in xylene is 0.8 g / ml.

[0029] (3) The method is the same as step (3) of Example 1. The reaction temperature is 80°C, the reaction time is 5 hours, the molar ratio of macromolecular initiator:catalyst:ligand:monomer is 1:1:3:380, and the concentration of monomer-2-hydroxyethyl acrylate is 0.3g / ml .

[0030] (4) The method is the same as step (4) of Example 1. Among them, the reaction temperature is 70°C, the reaction time is 6 hours, and the modified nano-S...

Embodiment 3

[0032] (1) The method is the same as step (1) in Example 1. Among them, the reaction temperature is 90°C, the reaction time is 5 hours, and nano-SiO 2 : The mass ratio of γ-methacryloxypropyltrimethylsilane is 1:0.3, nano-SiO in toluene 2 The concentration is 0.5g / ml.

[0033] (2) The method is the same as step (2) of Example 1. The reaction temperature is 80°C, the reaction time is 5 hours, the molar ratio of initiator:catalyst:ligand:monomer is 1:1:3:250, and the concentration of monomer methyl methacrylate in xylene is 1.0g / ml.

[0034] (3) The method is the same as step (3) of Example 1. The reaction temperature is 90°C, the reaction time is 4 hours, the molar ratio of macromolecular initiator:catalyst:ligand:monomer is 1:1:3:320, and the concentration of monomer-2-hydroxyethyl acrylate is 0.25g / ml .

[0035] (4) The method is the same as step (4) of Example 1. Among them, the reaction temperature is 70°C, the reaction time is 6 hours, and the modified nano-SiO 2 ...

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Abstract

The invention discloses a block copolymer / nano-SiO2 composite material and a preparation method thereof. The composite material comprises a block copolymer, namely polymethyl methacrylate-b-polyacrylic acid-2-hydroxyethyl ester, and nano-SiO2; and the preparation method of the composite material is as follows: synthesizing polymethyl methacrylate containing terminal group chlorine by adopting a reverse atom transfer free radical method, taking the prepared polymethyl methacrylate as a macromolecular initiator, and synthesizing the block copolymer, namely the polymethyl methacrylate-b-polyacrylic acid-2-hydroxyethyl ester, through a atom transfer free radical method; and adopting a silane coupling agent, namely gamma-methacryloxypropyltrimethoxy silane, to modify the nano-SiO2, and obtaining the activated nano-SiO2; performing surface grafting reaction on the activated nano-SiO2 and the block copolymer, namely the polymethyl methacrylate-b-polyacrylic acid-2-hydroxyethyl ester, and obtaining the block copolymer / nano-SiO2 composite material. Compared with the block copolymer, the composite material has higher thermal deposition temperature and better heat resistance.

Description

technical field [0001] The present invention relates to a kind of block copolymer / nanometer SiO 2 Composite materials and methods for their preparation. Background technique [0002] Due to its wide application, the preparation and modification technology of nano-silica has been greatly developed. In particular, it can be combined with polymer materials to obtain organic / inorganic composite materials with different properties. In order to improve the thermal properties of polymers , The improvement of mechanical properties provides a new way. However, due to the large specific surface area of ​​nano-silica, many unsaturated residual bonds, high surface energy, and easy agglomeration between particles, how to prepare nano-SiO with good dispersion and uniform particle size distribution 2 , become nano-SiO 2 Key issues in composite materials research. Generally speaking, the nano-SiO 2 Perform surface modification and then react with polymer materials. [0003] Block Copo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L53/00C08K9/06C08K3/36C08F293/00C08F8/42
Inventor 易国斌黄海亮张斯林文静康正
Owner GUANGDONG UNIV OF TECH
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