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Polyhedral oligomeric silsesquioxane amphiphilic block copolymer and preparation method thereof

A technology of block copolymer and siloxane group, which is applied in the fields of amphiphilic block copolymer and its preparation, amphiphilic macromolecular design and self-assembly morphology research, and achieves the effects of simple preparation, mild reaction conditions and less loss of POSS.

Inactive Publication Date: 2011-09-28
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, there is no report on the preparation of amphiphilic block copolymers with POSS as hydrophobic blocks by reversible addition-cleavage chain transfer polymerization.

Method used

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  • Polyhedral oligomeric silsesquioxane amphiphilic block copolymer and preparation method thereof
  • Polyhedral oligomeric silsesquioxane amphiphilic block copolymer and preparation method thereof
  • Polyhedral oligomeric silsesquioxane amphiphilic block copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Prepare MAiBuPOSS: CDB: AIBN = 25: 1: 0.33 toluene solution system, the monomer concentration is 0.5 mol / L, put it in a bottle, seal it, freeze and degas it three times, then put it in an oil bath at 65°C for 48 hours, and freeze it to stop the reaction. Take an appropriate amount of the reaction solution and dry it in vacuum. 1 According to HNMR, the conversion rate of the first monomer was 90.2%. According to the molar ratio of tert-butyl acrylate (tBA): polymethacryloxypropyl POSS (MCTA): initiator (AIBN) = 2400: 20: 1, the measured tBA and AIBN are added to the reaction solution, sealed Afterwards, freeze and degas repeatedly for 3 times, 65 ℃ oil bath for 12 hours, freeze to stop the reaction, add a small amount of toluene to dilute and precipitate with methanol, dry, add to excess petroleum ether and stir overnight, filter and dry to obtain polymethacryloxyiso Butyl POSS-tert-butyl acrylate block copolymer, pink solid, its 1 H NMR picture as figure 1 As shown, t...

Embodiment 2

[0029] Similar to Example 1, the difference is that the MAiBuPOSS:CDB:AIBN=15:1:0.33 toluene solution system is prepared in Step 1, and the rest are the same as Example 1. Obtain polymethacryloxypropyl isobutyl POSS-polyacrylic acid amphiphilic block copolymer ABCP2. 1 The conversion rate of the first monomer was determined to be 92.3% by H NMR.

Embodiment 3

[0031] Similar to Example 1, the difference is that the POSS monomer concentration in Step 1 is 0.3mol / mL, and the rest are the same as Example 1. Obtain polymethacryloxypropyl isobutyl POSS-polyacrylic acid amphiphilic block copolymer ABCP3. 1 The conversion rate of the first monomer was determined to be 85.6% by H NMR.

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Abstract

The invention discloses polyhedral oligomeric silsesquioxane amphiphilic block copolymer and a preparation method thereof, and relates to macromolecular copolymer. Polyhedral oligomeric silsesquioxane POSS is taken as a hydrophobic block, and polyacrylic acid is taken as a hydrophilic block. The preparation method comprises the following steps of: adding a POSS monomer, a chain transfer agent andan initiator into a solvent, performing freeze degassing in a reaction container, and introducing argon into the reaction container, sealing for reaction, stopping the reaction until liquid nitrogen is frozen to obtain the hydrophobic block of polyhedral oligomeric silsesquioxane POSS; and adding tert-Butyl acrylate, an initiator and a solvent, performing freeze thawing degassing, introducing argon, sealing for polymerization, stopping the reaction until liquid nitrogen is frozen, removing unreacted tert-Butyl acrylate by using a dissolving precipitated method, adding a solvent for dilution, precipitating by using a precipitator, drying, stirring, soaking and purifying in an excessive selective solvent, filtering, drying to obtain polyhedral oligomeric silsesquioxane POSS-poly(tert-butyl acrylate) block copolymer, adding a cosolvent and an acidolysis reagent, and performing rotary evaporation to obtain the product.

Description

technical field [0001] The invention relates to a polymer copolymer, in particular to an amphiphilic block copolymer with reversible addition-fragmentation chain transfer (RAFT) polymerization and POSS as a hydrophobic block and a preparation method thereof. The first block of the amphiphilic block copolymer is polymethacryloxypropyl POSS, and the second block is polyacrylic acid. The invention can be used for the design of amphipathic macromolecules and the study of self-assembly morphology. Background technique [0002] In the past 10 years, polyhedral oligomeric silsesquioxane (Polyhedral oligomeric silsesquioxane, POSS) has attracted more and more attention as an organic-inorganic hybrid nanomaterial. POSS has a cage structure, and its classic structural formula is (RSiO 1.5 ) n (n≥4, R=H, alkyl, aryl or organic functional group), between silicon dioxide (SiO 2 ) and silicone (R 2 SiO) n Between 1.5nm and 3nm in diameter, POSS has become one of the most useful raw ...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F230/08C08F220/18C08F8/12C08F2/38
Inventor 戴李宗杨仓杰邓远名陈珉罗伟昂曾碧蓉许一婷
Owner XIAMEN UNIV
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