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POSS (polyhedral oligomeric silsesquioxane) contained polyacrylate-polysiloxane block copolymer and preparation method thereof

A polysiloxane block and polyacrylate technology, which is used in biocide-containing paints, coatings, antifouling/underwater coatings, etc. Limited range and other problems, to achieve the effect of improving surface hydrophobicity, improving surface properties, and improving softness and hardness

Inactive Publication Date: 2012-11-14
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although ATRP polymerization is a very good method for preparing copolymers, ATRP polymerization requires relatively harsh reaction conditions, and heavy metal salts will also be introduced, which increases the operational difficulty of the product purification process.
It has also been reported that POSS is used as a raw material to prepare macromolecular RAFT reagents, and block copolymers are obtained by RAFT radical polymerization with acrylates, but the main chain of this copolymer is relatively hard, the glass transition temperature is high, and the scope of application is limited (Mya KY, Lin EMJ, Gudipati CS, Shen L, He CB. Journal of Physical Chemistry B, 2010,114: 9119-9127)
At present, there are few reports on the preparation of polyacrylate-polysiloxane block containing POSS groups by RAFT free radical polymerization method

Method used

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  • POSS (polyhedral oligomeric silsesquioxane) contained polyacrylate-polysiloxane block copolymer and preparation method thereof
  • POSS (polyhedral oligomeric silsesquioxane) contained polyacrylate-polysiloxane block copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (a) Weigh 30g of double-ended hydrogen-terminated polydimethylsiloxane (molecular weight: 1000), 28.6g of isopropanol, and 1.74g of propenyl alcohol, add them into a 250mL three-necked flask, add 68μL of platinum catalyst, and stir magnetically , react at 20°C for 1h, then raise the temperature to 6°C for 1.5h. Remove the solvent from the obtained liquid on a rotary evaporator, and dry it in vacuum to obtain a hydroxyl-terminated polydimethylsiloxane with a molecular weight of 2000;

[0028] (b) Add 10 g of hydroxyl-terminated polydimethylsiloxane with a molecular weight of 1000, 1.1 g of the catalyst dicyclohexylcarbodiimide (DCC), and 100 mL of anhydrous dichloromethane into a 250 mL single-necked flask, and then add 4.55 g trithiocarbonate (DDMAT). After the addition, it was stirred at room temperature for 72h. Add n-hexane for dilution, filter out insoluble matter, use a rotary evaporator to remove the solvent, centrifuge at a speed of 5000r / min for 5min, take the...

Embodiment 2

[0031](a) Weigh 30g of double-ended hydrogen-terminated polytrifluoropropylmethylsiloxane (molecular weight: 2000), 18.6g of isopropanol, and 0.87g of propenyl alcohol, add them to a 250mL three-necked flask, and then add 34μL of platinum catalyst , magnetically stirred, reacted at 30°C for 0.5h, then raised the temperature to 100°C for 0.5h. Remove the solvent from the obtained liquid on a rotary evaporator, and dry it in vacuum to obtain a hydroxyl-terminated polytrifluoropropylsiloxane with a molecular weight of 2000;

[0032] (b) Add 10g of hydroxyl-terminated polytrifluoropropylmethylsiloxane with a molecular weight of 2000, 2.0g of the catalyst dicyclohexylcarbodiimide (DCC), and 150mL of anhydrous dichloromethane into a 250mL one-necked flask , and then added 4.55 g trithiocarbonate (DDMAT). After the addition, it was stirred at room temperature for 72h. Add n-hexane for dilution, filter out insoluble matter, use a rotary evaporator to remove the solvent, centrifuge a...

Embodiment 3

[0035] (a) Weigh 30g of single-end hydrogen-terminated polydimethylsiloxane (molecular weight: 5000), 30g of isopropanol, and 0.70g of propenyl alcohol, and add them into a 250mL three-necked flask, then add 21μL of platinum catalyst, stir magnetically, React at 25°C for 1h, then raise the temperature to 65°C for 1h. Remove the solvent from the obtained liquid on a rotary evaporator, and dry it in vacuum to obtain a hydroxyl-terminated polydimethylsiloxane with a molecular weight of 5000;

[0036] (b) Add 10g of hydroxyl-terminated polydimethylsiloxane with a molecular weight of 5000, 1.8g of catalyst dicyclohexylcarbodiimide (DCC), and 120mL of anhydrous dichloromethane into a 250mL single-necked flask, and then add 4.55 g trithiocarbonate (DDMAT). After the addition, it was stirred at room temperature for 72h. Add n-hexane for dilution, filter out insoluble matter, use a rotary evaporator to remove the solvent, centrifuge at a speed of 5000r / min for 5min, take the upper la...

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Abstract

The invention discloses a POSS (polyhedral oligomeric silsesquioxane) contained polyacrylate-polysiloxane block copolymer and a preparation method thereof. The preparation method includes subjecting hydrogen-terminated polysiloxane and vinylcarbinol to reaction to obtain hydroxy-terminated polysiloxane; subjecting the hydroxy-terminated polysiloxane and carboxyl thiocarbonic acid ester to reaction to obtain polysiloxane macromolecular RAFT (reversible addition-fragmentation chain transfer polymerization) reagent; polymerizing the polysiloxane macromolecular RAFT reagent, acrylate monomer and POSS monomer with initiator to prepare the POSS contained polyacrylate-polysiloxane block copolymer. The method has the advantages of simple operation and mild reaction conditions, reaction products have better surface performance and bonding performance with substrates, and further, the reaction products can be used in low-surface-energy lyophobic coating materials and used for preparing ice and snow preventive and antifouling coatings.

Description

technical field [0001] The invention relates to a POSS-containing polyacrylate-polysiloxane block copolymer and a preparation method thereof, belonging to the technical field of organosilicon-modified acrylate copolymers. Background technique [0002] Silicone polymer has excellent hydrophobicity, low surface energy, good chemical stability, and is a very good surface protection material. Silicone materials have poor adhesion to substrate surfaces. The acrylic resin has very good adhesion to the surface of the substrate. Through the method of copolymerization or blending, the silicone material is introduced into the acrylic resin, and the acrylic resin is modified. The advantages of the two can be combined to obtain a new type of copolymer with excellent performance. Copolymerization of silicone materials and acrylates through living controlled free radical polymerization is a good solution. [0003] Living controllable radical polymerization can effectively control the m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/14C08F220/18C08F230/08C08F220/28C08G77/392C09D153/00C09D5/00C09D5/16
Inventor 袁晓燕祁恒治赵蕴慧李博
Owner TIANJIN UNIV
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