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Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material

A technology of nano-silica and hyperbranched polymers, which is applied in the coating and other directions, can solve the problems of insignificant anti-oxidation resistance, low mercapto group introduction, and limited addition, and achieve good transparency, simple synthesis process, The effect of improving dispersion

Active Publication Date: 2014-04-23
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, simply grafting small molecular mercapto compounds on the surface of nano-silica not only has the common problems of the above-mentioned modified nano-silica, but also the low grafting rate makes the introduction of mercapto groups low, and the anti-oxidation effect is not obvious. Addition in limited quantities in UV-curable coatings

Method used

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  • Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material
  • Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material
  • Preparation method of hyperbranched polymer-modified nano-silicon dioxide hybrid material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] a) Add 5g of nano-silica and 30mL of toluene into a 250mL four-neck flask equipped with a thermometer, agitator, and a condenser tube. After ultrasonically dispersing for 1 hour, add 5mL of water, 5mL of absolute ethanol and 100g of γ- The mixed solution composed of mercaptopropyltrimethoxysilane (KH590), the pH of the system is adjusted to 6 with acetic acid, the grafting reaction is carried out at 50°C for 10 hours, the product is filtered, washed and dried to obtain the modified nano-silica with mercapto groups on the surface , that is, the first generation of modified nano-silica.

[0030] b) Take 5g of the first-generation modified nano-silica and 30mL of toluene, ultrasonically disperse it in a 250mL four-necked bottle for 1 hour, add 50g of trimethylolpropane triacrylate and 0.05g of benzophenone, and React for 8 hours, filter, wash, and dry to obtain modified nano-silica whose surface is acrylate, that is, the second-generation modified nano-silica.

[0031] c)...

Embodiment 2

[0043] a) Add 3g of nano-silica and 30mL of xylene into a 250mL four-neck flask equipped with a thermometer, agitator, and a condenser tube. After ultrasonic dispersion for 1 hour, add 7mL of water, 4mL of absolute ethanol and 100g of γ under stirring. -Mixed solution composed of mercaptopropyltriethoxysilane (KH580), the pH of the system is adjusted to 5 with acetic acid, the grafting reaction is carried out at 50°C for 8 hours, the product is filtered, washed and dried to obtain the modified nano-dioxide Silicon, the first generation of modified nano-silica.

[0044] b) Take 3g of the first-generation modified nano-silica and 30mL of xylene, ultrasonically disperse it in a 250mL four-necked bottle for 1 hour, add 30g of pentaerythritol tetraacrylate and 0.05g of 2-hydroxy-2-methyl-1-benzene Base-1-acetone, react under ultraviolet light for 8 hours, filter, wash, and dry to obtain modified nano-silica with acrylate surface, that is, the second-generation modified nano-silica....

Embodiment 3

[0049] a) Add 4g of nano-silica and 15mL of isopropanol into a 250mL four-neck flask equipped with a thermometer, a stirrer, and a condenser tube. After ultrasonic dispersion for 1.5 hours, add 5mL of water, 5mL of absolute ethanol and 180g of γ-mercaptopropyltrimethoxysilane (KH590) mixed solution, adjusted the pH of the system to 5.5 with acetic acid, grafted at 50°C for 8 hours, filtered the product, washed, and dried to obtain a modified nanometer with mercapto groups on the surface. Silicon oxide is the first generation of modified nano-silica.

[0050] b) Take 3g of the first-generation modified nano-silica and 20mL of toluene, ultrasonically disperse it in a 250mL four-necked bottle for 0.5h, add 80g of 1,6-hexanediol diacrylate and 0.1g of 1-hydroxycyclohexylbenzene base ketone, reacted for 10 h under ultraviolet light irradiation, filtered, washed and dried to obtain modified nano-silica with acrylate surface, that is, the second-generation modified nano-silica.

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Abstract

The invention relates to a preparation method of a hyperbranched polymer-modified nano-silicon dioxide hybrid material. The preparation method comprises the following steps: grafting a mercapto group-containing silane coupling agent to the surface of nano-silicon dioxide, utilizing a surface mercapto group and polyfunctional acrylic ester to perform click reaction to form the modified nano-silicon dioxide with the tail end of the acrylic ester, further performing the click reaction with a polyfunctional mercapto compound to form the modified silicon dioxide with the tail end of the mercapto group, repeating the operation between the polyfunctional acrylic ester and the polyfunctional mercapto compound for multiple times, and forming a hyperbranched polymer on the surface of the silicon dioxide. The hyperbranched polymer-modified nano-silicon dioxide hybrid material prepared by the preparation method provided by the invention has the mercapto group at the tail end and a hyperbranched structure, when the hyperbranched polymer-modified nano-silicon dioxide hybrid material is applied in an ultraviolet curing coating, the heat resistance, the hardness, the wear resistance and other mechanical properties of the coating can be improved, and the hyperbranched polymer-modified nano-silicon dioxide hybrid material can particularly solve the problems of dispersion and migration of the nano-silicon dioxide in the ultraviolet curing coating and the problem of oxygen polymerization inhibition of the ultraviolet curing coating.

Description

technical field [0001] The invention relates to an organic-inorganic hybrid material, in particular to a preparation method of a hyperbranched polymer-modified nano-silica hybrid material. Background technique [0002] Nano-silica is an effective additive commonly used in UV-curable coatings to improve coating hardness, wear resistance, adhesion and other properties. However, due to the presence of a large number of hydroxyl groups on its surface, it is hydrophilic Oleophobic properties, direct addition to UV-curable coatings not only has poor compatibility and is difficult to disperse, but also nano-silica will absorb and reflect part of the UV light, which will affect the curing speed. Therefore, when using nano-silica in the UV curing system, it must be surface modified or modified. [0003] In order to improve the dispersion of nano-silica in UV-curable coatings and reduce its negative effects, polymerizable acrylates, tertiary amine structures or mercapto groups that c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C09D151/10
Inventor 凌丽霞吴建兵
Owner TAIYUAN UNIV OF TECH
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