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Silicon framework hyperbranched epoxy resin and preparation method thereof

An epoxy resin, skeleton technology, applied in the direction of epoxy resin glue, epoxy resin coating, adhesive type, etc., can solve the problems of low viscosity of hyperbranched epoxy resin, can not be reused, difficult to separate catalyst, etc. The effect of easy separation, avoiding pollution and low cost of raw materials

Active Publication Date: 2010-11-10
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The viscosity of the hyperbranched epoxy resin prepared by Zhang Daohong with trimellitic anhydride, diethylene glycol, ethylene glycol, diethylene glycol, and epichlorohydrin as the main raw material is low, but the heat resistance is not high (European Polymer Journal, 2006, 42 (3): 711-714)
In the Chinese patent application 200910062871.5, Zhang Daohong disclosed that a hyperbranched silicone resin with a terminal vinyl group or a terminal silicon-hydrogen bond was obtained by hydrolysis, and then a heat-resistant silicon-skeleton hyperbranched epoxy resin was obtained by oxidation or hydrosilylation reaction. Resin, there are a lot of acidic substances in the hydrolysis process, which is easy to cause pollution problems, and most of the hydrosilylation reaction catalysts in the prior art are homogeneous catalysts, and there are problems such as catalyst residues in the product that are difficult to separate and cannot be reused

Method used

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  • Silicon framework hyperbranched epoxy resin and preparation method thereof
  • Silicon framework hyperbranched epoxy resin and preparation method thereof
  • Silicon framework hyperbranched epoxy resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Dry natural halloysite at 120°C for 5h, after grinding, weigh 200g of halloysite and mix with 40g of hydrogen peroxide (concentration: 30wt%), soak for 24h, put it in an oven, bake at 120°C for 6h, and cool to Take it out after room temperature, then centrifuge at 3500rpm for 10min, take the light-colored solid in the upper layer and calcinate at 450°C for 8h, cool and grind to obtain purified halloysite. Dissolve 0.2g of analytically pure chloroplatinic acid in 30g of absolute ethanol, then add 100g of purified halloysite and 1.0g of analytically pure sodium bicarbonate, ultrasonicate at 700W for 20min, then magnetically stir at room temperature for 36h, and then After standing for 12 hours, the solvent was evaporated under vacuum at 60°C to obtain a loose powder, and then the powder was put into a Buchner funnel with a filter paper, washed 3 times with 20ml of distilled water each time, and the sodium chloride was washed out. The halloysite-supported platinum catalyst...

Embodiment 2

[0035] Dry the natural halloysite at 100°C for 8h, after grinding, weigh 200g of halloysite and mix with 60g of hydrogen peroxide (concentration: 30wt%), soak it for 12h, put it in an oven, bake it at 120°C for 6h, and cool to Take it out after room temperature, then centrifuge at 4000rpm for 10min, take the light-colored solid in the upper layer and calcinate at 600°C for 7h, cool and grind to obtain purified halloysite. Dissolve 0.5g of analytically pure chloroplatinic acid in 30g of analytically pure isopropanol, then add 100g of purified halloysite and 1.5g of analytically pure sodium bicarbonate, ultrasonicate at 900W for 15min, and then magnetically stir at room temperature 30h, after 10h at room temperature, spin off the solvent at 60°C under vacuum to obtain a loose powder, then put the powder into a Buchner funnel with filter paper, wash 3 times with 20ml of distilled water each time, and wash out the chlorine. sodium chloride, and then vacuum-dried at 60° C. to obtai...

Embodiment 3

[0037] Dry the natural halloysite at 110°C for 6h, after grinding, weigh 200g of halloysite and mix it with 50g of hydrogen peroxide (concentration: 30wt%), put it in an oven for 18h and bake at 120°C for 6h, cool to room temperature Take it out, and then centrifuge at 5000rpm for 10min, take the light-colored solid in the upper layer and calcinate at 700°C for 5h, cool and grind to obtain purified halloysite. Dissolve 1.5 g of analytically pure potassium chloroplatinate in 30 g of analytically pure n-butanol, then add 100 g of purified Elo and 2.5 g of analytically pure sodium bicarbonate, ultrasonicate for 10 min at a power of 1200 W, and then magnetically stir at room temperature After 24 hours, after standing at room temperature for 13 hours, the solvent was evaporated under vacuum at 60°C to obtain a loose powder, and then the powder was put into a Buchner funnel with filter paper, and washed 3 times with 20ml of distilled water each time to wash out the chlorine. sodium ...

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Abstract

The invention discloses a silicon framework hyperbranched epoxy resin and a preparation method thereof. Firstly, compound A containing two moles of silicon-hydrogen bond, compound B containing three moles of double bond and self-made halloysite supported platinum catalyst are uniformly mixed, and are stirred under the temperature of 30DEG C to 100DEG C to react for 5 to 10 hours, so that the double bond can fully reacts, and thereby hyperbranched organic silicon resin, the end group of which is the silicon-hydrogen bond, is obtained; then, compound C containing a epoxy group is added in the hyperbranched organic silicon resin, and is stirred under the temperature of 60DEG C to 120DEG C to react for 10 to 15 hours until the silicon-hydrogen bond fully reacts, hydroquinone as polymerization inhibitor is then added, and after vacuumization, the silicon framework hyperbranched epoxy resin is obtained. The method has the advantages of simple technique and easily obtained materials, and does need organic solvent and processes such as washing, thus avoiding environment pollution caused by conventional organic solvent and washing for preparing organic silicon resin, and the obtained product is expected to be applied to fields such as the strengthening and toughening of epoxy resin and solventless, low-volatility epoxy resin coating.

Description

technical field [0001] The invention relates to the technical field of hyperbranched epoxy resin preparation, in particular to a silicon skeleton hyperbranched epoxy resin and a preparation method thereof. Background technique [0002] The research on the synthesis of hyperbranched epoxy resin originated in 1993. PCT international application WO9317060 discloses that an aliphatic hyperbranched epoxy resin with higher viscosity can be synthesized by using dimethylolpropionic acid as raw material, trimethylolpropane and epichlorohydrin to react. The viscosity of the hyperbranched epoxy resin prepared by Zhang Daohong with trimellitic anhydride, diethylene glycol, ethylene glycol, diethylene glycol, and epichlorohydrin as the main raw material is low, but the heat resistance is not high (European Polymer Journal, 2006, 42 (3): 711-714). In the Chinese patent application 200910062871.5, Zhang Daohong disclosed that a hyperbranched silicone resin with a terminal vinyl group or ...

Claims

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Application Information

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IPC IPC(8): C08G59/02C08G77/38C08G77/12C08G77/08C09J163/00C09J183/04C09D163/00C09D183/04C08L63/00C08L83/04
Inventor 张道洪火文君王晶李廷成周继亮李琳张爱清李金林
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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