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A kind of high temperature resistant hyperbranched epoxy resin and preparation method thereof

An epoxy resin and high-temperature-resistant technology, which is applied in the field of hyperbranched epoxy resin and its preparation, can solve the problems of low glass transition temperature, low heat resistance, and difficult aerospace high-temperature resistant resins, etc., to achieve improved glass Transformation temperature, short reaction time, and low cost

Active Publication Date: 2020-09-15
WUHAN HYPERBRANCHED POLYMER RESINS SCI& TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the heat resistance and glass transition temperature of epoxy resins prepared by all technologies are still not high, and it is difficult to meet the requirements of aerospace high-temperature resistant resins, which inhibits the development of epoxy resins in structural materials and aerospace composite materials.

Method used

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  • A kind of high temperature resistant hyperbranched epoxy resin and preparation method thereof
  • A kind of high temperature resistant hyperbranched epoxy resin and preparation method thereof
  • A kind of high temperature resistant hyperbranched epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1 A kind of high temperature resistant hyperbranched epoxy resin, its preparation method step is as follows:

[0046] (a) 0.20mol trimethylolpropane (TMP), 0.15mol dicarboxyimide compound (A2-01), 0.15mol xylene and zinc acetate (the quality of zinc acetate is 0.5% of the total mass of TMP and A2-01) %) mixed evenly, stirred and reacted at 180°C for 10h, then vacuumized at 110°C to remove xylene to obtain a hydroxyl-terminated hyperbranched polymer (HHBP-06, containing 6mol hydroxyl groups per mole of HHBP-06), the number average The molecular weight is about 1500g / mol.

[0047] (b) Add 0.01mol HHBP-06, 0.12mol epichlorohydrin and 0.006mol tetrabutylammonium bromide into a three-necked flask, stir and react at about 120°C for 5 hours, and then vacuum out excess epichlorohydrin, Then add 0.06mol tetrahydrofuran and 0.012mol sodium hydroxide to the three-necked flask, then stir and react at -5~0°C for 8 hours, stop the reaction, let the layers stand, wash the ...

Embodiment 2

[0048] Embodiment 2 A kind of high temperature resistant hyperbranched epoxy resin, its preparation method step is as follows:

[0049] (a) 0.23mol tris (2-hydroxyethyl) isocyanurate (THEIC), 0.225mol dicarboximide compound (A2-02), 0.69mol xylene and tetrapropyl titanate (titanic acid The quality of tetrapropyl ester is 1.0% of the total mass of THEIC and A2-02) mixed uniformly, stirred and reacted at 140°C for 16h, and then vacuumized at 100°C to remove xylene to obtain a hydroxyl-terminated hyperbranched polymer (HHBP- 48, each mole of HHBP-48 contains 48mol hydroxyl groups), and the number average molecular weight is about 27000g / mol.

[0050] (b) Add 0.01mol HHBP-48, 1.92mol epichlorohydrin and 0.0024mol hexadecyltriethylammonium bromide into a three-necked flask, stir and react at about 130°C for 4 hours, and then vacuum out the excess ring Oxychloropropane, then add 1.92mol ethyl acetate and 0.096mol potassium hydroxide to the three-necked flask, then stir and react at...

Embodiment 3

[0051] Embodiment 3 A kind of high temperature resistant hyperbranched epoxy resin, its preparation method step is as follows:

[0052] (a) 0.04mol tris (2-hydroxyethyl) isocyanurate (THEIC), 0.09mol dicarboximide compound (A2-03), 0.06mol xylene, 0.02mol N-methylpyrrolidone and Tetrabutyl titanate (the quality of tetrabutyl titanate is 1.5% of the total mass of THEIC and A2-03) was mixed uniformly, stirred and reacted at 160°C for 14h, and then vacuumized at 120°C to remove xylene and N-formaldehyde Based on pyrrolidone, a carboxyl-terminated hyperbranched polymer (CHBP-06, containing 6 mol carboxyl groups per mole of CHBP-06) was obtained, with a number average molecular weight of about 3200 g / mol.

[0053] (b) Add 0.01mol CHBP-06, 0.6mol epichlorohydrin, and 0.006mol cetyltrimethylammonium bromide into a three-necked flask, stir and react at about 140°C for 3 hours, and then vacuum out the excess ring Oxychloropropane, then add 0.5mol dioxane, 0.4mol butyl acetate and 0.48...

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Abstract

The invention belongs to the technical field of epoxy resin and particularly discloses high temperature-resisting hyperbranched epoxy resin and a preparation method thereof. The preparation method comprises the following steps: enabling a dicarboxyl imide compound to react with a trihydroxy compound to prepare a carboxyl-terminated or hydroxyl-terminated hyperbranched polymer; then enabling the carboxyl-terminated or hydroxyl-terminated hyperbranched polymer to react with epoxy chloropropane under the action of a ring opening catalyst to obtain an addition product; carrying out ring closing reaction on the addition product under the action of an organic solvent and an alkaline catalyst to generate the high temperature-resisting hyperbranched epoxy resin with the molecular weight of 1800 to29000 g / mol. The preparation method disclosed by the invention adopts a simple technology; the product has the properties of low viscosity, high temperature resistance and self-reinforcing tougheningfunction and is expected to be applied to the fields of enhancing and toughening of the epoxy resin, electronic packaging, solvent-free high temperature resisting coatings and the like.

Description

technical field [0001] The invention relates to the technical field of hyperbranched epoxy resin and its preparation method, in particular to a high temperature resistant hyperbranched epoxy resin and its preparation method. Background technique [0002] The research on the synthesis of hyperbranched epoxy resin originated in 1993. The PCT international application patent (WO9317060) revealed that using dimethylolpropionic acid as raw material, trimethylolpropane and epichlorohydrin can be used to synthesize fat with higher viscosity family of sulfur-containing hyperbranched epoxy resins. The inventor of the present application (Zhang Daohong) invented nitrogen heterocycle hyperbranched epoxy resin, silicon skeleton hyperbranched epoxy resin and degradable hyperbranched epoxy resin (ZL200910029024.9, ZL200910029026.8, ZL200910062871) with high heat-resistant temperature .5, ZL201010224451.5, ZL201510855381.6). The preparation technology of the hyperbranched epoxy resin of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/04C08G59/12C08L63/00C09D163/00
CPCC08G59/04C08G59/12C08L63/00C09D163/00
Inventor 张道洪卢燕芬于成龙王怡莓张俊珩
Owner WUHAN HYPERBRANCHED POLYMER RESINS SCI& TECH CO LTD
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