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A kind of high temperature resistant phosphorus bromine type solvent-free epoxy adhesive and preparation method thereof

An epoxy adhesive, phosphorus bromine type technology, applied in the direction of adhesive, epoxy resin glue, adhesive type, etc., can solve the problems of high price, high cost of polyetherimide resin, unfavorable large-scale popularization and application, etc. To achieve the effect of convenient operation, environmental friendliness and good application prospects

Inactive Publication Date: 2016-09-07
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] (2) 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BAHPFP) and other monomers are expensive, resulting in high cost of polyetherimide resin (HPEI) and adhesives, which is not conducive to Large-scale promotion and application can only be limited to some special fields

Method used

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  • A kind of high temperature resistant phosphorus bromine type solvent-free epoxy adhesive and preparation method thereof
  • A kind of high temperature resistant phosphorus bromine type solvent-free epoxy adhesive and preparation method thereof
  • A kind of high temperature resistant phosphorus bromine type solvent-free epoxy adhesive and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Put 100.0 grams of ES216 epoxy resin, 4.0 grams of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 10.0 grams of tetrabromophthalic anhydride (TBPA) into the reactor, After reacting at 110°C for 1.5 hours, add 15.0 grams of hydrogenated bisphenol A epoxy resin, stir and mix evenly to obtain 129.0 grams of component A, which is designated as A1.

[0048] 2.0 g of 4,4'-bismaleimidodiphenylmethane and 16.0 g of 2,2-bis[4-(4-maleimidophenoxy)phenyl]propane and 32.0 g of organic Put the silicone resin (YASI) into the reaction kettle, react at 130°C for 30 minutes, add 35.0 grams of CE793, stir and mix evenly to obtain 85.0 grams of component B, which is designated as B1.

[0049] Put 129.0 grams of A1 component, 85.0 grams of B1 component, 200.0 grams of dodecenyl succinic anhydride, 60.0 grams of methyl tetrahydrophthalic anhydride, and 5.0 grams of 2,4,6-tris(dimethylaminomethyl)phenol into In the reaction kettle, stir and mix evenly to obtain 479.0 grams of...

Embodiment 2

[0051] Put 100.0 grams of ES216 epoxy resin, 30.0 grams of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 35.0 grams of tetrabromophthalic anhydride (TBPA) into the reactor, After reacting at 130°C for 0.5 hours, add 25.0 grams of hydrogenated bisphenol A epoxy resin and 45.0 grams of CE793, stir and mix evenly to obtain 235.0 grams of component A, which is designated as A2.

[0052] Put 2.0 grams of 4,4'-bismaleimidodiphenylmethane and 10.0 grams of silicone resin (YASI) into the reaction kettle, and after reacting at 110°C for 60 minutes, add 10.0 grams of hydrogenated bisphenol A epoxy resin and 20.0 grams of CE793, stirred and mixed evenly to obtain 42.0 grams of component B, denoted as B2.

[0053] Put 235.0 grams of A2 component, 42.0 grams of B2 component, 80.0 grams of methyltetrahydrophthalic anhydride, 3.0 grams of aluminum acetylacetonate and 15.0 grams of 1,8-diazabicyclo[5.4.0]undecene-7 into the reaction In the kettle, stir and mix evenly to obtai...

Embodiment 3

[0055] Take an appropriate amount of the high-temperature-resistant phosphorus-bromine type solvent-free epoxy adhesives of Example 1 and Example 2, namely HTPM-1 and HTPM-2, and apply them evenly on standard stainless steel test pieces respectively. After airing at room temperature for 10 minutes, stack Combined, clamped, put into a blast oven for curing: start from room temperature to 70°C, keep warm for 2 hours, continue to heat up to 120°C, keep warm for 1 hour, continue to heat up to 170°C, keep warm for 1.5 hours, naturally Cool to room temperature. The tensile shear strength (σ) test was carried out at room temperature (25°C) and high temperature (220°C) using an electronic tensile machine, and the results are shown in Table 1.

[0056] Take appropriate amount of high temperature resistant phosphorus bromine type solvent-free epoxy adhesive of embodiment 1 and embodiment 2 respectively, i.e. HTPM-1, HTPM-2, push the film on the polytetrafluoroethylene film, place it in ...

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Abstract

The invention relates to a high-temperature-resistant, phosphorus-bromine-type and solvent-free epoxy adhesive and a preparation method thereof. The adhesive consists of ES216 epoxy resin, tetrabromophthalic anhydride, DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), bismaleimide resin, organic silicone resin, a curing agent, an accelerator and an active diluent. The preparation method comprises steps as follows: (1) placing the ES216 epoxy resin, the DOPO and the tetrabromophthalic anhydride into a reaction kettle, adding a reactive diluent after the reaction, and evenly mixing the mixture to obtain a component A; (2) placing the bismaleimide resin and the organic silicone resin into the reaction kettle, adding the active diluent after the reaction, and evenly mixing the mixture to obtain a component B; (3) placing the component A, the component B, the curing agent and the accelerator into the reaction kettle, and evenly mixing the mixture to obtain the adhesive. The adhesive can be applied to adhesion of metal, ceramic, glass and composite materials, can also be applied to technologies of RTM, VARTM, pultrusion and the like to manufacture fiber-reinforced advanced composite materials and has a bright application prospect.

Description

technical field [0001] The invention belongs to the field of epoxy adhesives, in particular to a high-temperature-resistant phosphorus-bromine type solvent-free epoxy adhesive and a preparation method thereof. Background technique [0002] Epoxy resin is widely used in various fields of national economy: whether it is high-tech field or general technology field, whether it is national defense industry or civilian industry, and even people's daily life can see its traces. [0003] There have been many research reports on the epoxy resin adhesive system, and there are also many invention patents: [0004] Yan Rui, Yu Xinhai et al [Research on Preparation and Properties of New Epoxy Adhesives, Insulating Materials, 2012, 45(2): 12-14,18] disclosed a new type of epoxy resin adhesive and its preparation method, and its performance has been systematically studied. [0005] Yu Xinhai et al [Preparation and Performance Research of Silicone Epoxy System Adhesive, Insulating Materia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J163/00C09J183/08C08G59/14C08G59/62C08G59/58
Inventor 虞鑫海陈戚倪柳青洪颖王婧怡周志伟
Owner DONGHUA UNIV
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