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A kind of high temperature resistant phosphorus nitrogen type solvent-free epoxy matrix resin and preparation method thereof

A technology of epoxy matrix and epoxy resin, applied in the field of polymer resin, can solve the problems of high cost, high price, and unfavorable large-scale popularization and application of polyetherimide resin.

Inactive Publication Date: 2017-10-03
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] 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 application, can only be limited to some special fields

Method used

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  • A kind of high temperature resistant phosphorus nitrogen type solvent-free epoxy matrix resin and preparation method thereof
  • A kind of high temperature resistant phosphorus nitrogen type solvent-free epoxy matrix resin and preparation method thereof
  • A kind of high temperature resistant phosphorus nitrogen type solvent-free epoxy matrix resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 2.0 grams of 2,2-bis[4-(2,4-bismaleimidophenoxy)phenyl]propane tetramaleimide resin, 10.0 grams of 1,3-bismaleimide Aminobenzene and 35.0 grams of 2,2-bis[4-(2-trifluoromethyl-4-maleimidophenoxy)phenyl]propane, 8.0 grams of 9,10-dihydro-9- Oxa-10-phosphaphenanthrene-10-oxide was placed in a reaction kettle, heated to 120°C and stirred for 0.5 hours, then cooled to 80°C, 20.0 g of CE-793 was added, stirred and mixed evenly to obtain 75.0 Gram component A, denoted as A1.

[0038] Add 25.0 grams of dicyandiamide, 2.0 grams of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and 120 grams of N,N-dimethylformamide into the reaction kettle, and heat up to 130°C, stirred and reacted for 3 hours, distilled under reduced pressure, recovered the solvent, precipitated a solid product, and dried in vacuo to obtain 27.0 g of dicyandiamide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10 -Oxide copolymer (BDP), which is the B component, denoted as B1.

[0039] Add 50.0 grams of...

Embodiment 2

[0042] 6.0 grams of 1,4-bis(2,4-bismaleimidophenoxy) pyrene tetramaleimide resin and 4.0 grams of 2,2-bis[4-(2,4-dimaleimide Leimidophenoxy)phenyl]propane tetramaleimide resin, 10.0 grams of 2,2-bis[4-(2-trifluoromethyl-4-maleimidophenoxy ) phenyl]propane, 25.0 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide were put into the reaction kettle, heated to 110°C and stirred for 1 hour, then cooled to 80°C After ℃, add 200.0 grams of hydrogenated bisphenol A epoxy resin, stir and mix evenly to obtain 245.0 grams of component A, which is designated as A2.

[0043] Add 95.0 grams of dicyandiamide, 35.0 grams of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and 620 grams of N,N-dimethylformamide into the reaction kettle, and heat up to 150°C, stirred and reacted for 2 hours, distilled under reduced pressure, recovered the solvent, precipitated a solid product, and dried in vacuo to obtain 130.0 g of dicyandiamide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10 -Oxide ...

Embodiment 3

[0047] 10.0 grams of 2,2-bis[4-(2,4-bismaleimidophenoxy)phenyl]propane tetramaleimide resin, 30.0 grams of 4,4'-bismaleimide Iminodiphenylmethane and 10.0 g 2,2-bis[4-(2-trifluoromethyl-4-maleimidophenoxy)phenyl]propane, 50.0 g 9,10-dihydro -9-oxa-10-phosphaphenanthrene-10-oxide was put into the reaction kettle, heated to 120°C and stirred for 1 hour, then cooled to 80°C, and 20.0 grams of hydrogenated bisphenol A epoxy resin 200.0 Gram CE-793, after stirring and mixing uniformly, obtain 320.0 grams of A component, denoted as A3.

[0048] Add 25.0 grams of dicyandiamide, 5.0 grams of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, and 120 grams of N,N-dimethylformamide into the reaction kettle, and heat up to 140°C, stirred and reacted for 2.5 hours, distilled under reduced pressure, recovered the solvent, precipitated a solid product, and dried in vacuo to obtain 30.0 g of dicyandiamide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10 -Oxide copolymer (BDP), that is, th...

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Abstract

The invention relates to a high-temperature-resistant phosphorus-nitrogen solvent-free epoxy matrix resin and a preparation method thereof, comprising tetramaleimide resin, bismaleimide resin, DOPO, dicyandiamide, epoxy resin, SR‑ 22000 silicone resin, accelerator and reactive diluent composition. The preparation method includes: (1) put tetramaleimide resin, bismaleimide resin, and DOPO into a reaction kettle for reaction, cool down after the reaction is completed, add active diluent, and stir evenly to obtain component A; (2) Add dicyandiamide, DOPO, and N,N-dimethylformamide to the reactor to react to obtain component B; (3) Add epoxy resin and SR-22000 silicone resin to the reactor to react, After the reaction is completed, cool down, add active diluent, stir evenly to obtain component C; (4) Stir and mix components A, B, and C for reaction, cool down, add accelerator, and stir evenly. The invention has the advantages of simple operation, excellent comprehensiveness, environmental friendliness and good application prospect.

Description

technical field [0001] The invention belongs to the field of polymer resins, and in particular relates to a high-temperature-resistant phosphorus-nitrogen type solvent-free epoxy matrix resin and a preparation method thereof. Background technique [0002] Epoxy resin generally refers to a polymer prepolymer containing two or more epoxy groups, with aliphatic, alicyclic or aromatic chain segments as the main chain. It reacts with a curing agent to form a three-dimensional network thermosetting material, which has good performance and is used in various fields. There are many types of epoxy resins, which can be divided into five categories according to their chemical structure and the combination of epoxy groups, namely: glycidyl ethers, glycidyl esters, glycidyl amines, aliphatic epoxy compounds, alicyclic In addition, there are heterocyclic epoxy resins and mixed epoxy resins, that is, high-performance epoxy resins containing heterocyclic rings in the molecular structure an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L63/00C08L79/08C08L85/02C08G79/02
Inventor 虞鑫海吴冯洪颖王婧怡倪柳青
Owner DONGHUA UNIV