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High-temperature endurable active toughener powder used for epoxy resin and preparation method thereof

A technology for active toughening agent and epoxy resin, which is applied in the field of high-temperature-resistant active toughening agent powder for epoxy resin and its preparation, can solve the problems that have not yet been published in literature or patent reports, and achieve low cost and low molecular weight. Easy and mild reaction conditions

Inactive Publication Date: 2009-10-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The molecular structure and preparation method of the high temperature-resistant active toughening agent powder for epoxy resin disclosed by the present invention have not yet been published in the literature or patent reports

Method used

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  • High-temperature endurable active toughener powder used for epoxy resin and preparation method thereof
  • High-temperature endurable active toughener powder used for epoxy resin and preparation method thereof
  • High-temperature endurable active toughener powder used for epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 21.6 g (0.1 mole) of 3,3'-diamino-4,4'-dihydroxybiphenyl (DADHBP), 41.0 g (0.1 mole) of 2,2-bis[4-(4-aminophenoxy Base) phenyl] propane (BAPP), 62.0 grams (0.2 moles) of 3,3',4,4'-tetracarboxydiphenyl ether dianhydride (ODPA), 0.015 moles of isoquinoline and 1246 grams of o-cresol Put it into the reaction kettle, stir, heat up to the temperature range of 100°C-150°C, and after maintaining the reaction for 5 hours, pour it into 24920 grams of ethanol precipitating agent under high-speed stirring state while it is hot, and precipitate solid powder, filter and use Wash with ethanol for 2-3 times, soak in acetone for 5 hours, filter, wash with deionized water for 2-3 times, and dry to obtain 112.7 grams of 1DADHBP / 1BAPP / 2ODPA-PI white powder, which is a high-temperature-resistant active toughening agent for epoxy resin Powder (theoretical amount 117.4 grams), yield is 96%, and its Fourier transformation infrared spectrum (FTIR) is as figure 2 As shown, the thermogravimetr...

Embodiment 2

[0060] 21.6 g (0.1 mol) of 3,3'-diamino-4,4'-dihydroxybiphenyl (DADHBP), 82.0 g (0.2 mol) of 2,2-bis[4-(4-aminophenoxy Base) phenyl] propane (BAPP), 93.0 grams (0.3 moles) of 3,3',4,4'-tetracarboxydiphenyl ether dianhydride (ODPA), 0.01 moles of isoquinoline and 983 grams of o-cresol Put it in the reaction kettle, stir, heat up to the temperature range of 100°C-150°C, and after maintaining the reaction for 5 hours, pour it into the precipitating agent of 9000 grams of ethanol and 830 grams of isopropanol under high-speed stirring state while it is hot, Precipitate solid powder, filter, wash with ethanol 2-3 times, soak in acetone for 5 hours, filter, wash with deionized water 2-3 times, dry to obtain 183.9 grams of 1DADHBP / 2BAPP / 3ODPA-PI white powder, namely epoxy resin With high temperature resistant active toughening agent powder (theoretical amount 185.8 grams), yield is 99%, and its Fourier transformation infrared spectrum (FTIR) is as Figure 4 shown.

[0061] The molec...

Embodiment 3

[0064] 21.6 g (0.1 mole) of 3,3'-diamino-4,4'-dihydroxybiphenyl (DADHBP), 123.0 g (0.3 mole) of 2,2-bis[4-(4-aminophenoxy Base) phenyl] propane (BAPP), 124.0 grams (0.4 moles) of 3,3',4,4'-tetracarboxydiphenyl ether dianhydride (ODPA), 0.005 moles of isoquinoline, 0.002 moles of pyridine and 2148 grams Put o-cresol into the reaction kettle, stir, heat up to the temperature range of 100°C-150°C, and after maintaining the reaction for 5 hours, pour it into the precipitate of 20,000 grams of ethanol and 10,000 grams of isopropanol under high-speed stirring state while it is hot. In the analysis agent, a solid powder was precipitated, filtered, washed 2-3 times with ethanol, soaked in acetone for 5 hours, filtered, washed 2-3 times with deionized water, and dried to obtain 238.9 grams of 1DADHBP / 3BAPP / 4ODPA-PI white powder, Promptly epoxy resin is used high temperature resistant active toughening agent powder (theoretical amount 254.2 grams), and yield is 94%, and its Fourier tran...

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Abstract

The invention relates to a high-temperature endurable active toughener powder used for epoxy resin, which comprises a general molecular structural formula as right, wherein -R1- is the diatomic linking group of aromatic series binary primary amine containing phenolic hydroxyl groups and -R2- is the diatomic linking group of aromatic series binary estolide molecule. The preparation method thereof comprises the steps of mixing the aromatic series binary primary amine, 2,2-Bis[4-(4-aminophenoxy)phenyl]propane and the aromatic series binary estolide with the mol ratio ranging from 1:1-5:2-6 in phenol solvent to react with each other at a temperature ranging from 100 to 150 DEG C for 5 hours and then pouring the obtained products into a precipitator stirred at a high speed to precipitate solid powder which is then filtered, washed, marinated, filtered and dried for preparing the high-temperature endurable active toughener powder for epoxy resin. The preparation method has the advantages of simple process and low cost, is environmental friendly, can finish the preparation process in universal equipment, and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the field of high-temperature-resistant active toughening agent powder and its preparation, and in particular relates to a high-temperature-resistant active toughening agent powder for epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin has excellent bonding performance and molding processability, and its own epoxy group can be combined with various functional groups (such as primary amino group, secondary amino group, tertiary amino group, hydroxyl group, carboxyl group, amido group, urethane group, Mercapto group, acid anhydride group, etc.) react chemically, so it has excellent compatibility and compatibility; its cured product has excellent electrical insulation properties, chemical resistance, mechanical properties, etc. However, its heat resistance is relatively low. To improve its heat resistance, it is often necessary to modify it, such as increasing the crosslinking density and aroma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J3/14C08L63/00C08L79/08
Inventor 虞鑫海费斐徐永芬
Owner DONGHUA UNIV
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