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Preparation method of modified dicyclopentadiene type cyanate ester resin with low hygroscopicity

A technology of dicyclopentadiene-type cyanate ester and low hygroscopicity is applied in the field of preparation of modified dicyclopentadiene-type cyanate ester resin, and can solve the problems of high hygroscopicity, poor toughness, accelerated system aging, etc.

Active Publication Date: 2019-10-25
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, like other types of cyanate resins, the high crosslinking density of dicyclopentadiene type cyanate resins causes its cured products to be brittle and poor in toughness, thereby limiting its application range; and the existing cyanate resins Most of the resin toughening methods are to reduce its cross-linking density, but it will lead to high hygroscopicity, especially in a slightly higher temperature environment, water molecules penetrate into the resin, which will reduce the intermolecular force of the material in the resin, resulting in the resin's The decline in mechanical properties will accelerate the aging process of the system, causing the performance of the modified cyanate ester resin system to decline rapidly, thus losing the purpose of toughening modification

Method used

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  • Preparation method of modified dicyclopentadiene type cyanate ester resin with low hygroscopicity
  • Preparation method of modified dicyclopentadiene type cyanate ester resin with low hygroscopicity
  • Preparation method of modified dicyclopentadiene type cyanate ester resin with low hygroscopicity

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Experimental program
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Effect test

Embodiment 1

[0049] The preparation method of the modified dicyclopentadiene type cyanate resin with low hygroscopicity is:

[0050] Weigh 10g of dicyclopentadiene-type cyanate and add it to a three-necked flask equipped with an electric stirring device, add 1g of modifier D, heat up to 85°C, keep stirring and mix for 20min, then add 0.1g of catalyst dilauric acid dilaurate Butyl tin, heat up to 140°C, keep stirring at constant temperature for curing reaction for 30 minutes, and then obtain modified dicyclopentadiene cyanate resin; dicyclopentadiene cyanate viscosity is 30-150mpa·S / 25°C;

[0051] The infrared characterization of modified dicyclopentadiene type cyanate resin is as follows: IR(KBr): 1742(-NH-C(=O)-NH-), 1732(-COO-), 1562 / 1367(triazine ring), 1177(-O-Si-C-)cm -1 ;2271cm -1 At-OCN disappeared, 1742cm -1 -NH-C(=O)-NH- is a strong absorption peak, and the amino group on the modifying agent has undergone block polymerization with dicyclopentadiene cyanate.

Embodiment 2

[0053] The preparation method of the modified dicyclopentadiene type cyanate resin with low hygroscopicity is:

[0054] Weigh 10g of dicyclopentadiene-type cyanate into a three-necked flask equipped with an electric stirring device, add 1.5g of modifier D, heat up to 90°C, keep stirring and mix for 20min, then add 0.3g of catalyst dilauric acid For dibutyltin, heat up to 150°C, keep stirring at constant temperature to carry out curing reaction for 45 minutes, and then obtain a modified dicyclopentadiene cyanate resin; the viscosity of dicyclopentadiene cyanate is 30-150mpa·S / 25°C;

[0055] The infrared characterization of modified dicyclopentadiene type cyanate resin is as follows: IR(KBr): 1742(-NH-C(=O)-NH-), 1732(-COO-), 1562 / 1367(triazine ring), 1177(-O-Si-C-)cm -1 ;2271cm -1 At-OCN disappeared, 1742cm -1 -NH-C(=O)-NH- is a strong absorption peak, and the amino group on the modifying agent has undergone block polymerization with dicyclopentadiene cyanate.

Embodiment 3

[0057] The preparation method of the modified dicyclopentadiene type cyanate resin with low hygroscopicity is:

[0058] Weigh 10g of dicyclopentadiene-type cyanate into a three-necked flask equipped with an electric stirring device, add 1.2g of modifier D, heat up to 90°C, keep stirring and mix for 20min, then add 0.2g of catalyst dilauric acid Dibutyltin, heat up to 145°C, keep stirring at constant temperature for curing reaction for 35 minutes, and then obtain modified dicyclopentadiene cyanate resin; the viscosity of dicyclopentadiene cyanate is 30-150mpa·S / 25°C

[0059] The infrared characterization of modified dicyclopentadiene type cyanate resin is as follows: IR(KBr): 1742(-NH-C(=O)-NH-), 1732(-COO-), 1562 / 1367(triazine ring), 1177(-O-Si-C-)cm -1 ;2271cm -1 At-OCN disappeared, 1742cm -1 -NH-C(=O)-NH- is a strong absorption peak, and the amino group on the modifying agent has undergone block polymerization with dicyclopentadiene cyanate.

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Abstract

The invention discloses a preparation method of a modified dicyclopentadiene type cyanate ester resin with low hygroscopicity. Firstly, a modifier with toughening and water-resistant properties is prepared, the modifier has two amino groups, and can react with -OCN groups of a dicyclopentadiene type cyanate ester to carry out front-end polymerization, a soft segment is introduced to achieve the purpose of toughening, and at the same time, the modifier contains a large amount of organosilicone, the organosilicone is introduced by a block bonding manner, the organosilicone has a stable dielectric constant and dielectric loss in a relatively wide temperature range, has relatively high flexibility, and can greatly improve toughness of the cyanate ester, and at the same time, the organosiliconehas good oxidation resistance and low surface energy, the organosilicone is embedded in a space networking resin, and when the resin is cured, silicon atoms are released to the surface of the resin due to low surface energy of the organosilicone, so that the modified cyanate ester resin has good water resistance, and the problem that hygroscopicity is increased during a resin toughing process issolved.

Description

technical field [0001] The invention relates to the technical field of cyanate resin synthesis, in particular to a preparation method of a modified dicyclopentadiene type cyanate resin with low hygroscopicity. Background technique [0002] The development of packaging materials is developing in the direction of high purity, high reliability, high thermal conductivity, high drought resistance, high heat and humidity resistance, high bonding strength, low stress, low expansion, low viscosity, easy processing, and low environmental pollution. The substrate material uses phenolic or epoxy resin as the matrix, and the glass transition temperature of the material is only 130-170°C. Due to the constraints of material heat resistance and high temperature rigidity, it cannot be used in the IC packaging industry; cyanate (CE) resin is a A new type of high-performance thermosetting resin, the monomer of which contains two or more cyanate functional groups (-OCN), and forms a highly cro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C07F7/08
CPCC07F7/0838C07F7/0889C08G73/0644C08G73/065Y02P20/55
Inventor 季静静金中宝王跃彪朱芝峰
Owner YANGZHOU TECHIA MATERIAL CO LTD
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