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Preparing methods of liquid crystal epoxy resin oligomer and epoxy resin composition

A technology of epoxy resin and oligomers, which is applied in the field of polymer material preparation to achieve excellent adhesion, solve the problem of encapsulation cracks, and improve thermal conductivity

Inactive Publication Date: 2009-11-25
GUANGDONG RONGTAI IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] To sum up, the liquid crystal epoxy resins involved in the current patents published in China are all main chain liquid crystal epoxy resins, that is, the liquid crystal elements are on the main chain of the epoxy resin, and the liquid crystal elements are hung on the side chains No Chinese patent report yet

Method used

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  • Preparing methods of liquid crystal epoxy resin oligomer and epoxy resin composition
  • Preparing methods of liquid crystal epoxy resin oligomer and epoxy resin composition
  • Preparing methods of liquid crystal epoxy resin oligomer and epoxy resin composition

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Experimental program
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Embodiment 1

[0038] The present embodiment provides a kind of preparation method of liquid crystal epoxy resin oligomer, comprising:

[0039] Taking p-phenylphenol (required purity ≥ 99%), epichlorohydrin, phase transfer catalyst, sodium hydroxide and distilled water as raw materials, based on the amount of p-phenylphenol, according to the following raw materials and p-phenylphenol The mol ratio of getting other raw materials:

[0040] Epichlorohydrin: the molar ratio of p-phenylphenol=1~5:1, phase transfer catalyst: the molar ratio of p-phenylphenol=1 / 100~1 / 50:1, sodium hydroxide: p-phenylphenol Molar ratio=1~4:0.5~2, distilled water: molar ratio of p-phenylphenol=1 / 100~1 / 20:1;

[0041] Add white powdery p-phenylphenol in the reaction vessel, and add epichlorohydrin, dissolve, add phase transfer catalyst, add sodium hydroxide again, and add distilled water dropwise, carry out reaction according to following formula (1):

[0042]

[0043] The reaction proceeds in two stages:

[0044]...

Embodiment 2

[0091] An embodiment of the present invention provides a method for preparing an epoxy resin oligomer containing a side chain liquid crystal structure, the method comprising the following steps:

[0092] Take 187.4ml of epichlorohydrin, 39g of p-phenylphenol, and 1ml of distilled water, use 18-crown-6 ether as a phase transfer catalyst, the addition amount is 0.05g, add NaOH 10g, the first stage reaction temperature is 75°C, the reaction time For 4 hours, the second stage reaction temperature was 105°C, and the reaction time was 8 hours. After the reaction, the excess epichlorohydrin was evaporated under reduced pressure, and the product was dissolved in a mixed solvent of methanol: acetone=2: 1 (volume ratio), and added Activated carbon, decolorize, filter with suction, dissolve with methanol: acetone = 2: 1 (volume ratio) mixed solvent, place the solution in a freezing water bath at ~10°C, cool and crystallize for 3 hours, filter with suction, wash 3 times with deionized wate...

Embodiment 3

[0094] The third embodiment provides an epoxy resin composition containing side chain liquid crystal epoxy resin oligomers, including the following raw materials in parts by weight, including:

[0095] 30 parts by weight of the liquid crystal epoxy resin oligomer that embodiment one makes

[0096] 10 parts by weight of o-cresol novolac epoxy resin

[0097] 20 parts by weight of melamine modified novolac resin

[0098] Silica powder (quartz powder) 150 parts by weight

[0099] Curing accelerator 2~methylimidazole 0.5 parts by weight

[0100] Toughening agent CTBN 3 parts by weight

[0101] Silane coupling agent KH-560 1.5 parts by weight

[0102] Stearic acid (lubricant) 0.8 parts by weight

[0103] Preparation method: including surface treatment of silicon micropowder, mixing of components, melt kneading, cooling, crushing, pressing into cake, packaging and low-temperature storage. Among them, the surface treatment of silicon micropowder is sprayed on silicon micropowder...

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Abstract

The invention discloses a preparing method of liquid crystal epoxy resin oligomer and epoxy resin composition. The method comprises that: p-phenylphenol, epoxy chloropropane, phase transfer catalyst, sodium hydroxide and distilled water as raw materials are reacted to prepare the liquid crystal epoxy resin oligomer. The epoxy resin composition comprises: mixing the prepared liquid crystal epoxy resin oligomer and other raw materials based on weight proportionality: 10-30 parts of liquid crystal epoxy resin oligomers by weight, 10-30 parts of o-cresol-formaldehyde epoxy resins by weight, 5-25 parts of melamine modified linear phenol aldehyde resins by weight, 60-150 parts of spherical silicon micronized quartz powders by weight, 0.1-2 parts of curing accelerators by weight, 2-10 parts of flexibilizers by weight, 0.6-5 parts of resin acceptors by weight and 0.5-5 parts of lubricants by weight, which are mixed for smelting, crushed and demagnetizing to prepare the epoxy resin composition comprising side chain liquid crystal structure. The epoxy composition has good heat-resistant property and good physical mechanical property, is suitable for the encapsulations of large scale and grand scale integrated circuits.

Description

technical field [0001] The invention relates to the technical field of polymer material preparation, in particular to a method for preparing a liquid crystal epoxy resin oligomer and an epoxy resin composition. Background technique [0002] With the development of integrated circuits towards ultra-large-scale, high-density, high-power, high-precision, multi-functional directions and the rapid development of electronic packaging technology, the development direction of epoxy molding compounds (EMC) is moving towards high purity, high reliability, High thermal conductivity, high temperature welding resistance, high moisture resistance, high bonding strength and low stress, low expansion, low water absorption, low viscosity, low environmental pollution, easy processing and other directions. To prepare such a high-performance EMC, the two most important technologies are to use special epoxy resin and increase the filling amount of silica powder. The latter must ensure the good f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/23C07D301/28C08G81/00C08L63/04C08L61/14C08K13/06
Inventor 杨明山李林楷何杰羽信全罗海平徐文玉
Owner GUANGDONG RONGTAI IND
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