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Method for preparing epoxy resin with biphenyl structure

A technology of epoxy resin and biphenyl structure, which is applied in the field of preparation of epoxy resin containing biphenyl structure, can solve the problems of epoxy resin preparation process parameters and low thermal conductivity without disclosing biphenyl structure, and solve the problem of encapsulation Effects of cracks, low melt viscosity, and reduced water absorption

Inactive Publication Date: 2010-06-09
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] ④ High thermal conductivity: With the development of high-power electronic instruments, the problem of heat dissipation of packaging materials also arises, because packaging materials are epoxy resin composite materials and organic polymer materials with low thermal conductivity
Chinese patent ZL01141578.9 discloses the preparation route of epoxy resin containing biphenyl structure, and particularly emphasizes that the content of the undesired product tetramethyldiphenoquinone contained is lower than 0.5% (mass), but no details are disclosed. The specific preparation process parameters of epoxy resin containing biphenyl structure

Method used

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  • Method for preparing epoxy resin with biphenyl structure
  • Method for preparing epoxy resin with biphenyl structure
  • Method for preparing epoxy resin with biphenyl structure

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Embodiment 1

[0027] The embodiment of the present invention provides a method for preparing an epoxy resin containing a biphenyl structure, comprising the following steps:

[0028] Put 0.01-1 mole of phase transfer catalyst into the reaction vessel, add 2-5 moles of absolute ethanol to dissolve it, then add 5-100 moles of biphenol and 10-200 moles of epichlorohydrin, Heat to 50-110°C, stir and react for 3-15 hours, add half of the NaOH solution with a total mole number of 0.1-5, react for 3-15 hours, then add the remaining half of the NaOH solution, under vacuum at -0.09MPa Distill under reduced pressure to remove excess epichlorohydrin to obtain a light yellow product; after dissolving the light yellow product in a solvent, add a decolorizing agent, filter with suction, freeze and recrystallize the filtrate at low temperature, filter with suction again, and wash with deionized water for 2~ 3 times, after vacuum drying, the light yellow crystal is obtained, which is the epoxy resin contain...

Embodiment 2

[0068] Get epichlorohydrin 187.4ml, diphenol 29.04g, ethanol 12ml, use 18-crown-6 ether as a phase transfer catalyst, the addition is 0.1g, add NaOH solution twice, add 8g concentration for the first time 30% NaOH, adding 8g concentration for the second time is 15% NaOH, and temperature of reaction is 85 ℃, and total reaction time is 6 hours, after reaction finishes, depressurizes and distills excess epichlorohydrin, and product uses methyl alcohol: acetone= Dissolve in a 2:1 (volume ratio) mixed solvent, add activated carbon for decolorization, filter with suction, and then 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 , after suction filtration, wash 3 times with deionized water at room temperature, and dry the product in a vacuum oven at 60° C. for 8 hours to finally obtain a biphenyl-containing epoxy resin with a yield of 93%. The epoxy equivalent of this biphenyl-c...

Embodiment 3

[0070] Take 187.4ml of epichlorohydrin, 29.04g of biphenol, and 12ml of ethanol, use 18-crown-6 ether as a phase transfer catalyst, the addition amount is 0.2g, add NaOH in two times, the concentration of adding 8g for the first time is 30 % NaOH, adding 8g concentration for the second time is 15% NaOH, and temperature of reaction is 80 ℃, and total reaction time is 8 hours, after having reacted, decompression evaporates excessive epichlorohydrin, and product uses butanol: acetone= Dissolve in a 1:1 (volume ratio) mixed solvent, add activated carbon for decolorization, filter with suction, then dissolve with butanol: acetone = 1:1 (volume ratio) mixed solvent, place the solution in a freezing water bath at -20°C, cool and crystallize for 1 hour, suction filtration, and the product after washing 3 times with deionized water at room temperature was dried in a vacuum oven at 60° C. for 8 hours to finally obtain a biphenyl-containing epoxy resin with a yield of 90%. The epoxy equi...

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Abstract

The embodiment of the invention provides a method for preparing epoxy resin with a biphenyl structure, which comprises the following steps: placing 0.01-1mol of phase transfer catalyst (PTC) in a reaction vessel; adding 2-5 mol of absolute ethyl alcohol to dissolve the phase transfer catalyst; then adding 5-100mol of C12H10O2 and 10-200mol of epichlorohydrin; heating to 50-110 DEG C, stirring and reacting for 3-15h; taking NaOH solution, adding half volume of the NaOH solution, reacting for 3-15h, then adding the rest NaOH solution; performing reduced pressure distillation under the vacuum condition of minus 0.09MPa to remove redundant epichlorohydrin to obtain a faint yellow product; dissolving the faint yellow product by organic solvent, adding decolorizer, filtering, freezing and recrystallizing the filtrate; and filtering once again, washing the frozen and recrystallized product by deionized water, vacuum drying the frozen and recrystallized product to obtain faint yellow crystals, namely the epoxy resin with a biphenyl structure. The prepared resin can be used for encapsulating large-scale integrated circuits and electronic elements.

Description

technical field [0001] The invention relates to the technical field of preparation of special epoxy resins, in particular to a preparation method of epoxy resins containing a biphenyl structure. Background technique [0002] Epoxy resin has excellent physical and mechanical properties and electrical properties, and has a good cost performance ratio, so it is widely used as coatings, adhesives, composite resin matrix, electronic packaging materials, etc. In particular, epoxy resins have played a significant role in the packaging of electronic components and integrated circuits (ICs). At present, more than 95% of electronic components and integrated circuits are packaged with epoxy resin composite materials. The matrix resin used therein is mainly o-cresol novolac epoxy resin. [0003] At present, the development trend of packaging technology is: packaging is developing in the direction of small, thin, light, and high density; packaging structure is developing from single ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
Inventor 杨明山李林楷何杰羽信全罗海平肖强
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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