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Long-chain alkyl ester modified linear phenolic epoxy curing agent and preparing method thereof

A long-chain alkyl ester and novolac epoxy technology, applied in the field of online novolac epoxy curing agent and its preparation, can solve the problems of poor compatibility, unfavorable processing and packaging molding, etc., and achieve lower processing temperature and easy preparation , Improve the effect of processing fluidity

Active Publication Date: 2019-08-09
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the compatibility between the filler and the base material becomes poor, which is not conducive to processing and packaging molding, the present invention provides a long-chain alkyl ester modified novolak epoxy curing agent, and at the same time, provides a long-chain Preparation method of novolak epoxy curing agent modified by alkyl ester

Method used

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  • Long-chain alkyl ester modified linear phenolic epoxy curing agent and preparing method thereof
  • Long-chain alkyl ester modified linear phenolic epoxy curing agent and preparing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) add 200ml dichloromethane solvent to dissolve in 40.525g novolac tert-butylphenol resin (molecular weight is 500), N 2 Add 0.1ml of acid-binding agent triethylamine under the atmosphere, and stir in ice-water bath for 10min to obtain phenolic resin-dichloromethane solution;

[0027] (2) Slowly add 1.860 g of tridecanoic acid chloride dropwise into the phenolic resin-dichloromethane solution, at a slow rate of one drop per second, continue to stir for 3 hours, rise to room temperature and continue to stir for 1.5 hours to obtain long-chain alkyl ester modification phenolic resin-dichloromethane solution;

[0028] (3) Add 10 g of distilled water to the long-chain alkyl ester modified phenolic resin-methylene chloride solution to remove the acid-binding agent, separate the liquids to obtain the organic phase, remove the methylene chloride under reduced pressure, dry in a vacuum oven at 45° C. for 4 hours, and grind. The novolac epoxy curing agent modified by the long-...

Embodiment 2

[0031] (1) add 200ml dichloromethane solvent to dissolve in 40.525g novolac tert-butylphenol resin (molecular weight is 500), N 2 Add 0.1ml of acid-binding agent triethylamine under the atmosphere, and stir in ice-water bath for 10min to obtain phenolic resin-dichloromethane solution;

[0032] (2) Slowly add 1.972g myristic acid chloride dropwise into the phenolic resin-dichloromethane solution, the slow drop rate is 1 drop per second, continue to stir for 3.5h, rise to room temperature and continue stirring for 2h to obtain long-chain alkyl ester modification phenolic resin-dichloromethane solution;

[0033] (3) Add 10 g of distilled water to the long-chain alkyl ester modified phenolic resin-methylene chloride solution to remove the acid-binding agent, separate the liquids to obtain the organic phase, remove the methylene chloride under reduced pressure, dry in a vacuum oven at 45° C. for 4 hours, and grind. The novolac epoxy curing agent modified by the long-chain alkyl es...

Embodiment 3

[0036] (1) add 200ml dichloromethane solvent to dissolve in 40.525g novolac tert-butylphenol resin (molecular weight is 500), N 2 Add 0.1ml of acid-binding agent triethylamine under the atmosphere, and stir in ice-water bath for 10min to obtain phenolic resin-dichloromethane solution;

[0037] (2) Slowly add 2.423g octadecanoic acid chloride dropwise to the phenolic resin-dichloromethane solution at a slow rate of one drop per second, continue stirring for 2.5h, rise to room temperature and continue stirring for 1h to obtain long-chain alkyl ester modification phenolic resin-dichloromethane solution;

[0038] (3) Add 10 g of distilled water to the long-chain alkyl ester modified phenolic resin-methylene chloride solution to remove the acid-binding agent, separate the liquids to obtain the organic phase, remove the methylene chloride under reduced pressure, dry in a vacuum oven at 45° C. for 4 hours, and grind. The novolac epoxy curing agent modified by the long-chain alkyl es...

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Abstract

The invention relates to a long-chain alkyl ester modified linear phenolic epoxy curing agent and a preparing method thereof. The modified phenolic epoxy curing agent is prepared through substitutionreaction of linear phenolic resin and saturated fatty acid acyl chloride under action of an acid binding agent; the modified phenolic epoxy curing agent is one of ordinary linear phenolic resin and tert butylamine phenolic resin (the molecular weight is 500-1000); the saturated fatty acid acyl chloride is one of dodecyl acyl chloride to stearyl acyl chloride; a solvent is dichloromethane; the acidbinding agent is one of triethylamine and pyridine. The preparing method of the modified phenolic epoxy curing agent is the substitution reaction. The long-chain alkyl ester modified linear phenolicepoxy curing agent and the preparing method thereof have the advantages that the long-chain alkyl ester structure of the curing agent can lower the softening point of the linear phenolic epoxy resin and make the colloidal viscosity reduced due to the fact that introduction of long chains makes the free volume of a system increased and activity space of chain segments larger; meanwhile, the long-chain alkyl ester structure can have an internal plasticization effect and improve the processing fluidity of the epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a long-chain alkyl ester modified novolac epoxy curing agent and a preparation method thereof. Background technique [0002] There are various types of molding compounds, mainly including epoxy resin, phenolic resin, cyanate resin, polyimide, etc. Among them, epoxy molding compound is widely used in the field of electronic packaging due to its simple production process, low cost and reliable performance. , is the mainstream material in the field of semiconductor components and electronic packaging. In recent years, with the development of semiconductor components towards high integration, increased chip storage capacity, and complex structures, the performance requirements for epoxy molding compounds have also been greatly improved. In order to meet the needs of development, epoxy molding compounds are required to have higher thermal conductivity, insulatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G59/62
CPCC08G8/28C08G59/62
Inventor 徐卫兵张建英徐鹏周正发马海红任凤梅赵青洋
Owner HEFEI UNIV OF TECH
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