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P-tert-butyl phenolic epoxy resin and preparation method thereof

A technology of novolac epoxy resin and p-tert-butyl, which is applied in the field of p-tert-butyl novolac epoxy resin and its preparation, can solve the problems that the types of novolac epoxy resin need to be further expanded and the research on novolac epoxy resin is less, and achieve Good application prospects, reduced rigidity and melt viscosity, and high reaction yield

Inactive Publication Date: 2019-04-23
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies on alkyl-substituted novolac epoxy resins other than methyl, and the types of novolak epoxy resins need to be further expanded.

Method used

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  • P-tert-butyl phenolic epoxy resin and preparation method thereof
  • P-tert-butyl phenolic epoxy resin and preparation method thereof
  • P-tert-butyl phenolic epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) 40g p-tert-butylphenol-formaldehyde resin is dissolved in 200g epichlorohydrin, add 0.4g phase-transfer catalyst benzyl triethylammonium chloride, evacuate and circulate nitrogen for 3 times, stir and heat up to 70°C, constant temperature reaction for 6h for etherification reaction. After further adjusting the temperature of the system to 60°C, add 23.7g of a 40% NaOH alkali catalyst aqueous solution dropwise, adjust the vacuum of the system during the dropwise addition, and make the system The water contained in it is continuously and stably removed to reduce the hydrolysis of epichlorohydrin. After the dropwise addition is completed within 5 hours, the constant temperature reaction is continued for 2 hours to make the reaction complete. After the reaction is completed, use a 300-mesh filter cloth to filter out the salt generated by the reaction, and recover the epichlorohydrin from the filtrate under reduced pressure at 100-130° C. to obtain crude p-tert-butylphen...

Embodiment 2

[0030] (1) Dissolve 40g of p-tert-butylphenol-formaldehyde resin in 300g of epichlorohydrin, add 1.2g of phase transfer catalyst tetrabutylammonium bromide, vacuumize and circulate nitrogen for 3 times, stir and heat up to 100°C under nitrogen atmosphere , Constant temperature reaction for 3h etherification reaction. After further adjusting the temperature of the system to 90°C, add 16.0g of a 48% NaOH alkali catalyst aqueous solution dropwise, adjust the vacuum of the system during the dropwise addition, and make the system The water contained in it is continuously and stably removed to reduce the hydrolysis of epichlorohydrin. After the dropwise addition is completed within 2 hours, the reaction is carried out at constant temperature for 2 hours to complete the reaction. After the reaction is completed, use a 300-mesh filter cloth to filter out the salt generated by the reaction, and recover the epichlorohydrin from the filtrate under reduced pressure at 100-130° C. to obtai...

Embodiment 3

[0034](1) 40g p-tert-butylphenol-formaldehyde resin is dissolved in 400g epichlorohydrin, add 0.8g phase-transfer catalyst benzyltrimethylammonium chloride, vacuumize nitrogen circulation 3 times, stir and heat up to 90°C, constant temperature reaction for 4h for etherification reaction. After further adjusting the system temperature to 70°C, add 28.0g of KOH alkali catalyst aqueous solution with a mass fraction of 38%, adjust the vacuum degree of the system during the dropwise addition, and make the system The water contained in it is continuously and stably removed to reduce the hydrolysis of epichlorohydrin. After the dropwise addition is completed within 5 hours, the constant temperature reaction is carried out for 1 hour to make the reaction complete. After the reaction is completed, use a 300-mesh filter cloth to filter out the salt generated by the reaction, and recover the epichlorohydrin from the filtrate under reduced pressure at 100-130° C. to obtain crude p-tert-bu...

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Abstract

The invention relates to p-tert-butyl phenolic epoxy resin and a preparation method thereof. The preparation method is characterized by comprising the following steps: carrying out etherification reaction by taking p-tert-butyl phenolic resin and epichlorohydrin as raw materials under the action of a phase transfer catalyst; adding an alkali catalyst solution into an etherification product to carry out ring-closing reaction, removing water in a system through decompression azeotropy, filtering filtrate, and then recovering excessive epichlorohydrin under reduced pressure; adding the crude resin into a solvent for dissolution, dropwise adding a small amount of alkali catalyst solution for refining reaction, washing with water, and then recovering the solvent under reduced pressure to obtainthe p-tert-butyl phenolic epoxy resin. The prepared p-tert-butyl phenolic epoxy resin can reach a high softening point, has a high epoxy value and low hydrolyzable chlorine content, can be used for packaging electronic circuits and electronic components. The preparation method provided by the invention is simple in steps, high in reaction yield and suitable for industrial production, and has goodapplication prospect.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and relates to a p-tert-butylphenol-formaldehyde epoxy resin and a preparation method thereof. Background technique [0002] Novolac epoxy resin has phenolic resin as the main chain and side chain epoxy group as the crosslinking group, which has good physical properties, mechanical properties and process properties. Compared with bisphenol A epoxy resin, since the molecular structure contains more than 2 epoxy groups, the crosslinking density after curing is high, and the product's solvent resistance, heat resistance, chemical resistance and dimensional stability will increase relatively. Therefore, the resin is widely used in the semiconductor industry as the main bonding material for integrated circuits, electronic components and packaging materials for civil weak current products. However, the main molecular structure of traditional phenol novolac epoxy resins is dominated by benzene rings, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/08
CPCC08G59/08
Inventor 张源源骆昱晖梁天童志伟
Owner HUAIHAI INST OF TECH