Eugenol-based epoxy resin and preparation process and application thereof

A eugenol-based epoxy resin and preparation technology, applied in the field of epoxy resin, can solve problems such as difficult to meet high-quality application requirements, low yield of closed-loop products, high hydrolyzable chlorine content, etc., achieve excellent catalytic performance, improve Processing fluidity, effect of improving dielectric properties

Inactive Publication Date: 2019-03-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this reaction requires repeated extraction and washing, resulting in a large amount of waste liquid, and the yield of the closed-loop product is low, about 70%, and the content of hydrolyzable chlorine in the product is high, which is difficult to meet the needs of high-quality applications.

Method used

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  • Eugenol-based epoxy resin and preparation process and application thereof
  • Eugenol-based epoxy resin and preparation process and application thereof
  • Eugenol-based epoxy resin and preparation process and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Benzyltriethylammonium chloride aqueous solution (concentration: 20g / L, 100mL) was mixed with halloysite nanotubes (5g), and the water was removed by evaporation, and the remaining substance was heated in an ultrasonic microwave device at 120°C for 20min. The halloysite nanotube catalyst immobilized with benzyltriethylammonium chloride is obtained.

[0068] Under normal pressure, eugenol and epichlorohydrin (molar ratio 1:1) were added, and the halloysite nanotubes immobilized with benzyltriethylammonium chloride prepared in this example were added in proportion as catalyst (benzyltriethylammonium chloride). The molar ratio of ethylammonium chloride to eugenol=0.05:1), etherification ring-opening reaction was carried out at 100°C, and the reaction time was 2 hours to obtain chlorohydrin ether; when the system was cooled to about 60°C, add Sodium hydroxide (the molar ratio of sodium hydroxide to eugenol = 1.05:1), was added in batches within 3 hours, and the heat preserv...

Embodiment 2

[0074] Get the eugenol-based epoxy resin 100phr prepared in Example 1, isophorone diamine 13phr, 2-methyl-4-ethylimidazole 0.3phr, stir for 2 hours and mix uniformly, according to GB-T7124-1986 (adhesive pull Tensile shear strength test method) evenly spread on the surface of the steel sheet cleaned with acetone and fixed, cured at 80°C for 30 minutes, and cured at 150°C for 1.5 hours. The iron sheet bonding strength and iron sheet bonding modulus data of the obtained samples are listed in Table 1 below.

[0075] Stir the eugenol-based epoxy resin, curing agent, and curing accelerator according to the above raw material composition, and then cast it into a steel mold, vacuumize and defoam at 80°C for half a minute, cure at 80°C for 2 hours, and cure at 150°C 2 hours. The sample released from the mold has no bubbles, and the appearance is transparent without obvious defects. The limiting oxygen index and dielectric constant data of the obtained samples are listed in Table 1 b...

Embodiment 3

[0077] Benzyltriethylammonium chloride aqueous solution (concentration: 1000g / L, 50mL) was mixed with halloysite nanotubes (10g), and the water was removed by evaporation, and the remaining substance was heated in an ultrasonic microwave device at 150°C for 40min. The halloysite nanotube catalyst immobilized with benzyltriethylammonium chloride is obtained.

[0078] Under normal pressure, eugenol and epichlorohydrin (molar ratio 1:1) were added, and the halloysite nanotubes immobilized with benzyltriethylammonium chloride prepared in this example were added in proportion as a catalyst (benzyltriethylammonium chloride). The molar ratio of triethylammonium chloride to eugenol=0.05:1), etherification ring-opening reaction was carried out at 110°C, and the reaction time was 2 hours to obtain chlorohydrin ether; Add sodium hydroxide (the molar ratio of sodium hydroxide to eugenol = 1.05:1), add in batches within 3 hours, and keep warm for 4 hours; put the system to stand, cool and ...

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Abstract

The invention discloses a preparation process of eugenol-based epoxy resin. The preparation process comprises the steps that (1) eugenol, epichlorohydrin and a catalyst A are added under the normal pressure, etherification ring-opening reaction is conducted at the temperature of 90-120 DEG C, thus chlorinol ether is prepared, and the catalyst A is a halloysite nanotube immobilized with benzyl triethyl ammonium chloride; (2) when a system obtained through reaction in the step (1) is cooled to 40-80 DEG C, alkali is added into the system, heat preservation for reaction is conducted for 1-12 h,then still standing and cooling layering are conducted, and thus collected organic phase products are epoxidized eugenol; and (3) the epoxidized eugenol prepared in the step (2), siloxane containing hydrogen at the two ends, and a catalyst B are mixed, hydrosilylation is conducted, and thus the eugenol-based epoxy resin is prepared. According to the preparation process, the bio-based eugenol serves as an initial raw material, and a prepared eugenol-based epoxy resin curing material simultaneously has the excellent flame retardant property, bonding property and electrical property.

Description

technical field [0001] The invention relates to the field of epoxy resins, in particular to a eugenol-based epoxy resin and its preparation process and application. Background technique [0002] Epoxy resins have developed into a large class of thermosetting resins due to their excellent mechanical and electrical properties, and are widely used in adhesives, structural composite materials, electronic semiconductor packaging and other fields. However, its performance is greatly affected by the epoxy resin matrix. [0003] At present, the global annual output of epoxy resin is more than 2 million tons, among which bisphenol A epoxy resin is widely used, such as E44, E51, etc., accounting for more than 85% of the total output. Bisphenol A type epoxy resin is mainly prepared from bisphenol A and epichlorohydrin as raw materials. Although bio-based epichlorohydrin has been industrialized and its output is increasing, more than 67% of bisphenol A is still completely dependent on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C08G59/30
CPCC07F7/0812C07F7/0829C08G59/306
Inventor 范宏张先伟马中柱胡激江陈睿
Owner ZHEJIANG UNIV
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