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Bio-based epoxy resin as well as preparation process and application thereof

A technology based on epoxy resin and preparation process, which is applied in the fields of silicon organic compounds, chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, etc. Low and high hydrolyzable chlorine content, to achieve the effects of excellent catalytic performance, improved processing fluidity, and improved dielectric properties

Inactive Publication Date: 2019-02-26
江苏和和新材料股份有限公司
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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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  • Bio-based epoxy resin as well as preparation process and application thereof
  • Bio-based epoxy resin as well as preparation process and application thereof
  • Bio-based epoxy resin as well as preparation process and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Soak 5g of SBA-15 mesoporous molecular sieve in 100mL aminopropyltriethoxysilane coupling agent hydrolyzate (concentration 1wt%, adjust pH to 5 with glacial acetic acid, and let it stand for 2 hours); take out after soaking for 2 hours Dry;

[0075] Mix benzyltriethylammonium chloride aqueous solution (concentration: 20g / L, 100mL) with treated SBA-15 mesoporous molecular sieve (5g), remove the water by evaporation, and place the remaining material in an ultrasonic microwave device for 120 ℃ and heated for 20 min to obtain a SBA-15 mesoporous molecular sieve catalyst immobilized with benzyltriethylammonium chloride.

[0076] Eugenol and epichlorohydrin (molar ratio 1:1) were added under normal pressure, and the SBA-15 mesoporous molecular sieve catalyst (benzyltriethylammonium chloride) prepared in this example was added in proportion to the solid-loaded benzyltriethylammonium chloride. The molar ratio of ethylammonium chloride to eugenol=0.05:1), etherification ring-op...

Embodiment 2

[0082] Get the bio-based epoxy resin 100phr prepared in Example 1, isophorone diamine 13phr, 2-methyl-4-ethylimidazole 0.3phr, stir for 2 hours and mix well, according to GB-T7124-1986 (adhesive stretching 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.

[0083] Stir the bio-based epoxy resin, curing agent, and curing accelerator according to the above raw material composition, and then cast it in 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 for 2 hours Hour. 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 below.

Embodiment 3

[0085] Soak 10g of SBA-15 mesoporous molecular sieve in 500mL aminopropyltrimethoxysilane coupling agent hydrolyzate (concentration 3wt%, adjust pH to 5 with glacial acetic acid, and let it stand for 1 hour); take it out and dry it after soaking for 2 hours ;

[0086] Mix benzyltriethylammonium chloride aqueous solution (concentration: 1000g / L, 50mL) with treated SBA-15 mesoporous molecular sieve (10g), remove the water by evaporation, and place the remaining material in an ultrasonic microwave device for 140 ℃ and heated for 40 minutes to obtain the SBA-15 mesoporous molecular sieve catalyst solidly loaded with benzyltriethylammonium chloride.

[0087] Add eugenol and epichlorohydrin (molar ratio 1:1) under normal pressure, add the SBA-15 mesoporous molecular sieve catalyst (benzyltriethylammonium chloride immobilized with benzyltriethylammonium chloride prepared in this example) in proportion. The molar ratio of triethylammonium chloride to eugenol=0.05:1), etherification r...

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Abstract

The invention discloses a preparation process of bio-based epoxy resin, the preparation process comprises: 1), adding eugenol, epoxy chloropropane and a catalyst A under normal pressure, carrying outetherification open-loop reaction at the temperature of 90-120 DEG C to prepare chlorhydrin ether; wherein the catalyst A is a mesoporous molecular sieve catalyst immobilized with benzyl triethyl ammonium chloride; 2) cooling the system obtained in the step 1) to 40-80 DEG C, adding an alkali into the system, and carrying out heat preservation reaction for 1-12 hours, standing, cooling and layering, and collecting an organic phase product, namely epoxy eugenol; and 3) and mixing the epoxy eugenol prepared in the step 2) and siloxane containing hydrogen at the two ends with a catalyst B, and carrying out hydrosilylation reaction to prepare the bio-based epoxy resin. The preparation process disclosed by the invention takes the bio-based eugenol as an initial raw material, and the prepared bio-based epoxy resin cured product has excellent flame retardancy, adhesive property and electrical property.

Description

technical field [0001] The invention relates to the field of epoxy resins, in particular to a bio-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 pet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/30C07F7/08
CPCC08G59/306C07F7/0889
Inventor 张涛叶书怀马丹李诚吉和信钟程苟明明袁凯王亮邵博文胡雪敬
Owner 江苏和和新材料股份有限公司
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