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Preparation process of biobased epoxy resin, product and application

A technology based on epoxy resin and preparation process, which is applied in the direction of epoxy resin glue, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc. High, low yield of closed-loop products and other issues, to achieve excellent catalytic performance, improve dielectric properties, improve the effect of processing fluidity

Inactive Publication Date: 2019-03-22
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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  • Preparation process of biobased epoxy resin, product and application
  • Preparation process of biobased epoxy resin, product and application
  • Preparation process of biobased epoxy resin, product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Heat 0.1 mol of benzyldiethylamine, 0.1 mol of γ-chloropropyltriethoxysilane, 100 mL of ethanol, and 0.02 mol of potassium iodide to 75°C under nitrogen protection, react for 1.5 hours, and obtain the quaternary ammonium salt mother liquor after filtering the product , Add 50mL of quaternary ammonium salt mother liquor dropwise to 100mL of distilled water / ethanol (20ml of water, 80ml of ethanol) to obtain a mixed solution, adjust the pH of the mixed solution to 5.0 with glacial acetic acid, and after standing for 2 hours, add 40 grams of halloysite nano The tube is put into it, fully soaked for 1-3 hours, and the water is removed by evaporation, and the obtained product is halloysite nanotube functionalized with quaternary ammonium salt.

[0077] Add eugenol and epichlorohydrin (molar ratio 1:1) under normal pressure, add the halloysite nanotube of quaternary ammonium salt functionalization prepared in this embodiment in proportion as catalyst (benzyltriethylammonium chl...

Embodiment 2

[0083] Take the bio-based epoxy resin 100phr prepared in Example 1, 13phr of isophorone diamine, 0.3phr of 2-methyl-4-ethylimidazole, 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.

[0084] 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 be...

Embodiment 3

[0086] Heat 0.1 mol of benzyldiethylamine, 0.1 mol of γ-chloropropyltrimethoxysilane, 100 mL of methanol, and 0.02 mol of potassium iodide to 60°C under nitrogen protection, react for 1.5 hours, and filter the product to obtain a quaternary ammonium salt mother liquor. Add 50mL of quaternary ammonium salt mother liquor dropwise to 100mL of distilled water / methanol (20ml of water, 80ml of methanol), adjust the pH of this solution to 5.0 with glacial acetic acid, put 40g of halloysite nanotubes into it after standing for 2 hours, and fully After soaking for 3 hours, the water was removed by evaporation, and the obtained product was halloysite nanotubes functionalized with quaternary ammonium salts.

[0087] Add eugenol and epichlorohydrin (molar ratio 1:1) under normal pressure, add the halloysite nanotube of quaternary ammonium salt functionalization prepared in this embodiment in proportion as catalyst (benzyltriethylammonium chloride The molar ratio with eugenol=0.05:1), ethe...

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Abstract

The invention discloses a preparation process of biobased epoxy resin. The process comprises (1) adding eugenol, epoxy chloropropane and a catalyst A at normal pressure; performing etherification ringopening reaction at 90 to 120 DEG C to prepare chlorine alcohol ether, wherein the catalyst A is a quaternary ammonium salt functionalized halloysite nanometer tube; (2) after the temperature of a system obtained after the reaction in step (1) is lowered to 40 to 80 DEG C, adding alkali into the system; performing heat insulation reaction for 1 to 12h; then, performing still standing, cooling andlayering; collecting an organic phase product which is epoxidated eugenol; (3) mixing the epoxidated eugenol prepared in step (2), siloxane with hydrogen at two ends and a catalyst B; performing hydrosilylation to obtain the biobased epoxy resin. The preparation process disclosed by the invention has the advantages that biobased eugenol is used as initial raw materials; the prepared biobased epoxy resin curing articles simultaneously have excellent flame retardant performance, bonding performance and electric performance.

Description

technical field [0001] The invention relates to the field of epoxy resin, in particular to a preparation process, product and application of a bio-based epoxy resin. 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 o...

Claims

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Application Information

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IPC IPC(8): C07F7/08C08G59/30C09J163/00
CPCC07F7/0879C08G59/306C09J163/00
Inventor 张涛叶书怀李诚马丹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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