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Sulfur-containing epoxide resin and preparation method thereof

A technology of sulfur epoxy resin and epoxy resin, which is applied in the field of sulfur-containing epoxy resin and its preparation, can solve problems such as difficult large-scale application, shortened product storage period, and easy entanglement of molecular chains, and achieve gel The effect of shortening time, short reaction time and simple preparation process

Active Publication Date: 2013-06-12
SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sulfur-containing epoxy resins prepared by these two methods, because the hydroxyl groups have hydrogen bonds, make the molecular chains of the sulfur-containing epoxy resins easy to entangle, resulting in high product viscosity, and usually need to be diluted with organic solvents during application; in addition, due to the presence of hydroxyl groups , when used in an acid anhydride curing system, it is easy to cause the ring opening of the anhydride to make it unstable, and ultimately lead to a shorter shelf life of the product
Moreover, the traditional process for preparing sulfur-containing epoxy resin usually needs to add a large amount of organic solvents. After the reaction is completed, most processes require washing steps, which have certain pollution to the environment.
Using hydrosilylation reaction (ZL201010224451.5, ZL200910062871.5) can prepare epoxy resin or sulfur-containing epoxy resin with low viscosity and few hydroxyl groups, but the product cost of silicone is high, the efficiency is low, and the yield is not high. Long reaction time and high energy consumption make it difficult to apply on a large scale

Method used

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  • Sulfur-containing epoxide resin and preparation method thereof
  • Sulfur-containing epoxide resin and preparation method thereof
  • Sulfur-containing epoxide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Under the condition of 15-20°C, slowly add 0.1mol dimercapto m-benzene, 0.2mol glycidyl methacrylate, and 0.5% hydroquinone of the mass of glycidyl methacrylate in sequence, mix well and wait for 5-10 After stirring and reacting for 10 hours at 140°C, the unreacted glycidyl methacrylate was removed at 140°C under a vacuum of 2mmHg to obtain a light yellow liquid, which is the sulfur-containing epoxy resin. The number average molecular weight was 426g / mol, the viscosity at 25°C is 650cp, and the epoxy value is 0.47mol / 100g.

[0026] The structural formula of sulfur-containing epoxy resin is as follows:

[0027]

Embodiment 2

[0029] Under the condition of 10-15°C, slowly add 0.1mol dimercapto-p-benzene, 0.2mol glycidyl methacrylate, and 0.5% hydroquinone of the mass of glycidyl methacrylate in sequence, mix well and stir for 10- After reacting at 15°C for 8 hours, then remove unreacted glycidyl methacrylate at 140°C under a vacuum of 2 mmHg to obtain a light yellow liquid sulfur-containing epoxy resin. The number average molecular weight was 426g / mol, 25 The viscosity at ℃ is 600cp, and the epoxy value is 0.46mol / 100g.

[0030] The structural formula of sulfur-containing epoxy resin is as follows:

[0031]

Embodiment 3

[0033] Under the condition of 15-20°C, slowly add 0.1mol dimercapto o-phthalene, 0.2mol glycidyl methacrylate, and 0.5% hydroquinone of the mass of glycidyl methacrylate in sequence, mix well and then stir for 5- After reacting at 10°C for 4 hours, then remove unreacted glycidyl methacrylate at 140°C under a vacuum of 2mmHg to obtain a light yellow liquid sulfur-containing epoxy resin. The number average molecular weight was 426g / mol, 25 The viscosity at ℃ is 500cp, and the epoxy value is 0.47mol / 100g.

[0034] The structural formula of sulfur-containing epoxy resin is as follows:

[0035]

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Abstract

The invention relates to a sulfur-containing epoxide resin and a preparation method thereof. The sulfur-containing epoxide resin is obtained by reacting a dithiol compound and glycidyl methacrylate in a stirring way at -5-20 DEG C for 4-10 hours. Compared with the traditional sulfur-containing epoxide resin, the sulfur-containing epoxide resin prepared through the method disclosed by the invention is lower in viscosity and higher in storage stability, can be applied to the fields of environment-friendly low-volatilization paint, low-volatilization resin, solvent-free epoxide resin insulating paint, and the like and can be directly applied without being added with an organic solvent or an active diluent; and compared with bisphenol A epoxide resin, the sulfur-containing epoxide resin disclosed by the invention is much lower in viscosity, shortened in gelation time by about 20% during solidification, enhanced in tensile strength and bend strength by about 10% and obviously increased in glass transition temperature and hardly influences the toughness. Besides, the preparation method disclosed by the invention has the advantages of simpleness, low pollution and low cost.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin preparation, and in particular relates to a sulfur-containing epoxy resin and a preparation method thereof. Background technique [0002] The synthesis of traditional sulfur-containing epoxy resins is mainly obtained by (1) ring-opening and ring-closing reactions of mercaptans and epichlorohydrin or (2) reaction of epoxy resins with thiourea. The sulfur-containing epoxy resins prepared by these two methods, because the hydroxyl groups have hydrogen bonds, make the molecular chains of the sulfur-containing epoxy resins easy to entangle, resulting in high product viscosity, and usually need to be diluted with organic solvents during application; in addition, due to the presence of hydroxyl groups , when used in an acid anhydride curing system, it is easy to cause the ring opening of the anhydride to make it unstable, and ultimately lead to a shorter shelf life of the product. Moreover, the trad...

Claims

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Application Information

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IPC IPC(8): C07D303/16C07D301/00C08G59/30C09D163/00
Inventor 张道洪程新建井丰喜张俊珩张春琪刘蓉徐庆华顾建峰李斌
Owner SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL CO LTD
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