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A kind of sulfur-containing hyperbranched epoxy resin and preparation method thereof

A technology of epoxy resin and hyperbranched polymer, which is applied in the field of sulfur-containing hyperbranched epoxy resin and its preparation, can solve the problems of long reaction time, environmental pollution, low yield, etc., and achieve short reaction time and low reaction temperature , the effect of reducing viscosity

Active Publication Date: 2014-10-15
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of these sulfur-containing hyperbranched epoxy resins usually needs to add a large amount of organic solvents. After the reaction is completed, most of the processes need washing steps, which has certain pollution to the environment. In addition, the reported preparation technology of sulfur-containing hyperbranched epoxy resins ( Esterification reaction, hydrosilylation reaction, grafting reaction, group transfer polymerization reaction) have low efficiency, low yield, long reaction time and high energy consumption, high temperature and long time during curing

Method used

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  • A kind of sulfur-containing hyperbranched epoxy resin and preparation method thereof
  • A kind of sulfur-containing hyperbranched epoxy resin and preparation method thereof
  • A kind of sulfur-containing hyperbranched epoxy resin and preparation method thereof

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preparation example Construction

[0042] Preparation of Compound A3:

[0043]It is obtained by the esterification reaction of the corresponding trihydric alcohol with thioglycolic acid or mercaptopropionate, and the preparation of trimethylolpropane trimercaptoacetic acid ester (TMP-TEA) is taken as an example to illustrate its preparation process. Add 0.1mol trimethylolpropane, 0.45mol mercaptopropionic acid, and 1.6g p-toluenesulfonic acid to a four-neck flask equipped with a condenser, thermometer, water separator and stirrer, slowly raise the temperature to 160°C, and stir for 6 hours Or so, stop reacting. Add 20g of a saturated aqueous solution of sodium bicarbonate, then pour into a separatory funnel to separate layers, wash with 20ml of distilled water each time until the pH value is 6-7, and then rotate the oil layer at about 120°C with a vacuum of 2-3mmHg Impurities were removed to obtain 33.8 g of light yellow transparent liquid with a yield of about 95%. The remaining A3 compounds can be obtained ...

Embodiment 1

[0047] 0.1mol trimethylolpropane trimercaptoacetate (TMP-TEA) and 0.305mol hydroxyethyl acrylate-methacrylate (MA-EA-MMA) were stirred at -5-0°C for 5h, then MA was added - 0.5% hydroquinone of EA-MMA quality, and then remove excess MA-EA-MMA under the condition of 120°C vacuum degree of 2mmHg to obtain 3mol double bond-containing acrylate monomer (D3-A) ; Then add 0.31mol of dimercaptoethanolamine, stir and react at 20°C for 10h, and remove excess dimercaptoethanolamine at 120°C under a vacuum of 2mmHg to obtain the first generation of mercapto-terminated hyperbranched polymer NP1-HSH-A; Then add 0.61mol glycidyl methacrylate, stir and react at -5-0°C for 5h, then add 0.5% hydroquinone based on the mass of glycidyl methacrylate, and then keep the vacuum at 140°C under the condition of 2mmHg , to remove excess glycidyl methacrylate, to obtain the first generation of sulfur-containing hyperbranched epoxy resin (G1-A) light yellow liquid, test its number average molecular weight...

Embodiment 2

[0049] 0.1mol trimethylolpropane trimercapto propionate (TMP-TPA) and 0.32mol hydroxypropyl acrylate-methacrylate (MA-PA-MMA) were stirred at -5-0°C for 4h, then MA was added - 1.0% hydroquinone of PA-MMA quality, and then remove excess MA-PA-MMA under the condition of 120°C vacuum degree of 2mmHg to obtain 3mol double bond-containing acrylate monomer (D3-B) ; Then add 0.32mol dimercaptoisopropanolamine and stir and react at 40°C for 8h, then remove excess dimercaptoisopropanolamine at 120°C under a vacuum of 2mmHg to obtain the first generation of mercapto-terminated hyperbranched polymer NP1-HSH-B; then add 0.62mol glycidyl methacrylate, stir and react at -5-0°C for 4 hours, add 1.0% hydroquinone of GMA mass, and then add 1.0% hydroquinone at 140°C under the condition of a vacuum of 2mmHg The first generation of sulfur-containing hyperbranched epoxy resin (G1-B) light yellow liquid was obtained by removing the excess GMA. The number average molecular weight was 2300g / mol, th...

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Abstract

The invention belongs to the technical field of epoxy resins and preparation method thereof and in particular discloses a sulfur-containing hyperbranched epoxy resin and a preparation method thereof. The preparation method comprises the following steps: stirring and reacting a trithiol compound and a diolefin compound at the temperature of 10 DEG C below zero and 20 DEG C for 2-5 hours and preparing an acrylate monomer with polyfunctionality; stirring and reacting the monomer and bithiol secondary amine at the temperature of 20-80 DEG C for 5-10 hours and obtaining a first generation mercapto-terminated hyperbranched polymer NP1-HSH; stirring and reacting the NP1-HSH and methacrylic acid glycidyl ester at the temperature of 10 DEG C below zero and 20 DEG C for 2-5 hours and obtaining a first generation sulfur-containing hyperbranched epoxy resin; and sequentially carrying out the previous three reactions on NP1-HSH to prepare a second-fourth generation sulfur-containing hyperbranched epoxy resin with the molecular weight of about 2,000-30,000 g / mol. The method is simple in process and low in reaction temperature, the obtained product can reduce the curing temperature and is expected to be applied to the fields of reinforcing and toughening of epoxy resins, solvent-free coatings and the like.

Description

technical field [0001] The invention relates to the technical field of sulfur-containing hyperbranched epoxy resin and its preparation method, in particular to a sulfur-containing hyperbranched epoxy resin and its preparation method. A method for hyperbranched epoxy resins. Background technique [0002] The research on the synthesis of sulfur-containing hyperbranched epoxy resin originated in 1993. PCT international application WO9317060 discloses that an aliphatic sulfur-containing hyperbranched epoxy resin with higher viscosity can be synthesized by using dimethylolpropionic acid as a raw material, trimethylolpropane and epichlorohydrin. The inventor of this application (Zhang Daohong) used trimellitic anhydride, diethylene glycol, ethylene glycol, diethylene glycol, and epichlorohydrin as the main raw materials to prepare sulfur-containing hyperbranched epoxy resins. The viscosity is low, but the heat resistance is low. Not high (European Polymer Journal, 2006, 42(3):71...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02
Inventor 张道洪胡鹏高凌张俊珩周继亮张爱清
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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