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Preparation method of triglycidyl-meta-aminophenol epoxy resin

A technology of triglycidol and aminophenol, applied in the direction of organic chemistry, can solve the problems of exceeding the stoichiometric amount and impossible to achieve complete cyclization

Inactive Publication Date: 2015-04-01
SHANGHAI HUAYI RESINS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors think that the weak point of the prior art is that if the amount of sodium hydroxide used does not reach the stoichiometric amount, the triglycidyl-p-aminophenol does not have and cannot reach the degree of complete cyclization all the time. To meet or exceed the stoichiometric amount
[0005] Triglycidyl-m-aminophenol and triglycidyl-p-aminophenol belong to triglycidylamine compounds, but it has recently been found that triglycidyl-m-aminophenol can be used in the preparation of high temperature resistance, high strength, high modulus and High impact epoxies are more competitive

Method used

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  • Preparation method of triglycidyl-meta-aminophenol epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Fill epichlorohydrin 2944g and benzyldiethylammonium chloride catalyst 108g in the 5000mL four-neck round-bottomed flask that is equipped with stirrer, thermometer, nitrogen inlet pipe, dropping funnel, condensing tube and oil-water separator, in Stirring began to heat up, at the same time add m-aminophenol 432g, m-aminophenol was added dropwise in 5 times, the interval between each drop was 25min, after the dropwise addition of m-aminophenol was completed, reacted at 45°C for 6.5 hr, then add 480g of sodium hydroxide at 53°C / 0.065MPa under vacuum pressure, maintain the ring closure reaction for 2.5hr, then release the vacuum, evaporate epichlorohydrin, add 1800mL toluene to the reaction solution to extract triglycidyl-m-amino Phenol epoxy resin, after 3 times of water washing and delamination, get the oil phase, evaporate toluene to obtain reddish-brown liquid triglycidyl-m-aminophenol epoxy resin product, this resin has a viscosity (measured at 25°C) of 7500mPa S, The...

Embodiment 2

[0024] In addition to adding 3312 g of epichlorohydrin and 130 g of benzyltriethylammonium bromide in the addition reaction stage of step (1), the reaction temperature is 50 ° C, and the reaction time is 7 hr. Sodium 130g, 50 ℃ of temperature of reaction, tightness of vacuum 0.07MPa, outside the reaction time 2hr, other prescription and operating steps are all with embodiment 1, and the triglycidyl-m-aminophenol epoxy resin product that obtains has viscosity (25 ℃ measures ) 8000mPa S, epoxy equivalent 9.4eq / Kg; Based on 100 parts by weight of the above-mentioned triglycidyl-m-aminophenol epoxy resin product and 160 parts by weight of methyl endomethine tetrahydrophthalic anhydride Uniformly mixed and solidified according to the conditions of Example 1, the performance index of the sample is: Tg241 ° C, impact strength 20KJ / m 2 , Bending strength 190MPa, tensile strength 70MPa.

Embodiment 3

[0026] In addition to adding 2576 g of epichlorohydrin and 86 g of benzyltrimethylammonium chloride in the addition reaction stage of step (1), the reaction temperature is 45 ° C, and the reaction time is 6 hours. Sodium 512g, temperature of reaction 47 ℃, vacuum tightness 0.06MPa, outside reaction 3hr, other prescription and operating steps are all with embodiment 1, the triglycidyl-m-aminophenol epoxy resin product that obtains has viscosity (25 ℃ measures ) 7000mPa S, epoxy equivalent 9.0eq / Kg; Based on 100 parts by weight of the above-mentioned triglycidyl-m-aminophenol epoxy resin product and 140 parts by weight of methyl endomethine tetrahydrophthalic anhydride Uniformly mixed and solidified according to the conditions of Example 1, the performance index of the sample is: Tg241 ° C, impact strength 16KJ / m 2 , Bending strength 180MPa, tensile strength 50MPa.

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Abstract

The invention discloses a preparation method of triglycidyl-meta-aminophenol epoxy resin. The ideal epoxy resin is prepared by adopting low-temperature addition reaction and vacuum dehydration ring-closure reaction, wherein the mole ratio of raw materials, namely meta-aminophenol to epoxy chloropropane is 1:(7-9), one of or a mixture of more than two of groups formed by benzyl diethyl ammonium chloride, benzyl triethyl ammonium chloride, benzyl trimethyl ammonium chloride, benzyl diethyl ammonium bromide, benzyl triethyl ammonium bromide and benzyl trimethyl ammonium bromide is used as a catalyst, the reaction temperature is 45-55 DEG C, and the reaction time is 6-7 hours; during the ring-closure reaction, the mole ratio of sodium hydroxide to meta-aminophenol is 1:(3-3.5), the reaction is performed at a temperature of 45-55 DEG C and a pressure of 0.06-0.07 MPa for 2-3 hours, and the obtained epoxy resin has the viscosity (measured at 25 DEG C) of 7000-8000mPa.S and the epoxy index of 9.0-9.4eq / Kg; and after the epoxy resin is cured by using 140-160wt% of methyl methenyl tetrabydrophthalic anhydride, the physical and mechanical properties of the epoxy resin are as follows: Tg is 241 DEG C, the impact strength is 16-20KJ / m<2>, the bending strength is 180-190MPa, and the tensile strength is 50-70MPa.

Description

1. Technical field [0001] The present invention relates to the preparation method of triglycidyl aminophenol epoxy resin, relate to the preparation method of triglycidyl-m-aminophenol epoxy resin more precisely. 2. Background technology [0002] Triglycidyl-m-aminophenol epoxy resin of the present invention has following chemical structural formula: [0003] [0004] Triglycidyl-p-aminophenol epoxy resin has good compatibility with other epoxy resins due to its low viscosity. After curing, it is often used as a high-temperature resistant material. There are many domestic and foreign production, research institutions and units. Catalysts are mostly used in the addition reaction process. For example, the prior art JP-A-57-70881 uses lithium chloride (LiCl) as a catalyst. JP-4-139230 disclosed on May 13, 1992 that tetramethyl chloride ammonium or tetramethylammonium bromide as a catalyst. In the cyclization reaction process, the usage amount of sodium hydroxide is just dif...

Claims

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Application Information

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IPC IPC(8): C07D301/28C07D303/36C08G59/42
CPCC07D303/36C07D301/28C08G59/4223
Inventor 黄慧琳胡志强张庭浩
Owner SHANGHAI HUAYI RESINS CO LTD
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