Fluorenyl polyether sulfone resin with side chains containing benzoxazine and preparation method of fluorenyl polyether sulfone

A technology of fluorenyl polyethersulfone and benzoxazine, which is applied in the field of thermoplastic resin and its preparation, can solve the problems of small molecular weight and brittleness of polymers, and achieve good thermal and mechanical properties

Inactive Publication Date: 2013-07-17
三亚哈尔滨工程大学南海创新发展基地
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, traditional benzoxazine resins have defects such as brittleness and low molecular weight of polymers obtained by crosslinking, while polyethersulfon

Method used

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  • Fluorenyl polyether sulfone resin with side chains containing benzoxazine and preparation method of fluorenyl polyether sulfone
  • Fluorenyl polyether sulfone resin with side chains containing benzoxazine and preparation method of fluorenyl polyether sulfone
  • Fluorenyl polyether sulfone resin with side chains containing benzoxazine and preparation method of fluorenyl polyether sulfone

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] Example 1

[0023] Synthesis of Fluorenyl Polyethersulfone with Amino Side Chain

[0024] In a three-necked flask equipped with a stirring rotor, a water separator, a nitrogen inlet and a condenser tube, 3.04 g of 9,9-bis(4-aminophenyl)-2,7-dihydroxyfluorene, 1.48 g of anhydrous potassium carbonate and Dichlorodiphenylsulfone 2.87g, add 50mL of dimethyl sulfoxide and 20mL of toluene, pass nitrogen, and heat up to 160°C under stirring. After continuing the reaction for 3 hours, the reaction was terminated, the reaction solution was lowered to room temperature, filtered, the filtrate was added to water, the precipitate was precipitated, washed with water and ethanol, and finally vacuum-dried at 60° C. for 24 hours to obtain a white side chain containing amino groups. Polyethersulfone powder 4.78g, yield 87%.

[0025] NMR test results (500M, CDCl 3 , ppm): In the 1H NMR spectrum, δ=6.39~7.94ppm is the chemical shift of the proton on the benzene ring, and 4.99ppm is the ...

Example Embodiment

[0026] Example 2

[0027] Except the anhydrous potassium carbonate was changed to 1.65g and the dichlorodiphenyl sulfone was changed to 3.44g, the reaction temperature was changed to 180°C, and other conditions were the same as in Example 1, and finally 4.16g of fluorenyl polyethersulfone powder containing amino groups in the white side chain was obtained. , the yield is 75%.

Example Embodiment

[0028] Example 3

[0029] Synthesis of Fluorenyl Polyether Sulfones with Benzoxazine Groups in Side Chains

[0030] 1.5g of fluorenyl polyethersulfone, 0.94g of phenol, 30mL of xylene and 0.6g of paraformaldehyde synthesized in the side chain containing amino groups synthesized in Example 1 were successively added to the there-necked flask, the temperature was raised to 150°C, the reaction was performed for 6 hours, and the temperature was lowered. After reaching room temperature, the reaction solution was poured into ethanol, filtered, and the filter cake was washed with ethanol, and then vacuum-dried to obtain 1.2 g of fluorenyl polyethersulfone powder containing a benzoxazine group in the side chain of light yellow, with a yield of 60 %.

[0031] NMR test results (500M, CDCl 3 , ppm): In the 1H NMR spectrum, δ=6.77~7.81ppm is the chemical shift of the proton on the benzene ring, 5.29ppm is the O-CH on the oxazine ring 2 -N proton characteristic peak, 4.69ppm is Ar-CH 2 ...

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Abstract

The invention relates to fluorenyl polyether sulfone resin with side chains containing benzoxazine and a preparation method of the fluorenyl polyether sulfone resin. The preparation method includes steps of adding 9, 9-bi (4-ammonia phenyl)-2, 7-dyhydroxyl fluorene, anhydrous potassium carbonate and dichlorophenyl sulfone into a container, then adding dimethyl sulfoxide and toluene, feeding nitrogen gas, heating to the temperature of 150-200 DEG C, reacting for 2-4 hours, steaming toluene, continuously reacting for 2-4 hours at the identical temperature, filtering after reacting, adding filtrate into water, precipitating to obtain fluorenyl polyether sulfone with side chains containing amino, adding the fluorenyl polyether sulfone with side chains containing amino, monophenol, paraformaldehyde, chloroform or dimethylbenzene into the container, heating to the temperature 60-160 DEG C, reacting by reflux for 5-24 hours, adding reactant into ethanol, and precipitating to obtain fluorenyl polyether sulfone resin with side chains containing benzoxazine. The fluorenyl polyether sulfone resin with side chains containing benzoxazine can be used independently or used with other resin and has good thermal properties and mechanical properties.

Description

technical field [0001] The invention relates to a thermoplastic resin and a preparation method thereof. Background technique [0002] With the rapid development of aerospace, transportation, information transmission and other technical fields, people's requirements for polymer materials are also getting higher and higher. Excellent mechanical properties, heat resistance, weather resistance and electrical insulation have become the goals pursued by people. At the same time, people's research on polymer materials is constantly developing in the direction of lightweight, low cost, high performance and multifunctionality, and the key to achieving this goal requires high-performance resins with different structures. To be done. The development of high-performance resins can be attributed to three aspects: heat resistance, heat and humidity resistance, and toughness. These three properties are mutually restrictive. Increasing the cross-linking density of cross-linked polymers c...

Claims

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Application Information

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IPC IPC(8): C08G75/23
Inventor 刘文彬韩丽王军祁彦龙徐元
Owner 三亚哈尔滨工程大学南海创新发展基地
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