Synthesis, characterization and curing characteristics of single benzoxazine containing DOPO based on bisphenol A

doi:10.3969/j.issn.0438-1157.2014.09.055

CIESC Journal ›› 2014, Vol. 65 ›› Issue (9): 3705-3711.DOI: 10.3969/j.issn.0438-1157.2014.09.055

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Synthesis, characterization and curing characteristics of single benzoxazine containing DOPO based on bisphenol A

LIU Jianhua¹, SHI Tiejun¹, XU Guomei^1,2, WANG Quan¹, WANG Qidong¹

1 School of Chemical Engineering, Hefei University of Technology, Hefei 230009, Anhui, China;
2 Department of Materials and Chemical Engineering, West Anhui University, Lu'an 237012, Anhui, China

Received:2013-12-30 Revised:2014-03-14 Online:2014-09-05 Published:2014-09-05
Supported by:
supported by the National Natural Science Foundation of China (51273054).

含DOPO的双酚A-单苯并(口恶)嗪合成、表征及其固化特性

刘建华¹, 史铁钧¹, 徐国梅^1,2, 王权¹, 王启东¹

1 合肥工业大学化工学院, 安徽合肥 230009;
2 皖西学院材料与化工学院, 安徽六安 237012

通讯作者: 史铁钧
基金资助:
国家自然科学基金项目（51273054）。

Abstract

Abstract: Double benzoxazine based on bisphenol A（DBOZ）was synthesized from bisphenol A, aniline and paraformaldehyde, and the single benzoxazine containing DOPO based on bisphenol A（DBDO）was synthesized from DBOZ and DOPO. FT-IR, NMR (¹H NMR and ¹³CNMR) were used to characterize the chemical structure of DBOZ and DBDO. Curing characteristics were studied with DSC and thermostability was studied with TG. In N₂ atmosphere, the ring opening polymerization of DBOZ took place at about 205℃, and initial decomposition temperature was 312℃. At 373℃, the fastest decomposition was achieved. At 800℃, carbon residue was 37.19%. In N₂ atmosphere, initial decomposition temperature of DBDO was 353℃. At 443℃, the fastest decomposition was achieved. At 800℃, carbon residue was 39.60%.

Key words: synthesis, polymerization, thermostability, NMR, double benzoxazine based on bisphenol A, single benzoxazine containing DOPO based on bisphenol A

摘要： 以双酚A、苯胺、多聚甲醛为原料，合成了双酚A-双苯并(口恶)嗪（DBOZ），再用其与DOPO（9，10-二氢-9-氧杂-10-磷杂菲-10-氧化物）反应，合成了含DOPO的双酚A-单苯并(口恶)嗪（DBDO）。采用红外、核磁共振（氢谱核磁共振和碳谱核磁共振）等分析手段对DBOZ和DBDO的化学结构进行了表征；采用差示扫描量热仪对DBOZ和DBDO的固化特性进行研究，使用热重分析分析了所得聚苯并(口恶)嗪的热稳定性。结果表明：在N₂气氛中，DBOZ在205℃左右开环聚合，热分解温度为312℃，在373℃分解速度达到最快，在800℃时的残碳率为37.19%；在N₂气氛中，DBDO的热分解温度为353℃，在443℃分解速度达到最快，在800℃时的残碳率为39.60%。

关键词: 合成, 聚合, 热稳定性, 核磁共振, 双酚A-双苯并(口恶)嗪, 含DOPO的双酚A-单苯并(口恶)嗪

CLC Number:

O631

LIU Jianhua, SHI Tiejun, XU Guomei, WANG Quan, WANG Qidong. Synthesis, characterization and curing characteristics of single benzoxazine containing DOPO based on bisphenol A[J]. CIESC Journal, 2014, 65(9): 3705-3711.

刘建华, 史铁钧, 徐国梅, 王权, 王启东. 含DOPO的双酚A-单苯并(口恶)嗪合成、表征及其固化特性[J]. 化工学报, 2014, 65(9): 3705-3711.

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Synthesis, characterization and curing characteristics of single benzoxazine containing DOPO based on bisphenol A

含DOPO的双酚A-单苯并(口恶)嗪合成、表征及其固化特性

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