Synthesis, characterization and curing characteristics of double benzoxazine contained double DOPO based on bisphenol A

doi:10.3969/j.issn.0438-1157.2014.11.056

Abstract

Abstract: The bisphenol A contained double DOPO (2DO) was synthesized by using double benzoxazine based on bisphenol A(DBOZ) and DOPO. And the double benzoxazine contained double DOPO based on bisphenol A (2DD) was synthesized by using 2DO,aniline and paraformaldehyde. FT-IR, NMR were used to characterize the chemical structure of 2DO and 2DD. Curing characteristics were studied with DSC and thermostability was studied with TG. In N₂ atmosphere, initial decomposition temperature of 2DD was 353℃. At the temperature of 442℃, the fastest speed of decomposition was achieved. At the temperature of 800℃, carbon residue was 40.40%. Mass-change rate at the temperature of 300℃ was 3.97%. Compared with double benzoxazine based on bisphenol A,initial decomposition temperature increased by nearly 41℃,the fastest speed of decomposition increased by nearly 70℃ and carbon residue increased by nearly 3.21%.

Key words: synthesis, thermostability, NMR, bisphenol A, double benzoxazine

摘要： 以双酚A-双苯并(口恶)嗪(DBOZ)和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物 (DOPO)为原料,合成了双酚A-双DOPO(2DO),再用其与苯胺、多聚甲醛反应,合成了含双DOPO的双酚A-双苯并(口恶)嗪(2DD).采用红外、核磁共振等分析手段对2DO和2DD的化学结构进行了表征,采用差示扫描量热仪对DBOZ和2DD的固化特性进行研究,使用热重分析仪分析了所得聚苯并(口恶)嗪的热稳定性.结果表明:在N₂气氛中,含双DOPO的双酚A-双苯并(口恶)嗪热分解温度为353℃,在442℃分解速率达到最快,800℃时的残碳率为40.40%,300℃的质量变化为3.97%.与未引入DOPO的双酚A-双苯并(口恶)嗪树脂相比,其热分解温度提高了将近41℃,最大分解速率提高了将近70℃,残碳率提高了将近3.21%.

关键词: 合成, 热稳定性, 核磁共振, 双酚A, 双苯并(口恶)嗪

CLC Number:

O631

LIU Jianhua, SHI Tiejun. Synthesis, characterization and curing characteristics of double benzoxazine contained double DOPO based on bisphenol A[J]. CIESC Journal, 2014, 65(11): 4607-4613.

刘建华, 史铁钧. 含双DOPO的双酚A-双苯并(口恶)嗪合成、表征及其固化特性[J]. 化工学报, 2014, 65(11): 4607-4613.

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