Synthesis of novel boron containing benzoxazine and its thermal properties with epoxy resin blends

doi:10.11949/j.issn.0438-1157.20161816

Abstract

Abstract:

The boric acid ethanolamine ester (BAE) was synthesized using boric acid and ethanolamine. The synthesis of benzoxazine contained boron (BAE-BOZ) was synthesized by using BAE, phenol and paraformaldehyde. The BAE-BOZ are mixed with epoxy resin in different proportions, and then cured by high temperature. Using FT-IR, ¹H NMR and ¹³C NMR analysis of the chemical structure of BAE-BOZ, proved that the target product has been synthesized. Curing properties on BAE-BOZ was studied with DSC, the thermal stability of poly(BAE-BOZ) cured BAE-BOZ/E-51 were studied by using TG analysis. The results showed that the curing peak of BOZ appeared at 218℃, B and oxazine ring were combined by B O C, and the highest the boric content in BAE-BOZ was 8.67%, the initial pyrolysis temperature was about 302℃, and the carbon residual at 800℃ increased from 41.80% to 58.08%. The thermal decomposition temperature of BAE-BOZ/E-51 copolymer reached 343℃.

Key words: synthesis, benzoxazine, epoxy resin, thermal stability, thermosetting resin

摘要：

以乙醇胺、硼酸为原料合成硼酸乙醇胺酯（BAE），再用所得硼酸乙醇胺酯与多聚甲醛、苯酚反应，合成含硼苯并噁嗪（BAE-BOZ）。将所得BAE-BOZ高温固化，BAE-BOZ和环氧树脂E-51按照不同的质量比进行熔融共混，并经高温固化。采用FT-IR，¹H NMR 和¹³C NMR等分析了BAE-BOZ的化学结构，证明了产物为目标产物；采用DSC对BAE-BOZ的固化特性进行研究；采用TG 分析了含硼乙醇胺型苯并噁嗪poly（BAE-BOZ）和BAE-BOZ/E-51共聚物的热稳定性。结果表明：BAE-BOZ在218℃出现了固化峰；BAE-BOZ的硼含量达到8.67%，在N₂条件下，poly（BAE-BOZ）的热分解温度为302℃，在426℃时热分解速率最快，800℃的残炭率为58.08%，与未经硼改性的乙醇胺型苯并噁嗪（E-BOZ）相比，热分解温度提高40℃，残炭率提高了16.28%；BAE-BOZ/E-51共聚物的热分解温度达到343℃，热性能得到进一步提高。

关键词: 合成, 苯并噁嗪, 环氧树脂, 热稳定性, 热固性树脂

CLC Number:

O631

CHEN Yang, SHI Tiejun, QIAN Ying, HE Tao. Synthesis of novel boron containing benzoxazine and its thermal properties with epoxy resin blends[J]. CIESC Journal, 2017, 68(6): 2604-2610.

陈杨, 史铁钧, 钱莹, 何涛. 新型含硼苯并噁嗪的合成及其与环氧树脂共混热性能[J]. 化工学报, 2017, 68(6): 2604-2610.

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