新型含硼苯并噁嗪的合成及其与环氧树脂共混热性能

doi:10.11949/j.issn.0438-1157.20161816

化工学报 ›› 2017, Vol. 68 ›› Issue (6): 2604-2610.DOI: 10.11949/j.issn.0438-1157.20161816

• 材料化学工程与纳米技术 • 上一篇下一篇

新型含硼苯并噁嗪的合成及其与环氧树脂共混热性能

陈杨, 史铁钧, 钱莹, 何涛

合肥工业大学化学与化工学院, 安徽合肥 230009

收稿日期:2016-12-28 修回日期:2017-02-21 出版日期:2017-06-05 发布日期:2017-06-05
通讯作者: 史铁钧
基金资助:
国家自然科学基金项目（51273054）

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

CHEN Yang, SHI Tiejun, QIAN Ying, HE Tao

School of Chemical Engineering, Hefei University of Technology, Hefei 230009, Anhui, China

Received:2016-12-28 Revised:2017-02-21 Online:2017-06-05 Published:2017-06-05
Contact: 10.11949/j.issn.0438-1157.20161816
Supported by:
supported by the National Natural Science Foundation of China (51273054)

摘要/Abstract

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

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

中图分类号:

O631

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.

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.

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新型含硼苯并噁嗪的合成及其与环氧树脂共混热性能

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

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