| 含氰基和乙炔基苯并噁嗪树脂的固化行为及性能研究 |
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| 引用本文： | 李泽宇,王志德,周权. 含氰基和乙炔基苯并噁嗪树脂的固化行为及性能研究[J]. 北京化工大学学报(自然科学版), 2000, 49(3): 22. DOI: 10.13543/j.bhxbzr.2022.03.004 |
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| 作者姓名： | 李泽宇 王志德 周权 |
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| 作者单位： | 1. 华东理工大学 材料科学与工程学院 特种功能高分子材料及相关技术教育部重点实验室, 上海 200237;2. 北京航空材料研究院, 北京 100095 |
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| 基金项目： | 中央高校基本科研业务费（50321042017001）；国家自然科学基金（52173074） |
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| 摘 要： | 以4-氨基苯氧邻苯二甲腈（BZN）、间氨基苯乙炔（APA）和多聚甲醛为原料制备了含氰基和乙炔基的苯并噁嗪树脂（BZ-BPA）。利用差示扫描量热法（DSC）、傅里叶变换红外光谱法（F T-IR）、热重分析法（TGA）分析了BZ-BPA的固化行为，得到：BZ-BPA在固化反应过程中存在两个放热峰（225℃和274℃）；在氮气氛围下，BZ-BPA固化物热失重5%的温度（T d5）为502.6℃，800℃时质量残留率为79.8%；在空气氛围下，T d5为506.0℃，800℃时质量残留率为29.6%。采用Kissinger法计算得到两个固化反应的表观活化能（E）：E1=228.31 kJ/mol，E2=87.97 kJ/mol；由Ozawa法计算得到：E1=225.98 kJ/mol，E2=92.26 kJ/mol；固化反应接近一级反应。考察了石英纤维增强的BZ-BPA复合材料（QF/BZ-BPA）的力学性能和耐热性能，结果显示：QF/BZ-BPA的玻璃化转变温度（Tg）为476℃；在常温下其弯曲强度为764.2 MPa，层间剪切强度为57.3 MPa；在400℃热处理2 h后，其弯曲强度为614.5 MPa，层间剪切强度为38.1 MPa；400℃热处理10 h后，其质量损失仅为2.4%。以上结果表明BZ-BPA复合材料具有优异的力学性能和耐热性能。
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| 关 键 词： | 乙炔基 氰基 苯并噁嗪树脂 固化行为 耐热性 |
| 收稿时间： | 2021-12-20 |
Curing behavior and properties of a benzoxazine resin containing cyano and acetylene groups |
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| LI ZeYu,WANG ZhiDe,ZHOU Quan. Curing behavior and properties of a benzoxazine resin containing cyano and acetylene groups[J]. Journal of Beijing University of Chemical Technology, 2000, 49(3): 22. DOI: 10.13543/j.bhxbzr.2022.03.004 |
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| Authors: | LI ZeYu WANG ZhiDe ZHOU Quan |
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| Affiliation: | 1. Key Laboratory of Specially Functional Polymer Materials and Related Technology of Ministry of Education, School of Materials Science and Engineering, East China University of Science and Technology, Shanghai 200237;2. Beijing Aviation Materials Research Institute, Beijing 100095, China |
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| Abstract: | A cyano- and ethynyl-containing benzoxazine resin (BZ-BPA) has been prepared from 4-aminophenoxyphthalonitrile (BZN), m -aminophenylacetylene (APA) and paraformaldehyde. The curing behavior of BZ-BPA was analyzed by differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). There are two exothermic peaks (225 ℃ and 274 ℃) in the curing process of BZ-BPA. The temperature of 5% thermal weight loss (T d5 ) of BZ-BPA cured in nitrogen is 502.6 ℃, and the residual mass rate at 800 ℃ is 79.8%. T d5 in air is 506.0 ℃, and the residual mass rate at 800 ℃ is 29.6%. The apparent activation energies of the two curing reactions were obtained by the Kissinger method: E1=228.31 kJ/mol, and E2=87.97 kJ/mol. The apparent activation energies were also obtained by the Ozawa method: E1=225.98 kJ/mol, E2=92.26 kJ/mol. The curing process is close to a first-order reaction. The mechanical and thermal properties of quartz fiber-reinforced BZ-BPA composites (QF/BZ-BPA) were investigated. The glass transition temperature (Tg) of QF/BZ-BPA is 476 ℃. At room temperature, the flexural strength is 764.2 MPa, and the interlaminar shear strength is 57.3 MPa. After heat treatment at 400 ℃ for 2 h, the flexural strength was 614.5 MPa and the interlaminar shear strength was 38.1 MPa. After heat treatment at 400 ℃ for 10 h, the mass loss was only 2.4%. The above results indicate that the BZ-BPA composites have excellent mechanical properties and heat resistance. |
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| Keywords: | ethynyl cyano benzoxazine resin curing behavior heat resistance |
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