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杯芳烃改性低粘度高残炭酚醛树脂的研究

Study on Low Viscosity and High Char Yield Phenolic Resins Modified by Calixarenes

【作者】 沈红

【导师】 雷毅;

【作者基本信息】 四川大学 , 高分子材料, 2004, 硕士

【摘要】 本文合成了Resorcinarenes杯芳烃、对叔丁基杯[4]芳烃和含(口恶)嗪环的杯芳烃衍生物,并采用红处光谱(FTIR)、核磁共振氢谱(~1H-NMR)和差示扫描量热法(DSC)对它们的结构和性能进行了表征。 制备了两种酚醛树脂,即在氢氧化钠和氢氧化钾混合物的催化作用下合成出低粘度酚醛树脂,另外在氨水的催化下合成了氨酚醛树脂,并讨论了原料配比与酚醛树脂粘度的关系,用凝胶渗透色谱(GPC)对两种酚醛树脂的分子量及其分布进行了表征。以这两种热固性酚醛树脂为基础,分别加入一定比例的溶剂乙醇或活性稀释剂如苯甲醛、水杨醛、糠醇和糠醛等得到不同的树脂体系。在这些体系中再分别引入不同的杯芳烃,用布氏粘度计对各体系的粘度进行测量。 用DSC对酚醛树脂中引入了不同活性稀释剂和(或)杯芳烃的体系进行热固化行为的研究,从而推测各体系的固化原理和确定固化工艺。用热重分析法(TGA)对各酚醛树脂体系的固化物进行热性能的研究,结果表明以水杨醛为活性稀释剂的两种酚醛树脂中分别引入10%的含(口恶)嗪环的Resorcinarenes杯芳烃都可获得高残炭的树脂体系,且两者残炭相差不大。在氮气气氛中,700℃下它们的残炭率约为70%,比普通氨酚醛树脂提高了约11%。 最后,用TGA法对残炭率最高的热固性酚醛树脂体系进行热降解动力学的研究,并对热老化寿命进行估算,同时对流变性能进行了研究。

【Abstract】 Resorcinarenes, p-tert-Butylcalix[4]arene and oxazine derivative from Resorcinarenes were synthesized respectively and their molecular structure and performace were characterized by FTIR,H-NMR as well as DSC.A low viscosity resole was synthesized catalyzed by the compound of sodium hydroxide and potassium hydroxide ,then another resole was synthesized catalyzed by ammonia. The relationship of raw material ratio and the resole viscosity was discussed ,and their molecular weight and molecular weight distribution were characterized by GPC. Based on the two resoles , a certain proportion solvent ethanol , or reactive diluent such as benzaledhyde, salicylic aldehyde, furfuryl alcohol and furfural was added respectively in the two resoles obtaining various resole systems where different calixarenes were added further .The viscosity of various systems was measured by Bookfield viscosity meter.The cure characteristics of various resole systems added different reactive diluent and (or) calixarenes were researched by DSC. thus assuming cure mechanism and determinating cure technology. Thermal performances of various cured resole systems were studied by TGA which showed two resoles added respectively 10% oxazine derivative where salicylic aldehyde as a reactive diluent both have high similar char yield , performed in nitrogen atmosphere the char yield at 700℃ is about 70% which is higher 11% than general resoles catalyzed by ammonia.Finally, the thermal decomposition kinetics and thermal ageing lifetime of resole having the highest char yield were researched and estimated by TGA ,meanwhile the rheological behaviors were researched. Key words: calixarenes; resole; low viscosity; reactive diluent; char yield

  • 【网络出版投稿人】 四川大学
  • 【网络出版年期】2005年 01期
  • 【分类号】TQ323
  • 【被引频次】17
  • 【下载频次】457
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