Low-temperature gelling phenomenon for a class of slow-curing phthalonitrile-benzoxazine resin,Journal of Applied Polymer Science

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Low-temperature gelling phenomenon for a class of slow-curing phthalonitrile-benzoxazine resin
Journal of Applied Polymer Science ( IF 2.7 ) Pub Date : 2023-11-30 , DOI: 10.1002/app.54917
Xulin Yang _{1,

2,

3} , Ziyi Zhu ₁ , Pan Wang _{1,

2} , Wenwu Lei ₁ , Fei Zhong ₁ , Ying Li _{1,

2} , Kui Li _{1,

2} , Wei Feng _{1,

2}

Affiliation

Bifunctional phthalonitrile-benzoxazine (PNBZ) usually suffers from slow-curing characteristics. Recently, we unexpectedly observed a waste liquid containing PNBZ solution and excess ethylenediamine (EDA) had turned into a gel at room temperature. Since the report on the PNBZ gelling phenomenon below 150°C was rare, this accidental finding manifested the possible formation of PNBZ gel at low temperatures. By varying the EDA molar ratio, PNBZ gels with different microstructures were successfully realized at the low temperature of 50°C. Through the differential scanning calorimetry, thermogravimetric analyse (TGA), and Fourier transform infrared technique, the driving force behind the gel formation was found to be the low-temperature copolymerization between the amino group of EDA and the BZ ring of PNBZ, resulting in the amine-containing intermediate. PNBZ gel was thermally unstable, but was mechanically robust. The current method was also universal to realize polymer or composite gels for a class of slow-curing PNBZ resin (i.e., allyl-containing PNBZ gel and its carbon nanotube-filled composite gel). This study not only expands our understanding of the low-temperature polymerization behavior of PNBZ but also provides a versatile strategy for low-temperature preparation of PNBZ-based gels. Making the most of current approach, it is believed that multifunctional PNBZ-based gels will be developed for various applications.

中文翻译：

一类慢固化邻苯二甲腈苯并恶嗪树脂的低温凝胶现象

双官能邻苯二甲腈-苯并恶嗪 (PNBZ) 通常具有固化缓慢的特点。最近，我们意外地观察到含有PNBZ溶液和过量乙二胺（EDA）的废液在室温下变成了凝胶。由于PNBZ在150℃以下凝胶化现象的报道很少，这一偶然发现表明PNBZ凝胶在低温下可能形成。通过改变EDA摩尔比，在50℃的低温下成功实现了具有不同微观结构的PNBZ凝胶。通过差示扫描量热法、热重分析（TGA）和傅里叶变换红外技术，发现凝胶形成的驱动力是EDA的氨基与PNBZ的BZ环之间的低温共聚，从而产生凝胶含胺中间体。PNBZ 凝胶热不稳定，但机械性能稳定。目前的方法对于实现一类慢固化PNBZ树脂的聚合物或复合凝胶（即含烯丙基的PNBZ凝胶及其碳纳米管填充复合凝胶）也具有通用性。这项研究不仅扩大了我们对 PNBZ 低温聚合行为的理解，而且为低温制备 PNBZ 凝胶提供了一种通用策略。充分利用现有方法，相信将开发出适用于各种应用的多功能 PNBZ 凝胶。

更新日期：2023-11-30

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