Chen Yinjun, Zhang Huiyi, Majumdar Soumabrata, van Benthem Rolf A T M, Heuts Johan P A, Sijbesma Rint P
Department of Chemical Engineering & Chemistry, Institute for Complex Molecular Systems, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands.
Department of Chemical Engineering & Chemistry, Laboratory of Physical Chemistry, Eindhoven University of Technology, 5600 MB Eindhoven, The Netherlands.
Macromolecules. 2021 Oct 26;54(20):9703-9711. doi: 10.1021/acs.macromol.1c01389. Epub 2021 Oct 13.
The diamide-imide equilibrium was successfully exploited for the synthesis of dynamic covalent polymer networks in which a dissociative bond exchange mechanism leads to high processibility at temperatures above ≈110 °C. Dynamic covalent networks bridge the gap between thermosets and thermoplastic polymers. At the operating temperature, when the network is fixed, dynamic covalent networks are elastic solids, while at high temperatures, chemical exchange reactions turn the network into a processible viscoelastic material. Upon heating a dissociative network, the viscosity may also decrease due to a shift of the chemical equilibrium; in such materials, the balance between processibility and excessive flow is important. In this study, a network is prepared that upon heating to above ≈110 °C dissociates to a significant extent due to a shift in the amide-imide equilibrium of a bisimide, pyromellitic diimide, in combination with poly(tetrahydrofuran) diamines. At room temperature, the resulting materials are elastic rubbers with a tensile modulus of 2-10 MPa, and they become predominantly viscous above a temperature of approximately 110 °C, which is dependent on the stoichiometry of the components. The diamide-imide equilibrium was studied in model reactions with NMR, and variable temperature infrared (IR) spectroscopy was used to investigate the temperature dependence of the equilibrium in the network. The temperature-dependent mechanical properties of the networks were found to be fully reversible, and the material could be reprocessed several times without loss of properties such as modulus or strain at break. The high processibility of these networks at elevated temperatures creates opportunities in additive manufacturing applications such as selective laser sintering.
二酰胺 - 酰亚胺平衡被成功用于动态共价聚合物网络的合成,其中解离键交换机制导致在约110°C以上的温度下具有高加工性能。动态共价网络弥合了热固性聚合物和热塑性聚合物之间的差距。在操作温度下,当网络固定时,动态共价网络是弹性固体,而在高温下,化学交换反应使网络变成可加工的粘弹性材料。加热解离网络时,由于化学平衡的移动,粘度也可能降低;在这类材料中,加工性能和过度流动之间的平衡很重要。在本研究中,制备了一种网络,加热到约110°C以上时,由于双酰亚胺均苯四甲酸二酰亚胺与聚(四氢呋喃)二胺的酰胺 - 酰亚胺平衡发生移动,该网络会发生显著解离。在室温下,所得材料是拉伸模量为2 - 10 MPa的弹性橡胶,在约110°C以上的温度时,它们主要变成粘性的,这取决于组分的化学计量。通过核磁共振在模型反应中研究了二酰胺 - 酰亚胺平衡,并使用变温红外(IR)光谱研究了网络中平衡的温度依赖性。发现网络的温度依赖性力学性能是完全可逆的,并且该材料可以多次再加工而不会损失诸如模量或断裂应变等性能。这些网络在高温下的高加工性能为选择性激光烧结等增材制造应用创造了机会。