Elgoyhen Justine, Pirela Valentina, Müller Alejandro J, Tomovska Radmila
POLYMAT and Department of Applied Chemistry, Faculty of Chemistry, University of the Basque Country UPV/EHU, Avda Tolosa 72, 20018 Donostia-San Sebastián, Spain.
POLYMAT and Department of Polymers and Advanced Materials: Physics Chemistry and Technology, Faculty of Chemistry, University of the Basque Country UPV/EHU, Paseo Manuel de Lardizábal 3, 20018 Donostia-San Sebastián, Spain.
ACS Appl Polym Mater. 2023 Oct 20;5(11):8845-8858. doi: 10.1021/acsapm.3c01128. eCollection 2023 Nov 10.
The synthesis of waterborne thiol-ene polymer dispersions is challenging due to the high reactivity of thiol monomers and the premature thiol-ene polymerization that leads to high irreproducibility. By turning this challenge into an advantage, a synthesis approach of high solid content film-forming waterborne poly(thioether) prepolymers is reported based on initiator-free step growth sonopolymerization. Copolymerization of bifunctional thiol and ene monomers diallyl terephthalate, glycol dimercaptoacetate, glycol dimercaptopropionate, and 2,2-(ethylenedioxy)diethanethiol gave rise to linear poly(thioether) functional chains with molar mass ranging between 7 and 23 kDa when synthesized at 30% solid content and between 1 and 9 kDa at increased solid content of 50%. To further increase the polymers' molar mass, an additional photopolymerization step was performed in the presence of a water-soluble photoinitiator, i.e., lithium phenyl-2,4,6-trimethylbenzoylphosphinate, leading to high molar mass chains of up to 200 kDa, the highest reported so far for step grown poly(thioethers). The polymer dispersions presented good film-forming ability at room temperature, yielding semicrystalline films with a high potential for barrier coating applications. Nevertheless, affected by the polymer chemical repeating structure, which includes an aromatic ring, these thiol-ene chains can only crystallize very slowly from the molten state. Herein, for the first time, we present the successful implementation of a self-nucleation (SN) procedure for these types of poly(thioethers), which effectively accelerates their crystallization kinetics.
水性硫醇-烯聚合物分散体的合成具有挑战性,因为硫醇单体的高反应活性以及过早的硫醇-烯聚合会导致高度不可重复性。通过将这一挑战转化为优势,本文报道了一种基于无引发剂逐步生长声聚合的高固含量成膜水性聚硫醚预聚物的合成方法。双官能硫醇与烯类单体对苯二甲酸二烯丙酯、乙二醇二巯基乙酸酯、乙二醇二巯基丙酸酯和2,2-(乙二氧基)二乙硫醇进行共聚,当在30%固含量下合成时,得到摩尔质量在7至23 kDa之间的线性聚硫醚功能链,在固含量增加至50%时,摩尔质量在1至9 kDa之间。为了进一步提高聚合物的摩尔质量,在水溶性光引发剂即苯基-2,4,6-三甲基苯甲酰基次膦酸锂存在下进行额外的光聚合步骤,得到高达200 kDa的高摩尔质量链,这是迄今为止报道的逐步生长聚硫醚中最高的。该聚合物分散体在室温下具有良好的成膜能力,可得到具有阻隔涂层应用高潜力的半结晶膜。然而,受聚合物化学重复结构(包括芳香环)的影响,这些硫醇-烯链只能从熔融状态非常缓慢地结晶。在此,我们首次成功地对这类聚硫醚实施了自核化(SN)程序,有效地加速了它们的结晶动力学。