Romano Angela, Frattini Stefano, Miani Roberto, Gioia Claudio, Celli Annamaria, Sisti Laura
Department of Civil, Chemical, Environmental and Materials Engineering, University of Bologna, Via Terracini 28, 40131, Bologna, Italy.
Department of Physics, University of Trento, Via Sommarive 14, 38123, Povo, TN, Italy.
ChemSusChem. 2025 Apr 1;18(7):e202402154. doi: 10.1002/cssc.202402154. Epub 2024 Nov 28.
Developing polymers with labile bonds has attracted increasing attention since it can favor the chemical recycling into oligomers or even the starting monomers that could be recovered and re-used. Different chemical bonds can break upon exposure to external stimuli, such as thermal, UV, or chemical triggers. Among these, the acetal bond can degrade under mild acidic conditions. This study focuses on the synthesis of polymers constituted by acetal moieties suitable for triggered depolymerization. In particular, the solvent-less polyaddition of 1,4-butanediol and 1,4-butanediol divinyl ether was developed and optimized using a heterogeneous catalyst (Amberlyst 15) at 100 °C. The best reaction conditions in terms of catalyst loading and reagent ratio were determined through a Design-of-Experiment aiming to achieve high conversion, low polydispersity, and desirable molecular weight. The resulting material presented an amorphous character and thermal stability up to 220 °C. It was confirmed responsive in an acidic environment, being completely hydrolyzed in 42 days, while remaining stable at neutral and basic pH. The obtained results represent a proof of concept for the design of pH-responsive materials through solventless, and scalable processes. The acetal moiety may be further exploited to achieve architectures presenting a sustainable end-of-life by implementing a recycling-by-design approach for new adhesives or novel degradable thermosetting materials.
开发具有不稳定键的聚合物已引起越来越多的关注,因为它有利于化学循环为低聚物甚至可回收和再利用的起始单体。不同的化学键在受到外部刺激(如热、紫外线或化学触发因素)时会断裂。其中,缩醛键在温和酸性条件下会降解。本研究重点关注由适合触发解聚的缩醛部分构成的聚合物的合成。特别是,使用非均相催化剂(Amberlyst 15)在100°C下开发并优化了1,4 - 丁二醇和1,4 - 丁二醇二乙烯基醚的无溶剂聚加成反应。通过实验设计确定了催化剂负载量和试剂比例方面的最佳反应条件,旨在实现高转化率、低多分散性和理想的分子量。所得材料呈现无定形特征,热稳定性高达220°C。证实其在酸性环境中有响应,在42天内完全水解,而在中性和碱性pH下保持稳定。所得结果代表了通过无溶剂且可扩展的过程设计pH响应材料的概念验证。缩醛部分可通过对新型粘合剂或新型可降解热固性材料实施设计回收方法,进一步用于实现具有可持续生命周期结束的结构。