Druel Lucile, Kenkel Amelie, Baudron Victor, Buwalda Sytze, Budtova Tatiana
MINES ParisTech, PSL Research University, Center for Materials Forming (CEMEF), UMR CNRS 7635, CS 10207, 06904 Sophia Antipolis, France.
Institute of Thermal Separation Processes, Hamburg University of Technology, Eißendorfer Straße 38, 21073 Hamburg, Germany.
Biomacromolecules. 2020 May 11;21(5):1824-1831. doi: 10.1021/acs.biomac.9b01725. Epub 2020 Feb 13.
Cellulose aerogel microparticles were made via emulsification/nonsolvent induced phase separation/drying with supercritical CO. Cellulose was dissolved in NaOH-based solvent with and without additives in order to control solution gelation. Two emulsions, cellulose solution/oil and cellulose nonsolvent/oil, were mixed to start nonsolvent induced phase separation (or coagulation) of cellulose inside each cellulose droplet leading to the formation of so-called microgels. Different options of triggering coagulation were tested, by coalescence of droplets of cellulose solution and cellulose nonsolvent and by diffusion of nonsolvent partly soluble in the oil, accompanied by coalescence. The second option was found to be the most efficient for stabilization of the shape of coagulated cellulose microgels. The influence of gelation on particle formation and aerogel properties was investigated. The aerogel particles' diameter was around a few tens of microns, and the specific surface area was 250-350 m/g.
纤维素气凝胶微粒是通过乳化/非溶剂诱导相分离/超临界CO₂干燥法制备的。为了控制溶液凝胶化,将纤维素溶解在含或不含添加剂的基于NaOH的溶剂中。将两种乳液,即纤维素溶液/油乳液和纤维素非溶剂/油乳液混合,以引发每个纤维素液滴内纤维素的非溶剂诱导相分离(或凝聚),从而形成所谓的微凝胶。测试了不同的引发凝聚的方法,包括纤维素溶液液滴与纤维素非溶剂液滴的聚结,以及部分可溶于油的非溶剂的扩散并伴随聚结。发现第二种方法对于稳定凝聚的纤维素微凝胶的形状最为有效。研究了凝胶化对颗粒形成和气凝胶性能的影响。气凝胶颗粒的直径约为几十微米,比表面积为250 - 350 m²/g。