Enhanced Water Filtration Performance in Electrospun Cellulose Acetate Membranes via TEMPO-Mediated Cellulose Nanocrystal Incorporation and Hot Pressing

IF 5 3区工程技术 Q2 ENGINEERING, ENVIRONMENTAL

Journal of Polymers and the Environment Pub Date : 2025-08-25 DOI:10.1007/s10924-025-03659-5

Ane Arrizabalaga-Luzuriaga, Stefano Torresi, Ainara Saralegi, Arantxa Eceiza

{"title":"Enhanced Water Filtration Performance in Electrospun Cellulose Acetate Membranes via TEMPO-Mediated Cellulose Nanocrystal Incorporation and Hot Pressing","authors":"Ane Arrizabalaga-Luzuriaga, Stefano Torresi, Ainara Saralegi, Arantxa Eceiza","doi":"10.1007/s10924-025-03659-5","DOIUrl":null,"url":null,"abstract":"<div><p>Access to clean water is increasingly critical due to escalating pollution from industrialization and population growth. This study presents the development of advanced cellulose acetate (CA)-based membranes for water filtration through an integrated approach combining electrospinning, hot pressing, and cellulose nanocrystal (CNC) functionalization. A 12 wt% CA solution in a 4:1 acetone/acetic acid mixture was electrospun under optimized conditions (1 mL/h, 15 cm, 35–70% relative humidity) to produce uniform, bead-free nanofibrous mats. Subsequent hot pressing at 100 °C and 20 bar yielded denser membranes with enhanced mechanical durability and reduced pore size. Functionalization with CNCs and TEMPO-oxidized CNCs (CNC<sub>TEMPO</sub>) further improved performance. Structural characterization confirmed the successful TEMPO oxidation of CNCs, as evidenced by FTIR bands at 1730 and 1604 cm⁻¹ and a carboxyl content of 0.56 ± 0.04 mmol/g, enhancing nanocrystal dispersion and interfacial adhesion within the CA matrix. Moreover, SEM images showed denser and more homogeneous fiber morphology after hot pressing and CNC<sub>TEMPO</sub> incorporation, as well as higher tensile strength values, indicating structural reinforcement. These changes led to a reduction in water contact angle (from 104° to 37°) and filtration time from 100 min to under 30 s. Filtration tests showed improved rejection of 2.0 μm particles (92%) and efficient methylene blue dye removal (up to 95%) in membranes with 3 wt% CNC<sub>TEMPO</sub>. To the best of our knowledge, this is the first study to combine electrospinning, hot pressing, and TEMPO-oxidized cellulose nanocrystals in cellulose acetate membranes to simultaneously enhance wettability, mechanical stability, and filtration performance using a fully bio-based system. This integrated strategy offers a promising route for fabricating high-performance, multifunctional membranes for sustainable water treatment applications.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":659,"journal":{"name":"Journal of Polymers and the Environment","volume":"33 10","pages":"4485 - 4501"},"PeriodicalIF":5.0000,"publicationDate":"2025-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10924-025-03659-5.pdf","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Polymers and the Environment","FirstCategoryId":"5","ListUrlMain":"https://link.springer.com/article/10.1007/s10924-025-03659-5","RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"ENGINEERING, ENVIRONMENTAL","Score":null,"Total":0}

引用次数: 0

Abstract

Access to clean water is increasingly critical due to escalating pollution from industrialization and population growth. This study presents the development of advanced cellulose acetate (CA)-based membranes for water filtration through an integrated approach combining electrospinning, hot pressing, and cellulose nanocrystal (CNC) functionalization. A 12 wt% CA solution in a 4:1 acetone/acetic acid mixture was electrospun under optimized conditions (1 mL/h, 15 cm, 35–70% relative humidity) to produce uniform, bead-free nanofibrous mats. Subsequent hot pressing at 100 °C and 20 bar yielded denser membranes with enhanced mechanical durability and reduced pore size. Functionalization with CNCs and TEMPO-oxidized CNCs (CNC_TEMPO) further improved performance. Structural characterization confirmed the successful TEMPO oxidation of CNCs, as evidenced by FTIR bands at 1730 and 1604 cm⁻¹ and a carboxyl content of 0.56 ± 0.04 mmol/g, enhancing nanocrystal dispersion and interfacial adhesion within the CA matrix. Moreover, SEM images showed denser and more homogeneous fiber morphology after hot pressing and CNC_TEMPO incorporation, as well as higher tensile strength values, indicating structural reinforcement. These changes led to a reduction in water contact angle (from 104° to 37°) and filtration time from 100 min to under 30 s. Filtration tests showed improved rejection of 2.0 μm particles (92%) and efficient methylene blue dye removal (up to 95%) in membranes with 3 wt% CNC_TEMPO. To the best of our knowledge, this is the first study to combine electrospinning, hot pressing, and TEMPO-oxidized cellulose nanocrystals in cellulose acetate membranes to simultaneously enhance wettability, mechanical stability, and filtration performance using a fully bio-based system. This integrated strategy offers a promising route for fabricating high-performance, multifunctional membranes for sustainable water treatment applications.

Graphical Abstract

查看原文本刊更多论文

通过tempo介导的纤维素纳米晶掺入和热压增强醋酸纤维素电纺丝膜的水过滤性能

由于工业化和人口增长造成的污染不断升级，获得清洁水变得越来越重要。本研究介绍了通过结合静电纺丝、热压和纤维素纳米晶体（CNC）功能化的综合方法，开发先进的醋酸纤维素（CA）基水过滤膜。在优化条件（1 mL/h, 15 cm， 35-70%相对湿度）下，以12 wt% CA溶液为溶剂，以4:1丙酮/乙酸混合物静电纺丝，可制得均匀、无珠的纳米纤维垫。随后在100°C和20 bar下进行热压，得到了更致密的膜，增强了机械耐久性，减小了孔径。用cnc和tempo -氧化cnc （CNCTEMPO）功能化进一步提高了性能。结构表征证实了cnc的TEMPO氧化成功，FTIR波段在1730和1604 cm（⁻¹）和羧基含量为0.56±0.04 mmol/g证明了这一点，增强了纳米晶体的分散和CA基质内的界面粘附性。此外，SEM图像显示，热压和CNCTEMPO掺入后的纤维形态更致密，更均匀，抗拉强度值更高，表明结构增强。这些变化导致水接触角减少（从104°减少到37°），过滤时间从100分钟减少到30秒以下。过滤测试表明，在含有3 wt% CNCTEMPO的膜中，2.0 μm颗粒的截留率（92%）和亚甲基蓝染料的高效去除率（高达95%）有所提高。据我们所知，这是第一个将静电纺丝、热压和tempo氧化纤维素纳米晶体结合在醋酸纤维素膜上的研究，同时使用全生物基系统提高润湿性、机械稳定性和过滤性能。这种综合策略为制造高性能、多功能膜提供了一条有前途的途径，用于可持续的水处理应用。图形抽象

本文章由计算机程序翻译，如有差异，请以英文原文为准。

求助全文

约1分钟内获得全文求助全文

来源期刊

Journal of Polymers and the Environment 工程技术-高分子科学

CiteScore

9.50

自引率

7.50%

发文量

297

审稿时长

9 months

期刊介绍： The Journal of Polymers and the Environment fills the need for an international forum in this diverse and rapidly expanding field. The journal serves a crucial role for the publication of information from a wide range of disciplines and is a central outlet for the publication of high-quality peer-reviewed original papers, review articles and short communications. The journal is intentionally interdisciplinary in regard to contributions and covers the following subjects - polymers, environmentally degradable polymers, and degradation pathways: biological, photochemical, oxidative and hydrolytic; new environmental materials: derived by chemical and biosynthetic routes; environmental blends and composites; developments in processing and reactive processing of environmental polymers; characterization of environmental materials: mechanical, physical, thermal, rheological, morphological, and others; recyclable polymers and plastics recycling environmental testing: in-laboratory simulations, outdoor exposures, and standardization of methodologies; environmental fate: end products and intermediates of biodegradation; microbiology and enzymology of polymer biodegradation; solid-waste management and public legislation specific to environmental polymers; and other related topics.