Journal of Textile Research ›› 2026, Vol. 47 ›› Issue (02): 247-254.doi: 10.13475/j.fzxb.20251003001

• Dyeing and Finishing Engineering • Previous Articles     Next Articles

Preparation of different cellulose nanocrystals and their effects on functionality of composite membranes

ZHANG Tao1, ZHANG Fuli1(), GUO Hong2, LI Zhao2,3, LI Dan1, WANG Yazhou2, LIN Wei2   

  1. 1 PLA Naval Medical Center, Shanghai 200433, China
    2 College of Textile Engineering, Taiyuan University of Technology, Jinzhong, Shanxi 030600, China
    3 Wuhan Research Institute of Materials Protection Co., Ltd., China National Machinery Industry Corporation, Wuhan, Hubei 430000, China
  • Received:2025-10-15 Revised:2025-12-08 Online:2026-02-15 Published:2026-04-24
  • Contact: ZHANG Fuli E-mail:ly24112@163.com

Abstract:

Objective To achieve the high-value recycling of waste indigo denim and the preparation of functional materials, this study aims to clarify the role of indigo dye in the recycling process and explore a high-value technical pathway without complex decolorization. The feasibility of directly preparing functional cellulose nanocrystals (CNCs) without decolorization was successfully demonstrated, providing both a theoretical basis and technical support for the recycling of waste denim.

Methods Three types of CNCs (named W-CNCs, D-CNCs, and T-CNCs) were prepared by sulfuric acid hydrolysis from undyed denim, waste indigo denim and waste indigo denim decolorized by N, N-dimethylformamide (DMF). The microstructure, physicochemical properties and thermal stability of the three CNCs were characterized by SEM, XRD, FT-IR and TGA. The films were prepared by compounding the three types of CNCs with polyvinyl alcohol (PVA) at different mass ratios (1%, 3%, 5%, 7%, 10%), respectively. The mechanical properties, thermal stability and UV resistance of the resulting composite films were subsequently evaluated.

Results All three CNCs exhibited a rod-like morphology with no significant difference in dimensions and maintained a cellulose I crystal structure. Due to the retention of the characteristic functional groups of indigo dye, the D-CNCs suspension displayed a distinct blue color, whereas the W-CNCs and T-CNCs suspensions appeared milky white. Compared with raw cotton fibers, the thermal stability of all CNCs decreased significantly, and the presence of residual indigo dye did not markedly influence this trend. Functional analysis demonstrated that the tensile strength of the PVA composite film increased by 20.4% with the incorporation of 5% D-CNCs. When the D-CNCs content was elevated to 10%, the initial decomposition temperature of the composite film was raised by 8%. Moreover, with increasing D-CNCs loading, the transmittance of the composite film in the 200 - 400 nm UV range decreased substantially, resulting in a gradual enhancement of UV-blocking performance. Specifically, the UV absorption rates reached 96.39% and 98.5% at D-CNCs loadings of 5% and 10%, respectively.

Conclusion The residual indigo dye not only imparted distinctive chromatic properties to CNCs, but also demonstrated notable advantages in enhancing the mechanical properties, improving thermal stability, and conferring UV resistance to PVA composites. The technology proposed in this study for directly preparing functional CNCs from waste indigo denim can be extended to the field of textile waste recycling, providing low-cost raw materials for UV-resistant packaging materials and flexible composite materials. Furthermore, this study presented a viable technical pathway for the high-value recycling and reuse of waste indigo denim, offering promising environmental benefits and application prospects.

Key words: cellulose nanocrystal, recycling of waste textiles, decolorization, indigo dye, indigo denim fabric, composite membrane, UV resistance

CLC Number: 

  • TS102.9

Fig.1

Photographs of different fabric samples. (a) Indigo denim fabric;(b) Decolorized indigo denim fabric; (c) Grey cotton denim fabric"

Fig.2

SEM images and suspension photographs of different CNCs. (a) T-CNCs;(b) D-CNCs;(c) W-CNCs;(d) T-CNCs suspension;(e) D-CNCs suspension;(f) W-CNCs suspension"

Tab.1

Comparison of different CNCs sizes"

样品编号 样品名称 宽度/nm 长度/nm
1 T-CNCs 12.3±5.2 132±52
2 D-CNCs 14.7±4.4 154±66
3 W-CNCs 13.1±4.6 127±49

Fig.3

FT-IR spectra of T-CNCs, D-CNCs, W-CNCs and cotton fabric"

Fig.4

XRD patterns of T-CNCs, D-CNCs, and W-CNCs"

Fig.5

Comparison of TGA of T-CNCs, D-CNCs, W-CNCs, and cotton fabric"

Fig.6

Mechanical properties of pure PVA film and composite films with different contents of T-CNCs and D-CNCs. (a) Tensile Strength;(b) Elongation at Break"

Fig.7

Thermogravimetric curves of composite films with different amounts of T-CNCs and D-CNCs added. (a)TG curves;(b)DTG curves"

Fig.8

Light transmittance of composite films with different amounts of T-CNCs and D-CNCs added"

Fig.9

Photographs of composite membranes with different addition amounts of T-CNCs and D-CNCs"

[1] ALWALA W, PERJU A, SCHWARZ M, et al. The compostability of denim fabrics dyed with various indigos[J]. BioResources, 2024, 19(2): 2685-2700.
doi: 10.15376/biores
[2] MANIAN A P, MUELLER S, BECHTOLD T, et al. Quantification of indigo on denim textiles as basis for jeans recycling[J]. Dyes and Pigments, 2023, 216: 111327.
doi: 10.1016/j.dyepig.2023.111327
[3] ZHAO M Y, ZHOU Y, MENG J, et al. Virtual carbon and water flows embodied in global fashion trade - a case study of denim products[J]. Journal of Cleaner Production, 2021, 303: 127080.
doi: 10.1016/j.jclepro.2021.127080
[4] BUSCIO V, CRESPI M, GUTIÉRREZ-BOUZÁN C. A critical comparison of methods for the analysis of indigo in dyeing liquors and effluents[J]. Materials, 2014, 7(9): 6184-6193.
doi: 10.3390/ma7096184 pmid: 28788185
[5] WANG T, LIU B, XUE Y J, et al. Effect of textile waste on incineration behavior of dyeing sludge: combustion characteristics, gas emissions, kinetics[J]. Journal of Cleaner Production, 2024, 435: 140619.
doi: 10.1016/j.jclepro.2024.140619
[6] ABAGNATO S, RIGAMONTI L, GROSSO M. Life cycle assessment applications to reuse, recycling and circular practices for textiles: a review[J]. Waste Management, 2024, 182: 74-90.
doi: 10.1016/j.wasman.2024.04.016 pmid: 38643525
[7] RENDÓN-CASTRILLÓN L, RAMÍREZ-CARMONA M, OCAMPO-LÓPEZ C, et al. Efficient bioremediation of indigo-dye contaminated textile wastewater using native microorganisms and combined bioaugmentation-biostimulation techniques[J]. Chemosphere, 2024, 353: 141538.
doi: 10.1016/j.chemosphere.2024.141538
[8] SCOTT C A, SABER D A, NEIVANDT D J. Engineering a compostable isolation gown to reduce hospital-derived synthetic waste accumulation in landfill[J]. Environmental Technology & Innovation, 2024, 35: 103663.
[9] FAN W, WANG Q, RONG K, et al. MXene enhanced 3D needled waste denim felt for high-performance flexible supercapacitors[J]. Nano-Micro Letters, 2023, 16(1): 36.
doi: 10.1007/s40820-023-01226-y pmid: 38019340
[10] PINHO-LOPES M. Sand reinforced with recycled cotton textiles from waste blue-jeans: stress-strain response[J]. International Journal of Geosynthetics and Ground Engineering, 2022, 8(5): 59.
doi: 10.1007/s40891-022-00404-z
[11] KRAMENS J, VĪGANTS E, KANUKUNTLA S P, et al. Study of the application of pellets from textile material waste and biomass mixture in industrial and residental heating systems[J]. ENVIRONMENT TECHNOLOGIES RESOURCES Proceedings of the International Scientific and Practical Conference, 2023, 1: 86-92.
[12] TRACHE D, HUSSIN M H, HUI CHUIN C T, et al. Microcrystalline cellulose: isolation, characterization and bio-composites application: a review[J]. International Journal of Biological Macromolecules, 2016, 93: 789-804.
doi: 10.1016/j.ijbiomac.2016.09.056
[13] WANG S J, ZHANG T, ZHANG X L, et al. Development of 3D needled composite from denim waste and polypropylene fibers for structural applications[J]. Construction and Building Materials, 2022, 314: 125583.
doi: 10.1016/j.conbuildmat.2021.125583
[14] AKHLAGHI BAGHERJERI M, HAQUE A N M A, MONHEMI H, et al. Dissolution of denim waste in N-methyl morpholine-N-oxide monohydrate for fabrication of regenerated cellulosic film: experimental and simulation study[J]. Carbohydrate Polymers, 2024, 346: 122655.
doi: 10.1016/j.carbpol.2024.122655
[15] MO Y, HUANG X Y, YUE M, et al. Preparation of nanocellulose and application of nanocellulose polyurethane composites[J]. RSC Advances, 2024, 14(26): 18247-18257.
doi: 10.1039/d4ra01412j pmid: 38854830
[16] LI Z, ZHANG M L, LI F, et al. Recycling of waste denim: a stepwise utilisation strategy for clean decolourisation, opening and degradation[J]. Waste Management, 2025, 198: 12-20.
doi: 10.1016/j.wasman.2025.02.037 pmid: 40014882
[1] WANG Hongli, ZHANG Hui, LIU Jianyu, YU Haize, ZHANG Yaning, WANG Lili, XU Xuechao. Preparation and adsorption-photocatalytic performance of cotton-based biochar-ZIF-L(Zn)-chitosan/polypropylene composite membrane [J]. Journal of Textile Research, 2025, 46(09): 84-93.
[2] ZUO Zhuofan, LU Kailiang, LI Qianwen, ZHANG Wei. Optimization of treatment efficiency of indigo dyeing wastewater by electrocoagulation using Al-Mg alloy anodes [J]. Journal of Textile Research, 2025, 46(09): 197-204.
[3] LI Han, QIAN Jianhua, WENG Kexin, WANG Ao, DAI Hongxiang, SHAN Jiangyin. Preparation of woven fabrics from polyvinyl chloride fiber and their composite film structures and properties [J]. Journal of Textile Research, 2025, 46(08): 80-88.
[4] WEI Xuanxiang, FENG Yang, FAN Xiangyu, WU Minghua, YU Deyou. Yak wool decolorization using homogeneous advanced oxidation technology and its mechanism [J]. Journal of Textile Research, 2025, 46(06): 151-159.
[5] XIANG Wenlong, YANG Jingran, XIAO Xiaozhen. Preparation of Fe-Co bimetallic organic framework/rice husk composite material and its performance in dye decolorization [J]. Journal of Textile Research, 2025, 46(06): 178-186.
[6] ZHU Lin, WANG Zhanpeng, WU Baozhai, WANG Shaopeng, LIU Yiming, DAI Chengna, CHEN Biaohua. Decolorization of waste polyester fabrics by solvent extraction and its influence on glycolysis [J]. Journal of Textile Research, 2025, 46(01): 103-110.
[7] HUANG Tiantian, SONG Yuanzhu, ZHAO Bin. Tannic acid-based flame retardant multifunctional coating for surface finishing Lyocell fabrics [J]. Journal of Textile Research, 2024, 45(12): 152-158.
[8] HAN Bo, WANG Yulin, SHU Dawu, WANG Tao, AN Fangfang, SHAN Juchuan. Reactive dyeing using recycled dyeing wastewater [J]. Journal of Textile Research, 2023, 44(08): 151-157.
[9] WANG Wei, WU Jiaxin, ZHANG Xiaoyun, ZHANG Chuanjie, GONG Zhaoqing. Decolorization properties and mechanism of waste cotton fabrics for preparing cotton pulp [J]. Journal of Textile Research, 2023, 44(07): 175-183.
[10] LIU Dunlei, LU Jiaying, XUE Tiantian, FAN Wei, LIU Tianxi. Preparation and properties of superhydrophobic thermal insulating polyester nanofiber/silica aerogel composite membranes [J]. Journal of Textile Research, 2023, 44(07): 18-25.
[11] WANG Jing, LOU Yaya, WANG Chunmei. Preparation and decolorization of iron-based metal\|organic framework/activated carbon fiber composites [J]. Journal of Textile Research, 2022, 43(08): 126-131.
[12] YANG Wenbo, ZHANG Aojie, LIU Youyan, LI Qingyun. Adsorption and decolorization of Reactive Blue 4 by polyurethane foam-immobilized biosystem [J]. Journal of Textile Research, 2022, 43(08): 132-139.
[13] JIN Yaofeng, LIU Leigen, WANG Wei, LU Xin. Preparation and UV shielding of rutile nano-TiO2 by induction of nanocrystal-cellulose at room temperature [J]. Journal of Textile Research, 2022, 43(02): 176-182.
[14] WU Jiayin, WANG Hanchen, HUANG Biao, LU Qilin. Fabrication of fluorescent cellulose nanocrystals hydrogels for chloride ion response [J]. Journal of Textile Research, 2022, 43(02): 44-52.
[15] GAO Qiang, WANG Xiao, GUO Yajie, CHEN Ru, WEI Ju. Preparation and performance of cotton based Ti3C2Tx oil-water separation membrane [J]. Journal of Textile Research, 2022, 43(01): 172-177.
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
No Suggested Reading articles found!