Waste and Biomass Valorization

, Volume 10, Issue 7, pp 1913–1927 | Cite as

Extraction of Cellulose Nanocrystals with Structure I and II and Their Applications for Reduction of Graphene Oxide and Nanocomposite Elaboration

  • Faouzia Khili
  • Joao Borges
  • Pedro L. Almeida
  • Rabah Boukherroub
  • Amel Dakhlaoui OmraniEmail author
Original Paper


The aim of the present study is to investigate the effect of the hydrolysis process on the properties of nanocrystalline cellulose (NCC) isolated from different precursors and the subsequent use of the extracted NCC for the reduction of graphene oxide (GO). The raw materials (almond and peanut shells) chosen for the isolation of cellulose were selected on the basis of their abundance and their poorly investigation in the production of NCC. Microcrystalline cellulose (MCC) was firstly extracted by alkali and bleaching treatments, then hydrolyzed under different processes to produce NCC polymorphs with structure I (NCC-I) and NCC structure II (NCC-II). The Fourier transform infrared spectroscopy, the X-ray diffraction (XRD) and the 13C NMR studies of the alkali and bleached products confirmed the formation of cellulose type I with high purity and good crystallinity, while scanning electron microscopy (SEM) showed micrometric fibers with lengths reaching 80 µm. Sulfuric acid treatment of these microfibers results in NCC type I or II, depending on the hydrolysis process. SEM of the NCC samples exhibited nanorods with diameter and aspect ratio in the range of 20–40 and 20–25 nm, respectively. Thermogravimetric analysis (TGA) of the MCC and NCC products indicated stable materials with a degradation temperature reaching 240 and 200 °C for MCC and NCC, respectively. The other part of our work concerns the use of the obtained cellulose nanocrystals (type II) for the preparation of reduced graphene oxide composite (NCC/RGO), to demonstrate the reducing properties of the isolated NCCII.


Cellulose agrosources Cellulose nanocrystals Sulfuric acid hydrolysis Cellulose nanorods Graphene oxide Reduced graphene oxide composite 



This work was partly supported by The Tunisian Ministry of Higher Education and Scientific Research and the Portuguese Science and Technology Foundation through projects FCT/5964/27/5/2013/S, PTDC/FIS/NAN/0117/2014 and by FEDER funds through the COMPETE 2020 Program and National Funds through FCT - Portuguese Foundation for Science and Technology under the project UID/CTM/50025/2013/S and by the Portuguese Nuclear Magnetic Resonance Network (PTNMR).

Supplementary material

12649_2018_202_MOESM1_ESM.docx (2.9 mb)
Supplementary material 1 (DOCX 2958 KB)


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Copyright information

© Springer Science+Business Media B.V., part of Springer Nature 2018

Authors and Affiliations

  • Faouzia Khili
    • 1
    • 4
  • Joao Borges
    • 2
  • Pedro L. Almeida
    • 2
    • 3
  • Rabah Boukherroub
    • 4
  • Amel Dakhlaoui Omrani
    • 5
    • 6
    Email author
  1. 1.Unity of Research ‘Physics of Lamellar Materials and Hybrid Nanomaterials (PMLNH)’, Faculty of Sciences BizerteUniversity CarthageCarthageTunisia
  2. 2.Nova,I3N - CENIMAT, Departamento de Ciência dos Materiais, Faculdade de Ciências e TecnologiaFCT/UNLCaparicaPortugal
  3. 3.Área Departamental de FísicaInstituto Superior de Engenharia de LisboaLisboaPortugal
  4. 4.University of Lille, CNRS, Central Lille, ISEN, University of ValenciennesUMR 8520, IEMNLilleFrance
  5. 5.Department of Chemistry, Faculty of Sciences and Arts-KhulaisUniversity of JeddahJeddahKingdom of Saudi Arabia
  6. 6.Laboratory of Physical Chemistry of Mineral Materials and Their Applications, National Center of Research in Material SciencesCNRSMSolimanTunisia

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