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Preparation and Characterization of Regenerated Cellulose Using Ionic Liquid

Authors:
Vaniespree Govindan at Universiti Malaysia Perlis
Vaniespree Govindan
Salmah Husseinsyah at Universiti Malaysia Perlis
Salmah Husseinsyah
P.L. Teh at Universiti Malaysia Perlis
P.L. Teh
Faisal Tanjung at BMJpaperpack
Faisal Tanjung
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Abstract and Figures

Regenerated cellulose were prepared by dissolving cellulose in lithium chloride (LiCl) and dimethylacetamide (DMAc). The effect of MCC content on tensile properties and X-ray diffraction were studied. The results found that regenerated cellulose at 3wt% of MCC content have higher tensile strength. The Young's modulus of regenerated cellulose composite increased with increasing MCC content while elongation at break decreased. Crystallinity index of regenerated cellulose also increased as MCC content increased.
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Advances in Environmental Biology, 8(8) 2014, Pages: 2620-2625
AENSI Journals
Advances in Environmental Biology
Journal home page: http://www.aensiweb.com/AEB/
Corresponding Author: Salmah Hussiensyah. Universiti Malaysia Perlis, Division of Polymer Engineering, School of
Materials Engineering, 02600 Jejawi, Perlis, Malaysia.
Fax: 604-9798178. Email: irsalmah@unimap.edu.my
Preparation and Characterization of Regenerated Cellulose Using Ionic Liquid
Vaniespree Govindan, Salmah Hussiensyah, Teh Pei Leng, Faisal Amri
Universiti Malaysia Perlis, Division of Polymer Engineering, School of Materials Engineering, 02600 Jejawi, Perlis, Malaysia.
A R TI C LE I NF O
A BS T R AC T
Article history:
Received 28 February 2014
Received in revised form 25 May 2014
Accepted 6 June 2014
Available online 20 June 2014
Keywords:
Regenerated cellulose
Ionic liquid
Mechanical properties
X-ray diffraction (XRD)
Regenerated cellulose were prepared by dissolving cellulose in lithium chloride (LiCl)
and dimethylacetamide (DMAc). The effect of MCC content on tensile properties and
X-ray diffraction were studied. The results found that regenerated cellulose at 3wt% of
MCC content have higher tensile strength. The Young‟s modulus of regenerated
cellulose composite increased with increasing MCC content while elongation at break
decreased. Crystallinity index of regenerated cellulose also increased as MCC content
increased.
© 2014 AENSI Publisher All rights reserved.
To Cite This Article: Vaniespree Govindan, Salmah Hussiensyah, Teh Pei Leng, Faisal Amri, Preparation and Characterization of Regenerated
Cellulose Using Ionic Liquid. . Adv. Environ. Biol., 8(8), 2620-2625, 2014
INTRODUCTION
Cellulose is the most abundant bio-renewable material, with a long and well-established technological base
[12] and almost inexhaustible source of raw material for the increasing demand for environmentally friendly and
biocompatible products [30]. Cellulose is one of the most widespread biopolymer found globally, existing in a
variety of living species such as plant, animals, bacteria and some amoebas [18]. As shown in Fig.1, it has a
highly crystalline polymer of D-an-hydroglucopyranose units joined together in long chains by β -1,4-glycosidic
bonds [15].
Fig. 1: Schematics single cellulose chain repeat unit, showing the directionality of the 1–4.
However, processing and derivatization of cellulose are difficult in general, because this natural polymer is
neither meltable nor soluble in conventional solvents due to its hydrogen bonded and partially crystalline
structure. Therefore, present industrial production of regenerated cellulose and cellulose derivatives are in long
time dominated by polluting viscose process and heterogeneous processes, respectively (Klemm et al., 1998).
With increasing governmental regulations in industries, the need to implement “green” processes for cellulose
processing and to explore alternative routes for the functionalization of cellulose with simpler reagents and less
steps is getting increasingly important [2].
Since cellulose is difficult to process in solution or as a melt, because of its large proportion of intra- and
intermolecular hydrogen bonds, which strictly limit its processing and applications [1,23]. Therefore, many
organic and inorganic solvent systems such as N-methyl morpholine N-oxide (NMMO) [3] lithium chloride/1,3-
dimethyl-2-imidazolidinone (LiCl/DMI) [28] lithium chloride/N,N dimethylacetamide (LiCl/DMAc) [29] and
2621 Salmah Hussiensyah et al, 2014
Advances in Environmental Biology, 8(8) 2014, Pages: 2620-2625
phosphoric acid [17] have been investigated for regenerated cellulose fiber production. Nevertheless, most of
the systems still seem to be unsuccessful from an industrial viewpoint because of their toxicity and difficult
solvent recovery. Recently, ionic liquids (ILs), which are considered as desirable green solvents, have been
reported to be effective and promising cellulose solvents. [21,25,26,32]. Nowadays, ILs used for manufacturing-
regenerated cellulose fibers are arousing considerable commercial interest because of their superior dissolving
capacity, environmentally friendly properties, easy recycling and good recoverability [20,31,32].
In this research to investigated the effect of MCC content on tensile properties and X-ray diffraction of
regenerated cellulose using ionic liquid.
Methodology:
Materials:
In this research, microcrystalline cellulose (MCC) with particle size of 50µm was supplied by Sigma-
Aldrich, USA. Lithium Chloride (LiCl) and N, N Dimethylacetamide (DMAc) was obtained from Across,
Belgium. Acetone was supplied by Sigma –Aldrich.
Preparation of Regenerated Cellulose:
Cellulose was dissolve using DMAc/LiCl initially, involves an activation step in which the cellulose
structure is first swollen via solvent exchange. Microcrystalline cellulose (MCC) was immersed in distilled
water, twice in acetone and in DMAc for 40 minutes each, dried for 3 hrs at 80°C. The dissolution occurred by
immersing the MCC in DMAc solution with addition of 8 wt. % LiCl and stirred using magnetic stirrer at room
temperature for 30 minutes until the LiCl completely dissolved. The transparent gel film had formed after
removal of DMAc was immersed in distilled water for 30 minutes to regenerate cellulose and extract the
DMAC/LiCl co-solvent. Then the samples were dried at room temperature for 1 day.
X-ray diffraction (XRD):
XRD analysis was carried out using Bruked Ds Advance diffractometer equipped with X-ray Tube: Cu-Kα
(λ=1.5418Ao), analysed under normal atmospheric condition at room temperature. The relative amount of
crystallinity of the specimens was evaluated using crystallinity index (CI) [24]
Crystallinity Index(CI) = 100( I - I‟ ) / I
where I is the height of the peak assigned to (200) planes, typically located in the range 2θ = 21o–22o. I‟ is
the height of the peak assigned to (110) planes measured at 2θ = 18o-19o, which is where the maximum occurs
in a diffractogram for fully-amorphous cellulose.
Tensile Test:
Tensile test was carried out using ASTM D882, and Instron Universal Testing Machine model 5569 was
used. The tensile specimens with dimensions of 15 mm x 100 mm were used. The cross-head speed used was 10
mm/min and the test was performed at 25±30C.
RESULTS AND DISCUSSIONS
Fig. 2: Stress–strain curves for regenerated cellulose with different MCC content.
2622 Salmah Hussiensyah et al, 2014
Advances in Environmental Biology, 8(8) 2014, Pages: 2620-2625
Tensile Properties:
Typical stress-strain curves for regenerated cellulose is shown in Figure 2. It is noted that these stress-strain
curves are all non-linear. The non-linearity is typical for a regenerated cellulose film, as previously reported by
[6,7]. The result indicates MCC had significant effects on tensile properties of regenerated cellulose. The tensile
properties of the regenerated cellulose increased with increasing cellulose content, and reduced at cellulose
content of 4 wt%.
Figure 3 present the effect of MCC content on tensile strength of regenerated cellulose. It can be observed
that the addition of MCC increased tensile strength of the films. The highest tensile strength is contributed by 3
wt% of MCC concentration. As the content of MCC is further increased, the MCC/LiCl/DMAc mixture
becomes very viscous and the cellulose dissolution is incomplete. Therefore, at MCC content above 3wt% the
tensile strength is reduced. The decreament of tensile strength of regenerated cellulose with further MCC
content due to aggregation of MCC particles occurred. The similar result had been reported by Mahmoudian et
al., 2012; Röder et al., 2002; Ishii et al., 2003. They found that cellulose/LiCl/DMAc systems, when the phase
separation is slow, cellulose prefer to form molecular aggregates which caused reduction in tensile strength.
Fig. 3: Effect of MCC content on tensile strength of regenerated cellulose.
Figure 4 shows the effect of MCC content on elongation at break of regenerated cellulose. The elongation at
break of regenerated cellulose decreased with increasing MCC content. This attributed that increases of MCC
content increased the rigidity of regenerated cellulose. An increase in the crystalline content leads to an increase
in tensile strength and stiffness, but caused the detriment of the ductility. The similar result had been reported by
[6]. They found that when MCC content increased, elongation at break is reduced.
Fig. 4: Effect of MCC content on elongation at break at regenerated cellulose.
2623 Salmah Hussiensyah et al, 2014
Advances in Environmental Biology, 8(8) 2014, Pages: 2620-2625
Figure 5 illustrates the Young „s modulus of regenerated cellulose with different MCC content. Young‟s
modulus of the regenerated cellulose increased directly proportional with increasing MCC content. Addition of
cellulose content in regenerated cellulose film caused increased in stiffness which leads to modulus
improvement. As reported in previous study,Pullawan et al.,2010 stated that this reinforcement is thought to be
due to the presence of the stiff and strong MCC.
Fig. 5: Effect of MCC content on young modulus of regenerated cellulose.
X-ray diffraction (XRD):
The XRD diffraction intensity curves of regenerated cellulose with different cellulose content is shown in
Fig. 6. Table 1 shows the XRD of regenerated cellulose. The diffractograms of regenerated cellulose exhibit
sharp diffraction peaks with increasing cellulose concentration. The diffraction peaks at 2θ = 18o- 19o and 21o-
22o which were assigned to lattices [110] and [200]. From the Table 1, the crystallinity index of regenerated
cellulose is increased from 41.86% to 52.70% with increasing MCC content. The increased in MCC content
caused increased in transformation of cellulose I to cellulose II structure which is the reason of increased in
crystallinity. The similar results had been reported by [14,11] that the dissolution and regeneration of cellulose
produced different cellulose polymorphs: type I, type II cellulose and amorphous cellulose. Regeneration of
cellulose in H2O caused reorganisation and immobilisation of cellulose I into type II and amorphous cellulose.
Figure 7 illustrate the schematic structure of cellulose I and cellulose II.
Fig. 6: XRD patterns of regenerated cellulose at different MCC content.
2624 Salmah Hussiensyah et al, 2014
Advances in Environmental Biology, 8(8) 2014, Pages: 2620-2625
Table 1: XRD data for regenerated cellulose at different MCC content.
MCC (wt%)
Crystallinity index,CI (%)
1
41.86
2
44.70
3
52.40
4
52.70
Fig. 7: Schematic structure of cellulose I and cellulose II.
Conclusion:
In summary, an ionic liquid of DMAc/LiCL was found to be effective since it act as non-derivatizing
single-component solvent for cellulose. Tensile strength and Young‟s modulus of regenerated cellulose
increased with increasing MCC content, while the elongation at break decreased. The crystallinity index is
increased with increased MCC concentration in regenerated cellulose. The transformation of cellulose I to
cellulose II was observed by X-ray diffraction for the regenerated cellulose.
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  • Aug 2001
  • GREEN CHEM
A series of hydrophilic and hydrophobic 1-alkyl-3-methylimidazolium room temperature ionic liquids (RTILs) have been prepared and characterized to determine how water content, density, viscosity, surface tension, melting point, and thermal stability are affected by changes in alkyl chain length and anion. In the series of RTILs studied here, the choice of anion determines water miscibility and has the most dramatic effect on the properties. Hydrophilic anions (e.g., chloride and iodide) produce ionic liquids that are miscible in any proportion with water but, upon the removal of some water from the solution, illustrate how sensitive the physical properties are to a change in water content. In comparison, for ionic liquids containing more hydrophobic anions (e.g., PF6− and N(SO2CF3)2−), the removal of water has a smaller affect on the resulting properties. For a series of 1-alkyl-3-methylimidazolium cations, increasing the alkyl chain length from butyl to hexyl to octyl increases the hydrophobicity and the viscosities of the ionic liquids increase, whereas densities and surface tension values decrease. Thermal analyses indicate high temperatures are attainable prior to decomposition and DSC studies reveal a glass transition for several samples. ILs incorporating PF6− have been used in liquid/liquid partitioning of organic molecules from water and the results for two of these are also discussed here. On a cautionary note, the chemistry of the individual cations and anions of the ILs should not be overlooked as, in the case of certain conditions for PF6− ILs, contact with an aqueous phase may result in slow hydrolysis of the PF6− with the concomitant release of HF and other species.
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Primary wood processing: Principles and practice
Book
  • Jan 2006
This book is primarily a general text covering the whole sweep of the forest industries. The over-riding emphasis is on a clear, simple interpretation of the underlying science, demonstrating how such principles apply to processing operations. The book starts by considering the broad question "what is wood? " by looking at the biology, chemistry and physics of wood structure (first 4 chapters). This sets the scene. Next key chapters examine "wood quality"- explaining how and why wood quality can be so variable and implications for processing. Finally, in a series of chapters, various "industrial processes" are reviewed and interpreted. The 2nd Edition is a total revision. A few chapters remain relatively unchanged (no change for the sake of change). Many have been totally rewritten. All chapters have been written by specialists, but the presentation targets a generalist audience.
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Discrimination of Matrix-Fibre Interactions in All-Cellulose Nanocomposites
Article
  • Dec 2010
  • COMPOS SCI TECHNOL
All-cellulose nanocomposites are produced using dissolved microcrystalline cellulose (MCC) as the matrix and cellulose nanowhiskers (CNWs), produced by acid hydrolysis, as the reinforcement. These nanocomposites are then characterised using X-ray diffraction to determine their crystallinity, and Raman spectroscopy to discriminate the reinforcing phase (cellulose I) from the CNWs and the matrix phase (cellulose II) from the dissolved MCC. Mechanical testing of the composites shows that there is a significant systematic reinforcement of the matrix material with the addition of CNWs. Furthermore, Raman spectroscopy is used to show that distinct spectroscopic bands for each phase within the composite spectrum can be used to discriminate the effects of both reinforcement and matrix. It is shown that a Raman band located approximately at 1095cm−1 can be used to follow the micromechanical deformation of the CNWs and matrix, whereas another band located at 895cm−1 arises purely from the matrix. This spectroscopic fingerprint is used to gain insights into the complex interactions occurring in these potentially recyclable composite materials, and offers a way forward to optimising their properties.
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Preparation of regenerated cellulose/montmorillonite nanocomposite films via ionic liquids
Article
  • Feb 2012
  • CARBOHYD POLYM
a b s t r a c t Regenerated cellulose/montmorillonite (RC/MMT) nanocomposite films were successfully prepared in ionic liquid, 1-butyl-3-methylimidazolium chloride (BMIMCl) using solution casting method. The effect of MMT loading on the thermal, mechanical, gas permeability and water absorption properties of the nanocomposite films was investigated. X-ray diffraction analysis revealed a cellulose II crystalline struc-ture and well dispersed MMT in RC/MMT nanocomposite films. Presence of MMT enhanced the thermal and thermal-oxidative stability and char yield of RC. The tensile strength and Young's modulus of RC films improved by 12% and 40%, respectively with the addition of 6 wt.% MMT. RC/MMT nanocomposite films exhibited improved gas barrier properties and water absorption resistance compared to RC. The results demonstrated that there is a possible interface interaction between cellulose and MMT which yielded better thermal and mechanical properties of the nanocomposite films as compared to pure cellulose.
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An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer
Article
  • Oct 1959
An empirical method for determining the crystallinity of native cellulose was studied with an x-ray diffractometer using the focusing and transmission techniques. The influence of fluctuations in the primary radiation and in the counting and recording processes have been determined. The intensity of the 002 interference and the amor phous scatter at 2θ = 18° was measured. The percent crystalline material in the total cellulose was expressed by an x-ray "crystallinity index." This was done for cotton cellulose decrystallized with aqueous solutions containing from 70% to nominally 100% ethylamine. The x-ray "crystallinity index" was correlated with acid hydrolysis crys tallinity, moisture regain, density, leveling-off degree of polymerization values, and infrared absorbance values for each sample. The results indicate that the crystallinity index is a time-saving empirical measure of relative crystallinity. The precision of the crystallinity index in terms of the several crystallinity criteria is given. Based on over 40 samples for which acid hydrolysis crystallinity values were available, the standard error was 6.5%.
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1-Allyl-3-methylimidazolium Chloride Room Temperature Ionic Liquid: A New and Powerful Nonderivatizing Solvent for Cellulose
Article
  • Oct 2005
  • MACROMOLECULES
A new and highly efficient direct solvent, 1-allyl-3-methylimidazolium chloride (AMIMCl), has been used for the dissolution and regeneration of cellulose. The cellulose samples without any pretreatment were readily dissolved in AMIMCl. The regenerated cellulose materials prepared by coagulation in water exhibited a good mechanical property. Because of its thermostable and nonvolatile nature, AMIMCl was easily recycled. Therefore, a novel and nonpolluting process for the manufacture of regenerated cellulose materials using AMIMCl has been developed in this work.
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Elastic modulus of filled polymer composites
Article
  • Jul 1993
  • J APPL POLYM SCI
The elastic modulus of polyepichlorohydrin (PECH) filled with glass beads and wollastonite was studied. It was found that the elastic modulus of the composites depends not only on the volume fraction of the fillers but also on their size. Percolation theory was used to explain the experimental results. © 1993 John Wiley & Sons, Inc.
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All-cellulose nanocomposite
Article
  • Nov 2005
  • POLYMER
Cellulose-based nanocomposite films with different ratio of cellulose I and II were produced by means of partial dissolution of microcrystalline cellulose powder in lithium chloride/N,N-dimethylacetamide and subsequent film casting. The mechanical and structural properties of the films were characterised using tensile tests and X-ray diffraction. The films are isotropic, transparent to visible light, highly crystalline, and contain different amounts of undissolved cellulose I crystallites in a matrix of regenerated cellulose. The results show that, by varying the cellulose I and II ratio, the mechanical performance of the nanocomposites can be tuned. Depending on the composition, a tensile strength up to 240MPa, an elastic modulus of 13.1GPa, and a failure strain of 8.6% were observed. Moreover, the nanocomposites clearly surpass the mechanical properties of most comparable cellulosic materials, their greatest advantage being the fact that they are fully biobased and biodegradable, but also of relatively high strength.
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