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Development of Antibacterial PVA/CNF Nano-Biocomposite Film Adapting

Modified Solution Casting Method

Article  in  International Journal Of Engineering Research and General Science · February 2021

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Kritika Singh Somvanshi Prakash Gope

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International Journal of Research in Engineering and Science (IJRES)
ISSN (Online): 2320-9364, ISSN (Print): 2320-9356
www.ijres.org Volume 9 Issue 2 ǁ 2021 ǁ PP. 52-57

Development of Antibacterial PVA/CNF Nano-Biocomposite Film

Adapting Modified Solution Casting Method
Kritika Singh Somvanshi, Prakash Chandra Gope, Saurabh Tiwari
Research Scholar, Mechanical Engineering Department, College Of Technology, G. B. Pant University of
Agriculture and Technology, Pantnagar, Uttarakhand-263145.
Professor, Mechanical Engineering Department, College Of Technology, G. B. Pant University of Agriculture
and Technology, Pantnagar, Uttarakhand-263145.
Research Scholar, Mechanical Engineering Department, College Of Technology, G. B. Pant University of
Agriculture and Technology, Pantnagar, Uttarakhand-263145.

Abstract:
Solution casting method is the most prominent, effective and cheap method to fabricate thinner nano-
biocomposite films at laboratory-scale. But due to improper dispersion of fiber in matrix just by mixing or
stirring restricts its applicability. This modified method involves combination of ultrasonication process with
solution casting method to fabricate antibacterial PVA/CNF nano-biocomposite film. As a result, agitation of
cellulose nano fiber into already prepared polyvinyl alcohol solution increases due to generation of high shear
force. A homogeneously dispersed film with enhanced properties is prepared by adapting this technique.
Keywords: Solution Casting Method, Ultrasonication, Cellulose Nano Fiber (CNF), Nano-Biocomposite Films
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Date of Submission: 28-01-2021 Date of acceptance: 12-02-2021
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Graphical Abstract:

I. INTRODUCTION:
Awakening of human towards ecosystem sustainability, development of green technologies especially
in food packaging industries has become increasingly valuable for mankind. Almost all of the processed food
products employed petroleum derived plastics having shallow-life but prolonged in atmosphere for millennia
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causing immense threat to environment. In contrast with the past, agricultural residues are appealing source of
nano-cellulose which is abundant, ecological and economical replacement of other limited natural as well as
synthetic fibers [1]. Cellulose Nano Fibers have outstanding mechanical, thermal and antimicrobial properties,
renewability and high applicability after functionalization [2, 3]. Prominent agricultural crop Sugarcane
(Saccharum) has yield of about 1.8 billion tones per year contains 40-50% cellulose in bagasse which is
noticeably much more than various crop residues mainly wheat straw (33wt %), corn cobs (34wt %), corn stalks
(35wt %) and rice straw (36wt %) [4-6]. Sugar Cane Bagasse is a low value, plentiful and biodegradable residue
that makes it encouraging nano reinforcement in novel green composites [7]. A research study shows that the
alkaline and acidic extraction of bagasse from sugar cane yields 56% and 63% cellulose respectively [8].
Solution casting is the primeval fabrication technique invented by Eastman Kodak in the nineteenth century [9].
For the development of nano-biocomposite films solution casting is the simplest yet most flexible method,
particularly when used with water-soluble bioplastics. Typically solution casting is a low temperature process
offering consistent thickness, less haziness and entropy with high optical clarity [10]. In this process, fiber is
incorporated into already prepared biopolymer solution and the biocomposite film is developed by solvent
precipitation technique. Steady evaporation often led to accumulation of nano-fibers in the solution resulting
non-homogeneous dispersion and poor interaction between them [11]. Even though this approach provides a
favorable outcome but with biodegradable hydrophobic polymers the recommendation of this fabrication
technique is restricted [12]. The major goal of this research work is to develop nano-biocomposite films utilizing
polyvinyl alcohol and cellulose nano fiber from sugarcane bagasse by modifying solution casting method to
obtain its suitability in packaging applications [13, 14, 15, 16]. To fabricate nano-biocomposite film slightly
different methodology is described and enhanced properties are validated through results.

II. METHODOLOGY
2.1 Materials
Polyvinyl Alcohol Cold (M.W. 850000-124000, 99% degree of hydrolysis and viscosity 23-38 cP) and
Polyethylene Glycol 6000 (PEG) (M.M. 5000-7000 with melting range from 56-610C) were supplied from
HPLC, India. Antibacterial agent Chitosan (CHT) (M.W. 3800-20000), Acetic Acid, Sodium Hydroxide were
purchased from HIMEDIA, India. Cellulose Nano Fiber (CNF) from Sugarcane Bagasse was transported from
Maple Biotech pvt.ltd. India. The materials used are non-toxic, eco-friendly and bio-degradable in nature.

2.2 Functionalization of Cellulose Nano Fibers

Firstly the cellulose nano fiber from sugarcane bagasse was washed in deionized water to remove
undesirable particulate matter. It was dried in oven at 50 °C approximately for 8 h and then concealed in packets
at room temperature. After that, to eliminate residual lignin, hemicelluloe and other impurities fiber was stirred
in hot plate at 250rpm with aqueous solution of acetic acid (5wt. %) at 80 0C for 6h. The solution was cleaned
with distilled water until 7 pH is obtained, then the solution was filtered and oven-dried at 500C for 4h. Again
aqueous suspension of 5wt. % NaOH was prepared in 500mL distilled water and nano cellulose is refluxed for
24h at 800C in a magnetic stirrer. The refluxed solid particles were cooled to ambient temperature, and then the
CNF were continuously washed until the pH of solution was neutral and centrifuged at 6000rpm for 10min.
After 5 washings the centrifugation operation was paused. The functionalized cellulose nano fiber thus obtained
was then filtered and oven-dried in vacuum at 500C for next 24 h and was used as reinforcement in nano-
biocomposite film. Functionalization process of sugarcane bagasse CNF is graphically depicted in Figure 1.

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Fig.1 Pictorial Representation of Functionalization of CNF from Sugarcane Bagasse

2.3 Development of Antibacterial PVA/CNF Film

The 5wt. % PVA solution was first prepared by dissolving free-flowing powder of PVA in deionized
water at 400C by taking 5g of PVA powder in 95mL of water and stirred at 800C and 250rpm for 2 h in a hot
plate magnetic stirrer. Now the functionalized cellulose nano fibers were added to prepared PVA solution and
stirred for another 1h at same condition. Sugarcane bagasse cellulose was added at 30, 40 and 50wt. %
respectively to fabricate different nano-biocomposite films. Then obtained solution was sonicated for 30 min at
800C and 37% power without time lag in Ultrasonic Homogenizer Probe Sonicator. The 70wt. % Polyethylene
Glycol and 1.25gm chiosan were added to mixture and mechanically stirred at same temperature for next 60
min. The final suspensions were sonicated for 30min at same condition to obtained homogeneous solution and
remove any entrapped air bubbles. Finally the films were casted in glass petridish and dried in vacuum oven at
800C for 24h for complete removal of water. The resulting composite films were then peeled off and kept in the
desiccator to equilibrate the films for 24 h before characterization. A detailed flow chart discussing the
methodology to fabricate antibacterial PVA/CNF nano-biocomposite film from solution casting method by
modifying it with ultrasonication technique is presented in Figure 2.

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Fig. 2 Development of Antibacterial PVA/CNF Nano-Biocomposite Film Adapting Modified

Solution Casting Method

Table 1 represents the nomenclature of fabricated antibacterial nano-biocomposite films from Poly Vinyl
Alcohol (PVA) - 5wt. % and treated/untreated Cellulose Nano Fiber (CNF) - 40wt. % blended with
Polyethylene Glycol (PEG) - 70wt. % and Chitosan (CHT) - 1.25g by solution casting method as well as
adapting modified solution casting method by sonication process.

Table 1 Nomenclature of Developed Nano-Biocomposite Films

Abbreviation Full Name

PVA-1 Pure Poly Vinyl Alcohol Film without Sonication

PVA-2 Pure Poly Vinyl Alcohol Film with Sonication

PVA/CNF-11 PVA & Untreated CNF (40wt. %) Film Blended with PEG and CHT without Sonication

PVA/CNF-21 PVA & Treated CNF (40wt. %) Film Blended with PEG and CHT without Sonication

PVA/CNF-12 PVA & Untreated CNF (40wt. %) Film Blended with PEG and CHT with Sonication

PVA/CNF-22 PVA & Treated CNF (40wt. %) Film Blended with PEG and CHT with Sonication

III. METHOD VALIDATION

Ultimate tensile strength and Elongation at Break (%) of antibacterial PVA & CNF (Treated/Untreated)
films reinforced at 40wt. % and blended with PEG, CHT were determine on Universal Testing Machine
according to ASTM D882-12 standard. The highest tensile strength was recorded 80.47MPa in treated CNF
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followed by 70.13MPa in untreated CNF sample when casted with sonication process. Similarly, highest
percentage elongation was found 15.08% followed by 11.97% in the PVA/CNF-22 and PVA/CNF-12 samples
respectively. Thus by adapting modified solution casting method the enhancement in mechanical properties was
observed irrespective to functionalization of fiber. This may be attributed to good dispersion of fiber in matrix
increasing interfacial bonding between them as compared to solution casting method. Moreover, homogeneous
films were formed because no cavitations and agglomeration of fiber took place. Mechanical Properties of
developed films are presented through Bar Graph in Figure 3.

Fig.3 Effect of Sonication on (a) Ultimate Tensile Strength MPa and (b) Elongation at Break (%) of Developed
PVA/CNF Films at 40wt. % Reinforcement Treated and Untreated Both

IV. CONCLUSION
Ultrasonication process prevents the re-agglomeration of cellulose nano fiber in polyvinyl alcohol as
occurred in solution casting method. Moreover, consistent dispersed solution is prepared without any air
bubbles. Thus the developed antibacterial PVA/CNF film by adapting modifying solution casting technique has
enhanced mechanical properties. Thus this method can be used effectively in fabrication of nano-biocomposite
films.

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