High performance green barriers based on nanocellulose
© Nair et al.; licensee Chemistry Central Ltd. 2014
Received: 14 July 2014
Accepted: 24 October 2014
Published: 7 November 2014
Packaging materials are widely used to prevent food and drink, healthcare, cosmetics and other consumer goods against physical, biochemical, and microbiological deterioration. They should provide sufficient barrier against oxygen, water vapor, grease, and microorganisms. Currently, the packaging materials are largely based on glass, aluminum and tin, and fossil derived synthetic plastics. These materials possess high strength and barrier properties. However, they are unsustainable, some are fragile such as glass, and their weight adds to energy costs for shipping -. The global consumer packaging demand is valued at approximately US$400b-$500b and is one of the faster-growing markets, forecasted to grow at ~4% per year until 2015 .
With the increased environmental concerns over sustainability and end-of-life disposal challenges, materials derived from renewable resources have been strongly advocated as potential replacements . Cellulose is the most abundant polymer in nature and accounts for approximately 40% of lignocellulosic biomass. Cellulose paper-based packaging is lightweight, low-cost, and most important, sustainable. Unfortunately, common paper made from lignocelluloses does not provide sufficient barrier for water, oxygen or oil. Currently, paper based packages are made with unsustainable coatings of wax, plastics, or aluminum. Cellophane is the only cellulose based material (not modified or coated) currently used for barrier packaging due to its high gas barrier. However, the production of cellophane is via a viscose route which produces byproducts and uses reagents (CS2 and H2S) that are harmful to the environment .
The production of cellulose nanomaterial such as cellulose nanofibrils (CNFs) and cellulose nanocrystals (CNCs) have opened vast possibilities of utilizing cellulose based materials for packaging. Cellulose nanomaterial has diameter in the range of 2-50 nm with large surface area -. The ability to form hydrogen bonds resulting in strong network makes it very hard for the molecules to pass through, excellent for barrier applications . This review paper aim to summarize the recent developments in various barrier films based on nanocellulose with special focus on oxygen and water vapor barrier properties.
Nanocellulose and its preparation
Cellulose nanofibrils (CNFs) or microfibrils have diameter in the range of 2-50 nm and lengths up to several micrometers depending on their origin -. CNFs have exceptional optical and mechanical properties, and therefore can be used as a building block for a variety of high-performance materials -. Intensive mechanical treatment is required to disintegrate the cellulose fiber to nanofibrils . Several methods of mechanical fibrillation have been used for the production of CNFs such as homogenizers ,, microfluidizers , and grinders ,. Cellulose nanocrystals (CNCs) are often prepared by treating cellulose fiber with sulfuric acid or hydrochloric acid. Strong acidic condition leads to aggressive hydrolysis to attack the noncrystalline fractions within the cellulose fiber which results in the formation of low aspect cellulose fibril aggregates known as CNCs -.
Migration process of molecules through nanocellulose film
Where P is the permeability, D is the diffusion coefficient, and S is the solubility coefficient.
Where q is the amount of material passing through the film, l is the thickness, A is the cross sectional area, t is time, and Δp is the pressure difference between the two sides of film.
CNFs for barrier application
CNFs is a strong gas barrier material. Compared to CNCs, CNFs consists of crystalline and disordered regions. In most of the cases, crystallinity ranging from 40-75% has been reported for the CNFs obtained from softwoods and hardwoods ,,,. Saito and Isogai (2004) showed that the degree of crystallinity varied from 78-91% for CNFs produced from TEMPO oxidation of cotton linter . Films made purely of mechanically fibrillated CNFs have very high air and oxygen barrier property. The oxygen transmission rates (OTR) of CNF films with thickness of 21 μm were as low as 17 ± 1 ml m-2day-1. These values are competitive with other best synthetic polymers such as ethylene vinyl alcohol (EVOH) (3-5 ml m-2 day-1) and polyvinylidene chloride (PVdC) coated polyester films (9-15 ml m-2 day-1) of approximately same thickness with respect to OTR . Recently, Osterberg et al.  demonstrated a rapid method of making robust CNF films with high oxygen barrier property. The CNF solutions were first filtered followed by hot pressing at high pressure followed by air drying. At a relative humidity below 65%, the oxygen permeability of these films was below 0.6 cm3 μm m-2 d-1 kPa-1. However, oxygen permeability of CNF films increases with the increase in relative humidity. This is mainly due to the plasticizing and swelling of nanofibrils through the adsorption of water molecules at high relative humidities.
Oxygen permeability of nanocellulose film compared to those made form commercially available petroleum based materials and other polymers
WVTR of nanocellulose compared to commercially available petroleum based materials and other polymers
CNCs for barrier application
Contrary to CNFs, very few studies have been directed toward study of 100% pure CNC film or treated CNC films. Belbekhouche et al.  compared the gas barrier properties between CNF and CNC films. They found that the films made of CNCs were more permeable to oxygen than those made of CNFs. The oxygen molecules penetrated much more slowly within CNF film due to the higher fibril entanglements within the film which increased the tortuosity factor. CNCs, which have crystallinity greater than 60% combined with their ability to form a dense hydrogen bonded network can increase gas barrier property. Bacterial cellulose nanocrystals (BNCs) films present excellent oxygen barrier at low relative humidity, but their high moisture sensitivity results in dramatically decreased barrier when the relative humidity is higher than 70%. The oxygen permeability of 6.99 ± 10-22m3m/m2s Pa at 0% humidity increased to 5.97 ± 10-18m3m/m2s Pa at 80% humidity. However, this permeability was reduced by 97% and 74% when BNC films were coated with annealed PLA electro spun nanostructured fibers and 3-aminopropyl) trimethoxysilane (APTS), respectively . Herrara et al.  studied thin spin coated films made from CNCs prepared with sulfuric acid and hydrochloric acid. The hydrochloric acid made CNCs resulted in films with low permeability for oxygen, while the sulfuric acid made CNCS resulted in films with higher permeability.
CNCs have been studied as filler for various natural polymers for enhancing the barrier properties. Saxena et al.  produced nanocomposite film with low oxygen permeability by casting an aqueous solution containing xylan, sorbitol and nanocrystalline cellulose. Oxygen permeability of films prepared from xylan, sorbitol and 50% by weight of sulfonated CNC exhibited a significantly reduced oxygen permeability of 0.1799 cm3.m/m2.d.kPa compared with films prepared solely from xylan and sorbitol with an oxygen permeability of 189.1665 cm3.m/m2.d.kPa. Poly lactic acid (PLA) nano-biocomposites containing 5 wt% of nanocrystals exhibited the highest oxygen barrier. The OTR for PLA nanocomposites with 5% w/w of unmodified CNCs was 17.4 ± 1.4 cm3mm m-2 day-1, while that for modified CNCs with an acid phosphate ester of ethoxylated nonylphenol in a 1/4 (wt/wt) ratio was 15.8 ± 0.6 cm3mm m-2 day-1. Addition of 1 wt% of silver nanoparticles to these modified CNC- PLA composites further decreased the OTR to 12.6 ± 0.1 cm3mm m-2 day-1. The OTR values of ternary systems consisting of PLA, PHB (poly hydroxybutyrate) and 5 wt% unmodified CNCs was 15.3 cm3mm m-2 day-1, while that for modified CNCs with an acid phosphate ester of ethoxylated nonylphenol in a 1/1 (wt/wt) ratio was 13 cm3mm m-2 day-1. Water contact angle measurements showed that the ternary system had high hydrophobicity and the presence of sulphate groups with low polarity on the surface of CNCs increased the surface hydrophobicity of the final composite material .
CNCs were used as fillers in polyvinyl alcohol (PVOH) matrix. The addition of 5 wt% CNCs decreased the WVP of pure PVOH films from 0.61 ± 0.04 g.mm/kPa.h.m2 to 0.44 ± 0.01 g.mm/kPa.h.m2. The reinforcement of natural biopolymers with CNCs was found to reduce WVTR of the resulting nanocomposites. The films prepared using xylan as reinforcement polymer with 10% sulfonated CNCs exhibited a 74% reduction in specific water transmission properties compared with the film without CNCs and a 362% improvement compared with xylan films reinforced by 10% softwood kraft fibers. The xylan/sulphonated CNC nanocomposites showed a WVTR of 174 g/hm2. They also compared xylan films reinforced with CNC made from hydrochloric acid with those reinforced with sulphonated CNC. Even though, films showed a significant reduction in water transmission, the reduction was not as significant as those using sulfonated CNCs. The xylan/ hydrochloric acid made CNC films showed a WVTR of 281 g/hm2. Khan et al.  showed that the values of water vapor permeability (WVP) decreased sharply as the content of CNCs increased in the methyl cellulose based films. The WVP of control films (without CNCs) was 6.3 g.mm/m2.day.kPa, while those films in cooperated with 1 wt% CNC showed a permeability of 4.7 g.mm/m2.day.kPa.
Nanocellulose such as CNFs and CNCs have opened vast possibilities of utilizing cellulose based materials. The use of CNFs in films, composites, and coatings has found to substantially reduce the oxygen permeability within these materials. The oxygen barrier efficiency of pure CNF films is highly competitive and even be comparable with commercial synthetic polymers. The improvement of oxygen barrier properties by CNFs can be attributed to the dense network formed by nanofibrils with smaller and more uniform dimensions. Even though CNCs have higher crystallinity than CNFs, mechanically fibrillated CNF films were found have much lesser oxygen permeability than CNCs. The CNF films have higher entanglements within the film which increases the diffusion path for gas molecules. Also, nanocellulose has a strong reducing effect on water vapor diffusion due to its size, and swelling constraints formed due to rigid network within the films compared to cellulose fibers. The use of CNFs and CNCs in various natural polymer based composites has found to substantially reduce the gas permeability within these composites.
All the authors have contributed to the literature review and manuscript writing. All authors read and approved the final manuscript.
This work was partially supported by the USDA Forest Service R & D special funding on Cellulose Nano-Materials (2012).
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