Contents

Cover

Title page

Copyright page

Preface

Chapter 1: Montmorillonite Composite Materials and Food Packaging

1.1 Introduction
1.2 Polymer/MMT-Based Packaging Materials
1.3 Biopolymers and Protein/MMT-Based Packaging Materials
1.4 Ag⁺-Cu2⁺-Zn2⁺/MMT-Based Composites Packaging Materials
1.5 Metal Oxide/MMT-Based Packaging Materials
1.6 Natural Antioxidants/MMT Composite Materials for Food Packaging
1.7 Enzyme/MMT-Based Composites Packaging Materials
1.8 Conclusion
References

Chapter 2: Halloysite Containing Composites for Food Packaging Applications

2.1 Halloysite
2.2 Nanocomposites Containing HAL
2.3 Conclusion
References

Chapter 3: Silver Composite Materials and Food Packaging

3.1 Silver and Silver Compounds as Active Agents
3.2 Conclusions
References

Chapter 4: Zinc Composite Materials and Food Packaging

4.1 Introduction
4.2 Food Packaging
4.3 Polymers in Food Packaging
4.4 Nanotechnology
4.5 Nano-Fillers
4.6 Classification of Nano-Fillers
4.7 ZnO Nanoparticles
4.8 Composites
4.9 Conclusions
References

Chapter 5: Silicium-Based Nanocomposite Materials for Food Packaging Applications

5.1 Introduction
5.2 Nanosilica/Polymer Composites
5.3 Characterization of Polymer/Nancomposites
5.4 Conclusion
References

Chapter 6: Nanoiron-Based Composite Oxygen Scavengers for Food Packaging

6.1 Introduction
6.2 Characteristics of Oxygen Scavengers
6.3 Nanomaterials and Nanoiron
6.4 Nanoiron-Based Composite Oxygen Scavengers
References

Chapter 7: Carbon Nanotubes (CNTs) Composite Materials and Food Packaging

7.1 Introductions on Carbon Nanotubes
7.2 Polymer/CNTs Composite Materials
7.3 Safety Issues of CNTs and Polymer/CNTs Composites
7.4 Outlook
References

Chapter 8: Polymer/Graphene Nanocomposites for Food Packaging

8.1 Polymers for Food Packaging
8.2 Polymers for Steel Can Packaging
8.3 Water Permeation and Anticorrosion of Polymer Coatings
8.4 Polymer–Food Interactions
8.5 Polymer/Clay Nanocomposites
8.6 Polymer/Graphene Nanocomposites
8.7 Summary and Outlook
References

Chapter 9: Biodegradability and Compostability of Food Nanopackaging Materials

9.1 Introduction
9.2 Biodegradability and Compostability
9.3 Biodegradability and Compostability of Food Nanopackaging Materials
9.4 Conclusion
Conflicts of Interest
Acknowledgments
References

Chapter 10: Nanocellulose in Food Packaging

10.1 Antimicrobial Effectiveness of Biopolymeric Films/Coatings Containing Cellulose Nanostructures
10.2 Physicochemical Properties of Bio-Nanocomposites Materials Reinforced with CNC
10.3 Enhancement of the Mechanical Properties of Polymers with CNC
10.4 Enhancement of the Barrier Properties of Polymers with CNC
10.5 Research Works on CNC as Biodegradable Reinforcement and Barrier Component
10.6 Conclusion
References

Chapter 11: Nanocellulose in Combination with Inorganic/Organic Biocides for Food Film Packaging Applications – Safety Issues Review

11.1 Introduction
11.2 Nanocellulose in Flexible Film Food Packaging
11.3 Health and Environmental Toxicity Evaluations of Active Antimicrobial Packaging
References

Chapter 12: Composite Materials Based on PLA and its Applications in Food Packaging

12.1 Introduction
12.2 Synthesis of Polylactic Acid
12.3 Reinforcing Agents
12.4 Surface Modification of Fibers and Fillers
12.5 Nanostructures in the PLA Matrix
12.6 Processing Techniques
12.7 Properties Related to Packaging Applications
12.8 Recyclability of PLA
12.9 Biodegradation of PLA
12.10 Future Tendencies
References

Chapter 13: Nanomaterial Migration from Composites into Food Matrices

13.1 Introduction
13.2 Nanotechnology in the Food Industry
13.3 Nanoparticle Toxicology
13.4 Migration Assays and Current Legislation
13.5 Conclusion
Acknowledgments
References

Index

End User License Agreement

List of Illustrations

Chapter 1

Figure 1.1 Structure of Montmorillonite (available online).
Figure 1.2 Different types of polymer NCs. (Color figure available online.)
Figure 1.3 Illustration of the “tortuous pathway” created by incorporation of clay nanoplatelets into a polymer matrix film. (Image available online.)
Figure 1.4 Gas permeability of LDPE and LDPE/clay NCs for 1, 3, 5, and 7 wt% clay. Reprinted with permission from Reference [18].
Figure 1.5 Oxygen permeations of pure PS and PS/5wt% clay NCs. Reprinted with permission from Reference [25].
Figure 1.6 Surface plot of OTR and WVTR as a function of nanoclay, compatibilizer, and film thickness. (a) OTR at constant nanoclay; (b) OTR at constant compatibilizer; (c) OTR at constant film thickness; (d) WVTR at constant nanoclay; (e) WVTR at constant compatibilizer; (f) WVTR at constant film thickness. Reprinted with permission from Reference [29].
Figure 1.7 Structure of amylopectin and amylose which consist starch (image available online).
Figure 1.8 Effect of clay concentration on gel fraction (%) of starch/clay composites at different irradiation doses (left graph) and in relative water vapor transmission (right graph) (Reprinted with permission from Reference [39]).
Figure 1.9 Toast packaged with a biodegradable film based on cassava starch formulated with glycerol, sucrose, and inverted sugar as plasticizers (Reprinted with permission from Reference [42]).
Figure 1.10 Antimicrobial activity of starch films modified by clays Nanofil 2 and NanoBent ZR-1 against gram-negative bacteria: E. coli and P. fluorescens or gram-positive bacteria: S. aureus and L. innocua. Different letters for each sample indicate the significant difference at p < 0.05. (Reprinted with permission from Reference [43].)
Figure 1.11 Structures of cellulose, cellulose acetate, and cellulose acetate butyrate (images available online).
Figure 1.12 (a) Oxygen permeabilities of LUC–MMT nanocomposite films at 50% and 75% RH. (b) Effect of MTM content on the moisture content and water uptake of LUC–MTM films. Moisture content was measured after conditioning the films at 23 °C and 50% RH for 2 days. Water uptake was measured after immersing the films in water for 6 days and then calculating the weights of absorbed water and cellulose in the NCs (Reprinted with permission from Reference [46]).
Figure 1.13 Chitin and chitosan structure (image available online).
Figure 1.14 WVP values as a function of NaMMT content, dilution, and preparation methodology (reflux vs. no reflux) for (a) chitosan and (b) chitosan/glycerol-based films. Reprinted with permission from Reference [55].
Figure 1.15 (a) Water vapor permeability values and (b) oxygen transmission rate values for all tested CS/PVOH composite and CS/PVOH/clay nanocomposite films. Reprinted with permission from Reference [56].
Figure 1.16 (a) Specific growth rate m and (b) overall growth of E. coli, on films containing 30 wt% oleic acid (OL) or glycerol (GL) and 5 wt% NaMMT as a function of processing. Note that same letters identify samples that did not show significant differences for the corresponding property at p < 0.05. Reprinted with permission from Reference [57].
Figure 1.17 Oxygen permeation of PLA films coated by ink formulations with different clay Types. Reprinted with permission from Reference [68].
Figure 1.18 WVP of PLA films coated by ink formulations with different clay contents. Reprinted with permission from Reference [68].
Figure 1.20 Silver release (mg/kg of food simulant) versus time from PLA nanobiocomposites containing 1, 5, and 10wt% of silver-based nanoclay. Reprinted with permission from Reference [87].
Figure 1.21 Logarithm of the number of colony-forming units (CFU) as a function of the concentration of MtCu²⁺ nanoparticles in the films. The photograph above shows LB plates on E. coli containing different concentrations of MMTCu²⁺: (a) pure LDPE, (b) 1%MMTCu²⁺/LDPE, (c) 2%MMTCu²⁺/LDPE, (d) 3%MMTCu²⁺/LDPE, (e) 4%MMTCu²⁺/LDPE ASTM E-2149 method (Bruna et al. [90]).
Figure 1.22 Immobilizing M-TiO₂ particles on OMMT and different interactions between the hydroxyl groups of PVA chain and other polar groups. Reprinted with permission from Reference [95].
Figure 1.23 Lipid oxidation of beef packed with active films determined by measuring the TBARS during storage at 4 °C. Evaluation of antioxidant effectiveness of the following: (a) LDPE and EVA films controls and LDPE and EVA films spiked with the same concentration of natural extract; (b) EVA film control, EVA films spiked with different concentrations of natural extract, and EVA films spiked with the lowest concentration of functionalized nanoclays; (c) EVA film control and EVA films spiked with different concentrations of functionalized nanoclays. Reprinted with permission from Reference [121].
Figure 1.24 Comparative images of tested films (a); sample of meat packaged with blank film (b) and with active film (c). Reprinted with permission from Reference [122].
Figure 1.25 Picture of the active nanocomposite LLDPE film packaging production by the blow molding method attached to a high shear force twin-screw extruder. Reprinted with permission from Reference [124].
Figure 1.26 In vivo antimicrobial assay in B. cinerea-inoculated strawberries: (a) control without nanocomposite film and (b) with TPS/MMT/EOCs nanocomposite film containing 7.46 g kg^-1 of total EOCs (CRV: TML 50:50). Reprinted with permission from Reference [126].

Chapter 2

Figure 2.1 (a) Molecular and physical structure of HNT [4]. (b) Structures of halloysite-10 Å crystalline and halloysite nanotube. Reprinted with permission from Yuan et al. [5]. Copyright© 2008, American Chemical Society.
Figure 2.2 Main halloysite morphologies vs. Fe content. Addapted from Joussein et al. [7].
Figure 2.3 TEM images of HNT. Reprinted with permission from Rawtani and Agrawal [9].
Figure 2.4 (a) Pictures of bananas packaged with PE films and HNT/PE films containing 5 wt% HNTs. (b) Firmness of tomatoes packaged with PE films and HNT/PE films containing 5 wt% HNTs. Values at days 0 and 10 are not significantly different. Reprinted with permission from Erdinc Tas et al. [32].
Figure 2.5 Total aerobic count on chicken surfaces packaged with neat PE films (red) and PE/1wt% HNT nanocomposite films (green). Values for the initial time are not different. Reprinted with permission from Erdinc Tas et al. [32]. Copyright© 2017, Springer Science + Business Media New York.
Figure 2.6 Complete eradication of the fungus when the bread is stored 11 days in a package based on the new antimicrobial hybrid film compared with the neat LDPE in a storage experiment of fungi-inoculated sliced bread (preservative-free). Reprinted with permission from Shemesh et al. [33].
Figure 2.7 Antibacterial LDPE/(HNT/CV-TY) packaging film for hummus. Reprinted with permission from Krepker et al. [35].
Figure 2.8 E. coli count in hummus after the inoculation with (10² CFU mL^–1) and incubation with the respective film in a headspace assay (no direct contact) for 22 h at 37 °C. All experiments were carried in triplicates. Reprinted with permission from Krepker et al. [35]. Copyright© 2017 Elsevier Ltd. All rights reserved.
Figure 2.9 The mechanism for the physical adsorption (noncovalent functionalization) of SDS and BCP molecules onto the surface of HNTs and their effective dispersion in the PS matrix. Copyright© 2017 Lazaros Tzounis et al. [44] (Hindawi). This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Figure 2.10 Schematic representation of the entanglements between the grafted SEBS of HNT (Hal-S) and the SEBS-g-MA chains of the PA11/SEBS-g-MA blend. Reprinted with permission from Sahnoune et al. [59]. Copyright© 2017 Elsevier Ltd. All rights reserved.
Figure 2.11 Schematic diagram of a possible interaction mechanism between PLA and HNT. Addapted from De Silva et al. [81].
Figure 2.12 Biodegradation of neat PLA versus PLA/clay nanocomposites. Aspect of nanocomposites at different degradation stages and the variation of the degree of degradation and average molecular weight with degradation time Reprinted with permission from Ray [112]. Copyright© 2012, American Chemical Society.
Figure 2.13 Mechanical properties of starch and its nanocomposites. Adapted from Hedicke-Höchstötter et al. [117].
Figure 2.14 Results on the porosity test (time need to pass 100 cm³ air through hand sheets) on paper modified with halloysite, SiO₂, and TiO₂. Adapted from Lu et al. [118].

Chapter 3

Figure 3.1 Typical termogravimetric curves of S-PVA blend films (C) and those containing 0.1 and 0.3 %wt of AgNPs obtained by TGA analysis.
Figure 3.2 Typical UV-VIS spectra of S-PVA blend films (C) and those containing 0.1 and 0.3%wt of AgNPs after 1 (1W) and 5 (5W) storage weeks.

Chapter 4

Figure 4.1 Biodegradable polymer materials.
Figure 4.2 Classification of composites.
Figure 4.3 Schematic representations of nanocomposites.
Figure 4.4 Schematic representation of solution casting.
Figure 4.5 Schematic representation of in situ polymerization.
Figure 4.6 Schematic representation of melt extrusion.
Figure 4.7 SEM images of the ZnO-based composite films.
Figure 4.8 Mechanical properties of the different ZnO composite films.
Figure 4.9 Oxygen transmission rate of the different ZnO composite films.
Figure 4.10 WVTR properties of the different ZnO composite films.

Chapter 5

Figure 5.1 Structure of a nanosilica aerogel.
Figure 5.2 Scanning electron microscopy (SEM) images of SiO₂ particles prepared according to the Stober procedure. (a) 650 nm silica particles. (b) 240 nm silica particles [7].
Figure 5.3 SEM micrographs of the fractured surface of the PLA nanocomposites. (a) PLA+0.2 wt.% silica. (b) PLA+0.5 wt.% silica. (c) PLA+1 wt.% silica. (d) PLA+2 wt.% silica. (e) PLA+3 wt.% silica. (f) PLA+5 wt.% silica [4].
Figure 5.4 Schematic illustration of the solidification process of iPP/silica composites at the critical condition that inter-particle distance equals the end-to-end distance of iPP chains [93].
Figure 5.5 Number of spherulites vs. crystallization time of PLA and PLA/SiO₂ nanocomposites [86].
Figure 5.6 POM micrographs of spherulites in PLLA and PLLASN5 after crystallization at 115°C for 2, 4, and 9 min [81].
Figure 5.7 Wide-angle X-ray diffraction (WAXD) patterns of PLA and its corresponding silica nanocomposites [85].
Figure 5.8 WAXD patterns of (a) PP and (b) PP/silica (1 wt.%) obtained during cooling from 225 to 70 °C at 10 °C/min [92].
Figure 5.9 Tortuous path of a gas molecule in clay nanocomposites.
Figure 5.10 PLA films-neat and nanocomposites with different loadings of silica nanoparticles (from 0.2 to 3 wt.%).

Chapter 6

Figure 6.1 (a) SEM of nanoscale iron at a magnification of 1500; (b)SEM of nanoscale iron at a magnification of 300 k; (c) Secondary Electron Image (SEI) analysis (SEI were taken on the same region as of Figure 6.1b) of iron atom distribution

Chapter 9

Figure 9.1 Compostable materials identification flow chart according to ASTM D6400 [23].
Figure 9.2 Biodegradation in Natural Norman soil at 28°C. Poly(ethyl glyoxylate) (PEtG) (filled rectangle), control: cellulose (open circle), PEtG second addition (filled triangle). Results are expressed as the average of three replicates [35].
Figure 9.3 Response of the systems evaluated at different pH conditions: natural montmorillonite (NMnt), natural montmorillonite containing blueberry extract (NMnt+BE), modified montmorillonite (MMnt), modified montmorillonite containing blueberry extract (MMnt+BE), and blueberry extract (BE) [10].
Figure 9.4 Biodegradability in vegetal compost of cassava thermoplastic starch (TPS) films containing different concentrations of yerba mate extract (Y) (0, 5, and 20 wt.%, namely TPS, TPS-Y5, and TPS-Y20, respectively) [45].
Figure 9.5 Macroscopic appearance of biodegradation in soil of cassava thermoplastic starch (TPS) films with two different concentrations of starch (TPS75, TPS85) and TPS films with two different concentrations of starch containing citric acid (CA) (TPS75-CA and TPS85-CA) [48].
Figure 9.6 Biodegradability of poly(lactic acid) (PLA) and PLA + 1.5% nanoclays (Cloisite 30B) [57].
Figure 9.7 Gel permeation chromatography (GPC) of poly(lactic acid) (PLA and PLA + 3% nanoclays) (Cloisite 30B) before and after biodegradation in a composting medium [57].
Figure 9.8 Effect of organoclay (Cloisite 30B) content on biodegradability of polybutylene succinate (PBS) and its clay nanocomposites [65].
Figure 9.9 Influence of lignin incorporation and irradiation on the biodegradation of TPS-based films incubated in a controlled soil (kinetics of the CO₂ release fit by a first-order low CO₂ = C_max[1 -exp(-kt)]) [79].

Chapter 10

Figure 10.1 Scanning electron microscopy (SEM) of a wood fiber (a), TEM of wood CNCs (b), and TEM image of tunicate-CNCs (c) [10].
Figure 10.2 Schematic drawing of polymer network reinforced with MCC (left) vs CNC (right) [60].
Figure 10.3 Schematic drawing of the diffusion of gas permeant through the porous structure of polymer-CNC bio-nanocomposites [64].

Chapter 11

Figure 11.1 Serial dilution of four strains of yeast strains to test potency of c-CuNP. Growth inhibition is increased with the addition of soluble zinc to media.
Figure 11.2 Surface viability of S. cerevisiae (RM11) after exposure to a solid film. Colony forming units from three replicates were averaged and standard deviation graphed.

Chapter 12

Figure 12.1 PLA production. Numbers in bold brackets indicate the enzymes involved in the reaction. (1) Hexokinase, (2) phosphohexose isomerase, (3) phosphofructokinase I, (4) aldose, (5) triosphosphate isomerase, (6) glyceraldehyde 3-phosphate dehydrogenase, (7) phosphoglycerate kinase, (9) enolase, (10) pyruvate kinase.
Figure 12.2 Scheme classification of composites by their origin and biodegradability (modified from Goda et al. (17).
Figure 12.3 Classification of natural and synthetic fibers used as reinforcement.
Figure 12.4 Schematic representation of compression molding process.
Figure 12.5 Critical process parameters of compression molding method.
Figure 12.6 Description of extrusion process (a) and injection molding process (b).
Figure 12.7 Representation of extrusion blow molding.
Figure 12.8 Properties to be developed in food packaging materials.
Figure 12.9 Barrier properties of PLA in comparison to other common polymers, low-density polyethylene (LDPE), and polystyrene (PS) at 30 °C (a) N₂, (b) O₂, (c) CO₂, and (d) CH₄.
Figure 12.10 Alternatives of processing to recycle PLA.

List of Tables

Chapter 1

Table 1.1 Chemical composition of the main commercial montmorillonite cited.
Table 1.2 Antimicrobial activity of the barley protein (BP)/Cloisite Na+ composite films containing grapefruit seed extract (GSE) against the pathogenic bacteria. Reprinted with permission from Reference [76].

Chapter 2

Table 2.1 Types of synthetic polymers/halloysite systems.
Table 2.2 Bionanocomposites containing HNTs.

Chapter 4

Table 3.1 Examples of AgNPs synthesis using strong or green reduction methods.
Table 3.2 Crystalization temperature (T_c), glass transition temperature (T_g), entalphies of crystalization and melting (ΔHc, ΔHm,) and percentage of crystallinity (X) obtained by DSC of S-PVA blend films (C) and those containing 0.1 and 0.3%wt of AgNPs. Mean values ± standard deviation.
Table 3.3 Examples of different antimicrobial studies using silver species.

Chapter 4

Table 4.1 Overview of ZnO-based Composites.
Table 4.2 Mechanical properties of ZnO-based Composites.
Table 4.3 Antimicrobial activity test results of ZnO composite films against S. aureus and E. coli.

Chapter 5

Table 5.1 The dependence of tensile strength on different silica types (T120 and N999) and content for a prepared PLA material [70].

Chapter 7

Table 7.1 The mechanical properties and temperature of maximum thermal-degradation rate (T_max) of recently reported polymer/CNTs composite membranes.

Chapter 9

Table 9.1 Maximum heavy metal content for compostable materials according to various standards.
Table 9.2 Labeling and certification systems for compostability.
Table 9.3 Thermal degradation models [81, 82].

Chapter 10

Table 10.1 The different structural and mechanical characteristics of micro- and nanocellulose derivatives.

Chapter 11

Table 11.1 Level of required data upon submission of the Foof Contact Notification to the Office of Food Additive Safety and Applied Nutrition at the United States Federal Food and Drug Administration. The reported data addresses detailed mutagenic and carcinogenic potential of the proposed food contact substance. Requirements are based on the level of daily exposure to the proposed food contact substance per person.

Chapter 12

Table 12.1 Summary of previous reported work of polylactic acid and natural fiber biocomposites.
Table 12.2 Processing parameters and interval values recommended to process PLA resins^*.
Table 12.3 General physical properties of commercial PLA (NatureWorks^® Ingeo™ Biopolymer 2003D) for fresh food packaging and food serviceware (http://www.natureworksllc.com).

Chapter 13

Table 13.1 ENMs’ characterization techniques: Properties searched and methods currently in use [19, 20, 24].
Table 13.2 ENMs migrated from FCM – case studies.
Table 13.3 Toxicological tests by type of exposure and methodology applied.
Table 13.4 General regulation on packaging and materials in contact with food¹.
Table 13.5 Nanomaterials used in food contact materials and their regulation.

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Insights into Modern Food Science
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Library of Congress Cataloging-in-Publication Data
ISBN 978-1-119-16020-5

Preface

In recent years, consumer’s consciousness of the strong relationship between food quality and health has extensively impacted the packaging field. Nowadays, indeed, a packaging material is asked to match the handling and storage conditions with the quality and safety of foodstuffs. As a consequence, scientific literature and industrial R&D activities are plenty with attempts to develop new and effective materials that are able to preserve food from degradation in both normal and stressed environmental conditions, resulting in a consistent enhancement of their shelf-life. The packaging science is thus becoming an interdisciplinary research field, involving the expertise of chemists, physicists, engineers and biologists, with the ultimate aim to match the consumers’ expectation and government’s regulations.

The book is intended as an overview on the recent and more relevant insights in the application of composite materials on food packaging, emphasizing the scientific outcome arising from the physico-chemical properties of such engineered materials with the need of food quality and safety.

Composites, matching the properties of different components, allow the development of innovative and performing strategies for an intelligent food packaging, overcoming the limitations of using only a single material.

The book starts with the description of montmorillonite and halloysite composites, subsequently moving to metal-based materials with special emphasis on silver, zinc, silicium and iron. After the discussion about how the biological influences of such materials can affect the performance of packaging, the investigation of superior properties of sp² carbon nanostructures is reported. Here, carbon nanotubes and graphene are described as starting points for the preparation of highly engineered composites able to promote the enhancement of shelf-life by virtue of their mechanical and electrical features.

Finally, in the effort to find innovative composites, the applicability of biodegradable materials form both natural (e.g. cellulose) and synthetic (e.g. polylactic acid – PLA) origins, with the aim to prove that polymer-based materials can overcome some key limitations such as environmental impact and waste disposal.