PACKAGING TECHNOLOGY AND SCIENCE Packag. Technol. Sci. 2013; 26(Suppl.

1): 110 Published online 5 September 2012 in Wiley Online Library (wileyonlinelibrary.com) DOI: 10.1002/pts.1986

Chinese Packaging Institute -2012 Conference Fabrication and Characterizations of Zeolite blled Polyethylene Composite Films
By Zhen Huang,* Yu-hua Guo, Tian-ming Zhang, Xiao-hong Zhang and Li-ying Guo
Department of Packaging Engineering, Tianjin University of Commerce, Tianjin 300134, China

A series of low-density polyethylene (LDPE)/linear LDPE (LLDPE)/zeolite H-b composites at different zeolite contents up to 10 wt% were mixed after melt and blown into lm sheets. The resultant lms were characterized by using X-ray diffraction, scanning electron microscope and other physical property analyzers. X-ray diffraction results reect that either zeolite or polymer phase has maintained its regularly ordered microscopic structure without any observable deterioration. The scanning electron microscope morphological observation shows a good dispersion of zeolite in the PE matrix. Water vapour, oxygen and nitrogen transmission rates are all found to increase after introducing zeolite H-b. However, tensile strength, elongation, tear strength and puncture resistance are observed to obviously drop with successive increment of zeolite content. Composite lm clarity becomes poorer than the pristine lm as reected by the increase of the lm haze after adding zeolite H-b. Finally, the composite lms were used as packaging materials for fresh strawberries. The gas composition variations in the packages during 5 days reect that the O2 and CO2 contents have varied inside and they are apparently dependent on the zeolite loadings in the composite lms, subsequently affecting respiration rates of fruit. Our experiments suggest that there is a compromise between zeolite content and lm performances like mechanical, optical, barrier and packaging properties. Copyright 2012 John Wiley & Sons, Ltd.

Received 3 February 2012; Revised 21 May 2012; Accepted 29 May 2012 KEY WORDS: polyethylene; zeolite H-b; composite lms; barrier properties

INTRODUCTION Fresh fruits and vegetables harvested seasonally must be stored or packaged in suitable environments to prevent the possible degradation that may render them a lower quality or make them unsuitable for consumption. Among various preservation methods, physical packaging with polymeric lms is usually preferred as it necessitates the minimal processing of the produce so that it resembles its natural features to the maximum extent. As a feature of proper sealed packaging lms, a fresh fruit or vegetable is capable of creating modied atmosphere within the package due to the respiratory gases. These gases like oxygen, carbon dioxide, ethylene and water vapour can permeate through the packaging material at different rates and thus affect the quality of fresh food packed. Among various packaging materials, polyethylene is the most extensively used because of its easy availability, process ability, exibility and improved optical properties and seal strength. In addition, no other ingredient is required during processing of polyethylene. Recently, some investigators have studied the effect of zeolite on the performance of polyethylene packaging material as the zeolite is
* Correspondence to: Z. Huang, Department of Packaging Engineering, Tianjin University of Commerce, Tianjin 300134, China. E-mail: huangzhen50@yahoo.com Copyright 2012 John Wiley & Sons, Ltd.

Z. HUANG ET AL.

selectively permeable to different gaseous molecules like oxygen, nitrogen and carbon dioxide.18 To the best of our knowledge, zeolite is widely used to enhance the gas separation properties of the mixed matrix lms.9 It is worth noting that the lms, formed by incorporating zeolite particles into a properly selected polymer, exhibit much better gas separation properties as compared with conventional composites because of their unique phase morphology and high surface area.9 Furthermore, zeolite can be used for catalysts for the conversion of agriculture lm waste into useful hydrocarbon products.10 The challenge for these zeolite-lled composites is to improve the lm properties to meet the requirements for the purpose of suitable applications like packaging. Thus, knowledge about the relationship between properties and zeolite effects is required. In this study, PE/zeolite H-b composites were investigated in lm samples blown with different zeolite contents. Structural, mechanical, optical and barrier properties of the lms were studied and compared; moreover, these lms were tested for packaging fresh strawberries as they are a highly perishable fruit because of their physiological and morphological properties and their rapid postharvest responses.11,12 In this way, this study was aimed to investigate the effect of PE/zeolite H-b composites on air-packaged strawberries. EXPERIMENTAL Materials Commercial grade of low-density polyethylene (LDPE) (LD-163; Melt ow index (MFI), 5 g/10 min; density, 0.941 g/cm3) from SINOPEC Yanshan Chemical Corporation, Beijing, China, and linear LDPE (LLDPE) (FV-149M; MFI, 2 g/10 min; density, 0.931 g/cm3) from SKCorporation, Korea, were used at a mass ratio of 4:1 as the base polymer. Zeolite H-b, with a Si/Al ratio of 38 and a particle size of approximately 1 mm, was purchased from the Catalyst Plant of Nankai University, Tianjin, China. Compounding and lm blowing LDPE, LLDPE and zeolite H-b were melt-mixed to obtain pelletized composite using a twin-screw co-rotating extruder (LTE-26-52; Labtech Engineering Co. Ltd, Thailand) with a temperature prole of 155  C to 185  C during the compounding process. The obtained composite was then blown into 75-mm-thick lm samples using a double-layer co-extrusion lm blowing machine (SFM-200, L/D = 25 and D = 25 mm; Beijing Plastics Industry Co., Ltd, Beijing, China). Film blowing was performed at a temperature prole of 170  C to 190  C. To study the effects of zeolite content, a few PE/zeolite composite lms with different zeolite contents were prepared while the mass ratio of LDPE to LLDPE was kept at 4:1 for all composites. The compositions of these PE/zeolite H-b composite lms are summarized in Table 1. Characterization methods The PE/zeolite H-b composite lms obtained were examined by a few characterization methods given as follows. Morphology and structure analysis. Powder X-ray diffraction (XRD) analysis,13 performed on a Shimadzu XRD-6000 spectrometer using Cu Ka radiation (1.5406 ) with the samples scanned from 5 to 50 in steps of 0.02 , was carried out to investigate the composite microstructure and to conrm the presence of zeolite structure and whether zeolite affects the structure of the polymer matrix.
Table 1. Contents of PE/zeolite H-b composites prepared. Compositions (wt%) Samples
S0 S1 S2 S3 S4

LDPE
80.0 78.0 76.0 74.0 72.0

LLDPE
20.0 19.5 19.0 18.5 18.0

H-b
0.0 2.5 5.0 7.5 10.0

Copyright 2012 John Wiley & Sons, Ltd.

Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

ZEOLITEPE COMPOSITE PACKAGING FILMS

The cross-sectional morphology14 of the composite lm was examined with a scanning electron microscope (SEM; JEOL JSM-6700F). Before the SEM examinations, the sample strips were chilled in liquid nitrogen for at least 30 s and then folded with forceps to make a sharply broken cross section of the lms. The resultant lm was vertically adhered to an aluminium stub with a tape to render the lm cross-sectional surface parallel to the stub surface and gold coated under vacuum using a sputter coater. Mechanical properties. The tensile strength (TS)15 of the composite lms was determined on a universal testing machine at a rate of 200 mm/min. The defect-free strip sample was cut in a dumbbell shape with a size 15 100 mm, and 20 strips were prepared for each lm with 10 for transverse direction (TD) tests and the remaining for machine direction (MD) tests. Tear strength16 was determined using a universal testing machine at a rate of 200 mm/min, similar to the case of TS measurements. The samples were prepared with 10 strips for TD tests and the other 10 for MD tests for each lm. The puncture strength17 of plastic lms was evaluated using a pendulum impact tester. The sample was exposed, at right angle to its surface, to a semispherical punch of 12.7 mm in diameter at a controlled impact rate. The strength in joules is taken to be the maximum energy consumed at the moment of lm failure and is essentially a measure of the capacity of the lm to absorb energy. Optical properties. The haze and the transparency18 of the composite lms were quantitatively measured on a WGT-S tester (Labthink Technology Co., Ltd, Jinan, China) for more than 10 samples of each lm. Haze and transparency are two important parameters for transparent or translucent lms. The former refers to the percentage of the total transmitted light that, in passing through the sample, is scattered and/or refracted from the incident beam by more than 2.5 , whereas the latter is the percentage of incident light that, in passing through the sample, is deected by less than 0.1 from the axis of the incident light. It should be noted here that transparency is also called clarity because it is directly related to whether it is visible or not for the contents packed inside the lm bags. Barrier properties. Oxygen transmission rate (OTR) and nitrogen transmission rate (NTR)19 were tested using a manometric gas permeability tester (L100-5000; PBI Dansensor, Denmark). The test samples used were of circular shape with a diameter of 10 cm and stored before testing in desiccators. The test was performed at constant temperature and constant relative humidity (RH) of 23  C and 50% in this work. Water vapour transmission rate (WVTR)20 was determined using a water vapour permeability tester (L80-5000; PBI Dansensor). The lm separated the permeation cell into lower and upper chambers where the lower chamber was saturated with water vapour whereas the upper one was dried via a silica lter under air purge ow to a dened level of RH of 9.8%. The experiment was carried out in the room with a constant temperature of 23  C and a constant RH of 50%. Strawberries packaging. Strawberry fruit was obtained from a commercial fruit grower at Shandong province, China. Fruit was harvested at commercial maturity judged on the basis of fruit skin colour as it is considered as the best indicator of the harvest maturity in fruits. Therefore, fruit having a sharp-red skin colour was harvested and transported to the Packaging Engineering Laboratory of Tianjin University of Commerce, China. The fruit was sorted for uniformity in size, maturity and freedom from defects before packed in PE/zeolite H-b composite lms. The lms were cut into control sheets with a size of 25 25 cm for making plastic bags. For each lm variant, 10 replicate packs, each containing ve fruits, were tested. The randomly selected fruit was placed in a plastic tray, then loaded into lm bags and sealed through appropriate thermal treatment. The packed fruit was then transferred onto a home-made plastic mesh for avoiding any fruit injury and stored at ambient conditions (25  C28  C and 60%70% RH) to simulate marketing conditions. Figure 1 shows fresh strawberries packaged in PE/zeolite H-b composite lms blown in present study. The percentage concentrations of O2 and CO2 in the fruit bags were measured through a self-sealing rubber septum using a gas analyzer (Model Checkmate 9900 O2/CO2; PBI Dansensor). The gas composition was measured daily for 5 days. Statistical analysis. The experiment was carried out in a completely randomly way, and the results were subjected to ANOVA using Stastica Software 99 at a signicance level of P < 0.05. The standard deviation was then calculated, and all the data points were obtained in this work as mean values along
Copyright 2012 John Wiley & Sons, Ltd. Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

Z. HUANG ET AL.

Figure 1. Fresh strawberries packaged in PE/zeolite H-b composite lms. with a deviation within 10%, indicative of the reliability of the method used and the acceptable reproducibility of experimental results determined.

RESULTS AND DISCUSSION XRD analysis and SEM observations Figure 2 shows XRD patterns for PE lm and PE/zeolite H-b composite lms. As evidenced by the XRD results, there are two distinct diffraction peaks in 17 24 and 35 38 , respectively, for the S0 sample, which are probably related to crystalline features of LDPE/LLDPE materials used. The very high peak intensity conrms that the PE obtained is still highly structurally crystalline. Because PE is the substrate material, thus these two peaks are very clearly preserved in the XRD spectra for all composite samples. After adding zeolite H-b, a few more peaks at approximately 2 =7.16, 9.90 and 22.44 are observed, which are characteristic of the zeolite b structure and identical to those reported in the literature.13 Besides, with an increase in the zeolite content, the intensity of these peaks becomes more pronounced, as shown in Figure 2. On the other hand, the incorporation of zeolite particles has not been found to observably affect the crystalline structure of polyethylene matrices.

Figure 2. XRD patterns of PE/zeolite H-b composite lms.

Copyright 2012 John Wiley & Sons, Ltd. Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

ZEOLITEPE COMPOSITE PACKAGING FILMS

Figure 3 displays cross-sectional SEM images for the PE/zeolite H-b composite lms at 10 wt% zeolite loading, from which the particle distribution and morphologies may be examined. As we can see from Figure 3, zeolite H-b particles are generally homogeneously distributed throughout the whole polymer matrix, indicative of the feasibility of the melt mixing and co-extrusion lm blowing processes used. The lm thickness can also be approximately observed from Figure 3, and it is approximately 80 mm and agreeing rather well with the value for lm-blowing design. At high magnication, SEM image reects that zeolite particles used are generally uniform and have a particle size of approximately 1 mm. It is clearly observed that the zeolite particles are rather well contacted in the PE phases, indicative of good interfacial compatibility formed between dispersed phase and continuous phase. In contrast, Yong et al.14 reported that void-rich microstructures were created in polyimide lms after lled with only zeolite particles. Thus, we can deduce that some ne interfacial voids might have formed around zeolite particles as well.

Mechanical property measurements Table 2 presents zeolite/zeolite H-b composite lms. It can be seen that for PE/zeolite composite lms, the TS in two different direction tests rstly decreases with the zeolite content to 5.0 wt% of zeolite loading and then slightly increases. As for the MD TS, it is 22.2 MPa without adding zeolite but reduces to 15.8 MPa after introducing 5.0 wt% of zeolite. For the TD tests, the values are 20.9 and 14.5 MPa, respectively, for the lms without zeolite and at 5.0 wt% of zeolite loading. The decrease in lm TS may be mainly due to the decrease in the polymer content of the lms. One may note that the polymer content will drop correspondingly as the loading of zeolite H-b in the polymer matrix become higher, thus reducing the TS of the resultant lms with the zeolite content. After adding more zeolite, the melt mixing and co-extrusion lm-blowing method used here may have rendered the interfacial interactions between polymer macromolecules and zeolite particles slightly stronger, thereby recovering TS to an extent and reaching a plateau value. On the other hand, very ne voids around

Figure 3. Cross-sectional SEM images of the S4 lm sample: (a) low magnication and (b) high magnication.

Table 2. Mechanical properties of PE/zeolite H-b composite lms. TS (MPa) Films

S0 S1 S2 S3 S4

Elongation (%) TD TD
108 10 97 9 72 12 88 7 74 8

Tear Strength (kN/m) TD

98.6 5.4 99.5 4.3 90.7 6.1 89.4 3.2 82.1 5.1

MD
22.2 2.3 16.3 1.8 15.8 1.2 15.9 0.9 17.1 1.5

MD
445 36 322 25 291 13 280 18 291 21

MD
109.4 8.6 99.0 9.3 89.1 7.5 92.8 4.8 89.7 6.7

Puncture strength (J)

7.85 0.62 7.16 0.37 7.24 0.57 7.53 0.29 7.47 0.46

20.9 2.1 16.4 1.7 14.5 0.8 14.7 1.2 15.7 1.3

Copyright 2012 John Wiley & Sons, Ltd.

Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

Z. HUANG ET AL.

zeolite particles once created could contribute to the loss of lm TS. Similar observations have applied to percent elongation, tear and puncture strengths, as can be seen from Table 2. Although there are certain decreases in mechanical properties for these composite lms, they could still be used as exible packaging materials for storing fresh fruit. Optical properties For packaging applications, optical properties such as haze and clarity are of considerable importance in the development of polyethylene lms. Figure 4 shows the haze and transparency measurements for PE/zeolite H-b composite lms blown in current work. It can be seen that the pristine PE lm has a transmittance of approximately 85%, and the lm transmittance is reduced to 80% after adding zeolite. In contrast, the lm haze increases from 80% to 85% with introduction zeolite H-b. These results suggest that the addition of inorganic zeolite particles has adversely affected the lm optical properties. It is known to us that the high haze in PE lms has arisen from surface irregularities because of the extrusion roughness of the elastic melt ow effects and the crystallization roughness due to the presence of crystal aggregates.21 For the lm composites, the PE crystalline structure may not have been affected by the presence of zeolite H-b, but the zeolitic crystal structure is still retained in the lms as reected by XRD spectra. Then, the combined crystal aggregates of PE and zeolite H-b near the lm surface could subsequently make the composite lm surface smoothness worsen. In the meantime, the presence of rigid zeolite particles can affect the elastic melt ow at the exit of the extrusion die, possibly rendering the lm surface become relatively rougher. As a consequence, the composite lms have higher

Figure 4. Optical properties of PE/zeolite H-b composite lms: (a) haze and (b) transparency.
Copyright 2012 John Wiley & Sons, Ltd. Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

ZEOLITEPE COMPOSITE PACKAGING FILMS

haze and poorer transparency than the one without zeolite. However, one may note from Figure 1 that the clarity properties of the composite lms are still satisfactorily acceptable as they allow us to see what is contained within the packages. Barrier properties Table 3 displays the WVTR curve of PE/zeolite H-b composite lms at different zeolite loadings. Neat PE lm exhibits good resistance to water vapour transfer with a WVTR value of 5.66 g/m224 h due to the hydrophobic nature of polyethylene macromolecules. With the introduction of zeolite H-b into polymer matrices, the water vapour transmission rate increases considerably, and its value depends on the zeolite content added. As zeolite H-b loading is 5.0, 7.5, 10.0 wt%, the WVTR increases by approximately 46%, 55% and 78%, respectively. The signicant increase in WVTR for the PE composites may be mainly attributed to the large pore size of introduced zeolite H-b.13 Besides, the presence of aluminium element and hydrogen ion in the zeolite H-b might make itself slightly more hydrophilic than the PE substrate, possibly resulting in some increase in WVTR. In view of packaging fresh fruit and vegetables, the increase in WVTR may be helpful as water vapour, upon food respiration or retained water from washing, may transport readily to certain degree out of sealed lms to avoid condensing on the lm inner wall. Once water vapour is saturated inside the packaging, it will unavoidably attract the yield of bacteria and consequently shorten the life span for consumption. The gas permeation performance of PE/zeolite H-b composite lms was individually tested for N2 and O2. Table 3 shows the permeation results thus obtained for these composite lms with different zeolite loadings. As seen from Table 3, the PE substrate lm (S0) has an O2 transmission rate of 1880 ml/m224 h and N2 transmission rate of 760 ml/m224 h, respectively. After adding zeolite, the composite lm has higher OTR and NTR values compared with the lm without zeolite. In the case of the S3 lm with 7.5 wt% zeolite H-b, the OTR and NTR values are 2450 and 824 ml/m224 h, respectively. In addition, the ratio of OTR/NTR increases from 2.5 for the S0 lm to 3.0 for the S3 lm. As discussed earlier, XRD spectra of the composite lms reveal no obvious change in bulky PE crystallinity upon formation of the composites, which means that the changes in OTR or NTR are probably not due to the result of disruptions in polymer microstructures. Therefore, the gas permeation results could probably be attributed to the large pore size of zeolite H-b 13 introduced into the polymer matrix. Note that if some ne interfacial voids were created around zeolite particles, the gas transmission rate would also have increased. These barrier results suggest that the incorporation of porous zeolites in the conventional packaging lms may produce modied-atmosphere-packaging effect for fruits and vegetables. Packaging applications Figure 5 shows O2/CO2 concentration evolution in the packages for stored strawberries during 5 days for the PE/zeolite H-b composite lms. As can be seen, the respiratory rates of strawberry fruit increases with the progression of storage irrespective of the lms with or without zeolite loadings. The CO2 content in the packages are 2.02.4 times higher at 112 h than that at 20 h, but for the O2 content it is 4.4 and 2.1 times higher for the S0 and S4 lms, respectively. Thus, the respiration rates were modied during ambient storage to some extent, depending on the zeolite loadings. Figure 5 shows that at higher zeolite H-b loadings in the composites, higher O2 and lower CO2 content could be obtained. This may be explained as follows. During strawberry fruit respiration, O2 in the packages
Table 3. Permeation results of PE/zeolite H-b composite lms. WVTR Films
S0 S1 S2 S3 S4

NTR (ml/m 24 h)
2

OTR (ml/m224 h)
1880 48 2145 69 2333 24 2450 112 2605 85

(g/m 24 h)
2

4.66 0.14 4.57 0.28 6.79 0.49 7.23 0.37 8.30 0.63

760 9 789 18 815 21 824 27 845 16

Copyright 2012 John Wiley & Sons, Ltd.

Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

Z. HUANG ET AL.

Figure 5. O2/CO2 concentration changes in the packages for strawberries during storage for 5 days: (a) O2 and (b) CO2. was consumed whereas CO2 was generated. Hence, CO2 will permeate out and O2 will permeate into the packages based on concentration gradient. However, as discussed earlier, the gas permeation properties of the composite lms are different from each other because the one with higher zeolite content bears higher gas transmittance rate. As a result, more O2 or CO2 molecules can pass through the S4 lm with highest zeolite loading, leading to lowest CO2 content and highest O2 content inside the packages. Subsequently, the variations of gas concentrations in the packages could inuence the respiration rates of strawberry fruit affecting fruit quality. Our experiments show that the S4 lm with highest zeolite content had led to the best storing performance but at the cost of the lm clarity to certain extent for packaging fresh strawberry fruit. Therefore, there should be a compromise between zeolite content and lm performances like mechanical, optical, barrier and packaging properties and further work along this line will be carried out soon.

CONCLUSIONS In this article, we have fabricated numerous PE/zeolite H-b composite lms by using a double-layer co-extrusion lm blowing machine after having compounded LDPE/ LLDPE/zeolite H-b at different
Copyright 2012 John Wiley & Sons, Ltd. Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts

ZEOLITEPE COMPOSITE PACKAGING FILMS

zeolite contents through a twin-screw co-rotating extruder. The following conclusions can be drawn from the present study. 1. After incorporating zeolite H-b particles, the polyethylene composite lms exhibit considerable decrease in mechanical properties like TS, elongation, tear strength and puncture resistance, whereas the regularly ordered microscopic structure of either zeolite or polymer phase retains rather well as reected by XRD spectra. 2. The addition of zeolite H-b into the PE lm has shown a good dispersion of zeolite particles in the PE matrix as reected by SEM images, whereas the lm haze, possibly arising from surface crystal aggregations and the effect of rigid zeolite particles on the elastic melt ow, is seen to increase with zeolite loadings, subsequently making the lm surface smoothness worsen and the clarity poorer. 3. The PE/zeolite H-b composite lms exhibit obvious increase in water vapour, O2 and N2 transmission rates after introducing zeolites, possibly due to the large pore size of zeolite H-b. 4. The packaging application results for fresh strawberries show that the O2/CO2 composition had varied over time in the composite lm packages and higher zeolite H-b loadings had resulted in higher O2 content and lower CO2. These variations of gas compositions inside could modify subsequent respiration rates of strawberry fruit and possibly extend shelf-life of air-packaged strawberry fruit. 5. There are certain improvements in the barrier properties after adding zeolites, but the lm clarity and mechanical properties are sacriced. Thus, a compromise between the zeolite content and the lm properties should be taken into account, and more investigations are required to further achieve the integrated performance for these zeolite-lled composite lms.

ACKNOWLEDGEMENTS
The authors thank Tianjin University of Commerce for partially supporting this research.

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Packag. Technol. Sci. 2013; 26(Suppl. 1): 110 DOI: 10.1002/pts