Turkish J. Eng. Env. Sci.

27 (2003) , 1 – 9.
c TÜBİTAK

A New Protective Polyethylene Based Film Containing Zeolites for

the Packaging of Fruits and Vegetables: Film Preparation

S. Nur (AKTAŞ) DİRİM, Ali ESİN, Alev BAYINDIRLI

Middle East Technical University, Food Engineering Department,
06531, Ankara-TURKEY
e-mail: aliesin@metu.edu.tr

Received 25.01.2001

Abstract
To manufacture a polyethylene film containing zeolite particles for the packaging of foods six manufactur-
ing methods were tried: hot pressing, addition of zeolite to molten polyethylene and dissolved polyethylene
solution, coating polyethylene beads with zeolite in a revolving heating pan, extrusion of polyethylene beads
with zeolite and hot pressing of the extruded mix film. The experiments were repeated with three different
particle sizes of zeolites received from the Bigadiç mine belonging to Etibank. The film produced by the hot
pressing of co-extruded zeolite-polyethylene film was found to be quite satisfactory as a packaging material.

Key words: Packaging film, Polyethylene, Zeolite

Introduction lene gases which necessitates commodity diffusion re-

sistance and their effects on quality parameters to be
established together with the effect of temperature
Fresh fruits and vegetables harvested seasonally
on these. Such knowledge will enable the selection
in large quantities from different areas are mostly
of a suitable packaging material.
stored in suitable environments until marketed and
consumed. During storage and transportation, the Polyethylene is the most commonly used polymer
appropriate maintenance conditions should be prac- film for packaging with its advantages of being inert,
ticed since fresh fruit and vegetables are living permeable to gases and impermeable to water vapor
systems and very sensitive to deteriorative effects (Rooney, 1995). However, due to the large variety
(Kader, 1989). Packaging a food product is an oper- and variable properties of produce no single pack-
ation aimed to prevent most of the possible kinds of aging material can be said to be ideal for use with
degradation that render it unsuitable for consump- all produce. In order to achieve satisfactory perfor-
tion or of a lower sensorial value. Stability of a pack- mance with many produce-film combinations, highly
aged foodstuff greatly depends on the characteris- permeable porous patches were introduced. Among
tics of the packaging material and proper conditions these a commercial product FH T M film containing
of harvesting, storage and distribution (Mathlouthi natural zeolites embedded into polyethylene (Evert-
and Leiris, 1990). As a feature of proper packaging Fresh Co. Inc., Japan) was reported to be extremely
in a sealed package a fresh product creates a mod- suitable for extending the shelf life of produce. Al-
ified atmosphere by respiration and gas permeation though zeolites have unlimited uses in planting, an-
through the packaging material. Thus, suitable films imal feeding, waste treatment and solar heat collec-
for packaging should have desired levels of selective tors (Mumpton, 1983), in Turkey they are unfortu-
permeabilities to oxygen, carbon dioxide and ethy- nately being wasted in unrelated areas, e.g., as filling

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 (AKTAŞ) DİRİM, ESİN, BAYINDIRLI

material in cement. With regard to these and the surface. This was covered with another non-sticking
above facts considering the large amount of zeolite paper and hot pressed (Paul Weber Stgt. Uhlbach,
deposits of Turkey, in this study we aimed to produce Germany). The pressing temperature was measured
a packaging material using polyethylene and natural by means of four thermocouples placed into the press
zeolites. located as close as possible to the surface of the press.
Pressing was carried out at different temperatures
and different periods as given in Table.
Materials and Methods

In the production of the composite film, finely Table. Experimental parameters used for hot pressing.
ground natural zeolite was combined with commer-
cial polyethylene either in the form of extruded film Mass of zeolite per Temperature of Time of
or as beads. Polyethylene was purchased from the mass of Pressing Pressing
market as polyethylene beads (Petkim, Turkey) or polyethylene
as film with a thickness of 0.06 mm. Zeolite was (kg/kg) (◦ C) (minutes)
received from Etibank’s Bigadiç natural mineral re- 0.2 120 20
sources region in an an unprocessed form. In the re- 0.3 120 20
gion the purity is quite high, containing about 80% 0.4 120 20
ore and the rocks are mainly composed of clinop- 0.5 120 20
tilolite + heulandite with the remaining being erion- 0.6 120 20
ite, chabazite and analcime as determined by X-ray 1.0 120 30
diffraction analysis (Dokuz Eylül University). The 1.0 140 30
zeolite mineral was in the form of large pieces about 1.0 140 45
20 x 18 x 8 cm in dimension as received from the 1.0 145 20
region. These were first crushed in a jaw crusher 2.4 100 190
(Wedag BOCHUM, 1963, Karl Kolb, Frankfurt, Ger- 2.4 122 30
many) and then were ground with a hammer mill 5.0 120 250
(Laboratory Mill Model 4, Arthur H. Thomas Com- 5.0 145 30
pany, USA). The ground samples were classified into
three size ranges by sieving (Octagon 200 Test Sieve As an alternative procedure a similar test was
Shaker, Endocotts Limited, London). The three carried out by first spreading large zeolite parti-
ranges selected were -420 µ/+212 µ , -212 µ/+106 cles, i.e., -250 µ (60 mesh)/+177 µ (80 mesh) onto
µ and -106 µ/+53 µ, which shall from now on be polyethylene film. These were then pressed manu-
referred to as +212 µ, +106 µ and +53 µ respec- ally on the polyethylene surface in order to deform
tively. The natural zeolite samples were analyzed the surface. Upon creating sufficient surface rough-
in an X-ray diffractometer (Jeol JSDX-100 S4) and ness, the large particles were cleared from the surface
diffraction diagrams were obtained. For the analy- and the small particles were manually spread to fill
sis a CuKα lamp, a 30 kV working voltage and a 22 the cavities formed. The excess particles remaining
mA working current were used. In order to obtain on the surface were gently swept away. Then this
a zeolite + polyethylene film with suitable physical film was hot pressed for 30 min at 110 and 120◦C.
properties for packaging several methods were tried, In the second group of trials, zeolite was added to
which can be grouped into three. either melted or dissolved solutions of polyethylene.
In the first group of trials, hot pressing zeolite In the first part, polyethylene was melted and zeolite
particles on a polyethylene surface was attempted. was added to the melt. The experiment was started
In this method zeolite was embedded on the surface at 65◦C, whereafter about 80◦ C the film started to
of the polyethylene film confined between two plates soften. In the temperature range 120-145◦C shrink-
where the temperature of the plates and the applied age of the film took place and then in the range
pressure could be adjusted. Zeolite particles with 150-165◦C it started to melt. Between 190◦C and
dimensions less than 74 µ (200 mesh) were used for 205◦C it completely melted and slight mixing with
the experiments. A pre-weighed amount of polyethy- zeolite particles of an average size 74 µ could be
lene film was placed on a non-sticking paper and a achieved. The mixture was not perfectly homoge-
weighed amount of zeolite was spread onto the film neous at this temperature. The total time for heat-

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ing was 2 h. In order to obtain a film from this with zeolite gave rise to the second method, extru-
mixture, the mixture was spreaded by an automatic sion of polyethylene film with zeolite. In the first step
spreading machine (Automatic Film Applicator-133, of this method, zeolite covered polyethylene beads
Sheen Instruments Ltd., England). For this proce- were produced. For this purpose, polyethylene beads
dure several zeolite/polyethylene ratios, 0.5/10, 1/10 together with a large amount of ground zeolite of
and 2/10 (w/w), for the average zeolite particle sizes sizes +53 µ, +106 µ and +212 µ were mixed, and
of 74 µ were studied to determine the optimum ratio the mixture was slowly heated so that just the sur-
and particle size for spreading. face of the beads melted and ease the attachment of
In the second part polyethylene was dissolved in the zeolite particles to their surface. For this pur-
a solvent and zeolite was added to this solution. The pose, different temperatures in the range 140-150◦C
solvent used was xylene (Merck) as it is the most were tested. The optimum temperature of heating
suitable for polyethylene. According to this proce- was chosen as 145◦ C and further experiments were
dure, the most proper polyethylene to xylene ratio carried out at this temperature. Then the coated
was primarily determined by the several combina- bead samples were placed in an oven for 3 h at 145◦C
tions tried. These were 1/10, 1/9, 1/8, 1/7 and 1/6 (OV/160 CLAD, England) to ensure the attachment.
as mass ratios of polyethylene to xylene among which The amount of zeolite held by the beads was calcu-
1 part polyethylene per 10 parts of xylene proved to lated from the weight of the zeolite covered beads
be the best. Using this ratio polyethylene in the and the weight of the beads fed. This ratio was
form of sheets was put into xylene and the mixture checked for different trials and was found to differ
was kept at 75◦C for 1 h while mixing the solution by ± 0.01 kg/kg beads.
intermittently. Upon obtaining a homogeneous solu- Zeolite coated polyethylene beads were hot ex-
tion, zeolite with an average particle size of 74 µ was truded in an industrial extruder (Heminstone, 1977,
added. The amount of zeolite added was varied for Taiwan, Doğan Plastik, İzmir). The extruder die
different batches as 0.05, 0.1, 0.15, 0.2 and 0.25 parts exit temperature was 110◦C and the extruder tem-
of zeolite per 1 part of polyethylene. For a specific perature was 90◦ C, which were kept constant by a
ratio, the heterogeneous mixture was mixed continu- thermostat. The thickness of the film was adjusted
ously at 75◦ C for 10 min. Then the mixture formed by the feed rate, in this case being 30 kg/h. The
was poured as a thin film in a petri dish and dried in flow rate of the air was adjusted so that a blown col-
a vacuum oven at 80◦C until all xylene evaporated umn 3 m height and 0.5 m width was formed at the
leaving a thick and brittle film as a residue. Finally, extruder exit.
the obtained film was cut into very small pieces, i.e., The films prepared by extrusion as described
0.02 m x 0.05 m rectangular strips, placed between above contained large amounts of zeolite and their
heat stable and non-sticking papers and hot pressed flexibility was very low and some surface defects like
at 130◦ C for 5 min. holes caused by aggregates of zeolite was observed in
In the third group of trials, polyethylene beads some parts. For this reason, the films prepared thus
were coated with zeolite. To achive this we used were subjected to a curing process by hot pressing
a revolving heated pan (Armfield, FT12 Ball Mill, at 120◦C for 5 min.
England) with a stainless steel rotating pan directly After deciding on the method of film produc-
mounted onto the output shaft of a geared motor to tion, the film structures of the films produced by
give variable speed adjustments with the direction of this procedure were examined by image analysis (IA)
rotation easily reversible. Furthermore the complete and scanning electron microscope (SEM). The set-up
rotation of the pan could be set at different angles to used for this purpose consisted of three main parts
the to horizontal for satisfactory tumbling of the con- that were connected by several interfaces: a camera
tents of the pan. Zeolite particles of average size 74 µ (Cohu Inc.), a dual monitor image processing com-
to form the bed and enough polyethylene beads were puter equipped with image grabber (Targa, True-
placed into the pan and heated with the pan bottom vision) and an image processing software (Mocha,
immersed in an oil bath at 180◦C. With the action of Jandel Inc.). The images were directly taken by the
continuous mixing and heating, zeolite particles were camera using a KOWA vari-focal lens with a maxi-
attached to the softened surface of the polyethylene mum aperture ratio of 1:1.8. A standard 100 W light
beads. bulb was used for top lighting, while a UV source was
The positive result achieved in coating the beads used for bottom lighting in order to provide a higher

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intensity light than the room lighting. b. Mixing Zeolite Particles with Polyethy-
Analysis was performed by image acquisition and lene Melt and Polyethylene Solution
calibration in which an image captured and grabbed We also investigated the second possible alter-
on 256 gray levels is stored in the hard drive of a native for composite film production, complete mix-
computer with a standard format of 719 x 511 pixels ing of polyethylene and zeolite. According to trials
either as a color or monochrome value. After storing with different average zeolite particle sizes and ze-
the image, a scale value that is a function of the mag- olite/polyethylene ratios, the optimum particle size
nification is entered in order to convert the spatial and the mixing ratio for spreading was found to be
measurement value in pixels to centimeters. 74 µ and 1/10 (w/w), respectively. When the par-
For the same films, film structures were also ticle sizes were greater than 74 µ, they yielded a
examined by scanning electron microscope (SEM) very heterogeneous appearance and were also hard
(Met. Eng. Dept., METU). For SEM analysis, fine to spread. On the other hand, for smaller particle
representative samples from the three products of sizes it was necessary to employ greater amounts of
this study plus PE and FH films was used. Each film zeolite, which severely affected the density of the
was observed with x100 and x300 magnification. mix. Further, in determining the optimum zeo-
lite/polyethylene ratio the primary factor that af-
Results and Discussion fected the result was found to be spreadability.
When a sufficient amount of well mixed molten
The purpose of preparing polyethylene film embed- mixture was prepared at optimum conditions, i.e.,
ded with zeolite was to combine and increase the 1/10 (w/w) zeolite/polyethylene at 190-205◦C, we
individual advantages of both materials for use in tried to spread it as a thin film. With the instrument
food packaging. According to X-ray analysis with a available a number of drawbacks were observed. Pri-
diffractometer, natural zeolite samples contain more marily, the melt was highly viscous and too hot to
than 80% clinoptilolite + heulandite type zeolites. be used in the automatic spreader. This caused non-
This figure represents both types as the peaks given uniform thickness of the spread film and a sticking of
by these two types coincide. The resolution needs the material to the spreader blade due to the hard-
more detailed study, which is beyond the scope of ening of the material by rapid cooling. Thus, as a
this work. The results and assessment of the prod- means to hastening the process of spreading the melt
ucts prepared according to the different methods for on the flat surface as a thin film, manual operation
the manufacture of such a composite film are given of the blade was practiced. However, this was also
below. not successful, again owing to the increasing viscos-
a. Hot Pressing ity of the material by cooling. The main reason for
The films obtained by the process of embedding the failure of this method was the comparably high
ground zeolite particles with an average particle size temperature requirement of the process, i.e., around
of 74 µ on the surface of 60 µm and 100 µm thick melt temperature, whereas spreading had to be done
polyethylene films using a hot press at 100-145◦C did at room temperature with the existing spreader.
not yield a satisfactory product. This was primarily To eliminate the spreadability problem associ-
because the distribution of zeolite was not uniform ated with the phase change induced by cooling in
and the mechanical strength of the prepared films the previous method, a similar method less affected
was low where it resembled a kraft paper more than by temperature was tried. In this respect, as a suit-
a plastic film. When compared with the FH film, able solvent to dissolve polyethylene, xylene was se-
which appears to have the zeolite particles attached lected. For the necessary preliminary study the so-
to the surface by suitable means from one side of lute/solvent ratio and the temperature giving the
the film, a logical processing seemed to be spreading best solution was determined. This was obtained
hot particles on the warm softened film. However when a ratio of 1 part polyethylene per 10 parts
uniform spreading of the hot particles seemed to be xylene was used at 75◦ C. The reason for the selec-
a problem. In addition, it was not possible to ar- tion of this ratio was due to toxic nature of xylene
rive at the relevant time-temperature combination. and the neccessity that it be removed from the sys-
This was mainly because with the available manual tem. Therefore, when a homogeneous solution was
hot press it was not possible to adjust both of these obtained this ratio was choosen. Then, the other
parameters with sufficient accuracy. parameter zeolite/polyethylene ratio appeared to be

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the best when 0.1 of zeolite per gram of polyethylene successful coating of polyethylene beads, the beads
was used since zeolite amounts higher than this value should be immersed in a large amount of zeolite and
resulted in nonhomogeneous distribution. However, heated. The heating trials were done in an oven. For
the resulting mixture of the dissolved polyethylene each size group of zeolite particles used, the best re-
and zeolite was like a jelly, which again was not a sult was obtained as 3 h at 145◦ C. The mass ratio
spreadable fluid at the operation temperatures of the was high with large particles and quite low with the
spreading machine. This was most probably due to fine ones. The results as mass of zeolite per mass of
the rapid temperature drop from 75◦C to room tem- polyethylene beads at the end of 3 h at 145◦C with
perature and adsorption of some solvent by the zeo- respect to the average particle sizes of 53, 106 and
lite particles to yield a highly concentrated solution 212 µ were 1.082, 1.133 and 1.256 respectively.
of polyethylene in xylene. The resulting beads were found to be success-
Unsuccessful spreading due to solidification of the fully covered and hence were subjected to extrusion
mixture as a non-uniform layer on a plate by vapor- in an industrial extruder. However, because the ex-
izing the solvent appeared to be a suitable procedure truder was not specific for this composite material,
by which thick films, the could be obtained. To pro- the zeolite particles sedimented at the bottom and
cess these thick films into thin films hot pressing of formed aggregates that caused surface disorders. In
small strips cut from them seemed a possible solu- addition, the film was comparatively heavy for the
tion. extruders’ designed air pressure, which was not suf-
The films produced according to the above proce- ficient to blow the zeolite containing heavy films.
dure were relatively more successful than the previ- However, an intermediate zone in the extruded film
ous ones. The distribution of zeolite through the film showed promise.
was quite uniform and the obtained film was more This method was unsuccessful in terms of the loss
flexible and clear, and the thickness of the film could of material and non-uniformity of the produced films
be controlled easily by the amount of small pieces although it was an achievement in industrial appli-
to be pressed. However, because of the drawbacks cation.
of the utilization of a toxic solvent, time consump-
Although the extrusion of zeolite coated
tion and the need for additional equipment as well polyethylene beads as a film was unsuccessful, it
as provision for ventilation in the area comparatively
still was an achievement promising an improvement
giving rise to higher costs, industrial production by
with respect to thickness and uniformity. Therefore,
this method was not suitable feasible.
after discarding part of the film from both ends,
c. Coating Polyethylene Beads and Extru- the smooth intermediate zone of the extruded film
sion having uniform zeolite distribution was removed for
For industrial purposes, the idea of the employ- improvement by hot pressing.
ment of polyethylene beads in place of polyethy- The film obtained after pressing at 120◦C for 5
lene film seemed to be a more applicable process- min with the available equipment offered most of the
ing method. Thus, in further studies we planned to expected structural properties, especially flexibility
first attach zeolite particles onto the surface of the and uniformity in thickness and the distribution of
polyethylene beads and then have them extruded as zeolite particles in the film.
a film. As a means to compare the films produced by
We observed in the preliminary trials that it was the last method with the alternatives, image analy-
quite difficult to have zeolite particles attached to sis and SEM photographs were used. The images of
and kept on the surface of polyethylene beads. To the films +212 µ, +106 µ, +53 µ, FH and polyethy-
accomplish this polyethylene beads were added to a lene were magnified x10 and stored. The images of
bed of zeolite particles prepared in a revolving pan the polyethylene film purchased from the market and
and heated. Subsequent to several temperature-time that of the produced films given in Figures 1-4 ap-
studies in the pan, the best result for this method pear to be about the same. The zeolite particles can
was obtained as 1 h at 180◦ C using 53, 106 and 212 be seen on the pictures as embedded within the film
µ average sizes of the zeolite. This method was also structure. The image of the FH film (Figure 5) is
found to be unsuitable primarily because the pro- quite different from the others, implying a different
duction rate was very low. polymer structure, zeolite type and processing. The
From the previous trials we estimated that for a same results were obtained from the examination of

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SEM photographs (Figures 6-10). In addition, it can

be seen from the SEM photographs that there are no
holes between the zeolite particles and the polymer
film.

Figure 4. Film structure of polyethylene film.

Figure 1. Film structure of 212 µ film.

Figure 2. Film structure of 106 µ film. Figure 5. Film structure of FH film.

Figure 3. Film structure of 53 µ film.

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 (AKTAŞ) DİRİM, ESİN, BAYINDIRLI

Figure 6. SEM photograph of 212 µ film.

Figure 8. SEM photograph of 53 µ film.

1. Zeolite Coated Polyethylene Beads Pro-

duction
Industrially it is possible to produce such com-
posite films by using a twin-screw extruder. How-
ever, such equipment is costly to employ in research
work unless it is already available. Therefore, as an
alternative an equally effective method was deter-
mined in this study.
According to the desired production capacity, an
excess amount of ground zeolite particles of a size
smaller than 53 µ and polyethylene beads should be
placed in a tank of sufficient volume, in a ratio to
have all the beads kept buried in the zeolite par-
ticles. The tank should be suitable for continuous
Figure 7. SEM photograph of 106 µ film.
mixing and indirect heating so that its contents can
be heated to 145◦ C and kept at that temperature
In the light of the studies performed the follow- for 3 h while mixing continuously. The amount and
ing steps can be recommended for an industrial ze- purity of the raw materials are very important. The
olite containing polyethylene film production, which polyethylene beads should be pure and of high qual-
is schematically shown in Figure 11. ity. In the same manner, zeolite particles should be
composed of only one kind of zeolite so that the phys-
ical properties of the film can be easily controlled. As

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 (AKTAŞ) DİRİM, ESİN, BAYINDIRLI

an alternative design, a fluidized bed coating could

be studied.
2. Separation of the Coated Beads
The coated beads plus the excess zeolites should
go over a sieve to eliminate excess zeolite particles
for recycling.

Figure 10. SEM photograph of FH film.

Zeolites<53µ Polyethylene beads

∞
Mixing 3 h at 145°C

Figure 9. SEM photograph of PE film.

Zeolite Sieving

3. Extrusion into Film Coated Beads

The zeolite covered polyethylene beads should be
extruded through a straight die opening into a thick Extrusion
High Pressure Air
film. In the extruder, the air feed rate must be ad-
justed for such a material.
Film
4. Annealing Press
The raw film produced from the extruder should Annealing Press at 130 °C
be annealed by pressing at a specified temperature
around 130◦C and a convenient pressure depending Product Film

on the set thickness of the film so that a film with de-

sired thickness and properties can be obtained. For Figure 11. Schematic representation of the recommended
this purpose, hot rolls are recommended. process.

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 (AKTAŞ) DİRİM, ESİN, BAYINDIRLI

Conclusions life.

The present study aimed to find a suitable manu- Acknowledgments

facturing process to produce a zeolite polyethylene
composite packaging film of acceptable properties, The authors wish to express their thanks to the Sci-
which also makes use of natural Turkish zeolites. We entific and Technical Research Council of Turkey
found that such a film can be produced by extru- (TÜBİTAK) for its support in the later stages of this
sion and then annealing of zeolite-coated polyethy- study, Etibank Bigadiç Zeolite Mines Directorate for
lene beads prepared under specific conditions. How- its kindness in supplying the zeolites, Doğan Plas-
ever, for such a film to be acceptable in fruit and tik Sanayii for their efforts in the extrusion of the
vegetable packaging, additional properties increasing films, Prof. Dr. Uğur Köktürk (Mining Engineering
the shelf and storage life of the commodities are re- Department, Dokuz Eylül University) for his help in
quired. Thus, as a film combining the gas adsorptive analyzing zeolite samples and Prof. Dr. Bilgehan
property of zeolites with a very common food pack- Ögel (Metallurgical Engineering Department, Mid-
aging material, polyethylene shall be studied for its dle East Technical University) for his help in SEM
permeability to gases of interest that affect storage analysis.

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