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mechanical, optical,
printing, and flex-crack
properties of the
polyvinylidene chloride
coated biaxially
oriented polyethylene
terephthalate films
Abstract
This paper discusses a new method for development of transparent high barrier
biaxially oriented polyethylene terephthalate film via offline coating method. In the
present research, a more efficient coating method was employed which reduces
the cost of the developed film by 30–35% and minimizes the energy consumption
and saves the processing time of the film. Biaxially oriented polyethylene tereph-
thalate film was corona treated or chemically coated during processing thus elim-
inating one process step. Further, biaxially oriented polyethylene terephthalate
film was offline coated by polyvinylidene chloride dispersion for high barrier
properties and then laminated with polyethylene. Processing parameters, polyvi-
nylidene chloride coating formulations, and primer type were optimized based on
the coating feasibility, laminate bond strength, barrier properties, and ink adhesion
New Product Development, SRF Limited, Packaging Film Business, Indore, India
Corresponding author:
Akshay N Maikap, New Product Development, SRF Limited, Packaging Film Business, Indore, India.
Email: Akshay.Narayan@srf.com
Maikap et al. 159
Keywords
Biaxially oriented polyethylene terephthalate film, barrier properties, primer coat-
ing, lamination, polyvinylidene chloride coating
Introduction
Biaxially oriented polyethylene terephthalate (BOPET) films are a substrate
of choice for food packaging industry because of their excellent mechanical
and optical properties. High barrier protection against aroma, gas, and mois-
ture provides extended shelf life to the packaged food such as tea, coffee
powder, spices, meet, dairy product, alcoholic drink, sauces, snacks, biscuits,
etc. Food packaging film should have various requisites, i.e. protection
of food product from the loss of nutrients, functional properties,
color, aroma in order to preserve the taste and its appearance which is
expected by customers. Another function of package is transportation of
the product in a convenient manner, esthetic look, and clear information
about the product to consumer. To be used in packaging applications,
a polymer needs attributes such as high mechanical strength, thermal proper-
ties, transparency, barrier properties, and surface characteristics. High bar-
rier properties in polyethylene terephthalate (PET) film are generally
achieved by coating an aluminum layer using vacuum web metallization.
Oxygen transmission rate (OTR) in BOPET film is in the range of 120–
140 cc/m2/day and reduced down to 0.5–1 cc/m2/day in case of metalized
BOPET film. The major drawback in metalized BOPET film is lack of
transparency after metallization; hence film cannot be used for see through
packaging. Also metalized BOPET film has very poor flex crack resistance
which leads to pin holes after flexing which leads to inferior barrier properties
of the film.
Another method developed for high barrier see through packaging is coat-
ing of metal oxide, i.e. aluminum oxide (AlOx) or silicon oxide (SiOx) on the
BOPET film substrate, which offers a very high barrier against aroma, gas,
and moisture.1–3 However, the major drawback of metal oxide coated film is
160 Journal of Plastic Film & Sheeting 31(2)
lower flex crack resistance which leads to poor barrier properties. Also the
vacuum metallization process for metal oxide coating needs very high invest-
ment on equipments. Another method for barrier properties improvement of
BOPET films is mixing of nanoclay filled masterbatch via melt blend tech-
nique.4 Mixing of nanoclay into polymer matrix is associated with major
challenge, i.e. dispersion of nanoclay and to achieve intercalation/exfoliation
of clay platelets in the polymer matrix.
An alternative technique to develop transparent high barrier BOPET film
is coating of polyvinylidene chloride (PVDC) dispersion on the BOPET film
substrate. PVDC is one of the oldest and most widely used high barrier resins.
Coating PVDC dispersion on BOPET film can offer significant reduction in
OTR (4–8 cc/m2/day) as well as retaining transparency of the film.
Maximum barrier protection is achieved by a thin coating of PVDC copoly-
mer on the substrate film providing reduced permeability to oxygen and water
vapor. The film may be used for food packaging as well as for other appli-
cations such as cigarettes wrappers, lamination for boxes, and medicines.
With increasing PVDC latex concentration in coating solution, oxygen and
water vapor transmission rate (OTR, WVTR) value decreases. In contrast,
heat sealing, toughness, and flexibility properties decrease with increasing
vinylidene chloride concentration in PVDC coating solution.5,6
Conventional coating techniques such as gravure coating, dip coating, and
blade coating can be selectively employed for PVDC coating.
Advantages of PVDC coated BOPET film is transparency, high barrier,
excellent flex crack resistance as well as excellent abrasion resistance and
scratch resistance during processing. Another advantage of PVDC coated
BOPET film is suitability for high resolution graphic printing and lamination
process, thermal stability, and excellent processability. Consumption of
PVDC coated BOPET film is growing every year and the current global
demand of PVDC coated BOPET film is estimated as 2000–3000 MT/year.
PVDC coated BOPET film is currently used in laminated stand pouches
which are being used for packaging of high fatty acid content food, i.e.
baked food, chocolates, olives, etc.
However, the challenges in the PVDC coated BOPET film process is to get
good adhesion between the BOPET film substrate with PVDC. Thus, a
detailed research with varying primer coating or surface treatment on
BOPET film before PVDC coating is desired. Suitable primers for increased
adhesion with PVDC are possibly cross-linked polyurethane (PU) and copo-
lyesters which can form secondary bondage with chloride group of PVDC and
offer increases adhesion of PVDC with BOPET film. Another possible method
for increased adhesion between PVDC and BOPET film substrate is modifying
surface properties of BOPET film by corona treatment which leads to increase
in surface roughness (dyn/cm) of the film. Conventional method of developing
Maikap et al. 161
PVDC coated BOPET film is a complex three step process. Where in the first
step, BOPET film is manufactured followed by offline primer coating. After
that offline PVDC coating was done on BOPET film substrate. This three step
procedure is time-consuming process and requires very high energy consump-
tion, high oven temperature for drying of primer, and high processing time.7–18
The aim of this research work is to develop transparent high barrier
BOPET film via offline PVDC coating method with elimination of one pro-
cess step. In process development, one step of offline primer coating is elimi-
nated which can reduce the cost of the developed film up to 30% thereby
minimizing the energy consumption and also saved the process time by 25–
30%. Also, inline coating of primer before transverse direction orienter
(TDO) zone offers faster drying of the primer because TDO zones are
equipped with high velocity blowers and have high temperature setting that
is suitable for drying of primer. PVDC concentration in offline coating solu-
tion and primer type was varied and their corresponding effect on barrier
properties and other film properties was noted and discussed with detailed
description. The developed film was laminated with polyolefins, i.e. polyethyl-
ene (PE) or cast poly propylene and properties of the laminates were
investigated.
Materials
PET resin was synthesized in-house from purified terephthalic acid (PTA) and
monoethylene glycol (MEG) by polycondensation reaction at 260–280 C, in
presence of catalyst. PTA was purchased from Samsung, Korea and
Indorama, Thailand. MEG was purchased from Chemical India Company
(CIC), India. Properties of PTA and MEG are listed in Tables 1 and 2,
respectively.
162 Journal of Plastic Film & Sheeting 31(2)
Formula HO–CH2–CH2–OH
Mol. wt. (g/mol) 62.069
Purity (wt%) 99.90 min
Appearance Transparent, liquid
pH 6.50–7.50
Acid number (mg KOH/g) 0.01 max
Refractive index @ 20 C (%) 1.4318–1.4320
Density @ 20 C (g/cc) 1.1130–1.1140
Moisture content (%) 0.10 max
DEG content (%) 0.10 max
Ash content (ppm) 5 max
Boiling point range (5%, 95%) ( C) 197 min, 199 max
UV transmittance:
At 220 nm (%) 70 min
At 250 nm (%) 85 min
At 275 nm (%) 95 min
At 350 nm (%) 98 min
Maikap et al. 163
In-house developed PET resin has three types: additive PET resin, recycle
PET resin, and bright PET resin. Additive PET resin contains 0.4 wt% of
silica additive which provides antiblocking characteristics to the PET film.
Recycle PET resin is reextruded PET which is obtained from trimming waste
of PET film. Bright resin is virgin PET resin, without any additive. Resin
properties of bright, recycle, and additive PET resin are listed in Table 3.
Methods
Processing of BOPET film
BOPET film was processed by sequential biaxial stretching consisting of feed-
ing section, extrusion system followed by a casting unit, machine direction
orienter (MDO), inline coater, TDO, take-up and transfer section, and
winder. Coextruded BOPET film has three layered structure where each
layer consists of varying concentration of three different grades of polyester
resin (bright PET, recycle PET, additive PET resin). Feeding composition of
bright, recycle, and additive PET resin in twin screw extruder is listed in
Table 5.
Polyester resin melted in the extruders and then transferred to the three
layer extrusion die, the output of which is a three-layer film. The middle layer
is formed by the throughput of the main extruder while the throughput of the
coextruder 1 and 2 forms the two outer layers. Additive resin (silica content
0.4 wt%) offers antiblocking characteristics to the film during unwinding and
provides necessary friction in the film. The film coming out from the die falls
on chill roll, which is maintained at the temperature of around 25–30 C. The
film coming out of chill roll is called cast film. Cast film was stretched in two-
stage process (two gaps) to provide excellent mechanical properties and ther-
mal stability. In first stage, cast film enters into the MDO and stretched
(stretch ratio ¼ 3.2–3.5) in the machine direction (MD) and called as mono
film. Temperature profile in the MDO zones was in the range of 78–90 C.
Maikap et al. 165
reducing a process step, thus minimizing the energy consumption and mini-
mizing the process time for film development which is critical requirement for
industrial applications. Inline primer coating method has eliminated one pro-
cess step and reduced the final cost of the film by 30%. Also copolyesters and
PU-based primers are water soluble and free from any solvent related haz-
ards. This primer coating was done after stretching of the mono film in MDO
and before passing the film into TDO. TDO zones offer faster drying of the
primer coating due to their higher temperature setting and high air velocity.
Three different types of primer were coated on BOPET mono film. These are
aqueous solution of copolyester resins and PUs dispersion. These primers
offer excellent printability of BOPET film to various grades of inks, i.e.
vinyl ester, nitrocellulose, and PU-based inks. Also these primers are suitable
for solvent free as well as solvent-based adhesives used in lamination process.
Expt. no Film code PVDC (wt%) Water (wt%) Wax (phr) Sylobloc 45 (phr)
1. PT – – – –
2. PT-VC20 20 80 0.20 0.06
3. PT-VC30 30 70 0.40 0.12
4. PT-VC40 40 60 0.60 0.18
5. PT-VC50 50 50 0.80 0.24
6. PR – – – –
7. PR-VC20 20 80 0.20 0.06
8. PR-VC30 30 70 0.40 0.12
9. PR-VC40 40 60 0.60 0.18
10. PR-VC50 50 50 0.80 0.24
11. PC – – – –
12. PC-VC20 20 80 0.20 0.06
13. PC-VC30 30 70 0.40 0.12
14. PC-VC40 40 60 0.60 0.18
15. PC-VC50 50 50 0.80 0.24
16. PS – – – –
17. PS-VC20 20 80 0.20 0.06
18. PS-VC30 30 70 0.40 0.12
19. PS-VC40 40 60 0.60 0.18
20. PS-VC50 50 50 0.80 0.24
21. PV – – – –
22. PV-VC20 20 80 0.20 0.06
23. PV-VC30 30 70 0.40 0.12
24. PV-VC40 40 60 0.60 0.18
25. PV-VC50 50 50 0.80 0.24
PC: primer coating of copolyester WB-630 on BOPET film; phr: parts per hundred; PR: corona treated
BOPET film; PS: primer coating of copolyester WB-730 on BOPET film; PT: plain transparent BOPET
film (no treatment/primer coating); PV: primer coating of polyurethane on BOPET film.
Barrier properties
OTR of PVDC coated BOPET film was evaluated according to ASTM D3985
method by using MOCON OX-TRANÕ 2/21 at the test condition of 23 C
and 0% relative humidity (RH). WVTR of PVDC coated BOPET film was
evaluated according to ASTM F372 method by using MOCON
PERMATRAN-WÕ 3/33 at the test condition of 37 C and 90% RH.
Tensile properties
Tensile properties (tensile strength, tensile modulus, and % elongation) of
PVDC coated BOPET film was measured by using Tinius Olsen HD/WK
tensile tester, model H5KT according to ASTM D882 method.
Thermal shrinkage
Thermal shrinkage of the PVDC coated BOPET film was measured
according to ASTM D2838 test method. Samples were cut in the required
size (length ¼ 254 mm, width ¼ 254 mm) from different areas of the film.
Initial sample dimensions were measured and marked in MD and TD on
the film sample. Sample was placed in an oven at 150 C temperature for
30 min. Sample was removed and then allowed to cool at room tempera-
ture. Final sample dimensions in MD and TD were measured and the %
shrinkage in the film was calculated.
Optical properties
Haze (%) and transmittance (%) of the PVDC coated BOPET film was
measured by using haze guard from BYK Gardner USA, model No-4725,
according to ASTM D1003 method. Light that is scattered upon passing
through a film can produce a hazy or smoky field when objects are viewed
through the material. Transmittance (%) is the fraction of incident light at a
specified wavelength that passes through the sample.
Dyne test
Dyne test is used for the measurement of surface energy (dyn/cm) or wetting
tension. Test was done according to ISO8296. In the test various inks of
different dyne values were applied to the film surface to check the film’s sur-
face tension.
Maikap et al. 169
Ink test
Ink test was used to analysis the printability and bond strength of PVDC
coated BOPET films. A film sample of 30 cm 30 cm was cut and vinyl based
ink was drawn on the sample with the help of bar coater followed by drying
for 10 min. Tape test was done on the ink coated side by using 3M scotch
tape. The test is considered passed if there is no ink transfer from the film
surface to the 3M scotch tape.
Supplier Bostik India Pvt. Ltd Henkel, India Bostik India Pvt. Ltd
End group –OH group –OH group –N ¼ C ¼ O group
Solid content (%) 80 2 80 2 75 2
Solvent Ethyl acetate Ethyl acetate Ethyl acetate
Viscosity (mPa s) 4000–6000 3000–6500 100–700
Mixing ratio (parts by wt) 100 100 15
Figure 4. Barrier properties and coating thickness as a function of gravure roll mesh
size.
Figure 4 shows that with increased gravure roll mesh size, coating thick-
ness decreased and OTR and WVTR values increased. Thus, in order to
obtain high barrier (lower transmission rate), gravure roll of lower mesh
size (120 lines/in.) was selected. PVDC coated BOPET film was kept at 45–
50 C for 2–60 days for curing. With increased curing time, barrier properties
improved due to decrease in WVTR value. Increased curing time allows
higher cross-linking of PVDC resin and hence increased adhesion of PVDC
to primer coated BOPET film. WVTR value was leveled off after 7–12 days of
curing time. Thus, optimized curing time for PVDC coating was 7 days. Effect
of curing time on OTR and WVTR of PVDC coated BOPET film is shown in
Figure 5.
172 Journal of Plastic Film & Sheeting 31(2)
Figure 5. Effect of curing time on barrier properties of PVDC coated BOPET film
(where primer coating was polyurethane and PVDC concentration in coating solution
was 40 wt%).
Barrier properties (OTR and WVTR) of PVDC coated BOPET films are
presented in Figures 6 and 7, respectively.
Maikap et al. 173
Figure 6. OTR with increased PVDC concentration for various primer coated
BOPET film.
Figure 7. WVTR with increased PVDC concentration for various primer coated
BOPET film.
174 Journal of Plastic Film & Sheeting 31(2)
Figures 6 and 7 show that OTR and WVTR decreased with increased
PVDC concentration in coating solution. Also, different types of primer coat-
ing (copolyester resins and PU) have no significant difference in OTR and
WVTR values. Correlation of PVDC coating thickness (g/m2) with increased
PVDC concentration and OTR and WVTR of the film is presented in Table 8.
It can be seen from Table 8 that with increase in coating thickness, OTR and
WVTR decreased. Thus, barrier properties were improved with increased
coating thickness (g/m2) of the film. However, 40 wt% of PVDC concentra-
tion was selected as optimized concentration for coating process. Higher
PVDC concentration in coating solution leads to very high viscosity of the
solution and does not provide uniform coating. Very low PDVC concentra-
tion in coating solution did not offer significant increase in barrier properties.
Thus PVDC concentration in coating solution was varied above 20% and
below 50%.
Table 8. Resultant properties of various primers treated and PVDC coated BOPET film.
Tensile properties
Tensile properties of PVDC coated BOPET films were measured in MD and
TD and results are presented in Figure 8(a) to (d).
Figure 8. (a) Tensile strength in machine direction for PVDC coated BOPET films,
(b) tensile strength in transverse direction for PVDC coated BOPET films, (c) elongation
at break (%) in machine direction for PVDC coated BOPET films, and (d) elongation at
break (%) in machine direction for PVDC coated BOPET films. PC: primer coating of
copolyester WB-630; PR: corona treated; PS: primer coating of copolyester WB-730;
PT: plain BOPET film (no primer coating); PV: polyurethane primer coating on BOPET
film.
178 Journal of Plastic Film & Sheeting 31(2)
Figure 8. Continued.
Maikap et al. 179
Figure 8(a) and (b) shows the tensile strength of PVDC coated BOPET
films in MD and TD, while Figure 8(c) and (d) shows the % elongation at
break of PVDC coated BOPET film in MD and TD. It was observed that
increase in PVDC latex concentration in coating solution shows no significant
change in tensile strength and elongation of the BOPET film and results are
similar within the limit of standard deviation. It was also observed from
Figure 8(a) to (d) that tensile strength and elongation were almost similar
for the different primer coated films (copolyester and PU). Thus, PVDC con-
centration, coating thickness, and primer types are not adversely affecting the
BOPET film properties.
Thermal shrinkage
Thermal shrinkage (heat shrinkage) of the PVDC coated BOPET films was
measured at 150 C for 30 min, in MD and TD of the film and values are listed
in Table 8. Percentage shrinkage of the PVDC coated BOPET films was in the
range of 2.2–2.8% in MD and 0.1–0.6% in TD. Heat shrinkage value did not
change significantly with increased PVDC concentration (wt%) and coating
thickness.
Optical properties
Optical properties (% haze and % transmittance) of the PVDC coated
BOPET films were measured in MD and TD and results are shown in
Table 8 and Figure 9. Haze (%) was in the range of 3.0–6.9% for the film.
Percentage haze values were increased with increased coating thickness due to
higher PVDC concentration in coating solution. Table 8 also shows that haze
values did not change much with varying primer coating (copolyester and PU)
on BOPET film. Transmittance of PVDC coated BOPET films was in the
range of 90.0–90.1%.
180 Journal of Plastic Film & Sheeting 31(2)
Figure 9. Haze (%) in PVDC coated BOPET film. PC: primer coating of copolyester
WB-630; PR: corona treated; PS: primer coating of copolyester WB-730; PT: plain
BOPET film (no primer coating); PV: polyurethane primer coating on BOPET film.
Dyne test
Surface tension (dyn/cm) of PVDC coated BOPET film was measured and
results are listed in Table 8. PT grade film (without any surface treatment) has
very low value of surface tension (44 dyn/cm). Surface tension was increased
in corona treated and primer coated BOPET films. Increase in surface tension
in the primer coated film offers improved adhesion of PVDC coating to the
BOPET film substrate. Further PVDC coating on corona treated/primer
coated BOPET film has increased the surface tension value and it was
observed in the range of 68–72 dyn/cm. An increase in dyne value leads to
good printability in the BOPET films.
Bond Ink
Gelbo flexing OTR WVTR strength transfer to Laminate
Film type (number) (cc/m2/day) (g/m2/day) (g/25 mm) LDPE side structure
Table 9 shows laminate bond strength after gelbo flexing for PVDC coated
BOPET film. PS-40 (primer coating ¼ copolyester WB-730, PVDC concentra-
tion ¼ 40 wt%) film has highest bond strength of the laminate (230–245 g/
25 mm) compared to other primer coated BOPET film. High bond strength
in PS-40 film may be due to secondary bond formation between sulphonic
group present in WB-730 and chlorine group present in PVDC.
182 Journal of Plastic Film & Sheeting 31(2)
OTR and WVTR of laminate are shown in Figures 10 and 11, respectively.
OTR and WVTR values of the PS-40-based laminate were 6.0 0.1 cc/m2/day
and 4.5 0.1 g/m2/day, respectively. Laminate made from PS-VC-40 grade
BOPET film (primer coating ¼ copolyester WB-730, PVDC concentra-
tion ¼ 40 wt%) showed good printability (no ink transfer) and no
delamination.
Figure 10. OTR of laminate with increased number of gelbo flexing. PC: primer coating
of copolyester WB-630 on BOPET film; PR: corona treated BOPET film; PS: primer
coating of copolyester WB-730 on BOPET film; PT: plain transparent BOPET film (no
treatment/primer coating); PV: primer coating of polyurethane on BOPET film; VC-40
refers to the 40% concentration of PVDC in the coating solution.
Maikap et al. 183
Figure 11. WVTR of laminate with increased number of gelbo flexing. PC: primer
coating of copolyester WB-630 on BOPET film; PR: corona treated BOPET film; PS:
primer coating of copolyester WB-730 on BOPET film; PT: plain transparent BOPET film
(no treatment/primer coating); PV: primer coating of polyurethane on BOPET film; VC-
40 refers to the 40% concentration of PVDC in the coating solution.
Conclusions
In the present study a detailed method for development of offline PVDC
coated BOPET film was discussed. Present invention has following advantage
over conventional method of PVDC coated BOPET film development:
neat BOPET film and values were observed as 6–7 cc/m2/day (OTR) and 3–4 g/
m2/day (WVTR). Barrier properties were studied with increased curing time and
optimized curing time for 6 days. Different types of primer (copolyesters and
PUs) were coated on the BOPET film before PVDC coating and observed that
copolyester primer coated BOPET film has high laminate bond strength and ink
adhesion properties compared to the PU primer coated film. Based on the OTR
and WVTR and process capability the optimized PVDC concentration in coat-
ing solution was observed as 40–42 wt% for further production of the film.
Funding
This research received no specific grant from any funding agency in the public, com-
mercial, or not-for-profit sectors.
Conflict of interest
None declared.
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Biographies
Akshay N Maikap received his M.Tech. in Polymer Science and Technology
from Centre for Polymer Science and Engineering, I.I.T. Delhi. Currently, he
is working as Associate Vice President (New Product Development) in SRF
Limited (Packaging Film Business), Indore, India. He has 17 years work
experience in processing, characterization, and development of various spe-
cialty films for packaging applications.
Shikha Jain received her PhD in Polymer Science from Centre for Polymer Science
and Engineering, India Institute of Technology, Delhi, India. She has one year
research work experience as senior executive (New Product Development) in SRF
Limited, Indore, India. She has 5+ years academic research experience in polymer
processing, specialty coatings, nanocomposites, characterization and testing,
blends and structure properties correlation for material development.
Hari K Singh received his B.Tech. in Chemical Engineering from IIT (BHU),
Varanasi. He is currently working as Sr. Vice President, Global Manufacturing
Head and Country Head, Thailand. He is having 20þ years work experience is
BOPET film processing, coating, and specialty films for packaging applications.
Ashish Gupta received his B.E. in Polymer Science and Chemical Technology
from Delhi Technological University (Formerly Delhi College of
Engineering). He is currently Manager (New Product Development) in SRF
Limited (Packaging Film Business), Indore, India. He has four years’ experi-
ence in packaging film production and new product development.