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Effects of additives on fusion parameters of rigid PVC formulations

Article in Journal of Vinyl and Additive Technology · June 2008

DOI: 10.1002/vnl.20148

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Effects of Nanoclay and Additives on the
Fusion Characteristics and Thermal Stability
of Poly(vinyl chloride) Nanocompounds
Mehdi Moghri,1 Masis Akbarian2
1
Engineering Department, Islamic Azad University, Kashan Branch, Kashan, Iran
2
Polymer Engineering Department, Amirkabir University of Technology, Tehran, Iran
The effects of varying amounts of organically modified
nanoclay (NC), calcium stearate (Ca.St.), stearic acid
(St.Ac.), and an impact modifier (IM) on the fusion char-
acteristics of a rigid Poly(vinyl chloride) (PVC) nano-
compound were investigated by using the L9 orthogo-
nal method of experimental design. The materials
showed varying effects on the fusion parameters.
Thus, while the fusion time was lowered and the fusion
factor increased by NC, Ca.St., and IM, the reverse
was true with St.Ac. Effects on the minimum and maxi-
mum viscosities of formulations also varied with mate-
rial type. The behavior of the materials is discussed in
terms of their effects on the transformation of PVC
grains. Thermal stability and color change were sensi-
tive to NC content. J. VINYL ADDIT. TECHNOL., 15:92–98,
2009. ª 2009 Society of Plastics Engineers
INTRODUCTION
Polymer-(layered silicate) nanocomposites represent an
important class of engineering materials that have attracted
considerable attention from academic and industrial
researchers in the past few decades [1–3]. The increasing
interest in these materials is due to remarkable improve-
ments in some properties compared with those of the virgin
polymers and conventional particulate-filled microcompo-
sites, such as superior mechanical properties, gas perme-
ability, and flame retardancy. Sodium montmorillonite
(Naþ-MMT) is a type of clay with a layered silicate struc-
ture containing positively charged sodium ions within inter-
layers, and it is widely used as a reinforcement filler in pol-
ymers. To achieve increased properties, it is very important
for polymer molecules to enter the interlayers (intercala-
tion) and to separate the silicate layers (exfoliation), so as
to finely disperse the individual 1-nm thick sheets at the
nanoscale and strengthen the interfacial interactions
Correspondence to: Mehdi Moghri; e-mail: moghri@gmail.com
DOI 10.1002/vnl.20182
Published online in Wiley InterScience (www.interscience.wiley.com).
Ó 2009 Society of Plastics Engineers
JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—
—2009
between them and the polymer matrix. The inorganic lay-
ered silicate, however, is hydrophilic, and polymers are
mostly hydrophobic, so that in most cases, MMT-polymer
compatibility is not good enough for the polymer chains to
intercalate into the MMT galleries. To solve this problem,
inorganic MMT is always modified with compounds such
as alkyl quaternary ammonium salts [4, 5] by exchanging
the Naþ ions for cationic organic molecules.
Poly(vinyl chloride) (PVC) is a widely used thermo-
plastic polymer, and PVC-clay nanocomposites have been
prepared by melt blending using both Naþ-MMT and
organophilic montmorillonite (O-MMT). With Naþ-MMT
clay, the polarity of the PVC molecules permits the par-
tial insertion of PVC chains into the silicate interlayers,
thereby increasing the possibility of polar interaction
between electronegative chlorine atoms and Naþ ions
within the interlayer, but without exfoliation of the sili-
cate layers [6]. During the melt processing of polymer/O-
MMT nanocomposites, however, the silicate layers are
separated by the bulky alkylammonium compounds and
are better dispersed in the polymer matrix on the molecu-
lar level. Thus, because of the nanoscale effects, polymer/
O-MMT nanocomposites often exhibit more dramatic
improvements in mechanical and thermal properties than
their polymer/Naþ-MMT counterparts [7, 8]. This differ-
ence is attributed to the existence of partially intercalated
and partially exfoliated silicate layers in the polymer/O-
MMT composites, as compared with the partially interca-
lated and partially unexfoliated and disordered structures
found in polymer/Naþ-MMT composites [9], as shown by
X-ray diffraction and transmission electron microscopy
studies. A high degree of silicate-layer exfoliation, fol-
lowed by uniform and homogeneous dispersion of indi-
vidual silicate layers at the nanoscale within the polymer
matrix, is, therefore, a prerequisite for the formation of
authentic nanocomposites. These conditions are achieva-
ble with proper polymer and O-MMT combinations and
blending conditions. On the other hand, as in the case of
polymer/Naþ-MMT composites, silicate layers are not
 TABLE 1. Levels of variable parameters. TABLE 3. PVC formulation.

Ingredient Level 1 (phr) Level 2 (phr) Level 3 (phr) Ingredient Parts

Nanoclay 2 4 6 PVC-S (K-65) 100

Calcium stearate 0.2 0.4
Impact modifier 6 8
Stearic acid 0.1 0.3
separated, and the clay particles are mainly microdis-
persed, rather than nanodispersed, within the matrix.
In its powder form, PVC shows a variety of levels of
morphology [10]. Powder particles known as grains are
irregular in shape and are about 150 lm in diameter. Each
grain consists of many primary particles about 1 lm in
diameter, as well as some aggregates [11–13]. These pri-
mary particles are loosely packed together, porous, and com-
posed of domains 0.1 lm in diameter. In processing, grain
boundaries are eliminated, and primary particles are com-
pacted together. After significant interdiffusion, submicro-
particle boundaries disappear, and a three-dimensional net-
work of polymer chain entanglements is formed. This pro-
cess is referred to as the fusion or gelation of PVC [14],
which is accomplished during processing through the com-
bined action of heat, pressure, and shear and guides the proc-
essor to achieve a product with good mechanical properties.
Although of significant importance, little attention has
been directed in the literature to the influence of Naþ-
MMT and O-MMT on fusion characteristics and to the
simultaneous effects of additives on the state of fusion of
rigid PVC nanocomposites. Thermal stability studies,
however, have been adequately reported. Chen et al. [7]
have shown that the fusion time and temperature of rigid
PVC/Naþ-MMT nanocomposites decrease with increasing
Naþ-MMT content, whereas the reverse is true with rigid
PVC/O-MMT composites.
In our previous work [15], we reported the effects of
various heat stabilizers and lubricants on the fusion
parameters of rigid PVC formulations. In this article, we
present the results of our study on the effects of O-MMT
and some formulation additives on the fusion characteris-
tics and thermal stability of rigid PVC/O-MMT nanocom-
posites, using the L9 orthogonal array of the Taguchi
method of experimental design.
TABLE 2. L9 orthogonal array of variable parameters.
0.6 Tribasic Pb sulphate 0.8
10 Dibasic Pb stearate 0.5
0.5 Neutral Pb stearate 0.3
Calcium stearate 0.2–0.6
Stearic acid 0.1–0.5
Impact modifier 6–10
Nanoclay 2–6
EXPERIMENTAL
Materials
Suspension grade PVC of K-value 65, designated as
Vestolite S6558 and manufactured by Bandar-e-Imam pet-
rochemicals, Iran, with a weight-average molecular
weight of 90,000 and a number-average molecular weight
of 40,000 was used. The acrylic impact modifier (IM),
Paraloid KM-355, was a product of Rohm and Haas, Ger-
many, and the nanoclay (NC) was Nanofil19 that was
produced by Southern Clay Products, a subsidiary of
Rockwood Specialities, and organically modified by stear-
ylbenzyldimethylammonium chloride. All other ingre-
dients were commercial-grade products.
Design of Experiments
The application of design of experiments requires care-
ful planning, screening, prudent layout of the experiments,
and expert analysis of results. A standard statistical
method for the analysis of variance is used to determine
the reliability and accuracy of the experimental findings.
Through evaluation and screening of the effecting
parameters, it was decided to study the effects of varying
amounts of NC, stearic acid (St.Ac.), calcium stearate
(Ca. St), and IM as four design parameters at three levels,
using the appropriate 9-trial L9 orthogonal array design.
DesignExpert software (Version 7.0.2) was used for ana-
lyzing the results. Table 1 shows the different levels of
the variable parameters used in this study, and the L9 or-
thogonal array is shown in Table 2(phr ¼ parts by weight
per hundred parts of resin).

Nanoclay Calcium stearate Impact modifier Stearic acid

Run (phr) (phr) (phr) (phr)

1 2 0.2 6 0.1
2 2 0.4 8 0.3
3 2 0.6 10 0.5
4 4 0.2 8 0.5
5 4 0.4 10 0.1
6 4 0.6 6 0.3
7 6 0.2 10 0.3
8 6 0.4 6 0.5
9 6 0.6 8 0.1
FIG. 1. Effect of NC content on minimum torque.

DOI 10.1002/vnl JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—

—2009 93
 FIG. 2. Effect of NC content on maximum torque.
Preparation of Samples With Variable Formulation
Samples with variable ingredient contents were pre-
pared in a laboratory high-speed mixer. The PVC formu-
lation and the ranges of materials used, in phr, are shown
in Table 3. All ingredients were poured into the mixer
simultaneously and mixed for about 1 min to obtain the
dry blends. To study the fusion behavior of the mixtures,
the dry blends were processed at 1808C and 60 rpm for 5
min in a Brabender Plasticorder, Model PLV 153,
equipped with a 65-cc mixing chamber. The plastograms
were then evaluated to determine the effects of the formu-
lation ingredients on fusion.
Evaluation of Fusion Parameters
The method of evaluation of the fusion parameters is
based on the determination of fusion torque and, there-
after, the fusion level of the PVC formulations. The re-
sistance given by the test material against the rotating
blades in the measuring head is monitored as a measure
of viscosity. Details of plastogram features are described
in our previous work [15].
The fusion evaluation method used in the present study
is based on that of Muller [16].
The fusion quotient is defined as
Q ¼ B=A (1)
where Q is the fusion quotient, B is the maximum torque
after introduction of the dry blend (fusion peak) in m
g,
FIG. 3. Effect of NC content on fusion time.
94 JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—
—2009
FIG. 4. Effect of NC content on fusion factor.
and A is the minimum torque after introduction of the dry
blend in m
g. The fusion power effect, L, in m
g/min, is a
measure of fusion rate given by
L ¼ B=C (2)
where C is the time interval from introduction of the dry
blend to maximum torque (fusion time) in min. The
fusion factor, F, in m
g/min, is calculated from
F ¼ Q
L ¼ B2 =A
C (3)
By taking into account the viscosity ratio (Q) as well as the
fusion rate (L), fusion factor can be a useful parameter for
evaluating the efficiency of additives in promoting PVC
fusion. Higher values of F should indicate higher efficiency.
Evaluation of Thermal Stability
Thermal stability of melt-compounded formulations
was measured in static air by determining the time
required for color change of an indicator paper, due to
HCl release, at 2108C in a small glass tube.
RESULTS AND DISCUSSION
Figures 1–4 show the effects of varying amounts of
NC on minimum and maximum torques, fusion time, and
fusion factor. A sharp increase in fusion factor and a
reduction in fusion time are observed, while minimum
FIG. 5. Effect of Ca.St. content on minimum torque.
DOI 10.1002/vnl
 FIG. 6. Effect of Ca.St. content on maximum torque.
and maximum viscosities, as represented by minimum
and maximum torque values, show a steady increase with
NC loading. A change in NC content from 2 to 6 phr
results in a fusion factor increase from 378 to 1550 m
g/
min which is a 310% improvement. Additionally, fusion
time is reduced from 1.63 to 0.4 min in this range of NC
content.
The effect of Ca.St. on fusion behavior is less dramatic,
as shown in Figs. 5–8. If the amount of Ca.St. is increased
from 0.2 to 0.6 phr, the fusion factor shows an increase of
only 60%, with fusion time decreasing from 1.2 to 0.9 min,
after which it remains constant. The rates of increase in the
minimum and maximum torques with Ca.St. content are
also less pronounced. It is an obvious conclusion that both
Nc and Ca.St. are compatible with PVC and therefore
enhance grain fusion, which increases fusion level. From a
fusion perspective, the materials, therefore, may be classi-
fied as ‘‘internal’’ lubricants. However, the higher decrease
in fusion time and increase in fusion factor with NC are in-
dicative of its higher compatibility with PVC and, conse-
quently, its greater enhancement of grain fusion. Being
organically modified for good compatibility with PVC, NC,
in addition to its major role as an excellent reinforcing
agent, can also act as an efficient fusion promoter, given an
appropriate PVC formulation.
The increases in minimum and maximum fusion tor-
ques with increasing NC and Ca.St. content may be due
to decreases in the fusion temperature of the compounds
FIG. 7. Effect of Ca.St. content on fusion time.
DOI 10.1002/vnl
FIG. 8. Effect of Ca.St. content on fusion factor.
when the amounts of the materials are increased. Decreas-
ing fusion temperature results in increasing melt viscosity
of the PVC compounds.
The observations with NC in the present study are con-
trary to results reported by Chen et al. [7] in which the
fusion time and temperature of rigid PVC/O-MMT com-
posites were seen to increase, and melt viscosity
decreased, with increasing O-MMT content, whereas the
reverse was true with rigid PVC/Naþ-MMT nanocompo-
sites. The authors tried to explain the reason for this
behavior by suggesting that in the PVC/O-MMT nano-
composites, the organic modifier of O-MMT functions
more as a very effective internal lubricant that decreases
the frictional energy generated among the PVC particles
or between the PVC and O-MMT particles. The effective
fusion is thus prolonged, thereby increasing formulation
temperature and decreasing melt viscosity. The O-MMT
is shown to be partially intercalated and partially exfoli-
ated in the composite. In contrast, large quantities of polar
hydroxyl groups and silica-oxygen layers existing on the
surface of Naþ-MMT layers make the NC polar, thus
increasing its interaction with PVC chains and the friction
between the materials, thereby resulting in enhancement
of the fusion process. The Naþ-MMT is observed to be
partially encapsulated and partially intercalated in its
composites.
While the argument may be credible, it should be
pointed out that the above observations are related to
PVC formulations containing IM, liquid alkyltin heat sta-
FIG. 9. Effect of St.Ac. content on minimum torque.
JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—
—2009 95
 FIG. 10. Effect of St.Ac. content on maximum torque.
FIG. 12. Effect of St.Ac. content on fusion factor.

bilizer, and some known fusion retarders. Thus, the net

lower energy input attributable to lower friction of the
result in PVC/O-MMT composites could be a reduction in
polymer melt. This behavior, however, is sensitive to
the fusion-promoting capability of the O-MMT compo-
St.Ac. content and to the presence of other ingredients, as
nent. In contrast, lead-based heat stabilizers consisting of
seen in the slow decrease in fusion time (Fig. 11) and the
tribasic lead sulfate (TBLS) and dibasic lead stearate
increase in fusion factor in the 0.3–0.5 phr range (Fig.
(DBLS) and low levels of fusion-retarding ingredients
12). In the light of its overall effect on fusion, St.Ac.
constitute the features of the PVC formulations utilized in
could be regarded as an ‘‘internal-external’’ lubricant, i.e.,
the present study. The fusion-promoting behavior of NC
a fusion promoter as well as a retarder.
observed may, therefore, be a consequence of interactions
Effects of different amounts of IM on the fusion
among ingredients and possible synergistic reactions. In
parameters are depicted in Figs. 13–16. While the mini-
our previous study [15], it was found that TBLS, DBLS,
mum and maximum torques exhibit rapid and gradual
and Ca.St. were effective fusion enhancers through
increases, respectively, the slow rates of decrease in
decreasing the fusion time and increasing the fusion factor
fusion time and increase in fusion factor are noteworthy.
of rigid PVC compounds. It would therefore, be reasona-
In the range of 6–10 phr of IM, fusion time decreases
ble to assume that the presence of such ingredients would
slightly, from 1.13 to 0.9 min, whereas the fusion factor
have a positive effect on the fusion process of the PVC
starts to decrease after reaching a maximum at 8 phr. The
formulations used in the present study.
decrease might occur because beyond 8 phr, the IM may
Figures 9–12 show the effects of different amounts of
act as an ‘‘external’’ lubricant in combination with other
St.Ac. on the fusion parameters. The figures illustrate that
additives and thus lower the fusion level. Further evi-
while minimum and maximum torques decrease slightly
dence for this behavior is provided by the tendency to
with increasing St.Ac. loading, fusion time remains
level off of the maximum torque and fusion time curves
almost independent of St.Ac. content, decreasing by only
at 8 phr of the material.
0.1 min in the 0.1–0.5 phr range of the material. In this
The validity of the traditional classification of rigid
range of St.Ac. content, fusion factor shows an initial
PVC additives into ‘‘internal’’ and ‘‘external’’ lubricants
sharp decrease of 32% (from 1030 to 700 m
g/min) in the
has not gained much support recently, as evidenced by
0.1–0.3 phr range, followed by an increase in the 0.3–0.5
results published by Rabinovitch et al. [17] and by
phr range. In this respect, St.Ac. may exhibit ‘‘external’’
Summers [18]. Lubricant type designation is regarded as
lubrication properties from the fusion point of view,
irrelevant and, moreover, could not be decided on the ba-
thereby leading to a slower fusion process and a lowering
sis of effects on a few criteria such as melt viscosity and
of fusion rate. In fact, in the presence of St.Ac., applied
fusion, as is the case in this study. Other effects such as
shear on the sample is decreased. This decrease is due to
metal release, Tg variations, and haze, among others,

FIG. 11. Effect of St.Ac. content on fusion time. FIG. 13. Effect of impact modifier content on minimum torque.

96 JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—

—2009 DOI 10.1002/vnl
 FIG. 14. Effect of impact modifier content on maximum torque.
should also be considered. All additives commonly used
in rigid PVC formulations show, to a lesser or greater
extent, and either alone or in combination with other
ingredients, characteristics of both types of lubricants.
Thus, observed synergistic actions and mechanisms
involving various additives and lubricants in rigid PVC
formulations have led Summers [18] to consider the lubri-
cants as surfactants and slip agents.
From the lubricity point of view, it must be obvious
that the behavior of an additive is dependent upon the
type and amount of other lubricants and/or heat stabilizers
that are present in the mixture. The presence of additives
such as the effective fusion promoters TBLS and DBLS
and the weak fusion delayers neutral lead stearate and
St.Ac. can markedly affect the behavior of NC, Ca.St.,
and the IM, thereby changing the effects on PVC fusion.
It is well-known that PVC exhibits low thermal stabil-
ity and begins to dehydrochlorinate at about 1008C, a pro-
cess that induces the discoloration of the polymer [19].
Previous studies of PVC/O-MMT nanocomposites have
also reported that O-MMT modified with alkylammonium
salts can promote the dehydrochlorination of PVC during
melt processing [20–22], as opposed to the behavior of
PVC and PVC/Naþ-MMT nanocomposites, which kept
good processing stability. It has also been suggested that
the decomposition of the organic modifier and the subse-
quent catalytic effects on the HCl release are the main
reasons for the PVC discoloration [23]. The melt-blended
formulations used in the present study showed colors
FIG. 15. Effect of impact modifier content on fusion time.
DOI 10.1002/vnl
FIG. 16. Effect of impact modifier content on fusion factor.
ranging from near white for PVC to light pink for the
nanocomposites containing 2 phr of NC and almost brown
for those with 6 phr of NC, results indicating the
increased darkening of color with increasing NC content.
Similar color changes have been reported [21, 23–26],
although it is probable that the rate of color darkening in
the present work may have been masked to some extent
by the heat stabilizer system used. Additionally, within
each group of runs 1–3, 4–6, and 7–9 (Table 2), slight to
insignificant variations in color change were noted,
thereby indicating that NC was the sole formulation vari-
able with a major influence on discoloration.
The time at which polymer degradation occurs, as
ascertained from the release of HCl, reflects one of the
effects of NCs and has been used as a criterion for evalu-
ation of the thermal stability of PVC formulations [25,
26]. As shown in Fig. 17, the time to HCl evolution of
the composites decreases dramatically from that of pris-
tine PVC. Even with the 2-phr NC content, the time
decreases from nearly 16 to 6.5 min. This result is in
agreement with the color changes noted above, and it
indicates that the presence of organically modified NC
has an adverse effect on the thermal stability of PVC/O-
MMT nanocomposites. This observation agrees with
results obtained by Ren et al. [25] and by Beyer [26]
when using similar methods for the evaluation of thermal
stability. Again, within each group of runs 1–3, 4–6, and
7–9 (Table 2), slight variations in time to HCl release
FIG. 17. Effect of NC content on time to HCl evolution.
JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—
—2009 97
 were recorded, thus denoting NC as the most significant
formulation variable affecting thermal stability.
CONCLUSION
Within the limits of the effects on melt viscosity,
fusion parameters, and thermal stability of rigid PVC, the
above results can lead to the following conclusions:
1. Organically modified NC increases the minimum and
maximum melt viscosities, while reducing fusion time and
increasing the fusion factor.
2. The Ca.St. behaves similarly to the organically modified
NC but is a less effective fusion promoter.
3. Depending on its content, St.Ac. can act both as a pro-
moter and as a retarder of the fusion process.
4. The IM, in general, can have a positive effect on fusion,
although careful consideration should be directed to its
content in the formulations.
5. Organically modified NC adversely affects both color and
thermal stability, while Ca.St., St.Ac., and the IM have
much smaller effects.
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DOI 10.1002/vnl