International Journal of Advanced Research in Engineering and Technology (IJARET)

Volume 8, Issue 3, May - June 2017, pp. 01–11, Article ID: IJARET_08_03_001
Available online at http://www.iaeme.com/IJARET/issues.asp?JType=IJARET&VType=8&IType=3
ISSN Print: 0976-6480 and ISSN Online: 0976-6499
© IAEME Publication

THE HIGH CONCENTRATION COLORED

MASTERBATCH: INFLUENCE OF PARAFFIN
WAX AND PREMIXING PROCESSING METHOD
ON DISPERSION QUALITY
Lahcen Safraoui, Basma Benhadou, Abdellah Haddout, Mariam Benhadou, Mohamed
Benzhour
Laboratory of industrial management and energy and technology of plastics and composites -
ENSEM Casablanca Morocco
University Hassan II- Casablanca Morocco

ABSTRACT
Among major problems encountered by manufacturers of highly concentrated
color masterbatch is the poor dispersion of the pigment caused by the strong tendency
to build up agglomerations of powdered pigment particles. The aim of this study is to
characterize the effect of the conditions of the premixing process and the formulation
of the master batch of high concentration 40% on the quality of the dispersion. We
studied the influence of the speed, temperature, time and order of the introduction of
the premix ingredients and the use of a wetting agent on the dispersion quality by the
colouring strength measurement and pressure test by filtration. A study by optical
microscopy was considered.
Key words: Masterbatches, Processing parameters, Thermoplastics matrix, Coloration
process, Premixing, Dispersion quality, Wax.
Cite this Article: Lahcen Safraoui, Basma Benhadou, Abdellah Haddout, Mariam
Benhadou and Mohamed Benzhour The High Concentration Colored Masterbatch:
Influence of Paraffin Wax and Premixing Processing Method on Dispersion Quality.
International Journal of Advanced Research in Engineering and Technology, 8(3),
2017, pp 01–11.
http://www.iaeme.com/IJARET/issues.asp?JType=IJARET&VType=8&IType=3

1. INTRODUCTION
Masterbatches are widely used in the plastics industry to add color and other desired
properties to products [1, 3].Thanks to constant technological development, more efficient
processing plants, new fields of application, cost savings…, there is a daily demand for new
solutions and more efficient and sophisticated products. Only the objectives of masterbatches
producers remain the same: a higher concentration of pigment at the same time as a higher
dispersion quality. Plastic thin products such as strips, rope and filaments, which require the
use of high-concentration masterbatch for to be tinting, are most concerned with the degree of

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 Parametric Study of Stand-Off Distance on a Bridge Under Blast Loading

pigments dispersion or additives. Dispersion problems arise when the aggregate particles
interact to produce agglomerates [2].
Improved wettability of the particles with complete aggregate destruction leads to good
particle dispersion and this is demonstrated by the constancy of the number of particles as a
function of time [4].The problem that remains is the natural tendency of particles to reduce
their number over time because of the coalescence phenomena, linked to the attractive forces
that exist between the particles [5, 6]. The magnitude of the coalescence phenomena depends
on the pigment concentration volume, the particles physical properties, the environment
viscosity and temperature. The stability of pigment dispersion depends on the free energy of
overall interaction between the two dispersed pigment particles. The global interaction free
energy is a combination of Van der Waals interactions, electrostatic interactions and steric
interactions [7, 8].However, difficulties in pigment dispersion can be overcome by
particularly reducing the viscosity of the mixture [9, 10].
More the size of the pigment particle is smaller, more complete the capacities and inherent
properties of the particle will be and the better the results are expected [11].In many cases, the
base polymer in granules form alone is not sufficient to achieve the required dispersibility and
hence wetting agents and / or dispersants become necessary. Wetting and dispersing agents
are very effective and provide an easy way of making masterbatches with good pigment
dispersion.
The quality of the final dispersion depends on the optimization of many factors.
The quality of the dispersion final depends on the many factors optimization.In a previous
study [12], we showed that the screw configuration design and the temperature profile
strongly influenced the dispersion process. Another study is interested in manufacturing a
mono concentrated purple masterbatch based on dioxazine pigment, showed that a better
combination of processing parameters by the extrusion process to optimize pigment
dispersion and reduce clogging power.
The mixing process from three extrusions without filtration leads to a reduction in the
filter pressure value (FPV) of about 84%and an increase in the relative colouring strength
(RCS) of about 50%Compared to the standard production process (a single extrusion) for the
manufacture of a polyamide 6 monodispersed green masterbatch with a halogenated copper
phthalocyanine green pigment [14].
The modification of masterbatches formulation by the addition of waxes and / or powders
of micronized polyolefin make it possible to improve the quality of dispersion. Arno
Knebelkamp [15] has shown that using powders of micronized polyolefin obtained by
cryogenic grinding or with an air jet mill in the pigment concentrates formulation for coloring
plastics improves the pigment dispersion quality.
Andreas Seidel [16] proposed a method for improving the carbon black dispersion using a
wetting agent comprising low molecular weight wax, lignite and aliphatic or aromatic wax
oils, carboxylic acid esters, fatty acids and / or fatty alcohols. It has also shown that the
impact strength of notched specimen is significantly higher and the number of surface defects
is reduced compared to carbon black used alone.
The masterbatches manufacturing is a two-stage process: collecting ingredients and
mixing them, then processing them together by applying heat and shear to produce
homogenized granules. In general, variable speed mixers are used to produce a premix which
is then processed in twin screw extruders. This treatment depends on several key elements:
the formulation, the raw materials quality, and the mixture quality [17, 18].
A number of factors affect the product final quality relative to the dispersion level
obtained during the mixing process. Mixing time, blade speed, mixing temperature and the

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 Eldo Simon and Dr. M. Sirajuddin

order in which the ingredients are introduced are just a few of the factors influencing
dispersion [19, 20, 21].The effect of these factors is often difficult to determine because of the
strong interactions between them [3].
The aim of this study is to determine a precise way the impact of the different mixer
parameters on the masterbatch dispersion level. We studied the speed, the time, the
temperature and the ingredients introduction order on the dispersion quality. We also studied
the effect of using paraffin wax as a wetting agent in the masterbatch formulation as well as
its percentage on the dispersion degree.

2. EXPERIMENTAL PROCEDURE
2.1 Materials
The base polymer selected for this study was a polypropylene homopolymer PP GRAIN511A
issued by Sabic Belgium with an MFI of 25 g / 10 min (230 ° C and 2.16 kg), a melting
temperature of 155 ° C. The type of the red pigment used is PR 48: 3, sold by Hangzhou
AiBaiChemicalCo., Ltd. It is presented in powder form, density = 1.8, oil intake (ml / 100g)%
between 45-55, and light resistance= 8.The Licocene PP 1502 wax and Licocene PP6102 wax
softening temperatures are 86 ° C and 145°C respectively, provided by Clariant. These waxes
have been used as wetting agents to positively influence the dispersion degree.
Two formulas have been developed which are presented in Table 1.The presence of waxes in
the formulations is absolutely necessary in order to guarantee effective pigments wettability
and to limit the particles agglomerations constitution.
Table 1:Formulation details

Formulation 1 Formulation2
S. N° Ingredient
%w/w %w/w
1 PP GRAIN511A 22.5 22.5

2 Antioxidant B225 0,5 0,5

3 PP poudre 15 15

4 Cire Licocene PP 6102 0 20

5 CireLicocenePP 1502 20 0

6 Calcium Stearate 1 1

7 PR 48: 3 40 40

8 Plastaid – T 1 1

A double screw extruder type Nanjing Hisilicon Extrusion Equipment Co., Ltd. TSE40
with the following characteristics: L / D = 40, specific torque = 8.2 Nm / cm3 (30 kW at 600
rpm) and capable of operating at 600 rpm. The screw speed was set to 200 rpm. The different
formulations were premixed by a mixer type (power 58kw) capable of rotating up to 1000
rpm. The mixer speed was set at 100 rpm, 350 rpm, 500 rpm and 500 rpm and the mixing
time varied between 3 to 20 min.

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 Parametric Study of Stand-Off Distance on a Bridge Under Blast Loading

2.2 Filter test and relative coloring strength

Two characterization techniques of dispersion degree were developed in a previous study
[12],the filter pressure value (FPV) and an increase in relative colouring strength (RCS) were
used to evaluate the dispersion quality.

2.3 Reflection optical microscopy

To establish the relationships between the different parameters of the pre-mixing process and
addition of waxes on the one hand, and the dispersion degree on the other hand, we carried
out a series of observations under the reflective optical microscope, in order to characterize
the dispersion quality of our highly concentrated masterbatches.

3. RESULTS AND DISCUSSION

3.1 The dispersing agent: Type choice effect
A masterbatch is composed of a polymeric matrix in which a varied proportion (5-80%) of
pigments and / or colorants, dispersing waxes and other additives are included. The use of
special waxes - in particular high-quality wetting agents - and their optimum adaptation to the
pigments requirements, carrier systems and relevant processing technology enable efficient
and consequent realization. The choice of the wax type used appears necessary to achieve the
objectives. We have studied two waxes: PP LICOCENE 1502 and PP LICOCENE 6102.They
are used at 50% relative to the pigment percentage. The various formulas are introduced into
the mixer container in the order given in Table 1. The patch weight is 40kg. Both of two
formulas are mixed for 10 minutes with a rotating helix at a rate of 300 rpm. We have taken
as reference the formula without dispersing agent at a speed of 300 rpm.

Figure 1 The coloring strength evolution as a function of the wax type

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 Eldo Simon and Dr. M. Sirajuddin

Figure 2 The pressure evolution of the as a function of the wax type

Figures 1 and 2 represent successively the variation of the coloring strength and the
pressure by filtration as a function of the wax type chosen. The waxes stabilize the dispersion
and prevent any fine particles of pigment, formed during the dispersion process, from
reagglomerating as well as avoiding local overconcentration. The results clearly show that the
wetting agent type choice has a significant impact on the evolution of the coloring force and
the pressure, the wax which has a higher melt index shows better results.
Dispersion is the complete wetting of the pigment agglomerates - not only on the
agglomerate surface but also on all the particles surfaces, both inside and outside [22].Only
using special waxes allows the pigments optimum wetting, so that even the hollow and fine
spaces between the agglomerated particles become accessible to the wetting agent.
It is evident that a low viscosity wax may have advantages in this regard compared to a
higher viscosity wax. The pigmentpolarity, its particle shape, its size and its surface are
important factors in the selection and dosage of a suitable adjuvant, as well as its thermal and
mechanical properties [11, 22].
Due to the low viscosity, reduced by adding wax, longitudinal and lateral intensive mixing
in the double extrusion machine becomes easier. Even this aspect is of great importance, since
excellent mixing is among the prerequisites for effective wetting, dispensing and
homogenization of pigments and additive particles.

3.2Concentration effect of dispersing agent

The wetting efficiency depends mainly on the pigment surface tension properties and the base
polymer, as well as the resulting mixture viscosity [24].The absorption mechanism depends
on the pigment chemical nature and the type and volume of wetting agents used. The viscosity
plays an important role on the one hand, the use of a certain amount of wax is recommended
to improve substantially the wetting and pigments distribution. On the other hand, this
measurement results in a viscosity reduction of the concentrate melt and makes it possible to
increase the pigments concentration.
According to the pigment type, the optimum dispersion requires up to 40% of wax relative
to the pigment weight [91].Excessive wax amounts always result in migration and deposition
on the matrices [23], it is particularly advantageous in the pigment concentrate preparation
containing well-dispersed pigments with minimum fractions of polyolefin waxes.

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 Parametric Study of Stand-Off
Stand Off Distance on a Bridge Under Blast Loading

140 125.6 125.4

120.5 117.8
120 110
103.9

Coloring strength %
100
100
80
60
40
20
0
0% 10% 20% 30% 35% 40% 45%
Wax rate

Figure 3 The coloring strength evolution as a function of different levels of wetting agent

2 1.97
Filter pressue value(Bar/min)

1.94
1.95 1.91
1.9 1.86
1.85 1.81
1.8
1.74 1.74
1.75
1.7
1.65
1.6
0% 10% 20% 30% 35% 40% 45%
Wax rate

Figure 4 The pressure evolution as a function of different levels of wetting agent

Figures 3 and 4 show the coloring strength evolution and the pressure evolution for
different levels of dispersing agent relative to the pigment weight. These same figures show
that the increase in waxes volume fraction increase very substantially the coloring strength
and decreases the pressure
essure and consequently increases the masterbatch dispersion degree. The
wax percentage must be sufficient to avoid the pigment's particle agglomeration and ensure
good wetting of these particles in the mixture. We have found that the optimum dispersion
requires
quires up to 35% by the pigment weight. Increasing the wax content to values above 35%
does not always produce good results. Reducing the viscosity at certain values reduces the
shear effect generated by the screws during the extrusion step. The aim of thisthi work is to
prepare pigment concentrates having the lowest possible level of polyolefin waxes and at the
same time a good dispersion quality.

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 Eldo Simon and Dr. M. Sirajuddin

3.3 Mixer parameters effect

A series of experiments have been conducted to assess the importance of premixing
conditions
onditions of masterbatches, studytudy the influence of the mixer blade speed, after the
ingredients have been introduced into the container, batches
atches of 40 kg were mixed at 200 rpm,
300 rpm 400 rpm 500 rpm and 600 rpm for 5, 10 and 15 minutes. In addition we measured the
temperature of each prepared sample. Figure 5 shows the premixing conditions effect on
masterbatchess dispersion quality.

160
140
coloring strength %

120
100
80
60
Mixing time
40 min
20
0
300 400 500 600
Speed rpm

Figure 5 The coloring strength evolution as a function of time and of mixing speed

80

60
Tempeature °C

40

20 Mixing time
min
0
300 400 500 600
Speed rpm

Figure 6 The mixture temperature evolution as a function of time and of mixing speed.
The dispersion results obtained (Figure 5) and the monitoring of the mixture temperature
change (Figure 6) have shown that the parameter most relevant for the dispersion quality is
the mixture temperature. A higher temperature level has considerably improved the dispersion
degree. We have found that the higher the temperature, the more dust-free,
dust free-flowing
powder mixture is obtained. This can also offer the advantage of facilitating the masterbatches

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 Parametric Study of Stand-Off Distance on a Bridge Under Blast Loading

extrusion. In order to reach temperatures close to the wax softening point. We changed the
ingredients introduction order, in the first time we mixed PP grain, PP powder, antioxidant,
calcium Stearate and wax at a speed of 600rpm for 20min.The temperature obtained is 90 °
C., after adding the pigment and Plastaid-T also mixed at a speed of 600 rpm for 15 min to
reach a temperature of 80 ° C. When this temperature level is exceeded, the mixture presents
difficulties during extrusion. The figure. 7 shows the dispersion quality evolution obtained by
the new procedure. We noted a 56% increase in coloring strength when the pouch temperature
of the wax softening point is increased by heating the mixture. The pigment is moistened with
the wax, which makes the mixture virtually dust-free. In addition the pigment-wax mixture
forms a thin skin around the polymer granule, so that the wax functions as a binder. This
coating acts as a distance guard between the pigment particles. The wax particles in the
pigment particles vicinity and being substantially distributed have a high probability of
finding a place between the pigment particles, thus separating them from one another.
Consequently, these pigment particles will not form an agglomerate, which facilitates
pigments dispersion and finally stabilizes it.

Figure 7 The coloring strength evolution as a function of the new premixing procedure
The remarkable increase in the coloring strength allows a possible reduction in the amount
of pigment and wax. It is a way to have economic formulation costs and good performance
without treatment problems. The reduction of the wax content also makes it possible to reduce
the effect of migration on the granules surface which can affect the product quality during its
storage.

3.4 Microscopic analysis

In order to validate the results obtained previously on the interaction between the conditions
of the pre-mixing process and the formulation of the masterbatch on the one hand and the
dispersion quality on the other hand. We carried out a series of morphological analysis using
optical microscopy according to the parameters used.
Figure 8 shows the variation in the dispersion degree by a standard film with different
parameters studied. A better dispersion is presented for the new procedure used (FIG. 8F), we
have found that the agglomerates are almost disappeared and the film is characterized by a
more reddish contrast marking the increase in the coloring strength and consequently a better
dispersion. This corresponds to the results obtained above.

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 Eldo Simon and Dr. M. Sirajuddin

A B

C D

E F

Figure 8 Microscopic visualization of masterbatches with different mixture parameters

(A) Without wax, (B) with Licocene wax PP 6102, (C) with Licocene wax PP 1503 (D) Speed 300
rpm and time 10 min, (E) speed 600 rpm and time 20 min, (F) With the new protocol,

4. CONCLUSION
Dispersion is an inherent property of the pigment and the process used to produce the
masterbatch. Good dispersion is particularly required when the final application requires well-
required performance. A better understanding of the conditions effect of the mixtures
preparation before their treatment by extrusion is critical for better dispersion. This study
allowed us to show the formulation effect and the pre-mixing conditions on the dispersion

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 Parametric Study of Stand-Off Distance on a Bridge Under Blast Loading

level. The choice of the type and the rate wax used appear necessary. Using 17.5% of the
Licocene PP1502 wax considerably improves the dispersion degree. The application of a new
procedure, by increasing the mixture temperature to 90 ° C., makes it possible to increase the
colouring strength by 56% by improving the mixture quality, powdered and dust-free, the wax
acts as a binder and fixes the pigments particles on the polymer surface which facilitates the
dispersion.These results are validated by microscopic analyzes.

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