the high concentration colored …...color masterbatch is the poor dispersion of the pigment caused...

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http://www.iaeme.com/IJARET/index.asp 1 [email protected] 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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http://www.iaeme.com/IJARET/index.asp 1 [email protected]

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

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

http://www.iaeme.com/IJARET/index.asp 2 [email protected]

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

Eldo Simon and Dr. M. Sirajuddin

http://www.iaeme.com/IJARET/index.asp 3 [email protected]

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

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.

S. N° Ingredient Formulation 1

%w/w

Formulation2

%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

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

http://www.iaeme.com/IJARET/index.asp 4 [email protected]

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

Eldo Simon and Dr. M. Sirajuddin

http://www.iaeme.com/IJARET/index.asp 5 [email protected]

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.

Parametric Study of Stand

http://www.iaeme.com/IJARET/index.

Figure 3 The coloring strength

Figure 4 The pressure

Figures 3 and 4 show the coloring

different levels of dispersing agent relative to the pigment weight.

that the increase in waxes volume fraction increase very substantially the coloring strength

and decreases the pressure and consequently increases the masterbatch dispersion degree.

wax percentage must be sufficient to avoid the pigment's particle agglomeration and ensure

good wetting of these particles in the mixture.

requires up to 35% by the pigment

does not always produce good results.

shear effect generated by the screws during the extrusion step.

prepare pigment concentrates having the lowest possible level of polyolefin waxes and at the

same time a good dispersion quality.

100

0

20

40

60

80

100

120

140

0%

Co

lori

ng

str

eng

th %

1.97

1.6

1.65

1.7

1.75

1.8

1.85

1.9

1.95

2

0%

Fil

ter

pre

ssu

e valu

e(B

ar/

min

)

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

IJARET/index.asp 6 [email protected]

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

pressure evolution as a function of different levels of wetting agent

Figures 3 and 4 show the coloring strength evolution and the pressure

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

essure and consequently increases the masterbatch dispersion degree.

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

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 thi

prepare pigment concentrates having the lowest possible level of polyolefin waxes and at the

same time a good dispersion quality.

103.9110

120.5125.6 125.4

117.8

10% 20% 30% 35% 40%

Wax rate

1.941.91

1.86

1.74 1.74

10% 20% 30% 35% 40%

Wax rate

Off Distance on a Bridge Under Blast Loading

[email protected]

as a function of different levels of wetting agent

as a function of different levels of wetting agent

evolution and the pressure evolution for

These same figures show

that the increase in waxes volume fraction increase very substantially the coloring strength

essure and consequently increases the masterbatch dispersion degree. The

wax percentage must be sufficient to avoid the pigment's particle agglomeration and ensure

We have found that the optimum dispersion

Increasing the wax content to values above 35%

Reducing the viscosity at certain values reduces the

The aim of this work is to

prepare pigment concentrates having the lowest possible level of polyolefin waxes and at the

117.8

45%

1.81

45%

http://www.iaeme.com/IJARET/index.

3.3 Mixer parameters effect

A series of experiments have been conducted to assess the importance of premixing

conditions of masterbatches,

ingredients have been introduced into the container,

300 rpm 400 rpm 500 rpm and 600 rpm for 5, 10 and 15 minutes.

temperature of each prepared sample.

masterbatches dispersion quality.

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

Figure 6 The mixture temperature

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

powder mixture is obtained. This can also offer the advantage of facilitating the masterbatches

0

20

40

60

80

100

120

140

160

300

colo

rin

g s

tren

gth

%

0

20

40

60

80

300

Tem

pea

ture

°C

Eldo Simon and Dr. M. Sirajuddin

IJARET/index.asp 7 [email protected]

Mixer parameters effect

A series of experiments have been conducted to assess the importance of premixing

onditions of masterbatches, study the influence of the mixer blade speed,

ingredients have been introduced into the container, batches 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

temperature of each prepared sample. Figure 5 shows the premixing conditions effect on

s dispersion quality.

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

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

A higher temperature level has considerably improved the dispersion

We have found that the higher the temperature, the more dust

This can also offer the advantage of facilitating the masterbatches

400 500 600

Mixing time

Speed rpm

400 500 600

Mixing time

Speed rpm

[email protected]

A series of experiments have been conducted to assess the importance of premixing

tudy the influence of the mixer blade speed, after the

atches of 40 kg were mixed at 200 rpm,

In addition we measured the

premixing conditions effect on

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

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

A higher temperature level has considerably improved the dispersion

We have found that the higher the temperature, the more dust-free, free-flowing

This can also offer the advantage of facilitating the masterbatches

Mixing time

min

Mixing time

min

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

http://www.iaeme.com/IJARET/index.asp 8 [email protected]

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.

Eldo Simon and Dr. M. Sirajuddin

http://www.iaeme.com/IJARET/index.asp 9 [email protected]

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

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

http://www.iaeme.com/IJARET/index.asp 10 [email protected]

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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