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R E V I E W

TECHNICAL

I N F O R M AT I O N

PLASTICS

R2-02

Compounding Unplasticised PVC


(The Mixing Process)
Omya Applied Technology Services,
Segment Plastics

Mixing is an important operation in PVC compounding.


Some of the problems that occur during subsequent
processing can be avoided by optimising the mixing process.
Below, we summarise the important aspects of mixing, some
of the problems that often occur and suggested solutions.

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1. Introduction
PVC processing first requires a compounding process [1, 2], in which the PVC is
mixed with additives such as stabilisers,
lubricants, fillers and pigments to produce
a dry blend. It is important not only that all
components of the formulation should be
homogeneously mixed, but, in the ideal
case, that all components should bind to
the PVC particles.
In our experience, a number of problems in
processing can be traced back to agglomeration and separation resulting from an
inadequately compounded dry blend.
Poor mixing of the components is difficult
to correct subsequently and is often the
cause of problems such as fisheyes and surface flaws in semi-finished products.

Mix
Heat to 50C

The dry blend is cooled in a double wall,


water-cooled mixer. Low speeds are used
to avoid generating frictional heat [4, 5].

Add lubricant

It is particularly important to control the


speed of the rotor in the cooling chamber
to obtain optimum cooling times [6, 7].

Mix
Heat to 70C

Add stabilisers
Mix
Heat to 90C

Mix
Heat to 120C

Charge dry blend to cold


chamber
Cool
to 40C

It is important to match the filling volume


(about 70 to 80 %), the geometry of the
mixing blades and the rotational speed to
obtain optimum material flow with vortexing in the heating mixer.

Remove dry blend


from cold chamber

The vortex assists the homogeneous distribution of additives, while ensuring self cleaning of the mixing vessel and mixing
blade [4].

Mature
for 24 h

In practice, most mixers can only operate at


two speeds - slow and fast. However, for
optimum mixing, we recommend mixers
with infinitely variable speeds.
After the formulation has been heated to the
preset temperature (about 110 to 130 C),
the hot dry blend must be cooled to below
the melting point of wax (about 40 C) to

prevent agglomeration and allow it to be


stored.

Add fillers/pigments

In the hot mixer (also called a high-speed


mixer, fluid mixer or intensive mixer), the
compound is heated by intensive fluidisation at high circumferential speeds of 20 to
50 m/s of the mixing blade.

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Charge PVC powder

2. Hot/Cold Mixing
The most widely used process for preparing the dryblend PVC is discontinuous
compounding in a two-stage heating/cooling mixing process [3, 7]. In this case, the
PVC powder and additives are first heated
to about 120 C in a hot mixer and then
cooled to about 40 C in the cooling chamber.

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Final compounding and


processing of uPVC

The cooling water should be at a temperature of between 15 and 20 C. At lower


temperatures, atmospheric moisture may
condense on the walls of the chamber causing the dry blend particles to stick to them
and form an insulating layer, greatly reducing the cooling efficiency of the mixer and
generating agglomerates [7].
2.1. Optimum Mixing Process
A common practice is to put all the components into the hot mixer at the beginning of the mixing process. The mixer
blade rotates slowly at first, but is speeded
up subsequently to mix the compound and
heat it up to about 110 to 130 C.
As long as the compound produced is free
from defects, this is satisfactory. However, if
dispersion problems occur frequently, resulting in fisheyes, surface flaws and poor
mechanical properties, especially at higher
filler loadings, we recommend adding the
additives step by step. This often eliminates
or at least reduces the problems.
We consider the best procedure to be as
follows (see Figure 1):

First charge the PVC into the mixer. Mix


briefly and then start to add the other
components one at a time.

At about 50 C, add the one-pack stabiliser system. The low-melting lubricant that this contains will liquefy,
disperse homogeneously and bind to
the PVC particles together with the stabilisers.

If the stabilisers and lubricants are added


separately, it is best to add the lubricant at
50 C and then the solid stabilisers at
about 70 C.

Figure 1: Optimum Mixing Sequence for Highly Filled


PVC Formulations.

If the formulation contains liquids (Sn


stabilisers, epoxidised soya bean oil,
etc.), add them slowly at about 70 C
(inject them if possible). Adding them all

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at once runs the risk of agglomeration


and inhomogeneities.

At 75 to 80 C, the softening point of


the PVC is reached. The additives begin
to stick to the surface of the PVC particles. The molten lubricant promotes this
process, so that as the processing continues, they become almost completely
bound to the PVC particles.
At about 90 C, the CaCO3 and TiO2 pigment are added. If CaCO3 and TiO2 are
added earlier, some of the low-melting
lubricant may adhere to the surface of
the TiO2 or CaCO3 particles, especially
since these minerals have a larger specific
surface area than PVC [8]. Late addition,
particularly of TiO2, has the added benefit of reducing wear on the mixer blade
and vessel. This prevents colour discrepancies (greying) by metal particles.

Where the optimum mixing process is


used, a homogeneous dryblend is obtained, in which the additives are satisfactorily bound to the PVC. For processors, this
brings the following specific advantages

Free flowing compound

No segregation during storage, transport or metering

Low dust

Improved dispersion of the formulation


components

Reduction of wear on the mixing blades

Reduced residual moisture content in


the dry blend

Not all processors are able to adapt their


compounding process to meet optimum
mixing criteria. In such cases, we recommend a two-stage heating/mixing process in
which PVC, stabiliser and additives are first
loaded into the mixer and then subsequently the CaCO3 and TiO2 pigments, when the
temperature reaches about 90 C.
2.2 Double Batching
In the double batching process [9], some
(usually 50 %) of the PVC is mixed with the
total amount of additives in the hot mixer.
The rest of the PVC for the formulation is
then put into the cooling chamber, where it
is mixed with the premix from the hot mixer.

In the best case, this yields a mixture of virgin PVC particles without additives and
PVC particles containing twice the amount
of additives than that produced in a conventional (single batching) mixing process.
In the worst case, the additives are not
completely adsorbed by the PVC grains
(because the available surface area is too
small), and some of them remain in the dry
blend as separate fractions.
In both cases, differences in density between the particles may lead to separation
during storage, conveying and metering
[6]. This results in poor homogeneity and
has a negative effect on the subsequent
process [10], leading to inhomogeneities in
the final compounding [1, 2], variations in
the gelation of the PVC, and therefore to
poorer quality of the semi-finished product.

3. Troubleshooting during
Mixing
In uPVC processing, the numerous problems that may occur can have entirely different causes. Problems must therefore
always be dealt with on a specific case-bycase basis. Often, there is no obvious relationship between the processing problems
and the PVC compounding process. Table
1 lists some typical problems that arise
from inadequate mixing. Omya also offers
technical support.

4. Literature
[1] Krger, E., Aufbereiten von PVC,
Dissertation, Aachen, 1985.
[2] cpm GmbH, Grundstzliches und Problemlsungen fr die PVC-Extrusion, Grossefehn, 2000.
[3] Langenberg, H., Design of Heating Mixers
for Plastics Compounding, Kunststoffe/Plast
Europe 76 (1986) 5, pp. 406-409.
[4] Pahl, M. H., Mischen von Schttgtern,
in: Schttguttechnik in der Kunststoffindustrie, VDI-Gesellschaft Kunststofftechnik, Dusseldorf, 1998.
[5] Pahl, M. H., Solid-State Mixing of
Plastics, Kunststoffe/Plast Europe 76 (1986)
5, pp. 395-405.

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[6] Grosse-Aschhoff, M., Aufbereitung von


PVC fr die Fensterprofilextrusion
Verfahren und aktuelle Trends, 3rd Intern.
Plastics Window Congress 2000.
[7] Heine, J., PVC-Aufbereitung, MTI
Mischtechnik Industrieanlagen GmbH,
Detmold, 1999.
[8] Grosse-Aschhoff, M., Optimisation of
the PVC Mixing Process for Window
Profiles, Kunststoffe/Plast Europe 89 (1999)
2, pp.74-77.
[9] Grosse-Aschhoff, M., Double-Batching
in der Profilherstellung, Dissertation,
Paderborn, 1998.
[10] Eigruber, H., Plastics Special 7-8
(1999), pp. 38-44.

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Problem

Causes

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Solutions

Dry blend contains soft agglomerates that


can be crumbled between the fingers.
These agglomerates cause fisheyes in
semi-finished products.

Soft agglomerates can form in the raw


material as a result of transport and storage
Moisture absorption promotes the formation of such agglomerates

Increase the energy input to the mixer


(longer mixing time, higher speed of the
mixer blade, higher ultimate mixing
temperature [up to 130 C])
Check the material flow in the mixer
(does vortexing occur?)

Hard agglomerates in the dry blend cause


fisheyes in the semi-finished product

Caked material on the mixer wall and mixer


blades (see below)
Insufficient dispersion of the one-pack stabiliser

Check the raw materials


Is the mixer too full?
Check the material flow in the mixer
(see below); does vortexing occur?
Use the optimum mixing process

Caked material on the mixer wall and


mixer blades

Additives melt on the hot wall and mixer


blades and stick fast

Charge the PVC first, then the additives


(see 2.1)
Check the material flow in the mixer
(vortexing assists the distribution of
formulation components and promotes
self-cleaning of the mixer vessel and blades)

Mixer must be frequently cleaned

Caked material on the mixer wall and mixer


blades (see above)
Material deposits in mixer as a result of
inefficient material flow

Use the optimum mixing process


Check the material flow (see below)

Irregular gelation of the PVC [cf. 1, 2],


fisheyes

Inhomogeneities in dry blend

Use the optimum mixing process


Check the metering equipment and lines
(has separation occurred leading to
irregular, inhomogeneous dosing?)
Avoid double batching

Inhomogeneities/agglomerates during
the feeding of liquid components

Sudden addition of liquids runs the risk of


agglomeration/inhomogeneities

Add liquids slowly while the motor is


running, inject if possible

Dry blend generates dust


Separation of the dry blend on storage,
conveying or metering

Inadequate binding of the additive to the


PVC particles

Check the material flow in the mixer


(does vortexing occur?)
Increase the energy input to the mixer
(see above)
Use the optimum mixing process
Avoid double batching

Colour deviations/greying Dryblends


of the dry blend

Abrasion on the mixer blades

Only add the TiO2 later in mixing process,


at 90 C (see 2.1.)
Check regularly for wear of the mixer
blades

Inefficient material flow in the mixer


(poor vortexing)

Mixer is too full


Material flow altered by wear
to mixer blades

Match the amount of material in the mixer,


the mixer blades and mixer blade speed to
one another
Check mixer blades for abrasion

Table 1: Processing Problems that often Occur as a Result of Poor Mixing.

The information contained in this Technical Documentation relates only to the specific material designated herein and does not relate to use in combination with any other material or in any process. The
information provided herein is based on technical data that Omya believes to be reliable, however Omya makes no representation or warranty as to the completeness or accuracy thereof and Omya assumes no liability resulting from its use or for any claims, losses, or damages of any third party. Recipients receiving this information must exercise their own judgement as to the appropriateness of its use,
and it is the user's responsibility to assess the material's suitability (including safety) for a particular purpose prior to such use (March 2009).

Omya International AG
Baslerstrasse 42
4665 Oftringen
Switzerland

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E-Mail:
Internet:

+41-62 / 789 29 29
+41-62 / 789 26 36
plastics.info@omya.com
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