Dispersion Know How

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DISPERSION KNOW-HOW

VMA-GETZMANN GMBH
VMA‒GETZMANN
Research, development, production
and service in one factory
Since the foundation of the company the name VMA‒Getzmann has
been synonymous with the production of high‒quality and innovative
dispersion systems. The integration of progressive technology with
functional design as well as high quality, are characteristic of our
products.

Of course our dispersion systems are equipped with integrated


safety devices according to EC machinery directive 2006/42/EG.

4
Innovative dispersion and fine grinding
systems for laboratory, pilot plant
and production made in Germany

Our experience ‒ your advantage

Please visit us in our excellently equipped laboratory and pilot plant


for a personal product demonstration with your own products.
Our skilled engineers will be pleased to show you the impressing
range of services of our patented dispersing and grinding systems
DISPERMAT and TORUSMILL.

+49 2296 - 8030 • [email protected]

5
Disperrsiing
g in Laboratory, Piilot Plant annd
Prod
ducctionn with DISPEERMA AT Disssolvers

www.vma-getzmann.de
DISPERSING WITH DISPERMAT
DISSOLVERS

Contents
The Dispersion Process 8 Steps to Improve
1 Dispersion Results 14

The Doughnut Effect 9

The Rheological Behaviour


The Dispersing Effect of the of Millbases 15
Dissolver Disc on Agglomerates 10

Running the DISPERMAT


and Optimising Millbase
Formulations 11

Scaling up Laboratory
Results to Production 12

Circumference Velocity related


to the rotational Speed of the
Shaft for various Dissolver Disc
Diameters 13

7
1 THE DISPERSION PROCESS

The most frequent application of high speed dispersion is to incorporate extremely


fine solid particles into fluids, to produce colloidal suspensions.

Colloidal suspensions are characterised by their behaviour that the finely divided
small particles do not settle under the force of gravity. A sequence of related steps
take place during the dispersing process.

These are:

” The dispersion process:


wetting, mechanical size reduction,
product stabilisation
• the wetting of the surface of
the solid particles by the fluid
components of the millbase
• the mechanical breakdown
of associated particles leading to
smaller particles (agglomerates
and aggregates)
• the smaller particles generated during the dispersion are
stabilised, preventing renewed association (flocculation).

Special interaction between the solid particles and the fluid components of the
millbase determine their wetting and resistance to flocculation.

8
THE DOUGHNUT EFFECT

The best dispersion results with a DISPERMAT are obtained The doughnut effect develops because the millbase is
when the geometry of the dispersion container, the diameter, accelerated outwards from the tip of the dissolver disc.
the peripheral velocity and the height of the dissolver disc When it hits the wall of the vessel, the stream is divided
above the bottom of the vessel as well as rheological into two parts. The one going downwards flows back to
millbase properties are matched to one another. the middle of the dissolver disc along the bottom of the
After adding pigments and fillers to the resin solution, the dispersion vessel and rises up to hit the disc once again.
millbase is brought into a laminar rolling flow pattern by The second part flowing upwards has the same circular path,
increasing the speed of the shaft until no standing material which is limited in by the force of gravity and the rheological
can be seen at the wall of the container. properties of the millbase.
At the correct speed, a channel begins to form around the
shaft and a part of the dissolver disc becomes visible. At this
point, the millbase will form a doughnut-like flow pattern.

The doughnut-like flow pattern is a signal that the maximum


mechanical power possible is being transferred into the
millbase and furthermore that the millbase is being agitated
so that all the agglomerates will eventually reach the
dissolver disc.
” It all depends on the Doughnut

The flow pattern of the doughnut effect is greatly influenced


by the amount of pigment and filler in the millbase. When the
solids content is not high enough, the viscosity tends to be too
low. This leads to splashing and generation of bubbles during
dispersion.

In addition, the mechanical power input is limited and the


deagglomerating capability of the dissolver disc is affected.
Conversely, if the solids content is too high, then the viscosity
will be too high for the doughnut flow pattern to develop.

The flow of the millbase may also be hindered by a yield


value of viscosity. This will result in a tearing action of the
dissolver disc, which may at times even turn without having
contact with the millbase.

9
THE DISPERSING EFFECT OF THE DISSOLVER DISC
1 ON AGGLOMERATES

When the vanes of the disc are moved through the millbase When higher speeds are used, more mechanical power
at a high velocity, areas of higher and lower pressure are is introduced into the millbase. The best dispersion results
generated in front of and behind the vane. The alternating are obtained with the highest possible mechanical power
stress acting on the agglomerates in these areas facilitate input, as long as the doughnut flow pattern (laminar flow) is
their dispersion. In addition to this, a smashing impact should maintained.
be considered for larger agglomerates being hit by the edges
and the surfaces of the vanes. The mechanical power is a product of rotational speed and
However, a considerable share of the total dispersion work momentum (torque) of the shaft (π = 3,141...).
takes place at the surface of the dissolver disc. Due to the
fast movement of the blade, a gradient of shear builds up on
these surfaces in which the dispersion takes place.

The shear stress which acts particularly between the


lower disc surface and the bottom of the container largely
depends upon the distance between the two. The efficiency P=2πnM
of the shear gradient may be enhanced by decreasing this
separation since the shear rate within the gap is increased
and since a higher rotational speed may be chosen due to
the fact, that the change from laminar to turbulent flow takes
place at higher rotational speeds.

Circumference velocity related to the rotational


Geometry within the dispersion container speed of the shaft

D = Container diameter Dissolver disc–Ø in mm


The coloured
60 50 40 30 area indicates the
d = Dissolver disc diameter 30
25 optimum range of
a = Distance between
circumference velocity
dissolver disc and 20
Peripheral speed in m/s

20 between 18 – 25 m/s
bottom of container
f = Amount of millbase
f = 0,5 - 2d

10
a = 0,25 - 0,5d

0
d = 0,3 - 0,7D 10000 20000
D Speed rpm
10
RUNNING THE DISPERMAT AND OPTIMISING
MILLBASE FORMULATIONS

In practice, a simple procedure has proven to yield


satisfactory results:


First the liquid component is put into the dispersion container.
Then, under moderate agitation by the dissolver disc, High speed is built-in !
pigments and fillers are added slowly. The dissolver disc
speed can then be increased until the doughnut effect
is detected at a higher rpm (circumference velocities of
approximately 18-25 m/s).

After premixing, the walls of the dispersion container and the


At this stage, the capability of the DISPERMAT to transfer
shaft should be cleaned removed adhering millbase. high mechanical power into the millbase should be
Then the dispersion is carried out at high peripheral velocities
exploited. One must not be afraid to use high rotational
that guarantee the formation of the doughnut effect. speeds. If e.g. an dissolver disc of 25 mm diameter is used,
the DISPERMAT must be run at a
rotational speed of 15.000 rpm in
Recommended dissolver disc-0 in relation to viscosity and container size order to obtain peripheral velocities
of 20 m/s. The final dispersion result
250 is normally reached after 10 to 15
minutes.
200
175
Use of the dissolver for a longer
150 period of time is not likely to improve
125 the result. Sample analysis shows that
100 further deagglomeration does not take
90 place. The particle size of demanding
or difficult products can be reduced
80
further using a DISPERMAT bead mill
70 or basket mill.
60
Dissolver disc – Ø in mm

50 high-viscous µ > 5000 mPs

40 medium-viscous µ = 500 - 5000 mPs


30
low-viscous µ < 500 mPs
25
20
0,125 0,25 0,5 1 2 3 5 10 15 25 35 50 65
Container size in litres
11
SCALING UP LABORATORY RESULTS
1 TO PRODUCTION

v = circumference velocity m/s


π⋅d⋅n π = 3,141...
v=
d = diameter of the dissolver disc in m
60 n = revolutions of shaft in rpm

An important fact is that the dispersion disc, as this part is moved through the For a laboratory dissolver to reach
results obtained with a DISPERMAT millbase at the highest speed. the peripheral velocities necessary
can be scaled up to a production size It is for this reason, that the tip speed for dispersion, it must be able to run
dissolver. It was mentioned earlier (peripheral velocity) is to be considered at high speeds with utmost accuracy
that the dispersion depends upon the as the key parameter for scaling up and reproducibility. When using the
rate with which the agglomerates are laboratory results to production. dissolver discs of different diameters,
transported into the zones of shear This statement refers to the maximum the circumference velocities may easily
and on the mechanical power which is achievable degree of dispersion and be calculated by the following formula.
transferred into the millbase. not to the time necessary to obtain it.
The mechanical power is the parameter The DISPERMAT will normally be
that limits the maximum degree of faster in dispersing than a production
dispersion which can be achieved. The scale machine, as the distance of the
rate at which the transportation of the agglomerates must cover to reach
agglomerates into the vicinity of the the disc are shorter than in larger
dissolver disc takes place, determines equipment.
the time necessary to reach the
optimum dispersion result. Exact correlation between the
dispersion result with a DISPERMAT
The deagglomeration process mainly and a larger dissolver will naturally also
takes place within the area of shear depend upon comparable temperature
which surrounds the dissolver disc. conditions. For temperature control,
The most effective shearing conditions the use of a double wall temperature
12 are found at the tip of the dissolver control container is recommended.
CIRCUMFERENCE VELOCITY RELATED TO
THE ROTATIONAL SPEED OF THE SHAFT FOR
VARIOUS DISSOLVER DISC DIAMETERS

Please find here three useful examples of the relationship of the circumference velocity and the
shaft speed and the disc diameter.
The coloured area indicates the optimum range of circumference velocity between 18 - 25 m/s.

Example for a millbase volume Example for a millbase volume Example for a millbase volume
of 100 ml of 2500 ml of 30 litres

Dissolver disc–Ø in mm Dissolver disc–Ø in mm Dissolver disc–Ø in mm

250
225
200
150
125

100
60 50 40 30 90 80 70 60
30 30 30
25 50
20 40
20 20 20
Peripheral speed in m/s

Peripheral speed in m/s

Peripheral speed in m/s


10 10 10

0 0 0
10000 20000 5000 10000 3000 6000
Speed in rpm Speed in rpm Speed in rpm

container capacity 250 ml container capacity 5000 ml container capacity 30 litres


inner–Ø of container 65 mm inner–Ø of container 180 mm inner–Ø of container 440 mm
container height 85 mm container height 200 mm container height 440 mm
dissolver disc diameter 30 mm dissolver disc diameter 80 mm dissolver disc diameter 200 mm
shaft speed 11500 – 16000 rpm shaft speed 4300 – 6000 rpm shaft speed 1700 – 2400 rpm
peripheral velocity of disc 18 – 25 m/sec peripheral velocity of disc 18 – 25 m/sec peripheral velocity of disc 18 – 25 m/sec

13
1 STEPS TO IMPROVE DISPERSION RESULTS

In cases where the quality of dispersion does not meet the required standard,
the following parameters should be checked:

Duration of the Amount of Millbase Temperature


Dispersion Operation Better flow characteristics When dispersing, high
The quality of formulations may be achieved by using energy transfer into the
dispersed using a DISPERMAT with a more or less millbase in the container. millbase will lead to an
sufficient high speed generally reaches increase in temperature. In many cases
its final value after a short period of Dissolver Disc this destroys the flow characteristics of
time (approximately 10 -15 minutes). The use of smaller or larger the formulation. In addition, thermally
Increasing the dispersion time to more dissolver disc may lead to sensitive paint ingredients may be
than 20 minutes does not normally lead better results. harmed. Using a water cooled vessel
to improved results. will solve the problem.
Pigment and Filler
Doughnut Effect Concentration Raw materials
The doughnut flow pattern A high viscosity millbase of Partial re-formulation of the
should be maintained during tacky consistency with dilatant flow is paint using more suitable
the course of the whole dispersion. recommended this may be obtained by resins, pigments, fillers or
increasing the percentage of solids, but additives: It should be kept in mind,
Shaft Speed without destroying the doughnut flow that the DISPERMAT® is a dispersion
The mechanical power input pattern. device and not a piece of milling
should be optimised by machinery. Therefore it is incapable of
using the highest possible Flocculation grinding primary particles down to a
rotational speed and thereby the Does flocculation take place smaller size.
greatest peripheral velocity, without after dispersion?
destroying the doughnut flow pattern. If so, check additives. Additives
By adding suitable additives
Geometrical Vacuum the result of the dispersion
Considerations At a dispersion under process can be strongly improved.
The distance between vacuum high-viscous
the dissolver disc and the products can be produced to the
bottom of the vessel can be changed to greatest possible extend without air
obtain better results and to make higher bubble inclusions.
rotational speeds possible.

14
THE RHEOLOGICAL BEHAVIOUR OF MILLBASES

τ [Pa] τ [Pa]

D [1/s] D [1/s]

newtonian fluid: pseudoplastic substance:


Is a fluid whose viscoity is independent of the Viscosity decreases when the shear rate is
shear rate at which it is measured. increased.

plastic substance: dilatant substance:


Viscositsy decreases when the shear rate Viscosity increases when the shear rate is
velocity gradient in increased. increased

To obtain excellent dispersion results, the millbase must Millbase formulations are complex rheological systems, for
exhibit certain rheological properties. Unfortunately, the flow whose characterisation information concerning apparent
behaviour of a millbase may not be expressed by one single viscosity, plastic behaviour, yield stress, thixotropy, rheopexy,
parameter, such as the apparent viscosity. Viscosity is the dilantancy is needed.
measure of the internal friction of a fluid, and is a product
specific Constant Value which is defined as the quotient of low viscous μ < 500 mPs
shear stress (τ) and shear rate (D). medium viscous μ = 500 – 5000 mPs
Only Newtonian fluids retain a constant viscosity and are high viscous μ > 5000 mPs
independent of variations in shear rate (that is i.e. water,
mineral oil, etc.). All other substances which have a viscosity
which is dependent on shear rate are classified as Non- shear stress τ
Newtonian and are more commonly found than Newtonian
Viscosity μ = [Pa · s]
shear rate D
liquids. 15
Fine grrinding
g in Laboratoryy, Pilot Plant
annd Production with DISPERMAT and
TORU USMILLL
www.vma-getzmann.de
FINE GRINDING WITH DISPERMAT
AND TORUSMILL

Contents
Function and task
2
of the bead mill 18

The Step of Mechanical


Division in Dispersion 19

Pass and re-circulation


method 20 ‒ 21

Relationship between Power


Input and Dispersion Result 22 ‒ 23

Steps to Improve
Dispersion Results 24

Transfer of Laboratory Tests


to Industrial Production 25

17
2 FUNCTION AND TASK OF THE BEAD MILL

In many technical processes it is necessary to divide solid 3. The stabilisation of primary particles, agglomerates and
material into fine particles and distribute them evenly aggregates against renewed attraction
within a liquid carrier. This process is generally known as (= flocculation).
”dispersion”.

During dispersion, the adhesive forces that act between While the stabilisation against flocculation is primarily a
the extremely fine solid matter powder particles must be property of a colloid-chemical system, which depends on the
overcome. When the requirements on fineness are high or interaction of the liquid components (in varnishes for instance:
the solid matter is difficult to disperse, a dispersion with the binders, solvents and additives) with the solid matter parts
dissolver is often insufficient. (e.g. pigments and fillers) or on that of the solid particles
with each other, the dispersion machinery used plays a vital
Due to their ability to process a wide variety of solid matters part in the mechanical division and more important aids the
that are difficult to disperse, high speed bead mills have wetting process.
gained particular acceptance.
The actual dispersion system in a bead mill consists of a
In the dispersion process, three partial steps run in parallel: milling chamber and an agitator; the milling chamber is filled
with the grinding beads (material e.g. glass, zircon oxide,
steel) and the product to be dispersed. In the milling vessel,
1. The wetting of the surface of the solid matter to be the grinding medium is kept moving by the agitator, which
processed, by liquid components of the millbase. itself is driven by a motor.
The dispersion process takes place between the grinding
2. The mechanical division of agglomerates into smaller beads sliding on each other and between the rotor and/or
agglomerates and primary particles. the vessel sides and the grinding beads.

18
THE STEP OF MECHANICAL DIVISION
IN DISPERSION

Just like the dispersion, the mechanical imagine a batch bead mill, filled with a Those that are dispersed under these
process can be divided into three steps millbase which with progressing state conditions cause a visible increase in
of dispersion illustrates a measurable the colour strength. Those that have
• wetting change of a technical property. such a high stability that they are not
divided under the conditions of the
• mechanical division
maximum available shearing effect,
• flocculation stabilisation are still undispersed. By increasing the
speed, zones with stronger shearing
The step of mechanical division itself
effect develop where more stable
can also be separated. To enable the
agglomerates can also be dispersed.
agglomerates to be dispersed, they
Therfore, the colour strength may
must
continue to rise with increased speed.
• get into a dispersing situation,
Only after a sufficiently long dispersion
e.g. into the shearing zone
time combined with sufficiently high
between two grinding beads
speeds, can it be expected that
(spatial condition) and
all agglomerates are dispersed.
• be stressed enough so that they In paints, this may for instance be the Only then the spatial as well as the
break (energetic condition). colour strength, the gloss, the viscosity energetic conditions required for a full
or the fineness (to be measured with dispersion are met. Too low a speed
The mechanical division may be a Hegman Gauge according to DIN can generally not be compensated by
illustrated by comparing it with the 53203). longer dispersion and vice versa.
attempt to crack a nut with a hammer. Our example uses colour strength.
When all operating parameters,
In order to break the shell, the nut grinding bead filling quantity, bead
must be hit in the first place (spatial type, speed, cooling etc. are kept
condition), but it must also be hit hard constant, the measured colour strength
enough (energetic condition). For a reaches a finite value related to the
proper understanding it is important to time of dispersion.
realise that both conditions - spatial and Longer dispersion will not improve the
energetic - must be fulfilled at the same colour strength. Only by increasing the
time. Although this model may seem speed it is possible to further increase
rather trivial, it clearly demonstrates the the colour strength.
function of a dispersing machine.
In principle the validity of the model The reason for this behaviour is that in
can be proved with any dispersing a very long dispersion all agglomerates
instrument. have the opportunity to get into the
For reasons of simplicity, one should zones of the maximum shearing effect. 19
2 PASS AND RE-CIRCULATION METHOD

In principle, two methods can be distinguished in the


operation of the DISPERMAT SL bead mills. Either, the
complete millbase is collected after each pass through the
bead mill (single or multiple pass), or else the millbase is
fed directly back into the supply vessel from the outlet of the
milling chamber (re-circulation method).

In the single pass method, the product is filled into a


feed vessel and pressed through the milling chamber via
” Re-circulation preferred…

continuously adjustable pneumatic transport system or with Easily dispersible pigments can often be processed with the
the feed press. single pass method, whereas with pigments that are more or
In the re-circulation method, the product is filled into the feed difficult to disperse the re-circulation method is more efficient.
vessel and repeatedly pumped through the milling chamber
with an integrated, continuously adjustable pumping and Over a period of time the re-circulation method ensures , that
stirring system. every agglomerate will get into a dispersion situation.
Here, it has spatial and energetic condition and is dispersed.
The method of operation to be chosen depends on the type This means that the re-circulation system is more efficient
of task. and economic.

Schematic view of pass method Schematic view of re-circulation method

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20
21
Bead mill DISPERMAT SL‒nano
RELATIONSHIP BETWEEN POWER INPUT
2 AND DISPERSION RESULT

The higher the realised mechanical power input the higher


is the energy, brought into the container. It does not matter
Only mechanical power whether the power input which leads to the existing energy
density, is applied with a high speed and low torque or vice
input is important… versa.

To get all agglomerates at least one time in a zone of


highest energy density, which means that if the dispersion
Basic scientific research has shown that the mechanical condition with longer dispersion time does not change at
power that is transferred into the millbase is closely related a given bead filling charge and sufficient long dispersion
to the dispersion result. The mechanical power determines time, the dispersion result depends only on the amount of the
the energy that is transmitted by the agitator via the grinding mechanical power.
beads to the product.
The torque therefore depends directly on the flow
The power P is calculated from the speed n of the agitator characteristics of the millbase. If the viscosity changes during
and the torque M generated on the agitator according to the dispersion at constant speed, the power input changes
following equation: automatically.

P=2πnM Dispersion with constant speed

100%
P = power [Nm/s = J/s = W]
π = 3.141... Speed
n = speed [1/s]
M = torque [Nm] Temperature

Power

Torque

0%
Time
22
If the viscosity decreases during dispersion, the mechanical Apart from the agitator geometry and the viscosity of the
power drops, and if it increases, the mechanical power rises. millbase, the torque transmitted by the shaft onto the millbase
If the formulation is operated under a stronger cooling, the also depends on the type, quantity and size of the grinding
mechanical power input is higher due to the higher viscosity beads. High bead filling volumes increase the torque on
of the mill base. the agitator shaft and also increase the probability that
With a lower cooling the power input is correspondingly agglomerates come into a spatial dispersion situation.
lower.

This for example, is the reason why dispersion results may


literally depend on the season, because in winter, the cooling
water may be much colder than in summer!

The DISPERMAT SL solves this problem by enabling the


mechanical power input for dispersion to be pre-set.
During dispersion the torque of the rotor is continuously
measured and the speed controlled, so that the product of n
and M leads to precisely the pre-set mechanical power.

Dispersion with constant power Dependence of the dispersion result on the power input

100% 100%

Speed 1000 W
600 W
Temperature
300 W

Power 150 W

Torque

0% 0%
Time Time
23
2 STEPS TO IMPROVE DISPERSION RESULTS

The relationship between the effects of energy and time How can the dispersion result be improved ?
enables the dispersion process to be optimised.
If the required dispersion result is not achieved, it must first be increased dispersion time smaller beads or beads
determined whether this can be changed by increasing the with a higher density
dispersion time.
RPM increased the power input
by increasing the speed increased bead charge
The power input can be increased with higher speeds.
This will normally improve the dispersion. Smaller beads
and/or beads with a higher density beads (e.g. zircon oxide NM increased the power input modification of the
or steel) can also improve the dispersion result. by increasing the torque millbase (e.g. by using
additives)
Further, the bead charge can be increased to about 80%.
In order to operate the bead mill economically, dispersion improved cooling
should be made with as much solid matter as possible.
If after the dispersion there is some flocculation, a suitable
dispersing aid may help. A partial modification of the
millbase formulation by using
more suitable raw materials
can also be made.

24
Bead mill DISPERMAT RS
TRANSFER OF LABORATORY TESTS
TO INDUSTRIAL PRODUCTION

Considering the many influences on the spatial and energetic


conditions of dispersion and their difference in various bead
mills, it is not surprising to learn that the transfer of the results
from one machine to another is not automatically possible.
Even if the same bead mill is used, but with different discs,
the dwell time distribution of the millbase will be changed
and, despite the same number of passes (single pass) or
same dispersion time (re-circulation mode) the dispersion
result will also change.

Nevertheless, if different bead mills are to be compared with


each other, it is generally the case that production machines
have less adjustment possibilities. First, the typical result has
to be determined on a known millbase.

With this typical result (e.g. fineness), a test series should


be made with the DISPERMAT SL laboratory bead mill
with M‒control. The impeller speed should be adjusted
and the dispersion continued until the result matches that
which can be achieved in production. If a DISPERMAT SL
with C‒control is available, the tests should be made using
mechanical power input.
When comparable results have been achieved, the settings
on the DISPERMAT SL can be used to determine results that
are possible in production.

When milling with constant power input, not only can


complicated dispersion processes be performed in a
reproducible manner, but different dispersions can be
compared exactly.
The dispersion results from production machinery are easily
repeated with the DISPERMAT SL and formulations worked
out in the laboratory can be transferred into production. With
the DISPERMAT SL, problematic parameters like product
temperature, cooling water temperature or rheological
behaviour of the mill base, may be ignored as long as they
do not reach limits critical for the product.
25
Basket mill TORUSMILL SK
VMA‒GETZMANN GMBH
Euelerhammerstr. 13
51580 Reichshof
Germany
Tel +49 2296 - 8030
Fax +49 2296 - 80333
[email protected]
www.vma-getzmann.de

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