Plate out in PVC Extrusion – A

never ending Story?

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of filler, Influence of
Titanium dioxide lubricants and
and modifier soaps

Influence of extrusion Influence of water

Summary The lab method

The mechanisms

Cover of QUEEN’s Vinyl

“Innuendo” © EMI

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Bohemian Rhapsody

Is this the real life

Is this just fantasy
Caught in a landslide
No escape from reality
Open your eyes
Look up to the skies and see
I'm just a poor boy, I need no sympathy
Because I'm easy come, easy go,
A little high, little low,
Anyway the wind blows, doesn't really matter to me,
To me …

Dr.Mercury,
F. M. Schiller,
R. Taylor,
Dr. B. Pelzl,
J. Deacon,
R. Haberleitner
B. May (Queen)
(Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Plate out in the Die

Extrusion direction

Extruder drawing: G. Aylett &

Associate/AUS

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Plate out in the Die

Analytical results

Examples for profiles/%

Titanium 12 15 22 11 5 10 7 10 16
Lead 21 23 31 34 36 31 - - -
Calcium 15 11 5 8 13 12 17 19 12
Zinc - - - - - - 4 1 2
Organica 17 20 14 22 16 16 29 22 35
Chloride pos. pos. 8 pos. 0,3 0,4 pos. pos. pos.

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Plate out in the Calibrator

Extrusion direction Water Calibrator

Extruder steam

Water steam distillation

Exceed of solubility

Deposites

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Plate out analysis

Plate out composition: - inorganics

-- Chlorine
-- Calcium, Zinc, Lead
-- Titanium
- organics
-- short-chain fatty acids
-- low melting lubricants
-- costabilisers
-- antioxidants

Solution of problem: - optimisation of mixing, extruder set up …

- optimisation of dryblend and stabiliser compostion
- addition of antiplate out-additives

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Chemson’s method
Breaker Plate
#1
(Die)

#3

#4

Adaptor
#2

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Reliability of the Method

20

Derivative plot
C u m u la tiv e fr e q u e n c y
3
15

10 2

5 1

Average = 8.03
Std. deviation = 0.60 0 0
Standard error = 0.14
6,75 7,25 7,75 8,25 8,75 9,25
Plate out
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of Water

13

12
Plate out rating

11
10
9
8
7
0 0,1 0,2 0,3
phr water
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Dependency on phr PE wax
16 out
Plate 16 out
Plate
PE 1
14 14

12 12

10 10

8 8

6 6

4 4
0,1 0,2 0,3 0,4 phr PE0,5
1 0,1 0,2 0,3 0,4 phr CaSt
0,5
16 out
Plate 16 out
Plate
PE 1
14 14

12 12

10 10

8 8

6 6 PE 1

4 4
0,1 0,2 0,3 0,4 phr PbSt
0,5 190 191 192 193 194 195 MT/°C
196

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Dependency on phr PE wax
16 out
Plate 16 out
Plate

14 14

12 12

10 10

8 8

6 6

4 4
0,1 0,2 0,3 0,4 phr PE0,5
1 0,1 0,2 0,3 0,4 phr PE0,5
2

16 out
Plate 16 out
Plate

14 14

12 12

10 10

8 8

6 6

4 4
0,1 0,2 0,3 0,4 phr PE0,5
3 0,1 0,2 0,3 0,4 phr PE0,5
4

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 The test formulation

100,00 phr PVC [k=67]

1,00 phr processing aid
0,25 phr NLS
0,50 phr DBLS
3,00 phr DBLP
0,25 phr Calcium stearate
0,20 phr PE wax
0,20 phr oxidised PE wax
2,00 … 5,00 phr Titanium dioxide (Supplier A)
5,00 … 8,00 phr acrylic modifier
3,00 … 8,00 phr filler with coating

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of filler

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
3,50 phr Titanium dioxide (Supplier A)
6,50 phr acrylic modifier
235 Nm extrusion torque
215 Bar extrusion pressure 18
16
14
Plate out value
12
10
8
6
4
2
0
3,00 4,50 6,00 phr7,50
filler 9,00
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of filler

10

8
Plate out value

0
0,00 2,75 5,50 8,25 11,00 13,75
phr filler

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of Titanium dioxide

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
5,50 phr chalk
6,50 phr acrylic modifier
235 Nm extrusion torque
215 bar extrusion pressure 16
14
12
Plate out value
10
8
6
4
2
0
3,00 3,50 4,00 phr4,50
TiO2 5,00
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of Titanium dioxide manufacturer

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
5,50 phr chalk
6,50 phr acrylic modifier
3,50 or 7,00 phr Titanium dioxide
235 Nm extrusion torque
215 bar extrusion pressure

20

15

plate out
10
7,0 phr 5
3,5 phr
0
Supplier A Supplier B Supplier C
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of acrylic modifier

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
5,50 phr chalk
3,50 phr Titanium dioxide (supplier A)
235 Nm extrusion torque
215 bar extrusion pressure 18
16
14
Plate out value
12
10
8
6
4
2
0
5,00 6,00 7,00 phr modifier
8,00 9,00
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of extrusion torque

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
5,50 phr chalk
3,50 phr Titanium dioxide (supplier A)
6,50 phr acrylic modifier
215 bar extrusion pressure 18
16
14
Plate out value
12
10
8
6
4
2
0
215 225 235 245 Nm 255
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of extrusion pressure

100,00 phr PVC [k=67]

5,40 phr Lead stabiliser
5,50 phr chalk
3,50 phr Titanium dioxide (supplier A)
6,50 phr acrylic modifier
235 Nm extrusion torque 18
16
14
Plate out value
12
10
8
6
4
2
0
195 205 215 225 bar 235
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Influence of mixting procedure

18
16
14
12
Plate out

10
8
6
4
2
0
ng

ng

ng

ng
al

al

al

al
rm

rm

rm

rm
i

i
tch

tch

tch

tch
no

no

no

no
ba

ba

ba

ba
le

le

le

le
ub

ub

ub

ub
do

do

do

do
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Summary

1. Water increases the plate out both in die and calibrator.

2. Plate out decreases the gloss.
3. Lippoldt’s mechanism applies also to lead-based systems.
4. PE waxes, Calcium and Lead stearates form alloys!
5. The higher the filler dosage is the less plate out will result.
6. The more Titanium dioxide was added the more plate out will occur.
7. Acrylic modifier has probably no influence on the plate out.
8. A higher extrusion torque causes more plate out.
9. The extrusion pressure has no or only a small influence on plate out.
10. An increase of mass temperature causes in the most cases more plate out.
11. The plate out-method allows to characterise the processing window of waxes
and soaps.

Anyway the wind blows …

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 Thank you for your
kind attention

Cover of QUEEN’s Vinyl

“Innuendo” © EMI

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 DoE

Statistical Design of Rheological Experiments (1)

Variables: - metal soap Responses: - Extrusion torque

- internal lubricant - Extrusion pressure
- paraffin - Plate out

Number of Experiments: 8+1

Used Softeware: ECHIP

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 DoE

Statistical Design of Rheological Experiments (2)

- Metal soap 0.3 ... 0.6 phr

- paraffin 0.2 ... 0.7 phr

0.6
- internal 0.1 ... 0.6 phr

Paraffin

6
Mixture 1 2 3 4 5 6 7 8

0.
al
rn
te
in
soap 0.3 0.6 0.3 0.6 0.3 0.6 0.3 0.6
0 Metal soap 0.7
Wax B 0.2 0.2 0.7 0.7 0.2 0.2 0.7 0.7
Wax C 0.1 0.1 0.1 0.1 0.6 0.6 0.6 0.6

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 DoE

Statistical Design of Rheological Experiments (3) - Reliability

110 210 extrusion-pressure *

Fitted values

Fitted values
extrusion-torque
*
100 * *
180

* *
90 * *
***
*
150 *
80
* *
*
*
*
70 12
70 80 90 100 110 0 120 150 180 210
Observations Observations

Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow
 DoE

Statistical Design of Rheological Experiments (4) - Reliability

20 *
Fitted values Plate-out

15

*
*
** *
*
10 *
*

5
5 10 15 20

Observations
Dr. M. Schiller, Dr. B. Pelzl, R. Haberleitner (Chemson Group), Dr. Y. Salamonov (Elnova) Profiles 2006, Moscow