Plate out in PVC Extrusion A never ending Story?
Influence of filler, Titanium dioxide and modifier Influence of extrusion Influence of lubricants and soaps Influence of water Summary The lab method The mechanisms Cover of QUEEN s Vinyl Innuendo EMI
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. F. Mercury, M. Schiller, R. Taylor, Dr. B. Pelzl, J. Deacon, R. Haberleitner B. May (Queen) (Chemson Group), Dr. Y. Salamonov (Elnova)
Plate out in the Die Extrusion direction Extruder drawing: G. Aylett & Associate/AUS
Plate out in the Die Analytical results Examples for profiles/% Titanium 15 22 11 5 7 1 Lead 21 23 31 3 3 31 - - - Calcium 15 11 5 13 17 19 Zinc - - - - - - 1 2 Organica 17 20 1 22 1 1 29 22 35 Chloride pos. pos. pos. 0,3 0, pos. pos. pos.
Plate out in the Calibrator Extrusion direction Extruder Water steam Calibrator Water steam distillation Exceed of solubility Deposites
Plate out analysis Plate out composition: Solution of problem: - inorganics -- Chlorine -- Calcium, Zinc, Lead -- Titanium - organics -- short-chain fatty acids -- low melting lubricants -- costabilisers -- antioxidants - optimisation of mixing, extruder set up - optimisation of dryblend and stabiliser compostion - addition of antiplate out-additives
Chemson s method #1 (Die) Breaker Plate #3 # #2 Adaptor
Reliability of the Method C u m u la tiv e fr e q u e n c y 20 15 5 3 2 1 Derivative plot Average =.03 Std. deviation = 0.0 Standard error = 0.1 0,75 7,25 7,75,25,75 9,25 Plate out 0
Influence of Water 13 Plate out rating 11 9 7 0 0,1 0,2 0,3 phr water
Dependency on phr PE wax Plate 1 out 1 Plate 1 out 1 PE 1 Plate 1 out 1 0,1 0,2 0,3 0, phr PE 0,5 1 PE 1 Plate 1 out 1 0,1 0,2 0,3 0, phr CaSt 0,5 PE 1 0,1 0,2 0,3 0, phr PbSt 0,5 190 191 192 193 19 195 MT/ C 19
Dependency on phr PE wax Plate 1 out 1 Plate 1 out 1 0,1 0,2 0,3 0, phr PE 0,5 1 0,1 0,2 0,3 0, phr PE 0,5 3 Plate 1 out 1 Plate 1 out 1 0,1 0,2 0,3 0, phr PE 0,5 2 0,1 0,2 0,3 0, phr PE 0,5
The test formulation 0,00 phr PVC [k=7] 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) 5,00,00 phr acrylic modifier 3,00,00 phr filler with coating
Influence of filler 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 3,50 phr Titanium dioxide (Supplier A),50 phr acrylic modifier 235 Nm extrusion torque 215 Bar extrusion pressure 1 Plate out value 1 1 2 0 3,00,50,00 phr 7,50 filler 9,00
Influence of filler Plate out value 2 0 0,00 2,75 5,50,25 11,00 13,75 phr filler
Influence of Titanium dioxide 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 5,50 phr chalk,50 phr acrylic modifier 235 Nm extrusion torque 215 bar extrusion pressure Plate out value 1 1 2 0 3,00 3,50,00 phr,50 TiO 2 5,00
Influence of Titanium dioxide manufacturer 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 5,50 phr chalk,50 phr acrylic modifier 3,50 or 7,00 phr Titanium dioxide 235 Nm extrusion torque 215 bar extrusion pressure 20 7,0 phr 3,5 phr Supplier A Supplier B Supplier C 15 5 0 plate out
Influence of acrylic modifier 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 5,50 phr chalk 3,50 phr Titanium dioxide (supplier A) 235 Nm extrusion torque 215 bar extrusion pressure 1 Plate out value 1 1 2 0 5,00,00 7,00 phr modifier,00 9,00
Influence of extrusion torque 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 5,50 phr chalk 3,50 phr Titanium dioxide (supplier A),50 phr acrylic modifier 215 bar extrusion pressure 1 Plate out value 1 1 2 0 215 225 235 25 Nm 255
Influence of extrusion pressure 0,00 phr PVC [k=7] 5,0 phr Lead stabiliser 5,50 phr chalk 3,50 phr Titanium dioxide (supplier A),50 phr acrylic modifier 235 Nm extrusion torque 1 Plate out value 1 1 2 0 195 205 215 225 bar 235
Influence of mixting procedure normal double batching normal 1 1 1 2 0 Plate out double batching normal double batching normal double batching
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.. PE waxes, Calcium and Lead stearates form alloys! 5. The higher the filler dosage is the less plate out will result.. The more Titanium dioxide was added the more plate out will occur. 7. Acrylic modifier has probably no influence on the plate out.. A higher extrusion torque causes more plate out. 9. The extrusion pressure has no or only a small influence on plate out.. 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
Thank you for your kind attention Cover of QUEEN s Vinyl Innuendo EMI
DoE Statistical Design of Rheological Experiments (1) Variables: - metal soap - internal lubricant - paraffin Responses: - Extrusion torque - Extrusion pressure - Plate out Number of Experiments: +1 Used Softeware: ECHIP
DoE Statistical Design of Rheological Experiments (2) - Metal soap 0.3... 0. phr - paraffin 0.2... 0.7 phr Paraffin 0. - internal 0.1... 0. phr Mixture 1 2 3 5 7 soap 0.3 0. 0.3 0. 0.3 0. 0.3 0. 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. 0. 0. 0. internal 0. 0 Metal soap 0.7
Statistical Design of Rheological Experiments (3) - Reliability DoE Fitted values 1 extrusion-torque 0 90 0 70 70 0 90 0 1 Observations 10 150 0 0 150 10 2 Observations Fitted values 2 extrusion-pressure
Statistical Design of Rheological Experiments () - Reliability DoE Fitted values 20 15 Plate-out 5 5 15 20 Observations