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LW-16-18
Function of Waxes in
PVC Pipe Extrusion
Thomas C. Pedersen
Rheogistics LLC
Picayune, MS USA
2016 AFPM Lubricants and Waxes...
Rigid PVC Lubricants
• Paraffin waxes have been used for more than 40 years to
lubricate rigid PVC.
2016 AFPM Lubricants a...
Rigid PVC Lubricants
• Paraffin Waxes
• Calcium Stearate
• Polyethylene Waxes
• MontanWaxes – the earliest standard
• Hoec...
Rigid PVC Lubricants
• Prevent rigid PVC from degrading when heated and
sheared.
• Define rheology and control fusion.
• A...
Rigid PVC
•Most rigid PVC properties are affected
in one way or another by the lubricant
system.
•Getting and keeping thin...
PolyVinyl Chloride
Rigid PVC has great properties
• Typical 7000+ psi tensile strength
• Excellent stiffness
• Excellent i...
PVC Resin
2016 AFPM Lubricants and Waxes Meeting
PVC Compound
2016 AFPM Lubricants and Waxes Meeting
Processing Rigid PVC
• Rigid PVC products are formed by heating and compressing PVC compounds
into desired shapes.
• The c...
PVC Processing
The 0.7-1 micron PVC primary particles are thought to be
the primary flow units during rigid PVC processing...
Rigid PVC Fusion in Extrusion
2016 AFPM Lubricants and Waxes Meeting
Effects of Fusion Levels on Physical
Properties
Tensile Properties
• Increase with increasing fusion
Impact Properties
• P...
Extruder Energy Balance
2016 AFPM Lubricants and Waxes Meeting
Typical Rigid PVC Pipe Formulation
PVC Resin
Tin Stabilizer
Lubricants
Calcium Carbonate
Pigments
2016 AFPM Lubricants and...
2016 AFPM Lubricants and Waxes Meeting
Plastic Pipe Institute’s
TR-2 PVC Pipe Formulation
Ingredient Usage Level
PVC Resin...
Typical Rigid PVC Lubricant System
• Paraffinic Hydrocarbon Wax
• Refined from crude or synthetic based on ethylene or
met...
Plastic Pipe Institute
TR-2
Part A.3 Paraffinic HydrocarbonWax
Specification
2016 AFPM Lubricants and Waxes Meeting
2016 AFPM Lubricants and Waxes Meeting
Formulating waxes to meet
the PPI specification will
result in rigid PVC
formulations with different
processing characteri...
2016 AFPM Lubricants and Waxes Meeting
If formulating waxes for rigid PVC,
keep in mind what MarkTwain
said:
“It ain't wha...
2016 AFPM Lubricants and Waxes Meeting
The only reliable predictor of
hydrocarbon wax performance in
rigid PVC:
The size, ...
Typical Rigid PVC Lubricant System
• Paraffinic Hydrocarbon Wax
• Refined from crude or synthetic based on ethylene or
met...
Rigid PVC Lubricants
Product Options
• Individual Ingredients
• Combinations of multiple lubricants (Paraffin, oPE, etc.)
...
Fusion Characterization in the Lab
Torque Rheometer
• Fixed volume heated chamber
• Work imparted into PVC compound by mix...
Trial PVC Compound
• PVC Resin 100 parts
• Stabilizer 0.50 phr
• Wax 1.30 phr
• Calcium Stearate 0.65 phr
• Oxidized PEWax...
Paraffin Waxes
Paraffin waxes are mixtures of branched and straight chain molecules
Normal Straight Chain Content
CH3CH2CH...
Effect ofWax Molecule Size on Rheology
Carbon Number FusionTime FusionTorque Equil.Temp
26 166 sec 21.3 Nm >195°C.
32 352 ...
2016 AFPM Lubricants and Waxes Meeting
Lubricants are
Mechanical Stabilizers
• Lubricants prevent rigid PVC from degrading when
heated and sheared.
• Lubricants ...
Mechanical Stabilization of Rigid PVC
Recent Rheogistics Study
Could rigid PVC be processed without a conventional heat
st...
2016 AFPM Lubricants and Waxes Meeting
Plastic Pipe Institute’s
TR-2 PVC Pipe Formulation
Ingredient Usage Level
PVC Resin...
PPI PVC Pipe Range Composition
Lubrication Limits
2016 AFPM Lubricants and Waxes Meeting
Minimum
Allowable
Lubricants,
0.6...
Mechanical Stabilization of Rigid PVC
2016 AFPM Lubricants and Waxes Meeting
PipeGrade PVC Resin 100.0 parts
RX-165 Paraff...
Rigid PVC – Higher Stabilizer
2016 AFPM Lubricants and Waxes Meeting
0.50 phr
0.25 phr
Rigid PVC – Lower Stabilizer
2016 AFPM Lubricants and Waxes Meeting
0.125 phr
0.0625 phr
Rigid PVC – Lubricants Only
2016 AFPM Lubricants and Waxes Meeting
ZERO Tin
ReducingTin Stabilizer
• Shifts rheology
• Fusion time and torques remain remarkably similar
• Post fusion torque decrease...
Mechanical Stabilization of Rigid PVC
Color Development
2016 AFPM Lubricants and Waxes Meeting
Mechanical Stabilization of Rigid PVC
Color Development
• As the level of tin stabilizer is reduced, color develops
more q...
Conclusions
• The PVC Industry is a large application for paraffin and
hydrocarbon waxes.
• Simple alkanes (paraffin waxes...
Conclusions
• Waxes with carbon numbers of C30 to C34 work best as
primary PVC lubricants in North America’s tin stabilize...
Conclusions
• The lubricant system is adjusted to tune the formulation to
the heating and shearing characteristics of the ...
Conclusions
• Understanding and managing lubricant performance in
rigid PVC is very complex.
• The PVC industry requires i...
Conclusions
•The paraffin wax, calcium stearate, and
oxidized polyethylene wax long used in the
USA is an excellent starti...
References
T. C. Pedersen, “Process and Material Considerations in the Industrial
Application of Lubricants in Rigid PVC E...
2016 AFPM Lubricants and Waxes Meeting
Thank You!
Technology for Better Rigid PVC
Function of Waxes in PVC Pipe Extrusion
Function of Waxes in PVC Pipe Extrusion
Function of Waxes in PVC Pipe Extrusion
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Function of Waxes in PVC Pipe Extrusion

  1. 1. LW-16-18
  2. 2. Function of Waxes in PVC Pipe Extrusion Thomas C. Pedersen Rheogistics LLC Picayune, MS USA 2016 AFPM Lubricants and Waxes Meeting
  3. 3. Rigid PVC Lubricants • Paraffin waxes have been used for more than 40 years to lubricate rigid PVC. 2016 AFPM Lubricants and Waxes Meeting
  4. 4. Rigid PVC Lubricants • Paraffin Waxes • Calcium Stearate • Polyethylene Waxes • MontanWaxes – the earliest standard • Hoechst Wax E & OP • Esters of Montanic acid • Fatty Acid Esters • Derived from natural oils and fats • Amide Waxes • Ethylene bisstearamide wax 2016 AFPM Lubricants and Waxes Meeting
  5. 5. Rigid PVC Lubricants • Prevent rigid PVC from degrading when heated and sheared. • Define rheology and control fusion. • Allow the compound to be adjusted to the process. • The keys to better rigid PVC products and processing. 2016 AFPM Lubricants and Waxes Meeting
  6. 6. Rigid PVC •Most rigid PVC properties are affected in one way or another by the lubricant system. •Getting and keeping things right is a constant balancing act. 2016 AFPM Lubricants and Waxes Meeting
  7. 7. PolyVinyl Chloride Rigid PVC has great properties • Typical 7000+ psi tensile strength • Excellent stiffness • Excellent impact strength • Very good weatherability • Excellent cost performance 2016 AFPM Lubricants and Waxes Meeting
  8. 8. PVC Resin 2016 AFPM Lubricants and Waxes Meeting
  9. 9. PVC Compound 2016 AFPM Lubricants and Waxes Meeting
  10. 10. Processing Rigid PVC • Rigid PVC products are formed by heating and compressing PVC compounds into desired shapes. • The compound is compressed from a bulk density of approximately 0.50 gm/ml to a product density of approximately 1.40 gm/ml • PVC is heated to ca. 400°F by mechanical shear and heat transfer. • During processing, PVC is exposed to pressures of 2000 to 4000 psi. 2016 AFPM Lubricants and Waxes Meeting
  11. 11. PVC Processing The 0.7-1 micron PVC primary particles are thought to be the primary flow units during rigid PVC processing 2016 AFPM Lubricants and Waxes Meeting
  12. 12. Rigid PVC Fusion in Extrusion 2016 AFPM Lubricants and Waxes Meeting
  13. 13. Effects of Fusion Levels on Physical Properties Tensile Properties • Increase with increasing fusion Impact Properties • Peak at an intermediate level of fusion 2016 AFPM Lubricants and Waxes Meeting
  14. 14. Extruder Energy Balance 2016 AFPM Lubricants and Waxes Meeting
  15. 15. Typical Rigid PVC Pipe Formulation PVC Resin Tin Stabilizer Lubricants Calcium Carbonate Pigments 2016 AFPM Lubricants and Waxes Meeting
  16. 16. 2016 AFPM Lubricants and Waxes Meeting Plastic Pipe Institute’s TR-2 PVC Pipe Formulation Ingredient Usage Level PVC Resin 100.0 parts Tin Stabilizer 0.30 – 1.00 phr Paraffin Wax 0.60 – 1.50 phr Polyethylene Wax 0.00 – 0.30 phr Calcium Stearate 0.40 – 1.50 phr Calcium Carbonate 0.00 – 5.00 phr Titanium Dioxide 0.50 – 3.00 phr Process Aid 0.00 – 2.00 phr
  17. 17. Typical Rigid PVC Lubricant System • Paraffinic Hydrocarbon Wax • Refined from crude or synthetic based on ethylene or methane • Typical C32H66 • Calcium Stearate • Calcium salt of acid from natural fats and oils • Ca(C18H35O2)2 • Oxidized PEWax • Ethylene based • C100+H200+O? 2016 AFPM Lubricants and Waxes Meeting
  18. 18. Plastic Pipe Institute TR-2 Part A.3 Paraffinic HydrocarbonWax Specification 2016 AFPM Lubricants and Waxes Meeting
  19. 19. 2016 AFPM Lubricants and Waxes Meeting
  20. 20. Formulating waxes to meet the PPI specification will result in rigid PVC formulations with different processing characteristics and physical properties. 2016 AFPM Lubricants and Waxes Meeting
  21. 21. 2016 AFPM Lubricants and Waxes Meeting If formulating waxes for rigid PVC, keep in mind what MarkTwain said: “It ain't what you don't know that gets you into trouble. It's what you know for sure that just ain't so.”
  22. 22. 2016 AFPM Lubricants and Waxes Meeting The only reliable predictor of hydrocarbon wax performance in rigid PVC: The size, shape, and numbers of wax molecules.
  23. 23. Typical Rigid PVC Lubricant System • Paraffinic Hydrocarbon Wax • Refined from crude or synthetic based on ethylene or methane • Typical C32H66 • Calcium Stearate • Calcium salt of acid from natural fats and oils • Ca(C18H35O2)2 • Oxidized PEWax • Ethylene based • C100+H200+O? 2016 AFPM Lubricants and Waxes Meeting
  24. 24. Rigid PVC Lubricants Product Options • Individual Ingredients • Combinations of multiple lubricants (Paraffin, oPE, etc.) • Total systems include paraffin, oPE, and calcium stearate • Dust free, free flowing, fully melting calcium stearate 2016 AFPM Lubricants and Waxes Meeting
  25. 25. Fusion Characterization in the Lab Torque Rheometer • Fixed volume heated chamber • Work imparted into PVC compound by mixing blades • Measure torque required to turn the blades and melt temperature 2016 AFPM Lubricants and Waxes Meeting
  26. 26. Trial PVC Compound • PVC Resin 100 parts • Stabilizer 0.50 phr • Wax 1.30 phr • Calcium Stearate 0.65 phr • Oxidized PEWax 0.15 phr • Calcium Carbonate 5.00 phr • Titanium Dioxide 0.50 phr 2016 AFPM Lubricants and Waxes Meeting
  27. 27. Paraffin Waxes Paraffin waxes are mixtures of branched and straight chain molecules Normal Straight Chain Content CH3CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH3 Branched or “Non-normal” Content CH3 CH3CH2CH2CH2CH2CH2CH2CH1CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH1CH2CH2CH2CH2CH2CH2CH2CH3 CH2 CH2 CH3 Over 1,000,000 different C32+ H66+ molecular structures are possible. 2016 AFPM Lubricants and Waxes Meeting
  28. 28. Effect ofWax Molecule Size on Rheology Carbon Number FusionTime FusionTorque Equil.Temp 26 166 sec 21.3 Nm >195°C. 32 352 sec 15.2 Nm 188°C. 40 2,120 sec 10.1 Nm 188°C. 100+ (PEWax) 182 sec 18.9 Nm >195°C. 2016 AFPM Lubricants and Waxes Meeting C26 more soluble in rigid PVC. C40+ insoluble in rigid PVC.
  29. 29. 2016 AFPM Lubricants and Waxes Meeting
  30. 30. Lubricants are Mechanical Stabilizers • Lubricants prevent rigid PVC from degrading when heated and sheared. • Lubricants are often adjusted to eliminate shear burning issues. • In the USA, many rigid PVC formulations run very low levels of tin stabilizer and rely on lubrication for adequate stability. 2016 AFPM Lubricants and Waxes Meeting
  31. 31. Mechanical Stabilization of Rigid PVC Recent Rheogistics Study Could rigid PVC be processed without a conventional heat stabilizer? What happens when heat stabilizer is reduced or eliminated? 2016 AFPM Lubricants and Waxes Meeting
  32. 32. 2016 AFPM Lubricants and Waxes Meeting Plastic Pipe Institute’s TR-2 PVC Pipe Formulation Ingredient Usage Level PVC Resin 100.0 parts Tin Stabilizer 0.30 – 1.00 phr Paraffin Wax 0.60 – 1.50 phr Polyethylene Wax 0.00 – 0.30 phr Calcium Stearate 0.40 – 1.50 phr Calcium Carbonate 0.00 – 5.00 phr Titanium Dioxide 0.50 – 3.00 phr Process Aid 0.00 – 2.00 phr
  33. 33. PPI PVC Pipe Range Composition Lubrication Limits 2016 AFPM Lubricants and Waxes Meeting Minimum Allowable Lubricants, 0.60/0.00/0.40 Maximum Allowable Lubricants, 1.50/0.30/1.50
  34. 34. Mechanical Stabilization of Rigid PVC 2016 AFPM Lubricants and Waxes Meeting PipeGrade PVC Resin 100.0 parts RX-165 Paraffin Lubricant 1.30 phr RX-215 Oxidized Polyethylene 0.15 phr Calcium Stearate 0.65 phr Calcium Carbonate 5.00 phr Titanium Dioxide 1.00 phr 19% MethylTin Stabilizer 0.50 phr, 0.25 phr, 0.125 phr, 0.0625 phr and zero Processed on a BrabenderTorque Rheometer for one hour (65 gram charge, 60 rpm, 175° set point, no cooling)
  35. 35. Rigid PVC – Higher Stabilizer 2016 AFPM Lubricants and Waxes Meeting 0.50 phr 0.25 phr
  36. 36. Rigid PVC – Lower Stabilizer 2016 AFPM Lubricants and Waxes Meeting 0.125 phr 0.0625 phr
  37. 37. Rigid PVC – Lubricants Only 2016 AFPM Lubricants and Waxes Meeting ZERO Tin
  38. 38. ReducingTin Stabilizer • Shifts rheology • Fusion time and torques remain remarkably similar • Post fusion torque decrease occurs quicker • Longer term melt torque and temperature remain remarkably stable • Melt exhibits more “chatter” 2016 AFPM Lubricants and Waxes Meeting
  39. 39. Mechanical Stabilization of Rigid PVC Color Development 2016 AFPM Lubricants and Waxes Meeting
  40. 40. Mechanical Stabilization of Rigid PVC Color Development • As the level of tin stabilizer is reduced, color develops more quickly. • When tin stabilizer is not present, early pinking becomes an issue. 2016 AFPM Lubricants and Waxes Meeting
  41. 41. Conclusions • The PVC Industry is a large application for paraffin and hydrocarbon waxes. • Simple alkanes (paraffin waxes) are very versatile and effective primary lubricants for rigid PVC. 2016 AFPM Lubricants and Waxes Meeting
  42. 42. Conclusions • Waxes with carbon numbers of C30 to C34 work best as primary PVC lubricants in North America’s tin stabilized formulations. • In addition to their role in managing rheology, lubricants serve as mechanical stabilizers. • Rigid PVC free of conventional heat stabilizers may be processed under certain conditions. 2016 AFPM Lubricants and Waxes Meeting
  43. 43. Conclusions • The lubricant system is adjusted to tune the formulation to the heating and shearing characteristics of the customer’s processing equipment. • Changes in any material or any piece of equipment in a customer’s plant results in the need for a lubricant adjustment. 2016 AFPM Lubricants and Waxes Meeting
  44. 44. Conclusions • Understanding and managing lubricant performance in rigid PVC is very complex. • The PVC industry requires in-depth technical support and service. 2016 AFPM Lubricants and Waxes Meeting
  45. 45. Conclusions •The paraffin wax, calcium stearate, and oxidized polyethylene wax long used in the USA is an excellent starting point for alternate stabilization systems. 2016 AFPM Lubricants and Waxes Meeting
  46. 46. References T. C. Pedersen, “Process and Material Considerations in the Industrial Application of Lubricants in Rigid PVC Extrusion”, Journal ofVinyl Technology, 6, 104 (1984) J.W. Summers, “Lubrication Mechanism in Poly (Vinyl Chloride) Compounds: Understanding theThree Distinct Roles of Lubricants” Antec 2006, Society of Plastics Engineers. P. Benjamin, “The Influence of Processing on the Properties of PVC Pipe”, International Conference on PVC Processing, 6 & 7 April 1978,The Plastics and Rubber Institute. TR-2, Plastic Pipe Institute PVC Pipe Range Composition, List of Qualified Ingredients, 19 March 2013, Plastics Pipe Institute, Irving,TX USA 2016 AFPM Lubricants and Waxes Meeting
  47. 47. 2016 AFPM Lubricants and Waxes Meeting Thank You! Technology for Better Rigid PVC
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Function of Waxes in PVC Pipe Extrusion

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