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Optimization of Flame Retarded PP-Copolymer Compounds. By: Or Kariv Advisors: Dr. Fabian Rios Yoav Bar-Yaakov, Bromine Compounds LTD. Objectives. Finding an optimal formulation of PP copolymer with bromine based FR. Studying the influence of the FR on the compound’s properties.

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slide1

Optimization of Flame RetardedPP-Copolymer Compounds

By: Or Kariv

Advisors: Dr. Fabian Rios

Yoav Bar-Yaakov, Bromine Compounds LTD.

objectives
Objectives
  • Finding an optimal formulation of PP copolymer with bromine based FR.
  • Studying the influence of the FR on the compound’s properties.
  • Studying the influence of IM processing conditions on the compound.
introduction
Introduction
  • PP is known for its good mechanical and processing properties, but also for its high flammability.

Bromine FRs

  • C-Br present low bonding energy and therefore Br can readily be released.
  • FR molecular structure depends on the thermal stability required for the polymer.

Aromatic compounds high thermal stability

Aliphatic compounds high flame retardant efficiency

fr properties
FRproperties

FR-370

Tris- tribromoneopentyl phosphate

  • Thermal stability fits polymer processing temperature
  • Good synergy with the matrix
  • Good dispersion within the matrix
  • Non “blooming”
  • Good flame retardancy
  • Chemical flame inhibiting mechanism
slide5

Mechanism

Chain Scission & Flame poisoning: a competing reaction of HBr, with the radicals to create a less reactive radicals.

experimental
Experimental
  • Materials:
      • PP copolymer- grade SE- 50E ex by Carmel Olefins
      • FR-370- Tris- tribromoneopentyl phosphate by Bromine Compounds Ltd.
      • Free radical source (C-C initiator)
  • Equipment:
      • Injection molding machine, Arburg 500-150
      • Twin-screw extruder, Berstroff L/D=32
slide7

Methodology

  • Studying the influence of additives.
  • Optimized formulation:
  • UL-94: V-0 rating
  • Minimum additives content
  • Optimal balance of properties
  • Studying the effect of IM conditions.

Stage one-

Stage two-

slide8

Stage one:

Selecting the optimal formulation

Reference formulations:

results flammability properties
Results: Flammability Properties

LOI- limited oxygen index

  • Significant increase in the presence of FR
  • C-C influence insignificant.
results thermal properties
Results: Thermal Properties

HDT- heat deflection temperature

  • FR exhibits a significant increase of HDT
  • C-C has inverse effect

by causing the crystallinity degree to decrease

results rheological properties
Results: Rheological Properties

MFI- melt flow index

  • FR exhibits a plasticizing effect in high temperature
  • C-C causes MW reduction
results mechanical properties
Results: Mechanical Properties

Izod impact test

  • The FR causes a significant decrease of impact strength

Particles locate at amorphous phase and cause stress concentration

results mechanical properties1
Results: Mechanical Properties

Tensile modulus

  • FR causes a stiffening effect at room temperature
  • C-C causes MW reduction
finally
Finally…

Choosing optimal formulation

Balance between additives concentrations and properties

Minimum costs

Formulation Hcc14:

14% Br, 1.6% C-C

stage two doe for injection molding conditions
Stage two:DOE for injection molding conditions
  • Formulations: Hcc14 and 0cc20.

Independent variables:

  • A- Screw RPM
  • B- Back pressure
  • C- Injection speed
  • D- Melt temperature
  • E- Mold temperature
  • F- Holding pressure

Dependant variables:

  • Tensile strength
  • Tensile modulus
  • Impact strength
  • DSC: melting temperature

melting enthalpy

A six variables, two level screening design

slide17
Results
  • No reliable results were obtained from the experiment.

The reason

  • Experimental error larger than variables effects.
  • Little control over formulations processing.

Explanation

  • Plasticizing effect of the FR on polymer causing difficult processing.
doe results
DOE results

Smaller than experimental error → 0

Marginal → 0

conclusions
Conclusions
  • FR content affects polymer properties significantly.
  • FR content can be reduced by adding free radical source while maintaining flammability level.
  • Mechanical and rheological properties decrease.
  • Thermal properties increase.
  • An optimal formulation for flame retardant PP copolymer contains 14% Bromine (20% FR-370) and 1.6% C-C initiator.
  • While these compounds exhibit good FR properties, they are extremely difficult to process, limiting their commercial applications.
  • DOE analysis can be performed only on fully controllable processes.
further research
Further Research
  • More extensive research on the rheological properties of PP copolymer- FR compounds is required, using capillary and dynamic rheometers.
  • A capillary rheometer will show how viscosity changes with higher shearing rates similar to IM process, as opposed to MFI.
  • The processing problems of these compounds should be addressed, researched and improved to obtain compounds which are more commercially usable.
for all the help and support
For all the help and support…

Ita Finberg, Yaniv Hirschsohn, Izik, Meir & Smadar

Dr Iftah Nir, Dr Amos Ofir & Dr Anna Dotan

And especially to

Dr Fabian Rios from Shenkar

Yoav Bar- Yaakov and Racheli Rotem from ICL-IP

THANK YOU!

references
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