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  • Recent developments in flame retardants for sustainable fire safety solutions:

    Emerald Innovation 3000 polymeric flame retardant

    Presentation to AMI Masterbatch 2013 Patrick Jacobs, Technical Business Service EMEA Great Lakes Solutions, a Chemtura business

  • 2

    Agenda

    Chemtura / Great Lakes Solutions Overview

    Greener Innovation Strategies

    Emerald InnovationTM 3000 Polymeric Flame Retardant

    Introduction: structure

    Fire performance vs. HBCD / other aliphatic FRs

    Thermal stability in MB and at use levels

    Conclusions

  • Global specialty chemical company listed on the New York Stock Exchange (CHMT)

    Major markets served are energy, electronics, transportation, and agriculture

    Committed to global sustainability and engineering chemical solutions that meet our customers evolving needs

    More than 4,300 employees worldwide

    Manufactures in 31 countries and sells products in more than 100 countries

    Global headquarters in Philadelphia, Pennsylvania

    Regional headquarters and shared service centers in Sao Paulo, Brazil; Shanghai, China; Middlebury, Connecticut; and Manchester, United Kingdom

  • 4

    Great Lakes Solutions, an Industry Leader

    Electrical &

    Electronics

    Insulation &

    Furniture

    Automotive

    Fumigation Energy: Oilfield &

    Mercury Control

    Fine Chemical/

    Pharmaceutical

    Biocides Automotive Tires

    Fumigation

    Biocides

    Other

    Insulation &

    Furniture

    Electrical & Electronics

    Auto

    Fine Chem/ Pharma

    Energy

    Flame

    Retardants

    Brominated

    Performance

    Products

    KE

    Y B

    US

    INE

    SS

    ES

    INDUSTRIES SERVED

    Mercury control

    Greener innovation

    Rapid growth in electronics

    Flame retarded energy efficient

    thermal insulation

    Increased global fire safety

    standards

    KE

    Y G

    RO

    WT

    H

    DR

    IVE

    RS

  • 5

    How Do We Move Toward Environmentally Friendly, Sustainable FR Solutions?

    Great Lakes Solutions is applying a Greener is Better philosophy...

    Greener Innovation

  • 6

    Greener FR Design Strategy

    Greener alternatives that Achieve targeted fire safety standards

    Meet or exceed baseline performance and manufacturability

    Are cost effective based on total system cost

    Minimize transition costs

    Strive for zero environmental release VECAP to prevent release from manufacture to fabrication

    Durable & recyclable to allow low-risk rework and recycling

    Structures that are inherently Not persistance

    Not bioavailable

    Not toxic

  • 7

    The polymeric structure of Emerald Innovation 3000 renders it not readily bioavailable*, thus addressing the environmental concerns that threaten the sustainability of many current products.

    Emerald Innovation 3000 is an efficient, sustainable replacement for HBCD requiring minimal modification to current formulations or production processes.

    Applicable fire safety standards covering polystyrene foam insulation can be achieved with Emerald Innovation 3000.

    Synergists commonly used for EPS and XPS production are compatible with Emerald Innovation 3000.

    Our strategy of greener innovation provides you with proven, sustainable alternatives

    The Value of Emerald Innovation 3000

    * Per criteria described in US Federal Register notice 40 CFR 723

  • 8

    Results of Screening Versus Design for The Environment Assessment Framework

    vL= very Low

    L= Low

    vH= very High

    NE= no evidence

    Source: Davis, J.W. et. al., Strategic Approach Towards Developing More Environmentally

    Sustainable Flame Retardants, 12th Workshop on Brominated and Other Flame Retardants,

    2011

    PolyFR = Emerald Innovation 3000

    Persistent by Design, Required for Service Life &

    Stability

    Low to Very Low in All Health and Environmental Effects

  • 9

    Emerald Innovation 3000

    Property Emerald Innovation 3000

    Appearance Compacted powder

    Bromine, % 64

    Softening point, 0C 120

    5% wt loss, 0C (Thermogravimetric Analysis (@ 10 0C/min under N2)

    2620C

  • 10

    Emerald Innovation 3000 Flammability Performance Compared to HBCD

    Emerald Innovation 3000 demonstrates comparable fire retardant efficiency versus HBCD at similar bromine levels

  • 11

    Comparison to Partially Aliphatic Bromine Source

    Formulation % Br % Synergist DIN 4102 B2 Swiss Fire Testing

    (5.1)

    HBCD 1.60 - Pass Pass

    Emerald Innovation 3000 1.00 0,2 Pass Pass

    FR1 1.90 0,25 Fail Fail

    FR1 2,40 0.30 Fail Fail

    Data provided by the Dow Chemical Company

    FR1 = Tetrabromobisphenol A bis (2,3-dibromopropyl ether), a.k.a. PE-68

    Synergist = An organic compound having labile C-C linkages capable of generating radicals in the early

    stages of ignition process which can reduce the molecular weight of the host polymer.

    Aliphatic C-Br bonds are the key to efficiency in PS foams

    Only one half of the bromine in FR1 is aliphatic

    FR1 is not effective at >50% higher load level

  • 12

    Thermal Stability Testing

    Emerald Innovation 3000 is an efficient FR for extruded polystyrene (XPS) but lacks thermal stability, like HBCD, during processing

    Goal is to determine a suitable stabilization package for processing Emerald Innovation 3000.

    All formulations were run on a single screw extruder for multi-pass evaluation in Polystyrene Nova PS1600 @ 200C

    Pellets from extrusion pass 1, 3 & 5 were set aside for melt flow and color determination on molded plaques

  • 13

    Color and MFI Data 24-01 24-02 24-03 24-04 24-05 24-06 24-07 24-08 24-09 24-10

    % Emerald InnovationTM 3000 - 2 2 2 2 2 2 2 2 2 % Epon 164 - - 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 % Anox 20 - - 0.1 0.1 0.15 - - - 0.1 - % Naugard 445 - - - 0.1 0.15 - 0.1 0.15 - - % TBM6 - - - - - 0.1 0.1 0.15 - - % Ultranox 626 - - - - - - - - 0.1 - % Irganox 565 - - - - - - - - - 0.2 % Nova PS 1600 100 98 97.7 97.6 97.5 97.7 97.6 97.5 97.6 97.6 Color Values YI D1925

    1st Pass 2.04 10.12 5.72 3.23 2.50 3.80 4.75 4.53 0.04 4.65 3rd Pass 3.51 22.90 7.62 6.01 5.24 8.60 7.82 8.25 1.11 8.03 5th Pass 3.95 44.27 7.80 9.15 7.37 13.77 12.17 12.67 2.31 11.52

    WI CIE 1st Pass 70.52 39.07 50.45 57.16 58.26 56.58 53.69 53.97 66.02 52.39 3rd Pass 64.23 -2.55 42.88 47.49 48.8 40.32 43.13 42.18 61.34 40.79 5th Pass 63.06 -75.81 41.78 36.8 41.46 24.64 29.92 28.83 56.71 29.42

    MFI @ 200C/5kg, g/10min 1st Pass 7.04 7.62 6.09 5.55 5.86 5.86 5.08 6.08 5.39 5.71 3rd Pass 7.85 8.79 6.11 6.23 6.15 6.38 6.53 6.58 5.64 6.16 5th Pass 8.67 9.67 6.64 6.58 6.87 7.04 7.40 7.47 5.69 6.38

  • 14

    Yellowness Index

    0

    5

    10

    15

    20

    25

    30

    35

    40

    45

    50

    1st pass

    3rd pass

    5th pass

    0.1% Anox 20/0.1% Ultranox 626/ 0.2% Epon 164 appears to be most effective

  • 15

    Processing at Higher Temperature

    Extruder Temperature Profile, C 200, 230, 260, 260 250, 260, 260, 260

    % Emerald Innovation 3000 2 2

    % Epon 164 0.4 0.4

    % Anox 20 0.1 0.1

    % Ultranox 626 0.2 0.2

    % Nova PS 1600 97.3 97.3

    YI D1925 6.57 18.97

    WI CIE 44.12 6.67

    MFI @ 200C / 5kg / g/10min 5.96 6.16

    Increasing the Stabilization package and using a gradually increasing temperature profile in extrusion allows for processing at higher temperatures

  • 16

    Emerald Innovation 3000 thermal stability testing vs. stabilised HBCD

    Masterbatch samples

    62.5% FR + Epon 164/Anox 20/Ultranox 626 (6.25%/3.125%/3.125%)

    Extrusion temps: 190, 195, 200, 200C

    Masterbatch pellets pressed via compression molding into thin plaques

    Compression molding carried out at 150C

  • 17

    Emerald Innovation 3000 thermal stability testing vs. HBCD

    Emerald Innovation 3000 MB Stabilised HBCD MB

    Masterbatch compression molded

  • 18

    Masterbatch pellets subject to oven aging at 200C for 30 min.

    Let-down in Polystyrene (zinc free) @ 2% FR loading Let-down samples injection molded into 0.8mm plaques and

    subject to oven aging at 200C for 30 min.

    Emerald Innovation 3000 thermal stability testing vs. HBCD

  • 19

    Stabilised HBCD MB Emerald Innovation 3000 MB

    Emerald Innovation 3000 thermal stability testing vs. HBCD

    Masterbatch pellets subject to oven aging

  • 20

    Stabilised HBCD Emerald Innovation 3000

    Emerald Innovation 3000 thermal stability testing vs. HBCD

    Let-down at 2% and subject to oven aging

  • 21

    Summary

    Emerald Innovation 3000 is a highly efficient fire safety solution for XPS foam insulation.

    An optimized stabiliser solution (0.1% Anox 20/0.1% Ultranox 626 along with 0.2% Epon 164) has been developed for XPS containing Emerald Innovation 3000.

    This stabilisation package produced an excellent balance of Yellowness Index, Whiteness Index and MFI of Polystyrene after 5 extrusion passes.

    Emerald Innovation 3000 stabilised with the optimized package has a better thermal stability compared to stabilised HBCD.

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