“Aesthetics and Performance: FEVE Fluoropolymer Resins for Powder Coatings” Bob Parker D+D Webinar April 25, 2013

Outline: FEVE Powder Resins Overview of “FEVE” resin technology Determination of best properties for an FEVE powder coating resin Introduction of FEVE resin for powder coatings Testing results of formulations made with FEVE powder resin 2nd Generation FEVE Powder Coating Resin

What is an FEVE Fluoropolymer??? FEVE Powder Resins What is an FEVE Fluoropolymer??? A hybrid fluoropolymer resin with the ability to be used in standard coatings formulations like any other conventional coating resin A high performance resin that can withstand severe ultraviolet light exposure 2-3 times longer than conventional coatings resins

FEVE Fluoropolymer Resins FEVE Powder Resins FEVE Fluoropolymer Resins “FEVE” is abbreviation for “Fluoroethylene Vinyl Ether” resins for coatings Known for their high performance properties: Exceptional resistance to UV degradation Superior Chemical Resistance Excellent Thermal Resistance - Known for their unique formulation properties: 1) Solvent soluble 2) Can be cured at ambient temperature with isocyanates 3) Can achieve high gloss formulations

Fluoroethylene Vinyl Ether (FEVE) Resins FLUORINATED SEGMENTS: Weatherability, durability, chemical resistance VINYL ETHER SEGMENTS: Gloss, solubility, crosslinking

Target Properties/Characteristics for an FEVE Powder Coating Resin FEVE Powder Resins Target Properties/Characteristics for an FEVE Powder Coating Resin Properties Characteristics Melting Point Can Simplify Extrusion of the Powder Coating Formulation During Manufacture Tg (Glass Transition Temperature) Important in the Retention of Powder Properties when in Storage Type of Crosslinkable Functional Group Can affect the Shelf Life of the Powder Coating Degree of Functionality Affects Film Performance

Test for Choosing the Best Tg for the FEVE Powder Resins Test for Choosing the Best Tg for the FEVE Powder Resin: 1) Prepare powder coatings using several FEVE resins with different Tg properties 2) Place coatings in cylinders and apply 40 gm/cm² force. 3) Place cylinders in 40⁰ C. oven for 24 hours. 4) Check physical state of powder coatings.

Physical State of the Powder Coating FEVE Powder Resins Relationship of Tg of Resin and Blocking Properties of the Powder Coating Tg of Powder Resin (⁰C.) Physical State of the Powder Coating 40 Fused Hard Lump 45 Fused Hard Lump 50 Fused Soft Lump 55 Retained Powder State

Hardener for Crosslinking FEVE Powder Resins Connection between Cure System of FEVE Powder Resin and Shelf Life of Coatings Functional Group Hardener for Crosslinking Shelf Life Hydroxyl (-OH) Isocyanate, Melamine 2 years Carboxyl (-COOH) Epoxy, triglycidyl isocyanurate 1-1.5 years Glycidyl (epoxide ring) Amine, acid 3 months Hydroxyl functionality is the best choice!

Common properties of 1st Generation FEVE Powder Resin FEVE Powder Resins Common properties of 1st Generation FEVE Powder Resin

Typical Powder Coating Formulation FEVE Powder Resins Typical Powder Coating Formulation Flow Promoter: Eliminates surface imperfections Benzoin: Eliminates pinholes caused by out-gassing

Typical Laboratory Manufacturing Procedure: FEVE Powder Resins Typical Laboratory Manufacturing Procedure: Add all ingredients together; premix with blade mixer Extrusion of powder coating premix: a. twin screw extruder w/ 16 mm Bore size b. 250 RPM @ 120⁰C. Grinding with Blade Mixer Filtering of powder through 3 sieves → 180 micron 125 micron 90 micron

FEVE Powder Resins Effect of Different Catalysts on Gloss *1 – used 500 gram weight and ½” diameter ball *2 – ISO 2409 cross cut adhesion test *3 - visual check for degree of orange peel; 1=highest and 10=lowest Crelan Ui: IPDI NCO adduct; E-Caprolactam blocked Crelan TPLS2147: IPDI NCO adduct; internally blocked Bismuth Octoate is best catalyst!

Advantages of FEVE Powder over Conventional Powder resins FEVE Powder Resins Advantages of FEVE Powder over Conventional Powder resins Produces a hard film - higher than 2H pencil hardness Has stronger Chemical Resistance to acids, bases, and solvents Demonstrates significant anti-graffiti properties Exceptional Weatherability properties Highly Transparent film - translates to a high transmittance of a wide spectrum of light rays Impact on application productivity - FEVE resin has least impact on comtamination

FEVE Powder Resins Anti-graffiti Performance Test: Application of marker for 24 hours; attempted removal with Xylene

FEVE Powder Resins QUV B313 Weatherometer Exposure

FEVE Powder Resins Xenon Arc Weatherometer Exposure

FEVE Powder Resins Dipla Metal Weatherometer (DMW) Manufactured by Kato, Inc., which is based in Japan

Dipla Metal Weatherometer FEVE Powder Resins Dipla Metal Weatherometer

Exterior 10 year exposure: FEVE Powder Resins Exterior 10 year exposure: Test type : Inland weathering Test location : Miami , Florida (26°N) Exposure period : 11/30/2000 – 11/22/2010 Type of test : 45°Direct Global Radiant energy : Total: 62,281 MJ/m2(total) ; 1,488,552 Langleys UV : 2,863 MJ/m2(295-385nm)

Exposed Powder Coating Formulation: FEVE Powder Resins Exterior 10 year exposure: Exposed Powder Coating Formulation: Powder Resin : Lumiflon LF710F Hardener : Crelan VP LS2256 / Bayer Color : Brown Results of Exposure: 60⁰ Gloss retention (%): 60.3 Color Change (ΔE): 2.3

2nd generation FEVE powder resin: FEVE Powder Resins 2nd generation FEVE powder resin: Introduced 3 years ago Improved flow and leveling vs. 1st generation FEVE resin Improved impact resistance and flexibility vs. 1st generation FEVE resin Comparable to 1st generation FEVE resin in terms of hydroxyl functionality and Tg

FEVE Powder Resins PROPERTIES 1st generation FEVE resin 2nd generation Film Thickness (microns) 50-70 20⁰ Gloss 50 51 60⁰ Gloss 80 78 Leveling (PCI Standard) 2.5-3.5 6-7.5 Gloss retention after 6000 hours (QUV-B313 exposure) 87% 84% Mandrel Bend (mm) >8 3 Direct Impact (inch-lbs) 15 30 Reverse Impact (inch-lbs) 10 25 Cross-cut Adhesion (ISO 2409)

FEVE Powder Resins Summary: FEVE powder coating resins demonstrate exceptional resistance to UV degradation when used in powder coating formulations. while exhibiting the standard physical properties necessary for manufacturing a stable and easily applied powder coating formulation.