Optimization of SPF with Isocyanate Compatible Silicone Surfactants. Ray Geiling September 2013

Optimization of SPF with Isocyanate Compatible Silicone Surfactants Ray Geiling September 2013

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

SPF Performance Optimization of Closed-Cell SPF Physical Properties are very important Density Insulation Values Percent Closed-Cell Content Compressive Strength, Etc However, equally important is the optimization of the application properties Ease of Application Flow Properties Efficiently cover the substrate and fill gaps improving air barrier properties Reduced Gun Clogging or Plugging, Etc

Why Improve SPF Flow Properties Potential Benefits of Improving SPF Flow Properties Improve Efficiency of SPF to: Flow into irregular shaped areas Fill Gaps Nooks and Crannies Reducing Spray Gun Clogging and Plugging Improving these application properties may result in enhancing the ease of application for the SPF contractor. Potential Economic Advantage Less Gun Plugging = Less Down Time Less Touch Ups = Less Installation Time

Improved Flow: Attic Nooks and Crannies Efficiently Fill Hard to Reach Places

Improved Flow Gap Filling Improved Air Barrier Gaps Created Between Roof Deck and Truss

Spray Gun Tip

Research Questions Can isocyanate compatible silicone surfactants significantly lower pmdi surface tension and improve flow properties of SPF? If they can, will the improvements be realized if the surfactant is formulated into the Polyol Resin Blend rather than the pmdi? Will simply increasing the use level of the existing surfactant formulated into the Polyol Resin Blend improve flow properties?

SPF Formulation Standard 2.0 pcf Closed-Cell SPF Standard pmdi Ingredient % pmdi Value Polyester Polyol Blend 69.2 Flame Retardants TCPP & PHT 4-Diol 15 Catalyst Package DMEA & PMDETA 4.5 Tegostab B 8408 1 Isocyanate Equivalent Weight 135 NCO Content 31 Functionality 2.7 Viscosity @ 25C 190 HFC-245fa 8 Water 2.3

Silicone Surfactant Structure OH Functional vs. Non-OH Functional Vs. OH OH OH Reactive with pmdi Non-Reactive with pmdi

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Surface Tension: Liquid Spreading Low Medium High Surface Tension

Dynamic Surface Tensiometer Maximum Bubble Pressure Dynamic Tensiometer Change the Bubble Rate Formation to Increase Bubble Speed Work = y * Δ Area Page 23

pmdi Surface Tension Reduciton Faster Dynamics Slower Dynamics

pmdi Spreading Properties Standard pmdi pmdi Lower Surface Tension pmdi Spreading Area Increases with a Decrease in Surface Tension

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Evonik developed a new flow test to compare & contrast the flow performance of various surfactants Key Components Flow Test Bucket Spray Table

170oz. DMF-170Food Bucket International Paper Flow Testing 1.25 Drill Saw Bit Flow Test Bucket

Spray Table Set Up 9 inches 18 inches

Flow Test

Flow Samples Low Flow High Flow

Percent Flow Calculations Percent Flow % Flow = (g) SPF Flow * 100% (g) SPF Sprayed Percent Improved Flow % Improved Flow = % Flow Sample - % Flow Standard * 100% % Flow Standard

Agenda 1. Introduction 2. pmdi Surface Tension Reduction 3. New Flow Test Method Introduction 4. High Pressure SPF Performance Results 5. Conclusions

Evonik Spray Foam Equipment Hopewell, VA. Graco Reactor E-20 Spray Foam Machine Static Pressure ~ 1200 psi Dynamic Pressure ~ 1000 psi Temperature: A, B, and Hose Equally 110 F and 120 F Graco Fusion AP Gun 01 Spray Tip Page 34

Sample Preparation Conditions Physical Property Samples Cardboard Single pass at a thickness of 2 inches Cured for 24hrs. prior to testing Properties Tested Density K-factor, R-Value Percent Closed-Cell Content

Experimental Design Initial screening of 6 different surfactants evaluated at 1% use level in pmdi pmdi vs. pmdi + Surfactant Properties Measured Percent Flow Physical Values Density, R-Value, and Percent Closed-Cell Content The best performing surfactant was selected for further optimization Evaluated at different use levels and two processing temperatures 0%, 0.25%, 0.50% and 1.0% 110 F and 120

Standard 2.0 pcf System Performance Surfactant in Polyol pmdi Temp. % Flow Density k-factor R-Value % Closed- Cells 1% Tegostab B 8408 Standard 110 F 3.7 1.96 0.1523 6.6 95 1% Tegostab B 8408 Standard 120 F 3.8 1.97 0.1524 6.6 91

Surfactant Screening in pmdi Tegostab B 8408 in Polyol 1% Surfactant in pmdi % Flow % Improved Flow R-Value % Closed-Cells 1% NONE STANDARD 3.7 0 6.6 95 1% A-1 3.5-10 6.6 98 1% A-2 4.6 18 6.5 94 1% A-3 4.6 18 6.4 95 1% A-4 5.5 41 6.5 97 1% A-5 6.5 67 6.5 96 1% A-6 7.5 92 6.5 93

Surfactant Screening in pmdi Tegostab B 8408 in Polyol 1% Surfactant in pmdi % Flow % Improved Flow R-Value % Closed-Cells 1% NONE STANDARD 3.7 0 6.6 95 1% A-1 3.5-10 6.6 98 1% A-2 4.6 18 6.5 94 1% A-3 4.6 18 6.4 95 1% A-4 5.5 41 6.5 97 1% A-5 6.5 67 6.5 96 1% A-6 7.5 92 6.5 93

Surfactant Screening in pmdi Tegostab B 8408 in Polyol 1% Surfactant in pmdi % Flow % Improved Flow R-Value % Closed-Cells 1% NONE STANDARD 3.7 0 6.6 95 1% A-1 3.5-10 6.6 98 1% A-2 4.6 18 6.5 94 1% A-3 4.6 18 6.4 95 1% A-4 5.5 41 6.5 97 1% A-5 6.5 67 6.5 96 1% A-6 7.5 92 6.5 93

Surfactant Screening at 1% in pmdi: Sprayed at 110 F + 92%

Surfactant A-6 Optimization Evaluate Levels in pmdi 0% 0.25% 0.5% 1.0% Effects of Temperature 110 F vs. 120 F

Performance of A-6 at 110 F & 120F Different Use Levels Performance of A-6 @ 110 F % B 8408 in Polyol % A-6 in pmdi % Flow % Improved Flow Density k-factor R-Value % Closed-Cells 1% 0% 3.7 0 1.96 0.1523 6.6 95 1% 0.25% 4.6 24 1.95 0.1529 6.5 92 1% 0.5% 4.5 22 1.96 0.1517 6.6 93 1% 1% 7.5 92 2.01 0.1539 6.5 93 Performance of A-6 @ 120 F % B 8408 in Polyol % A-6 in pmdi % Flow % Improved Flow Density k-factor R-Value % Closed-Cells 1% 0% 3.8 0 1.97 0.1524 6.6 91 1% 0.25% 5.6 47 1.96 0.1553 6.5 93 1% 0.50% 5.7 50 1.93 0.1555 6.4 91 1% 1% 4.3 13 1.94 0.2109 4.7 68

Cell Opening at 1% at 120 F Open Cells

A-6 % Flow and R-Value X X

A-6 % Flow and R-Value 0.25% 0.5% X X

A-6 % Flow and R-Value ~ 24% Improved Flow @ 110 F X X

A-6 % Flow and R-Value ~ 50 % Improved Flow @ 120 F X X

Optimization Results Use Level Between 0.25% - 0.5% Flow Improvement Up to 24% at 110 F Up to 50% at 120 F

A-6 Testing in B-Side 0% in pmdi Will the improvements be realized if the surfactant is formulated into the Polyol Resin Blend rather than the pmdi? All Tests at 120 F Most Sensitive Condition Scenarios Tested in B-Side 1% B 8408 + 1% A-6 1% A-6 Only 1% B 8408 + 0.25% A-6 1.25% Standard B 8408 * 0.75% B 8408 + 0.25% A-6

A-6 Formulated into Polyol Blend % B 8408 in Polyol % A-6 in Polyol % Flow Flow vs. Control Density k-factor R-Value % Closed-Cells 1% 1% 17.2 353 1.97 0.2146 4.7 40 0% 1% 10 163 1.98 0.2622 3.8 29 1% 0.25% 8.8 132 1.93 0.1547 6.5 90 0.75% 0.25% 8.7 129 1.92 0.1556 6.4 86 1.25% 0% 6.6 74 1.94 0.1532 6.5 90 1% 0% 3.8 0 1.97 0.1524 6.6 91

A-6 Formulated into Polyol Blend 353% 4.2

A-6 Formulated into Polyol Blend 353% 4.2 X

A-6 Formulated into Polyol Blend R-Value 3.8 X

A-6 Formulated into Polyol Blend X X

A-6 Formulated into Polyol Blend 86% Closed-Cell X X X

A-6 Formulated into Polyol Blend X X X

Comparing A-6 in pmdi vs. Polyol

Comparing A-6 in pmdi vs. Polyol 1% B 8408 in Polyol + 0.25% A-6 pmdi +47%

Comparing A-6 in pmdi vs. Polyol +47% 1.25% B 8408 in Polyol + 74%

Comparing A-6 in pmdi vs. Polyol 1% B 8408 + 0.25% A-6 in Polyol + 132% +47% + 74%

Comparing A-6 in pmdi vs. Polyol 1% B 8408 + 0.25% A-6 in Polyol + 132% +47% + 74%

Answering the Question we Started With Can isocyanate compatible silicone surfactants significantly lower pmdi surface tension and improve flow properties of SPF? YES: 3 of 6 surfactants improved flow by 40% or more Surfactant A-6 being the best If yes, will the improvements be maintained if surfactant is formulated into the Polyol Resin Blend vs. the pmdi? YES: A-6 in the Polyol Resin Blend improved flow 132% Will increasing the use level of the standard surfactant improve flow properties? YES: Adding an additional 0.25% B 8408 improved flow by 74%

Conclusions The organic modification of Surfactant A-6 is more important than it s isocyanate compatibility to improve flow Improves flow properties in greater magnitude than the other surfactants evaluated All non-hydroxyl surfactants in the A-Side reduced gun clogging Based on observations but not quantified 5 samples with no A-Side surfactant vs. 10 with Surfactant A-6 could be a powerful additive for SPF systems Improving flow properties whether in A-Side or B-Side Reducing gun clogging and plugging if in the A-Side

Isocyanate Compatible Surfactants Sample A-1 A-2 A-3 A-4 A-5 A-6 Siloxane chain length MEDIUM LOW HIGH MEDIUM LOW MEDIUM Degree of backbone modification MEDIUM HIGH LOW MEDIUM HIGH MEDIUM Polyether chain length LOW LOW HIGH MEDIUM MEDIUM MEDIUM Propylene oxide content LOW LOW HIGH MEDIUM HIGH HIGH Additional organic pendants NO NO NO NO NO YES No Hydroxyl Functional Groups

pmdi Surface Tension Reduciton Faster Dynamics Slower Dynamics