DMPA® Polyol HA-0135 in Solvent Free Polyurethane Dispersions Guide Formulation DMPA® Polyol HA-0135 ▪ North America 340 Mathers Road Ambler PA 19002 USA Tel: +1 215 773 9280 (Toll Free 888 519 3883) Fax:+1 215 773 9424 TECHNICAL BULLETIN #2 DMPA® Polyol HA-0135 is a linear polyester polyol that contains both hydroxyl and acid functionality. The structure of DMPA® Polyol HA-0135 has been specifically designed to achieve maximum hydrolytic stability in water-borne applications. DMPA® Polyol HA-0135 can be used to formulate high solids and NMP free polyurethane dispersions. ▪ Europe Suite 4, Fairview Court Technical Data Fairview Road Appearance Cheltenham, Glos. GL52 2EX UK Tel: +44 1242 255 772 Fax: +44 1452 450 303 Please send e-mail enquiries to: [email protected] Website: www.geosc.com Typical Properties Clear / lightly hazy viscous liquid Acid Value, mgKOH / g (as supplied) 100 - 115 Hydroxyl Number, mgKOH / g (as supplied) 100 - 115 Non-volatile, % Brookfield Viscosity @ 100% NV Density @ 25°C, grams / litre 98 min @ 25°C 4000 - 8000 P @ 55°C 150 - 350 P @ 75°C 60 - 80 P 1200 - 1235 Colour, APHA 450 max Moisture, % 0.5 max DMPA® Polyol HA-0135 - Technical Bulletin #2 Table 1 - Pre-polymer Formulation Material Wt. (g) DMPA® Polyol HA-0135 Diexter-G IA66-120 CHDM 1 2 ® Desmodur W 3 Eqv. Wt. 85.0 500 (OH) 500 (COOH) 0.170 0.170 184.0 467 (OH) 0.394 8.4 72.12 0.116 147.0 MEK Eqv. # 131 (NCO) 1.122 83 TEA (for neutralization) 14.5 De-ionised water (I) 397.5 Ethylene diamine 10.6 De-ionised water (II) 101 0.143 30.03 0.353 70 Total 1000 Properties NCO/OH 1.65 Non-volatile % 84 Acid value, mg KOH / g 18.8 Free NCO % 3.6 Brookfield Viscosity @ 20 rpm RVT#5 @ 65°C @ 60°C @ 55°C 2800 cP 4000 cP 4800 cP 1 hydroxyl terminated saturated linear polyester which is a poly(hexamethylene adipate/isophthalate) glycol, product of Coim USA, Inc. 2 3 Desmodur® W is a product of Bayer CHDM is a product of Eastman Part I: Synthesis of NCO-terminated Pre-polymer 1. Charge DMPA® Polyol HA-0135, Diexter-G IA66-120, CHDM and MEK into a round bottom flask equipped with agitator, inert gas sparging tube, temperature controller and a water-cooled condenser. 2. Heat the contents to 55-65°C. Once the solution is homogeneous, slowly add Desmodur® W. Once the addition is completed, continue to hold at 80-85°C until the % NCO endpoint has been obtained. Note: % NCO is determined by the di-n-butylamine titration method. NCO endpoint is 3.3 to 3.7% 3. When NCO content is between 3.3 and 3.7%, allow the pre-polymer solution to cool to 55-65°C. 4. At 65°C, begin transferring the pre-polymer solution to an appropriate dispersion vessel equipped with a high-speed dispersing agitator. 2 DMPA® Polyol HA-0135 - Technical Bulletin #2 Part II: Neutralization, Chain Extension & Dispersion 1. Once the pre-polymer is transferred, begin agitation at 100-120 rpm and charge TEA (triethylamine). Allow sufficient time for the amine to mix in, approximately 10 minutes. (Agitator: IKA RW 28 Basic equipped with cowles blade). 2. Pre-mix ethylene diamine and de-ionised water and charge to an addition funnel. 3. Increase the agitation to 300-400 rpm and begin charging de-ionised water at a rate sufficient to maintain a vortex. 4. Once the pre-polymer is dispersed, begin the addition of the ethylene diamine solution prepared in step 2. Add the solution to the dispersion at a continuous rate over a 20-30 minute period. 5. After step 4 is completed, reduce the agitator speed and continue to mix for an additional 20-30 minutes. 6. Adjust pH to 8.0 with additional TEA. 7. Transfer the dispersion to a reactor equipped with agitation, temperature controller, inert gas sparge, condenser, distillation receiver and vacuum. Begin heating the solution to 80°C with moderate to low inert sparge. 8. At 80°C, begin to apply vacuum as needed until approx. 85-100 grams of distillate is collected. Table 2 - MEK Dispersion Properties MEK Dispersion properties Non-volatile (hot plate) % 43.5 pH 8.0 Viscosity @ 25°C KU-2 Viscometer Kreb Units cP 85.1 966 Brookfield RVT #2 @ 5 rpm 3680 Density @ 25°C, g / ml 1.07 Appearance Translucent Stability 4 weeks @ 60°C (with no precipitate) - 0.5 pH Film properties 0.05 mm on glass Sward Hardness 1 day / 1 week 34 / 36 3 DMPA® Polyol HA-0135 - Technical Bulletin #2 Table 3 - Distilled Dispersion Properties Distilled Dispersion properties Non-volatile (hot plate), % 45.5 pH 8.02 Viscosity @ 25°C KU-2 Viscometer Kreb Units cP 114 2350 Brookfield RVT #2 @ 5 rpm, cP 5440 Stability 4 weeks @ 60°C (with no precipitate) - 0.5 pH Film properties 0.05 mm on glass Sward Hardness 1 day / 1 week 32 / 38 DMPA® is a registered trademark of GEO Specialty Chemicals All information and data, including the formulations and procedures discussed herein, are believed to be correct. However, this should not be accepted as a guarantee of their accuracy, and confirming tests should be run in your laboratory or plant. No statement should be construed as a recommendation for any use which would violate any patent rights. Sales of all products are pursuant to terms and conditions included in GEO Specialty Chemicals sales documents. Nothing contained therein shall constitute a guarantee or warranty with respect to the products described or their use. Safety information regarding these products is contained in their Material Safety Data Sheets. Users of these products are urged to review and use this information. 4 Revised: December 2014
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