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DMPA® Polyol HA-0135 High Solids

Polyurethane Dispersions Using


Desmodur I - Guide Formulation

DMPA® Polyol HA-0135 TECHNICAL BULLETIN # 3

DMPA® Polyol HA-0135 is a linear polyester polyol


that contains both hydroxyl and acid functionality.
The structure of DMPA® Polyol HA-0135 has
GEO Specialty Chemicals, Inc.
been specifically designed to achieve maximum
Paints & Coatings Group
hydrolytic stability in water-borne applications.
▪ Customer Service (USA)
340 Mathers Road DMPA® Polyol HA-0135 can be used to formulate
Ambler PA 19002
high solids and NMP free polyurethane dispersions.
USA
Tel: +1 215 773 9280
(Toll Free 888 519 3883) Technical Data Typical Properties
Fax:+1 215 773 9424 Appearance Clear / slightly hazy
E-mail: TRIMET@geosc.com viscous liquid

Acid Value (as supplied) 100 - 115


GEO Specialty Chemicals, Ltd. Hydroxyl Number (as supplied) 100 - 115
▪ Customer Service (Europe)
Non-volatile % 98 min
Unit C, Pate Court, North Place
Cheltenham, Glos. GL50 4DY Brookfield Viscosity @ 25°C 4000 - 8000 P
UK @ 100% NV
@ 55°C 150 - 350 P
Tel: +44 1242 255 772 @ 75°C 60 - 80 P
Fax: +44 1242 262 804
E-mail: TRIMET-EU@geosc.com Density @ 25°C, grams / litre 1200 - 1235

Colour, APHA 450 max

Website: www.geosc.com Moisture % 0.5 max


DMPA® Polyol HA-0135 - Technical Bulletin #3

Table 1 - Pre-polymer Formulation

Materials Wt. (g) Eq. Wt. Eq. No.


DMPA® Polyol HA-0135 103.1 500 (OH) 0.206
500 (COOH) 0.206
Diexter-G IA66-120 1 223.3 467 (OH) 0.478

CHDM 2 10.4 72.12 0.144

Desmodur I 3 151.5 111.1 (NCO) 1.364

NMP 4 120.0
TEA (for neutralization) 18.5 101.0 0.183
Di-ionised water (I) 267.0

Ethylene diamine 13.2 30.03 0.440


Di-ionised water (II) 93.0
TOTAL 1000
Properties
NCO/OH 1.65
Non-volatile % 80.3
Acid value 18.6
Free NCO % 3.7
Brookfield Viscosity @ 65°C 1600 cP
RVT#5 @ 20 rpm @ 60°C 2560 cP
@ 55°C 3600 cP

1 3
Diexter-G IA66-120 is a product of Coim USA Desmodur I is a product of Bayer
2 4
CHDM is a product of Eastman NMP is a product of Lyondell

Part I: Synthesis of NCO-terminated Pre-polymer


1. Charge DMPA® Polyol HA-0135, Diexter-G IA66-120, CHDM and NMP into a round
bottom flask equipped with agitator, inert gas sparging tube, a temperature controller
and a water-cooled condenser.

2. Heat the contents to 70-80°C. Once the solution is homogeneous, slowly add
Desmodur I. After 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 #3

Part II: Neutralization, Chain Extension and Dispersion


1. Once the pre-polymer is transferred, begin agitation at 100-120 rpm and charge TEA
(tri-ethylamine). Allow sufficient time for the amine to mix in, approximately 10 minutes.
(Agitator: IKA RW 28 Basic equipped with cowels 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.

Table 2 - Dispersion Properties

Dispersion properties
Non-volatile (hot plate) % 52.1
pH 8.0
Viscosity @ 25°C KU-2 Viscometer
Kreb Units 102
cP 1723

Brookfield RVT #2 @ 5 rpm, cP 5440


Density @ 25°C g / ml 1.07
Appearance opaque
Stability 4 wks @ 60°C - 0.5 pH
( with no precipitate)

Film properties 0.05 mm on glass


Sward Hardness
1 day / 1 week 26 / 26

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 con-
strued 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.

3 Revised: October 2009

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