Low-temperature curing coating compositions
a technology of coating compositions and curing temperatures, applied in the direction of coatings, adhesive types, electricly conductive paints, etc., can solve the problems of tin and lead catalysts being tin and lead catalysts have been subject to a number of regulatory restrictions, and previous blocked polyisocyanates that unblock at relatively low temperatures have been difficult to make,
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example 1
Preparation of Dibutylglycolamide (“DBGA”) Blocked Polyisocyanate Curing Agent (Ratio of Isocyanato Groups from Toluene Diisocyanate to Blocking Groups from Trimethylol Propane and DBGA: TDI / TMP / DBGA=10 / 5 / 5)
[0146]
Amount#MateriallbsKg1Toluene diisocyanate7568.803433.152Methyl isobutyl ketone4249.601927.583Dibutyltin dilaurate1773.60 gm1773.60 gm4Trimethylol propane2000.00907.185Methyl isobutyl ketone1000.00453.596Dibutyl glycolamide18816.003998.877Methyl isobutyl ketone1000.00453.598Bisphenol A polyol2137.50969.559DOWANOL PPH22850.001292.7410Methyl isobutyl ketone2205.001000.171Prepared according to Example 1 of U.S. Pat. No. 4,452,9302Available from DOW Chemicals
[0147]A dibutylglycolamide blocked polyisocyanate curing agent was prepared as follows: Charges 1, 2 and 3 were combined in a flask set up for total reflux with stirring under nitrogen and heated to 35° C. Charge 4 was then added in four equal portions with a 30-minute hold following each addition. Following addition of char...
example 2
Preparation of a Cationic Amine-Functionalized Resinous Dispersion using the DBGA Blocked Polyisocyanate Curing Agent of Example 1
[0148]
Amount#MateriallbsKg1EPON 82819660.004381.702Bisphenol A4237.001921.873Methyl isobutyl ketone (“MIBK”)1161.00526.624Ethyl triphenyl phosphonium bromide9.704.405Dowanol PPh21435.00650.906Methyl isobutyl diketimine of diethylene1015.00460.40triamine (72.7% solids in MIBK)37Methyl ethanol amine866.00392.818DBGA Blocked Crosslinker418060.008191.87990% Formic acid606.00274.8810DI Water13184.005980.1611DI Water32090.0014555.771Difunctional bisphenol A / epichlorohydrin derived liquid epoxy resin2 Available from DOW chemical company3Reaction product of diethylene triamine and methyl isobutyl ketone produced by combining diethyelen triamine and excess methyl isobutyl ketone in a reactor equipped with a mechanical stirrer, temperature probe, and a condenser with a Dean Stark trap filled with methyl isobutyl keton attached and heating the mixture to reflux. Wat...
example 3
Synthesis of N-Butyl Glycolamide Blocking Agent
[0150]An N-butyl glycolamide blocking agent was prepared according to the following procedure: 1,000.43 g of glycolide (commercially available from AK Scientific, Inc.) was charged into a 3000-mL, 4-necked round bottom flask equipped with a stirrer, a condenser, a nitrogen inlet, and a thermocouple. Agitation and a nitrogen flow of 0.2 standard cubic feet (scft) / minute were started. 1,266.59 g of Mono-N-butylamine (commercially available from Eastman Chemical Company) was added to the flask over 4.5 hours at a rate such that the reactor temperature did not exceed 65° C. An ice bath was also placed under the flask during the addition to control the reaction temperature. After completion of the addition, the reaction mixture was heated to 80° C. and held for 4 hours until the MEQ amine is less than 0.2 as measured by titration using a Metrohm 751 PGPD Titrino with 0.1 N Perchloric acid in glacial acetic acid as the titration reagent. A sl...
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