Low-temperature curing coating compositions
A composition and coating technology, applied in conductive coatings, electrophoretic coatings, polyurea/polyurethane coatings, etc., can solve problems such as toxicity, crystallization, and difficulty in disposal
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Embodiment 1
[0172] Preparation of dibutylethanolamide ("DBGA") blocked polyisocyanate curing agent (ratio of isocyanato groups from toluene diisocyanate to blocking groups from trimethylolpropane and DBGA: TDI / TMP / DBGA =10 / 5 / 5)
[0173]
[0174]
[0175] 1 Prepared according to Example 1 of U.S. Patent No. 4,452,930
[0176] 2 Available from DOW Chemicals
[0177] The dibutylethanolamide blocked polyisocyanate curing agent was prepared as follows: Charges 1, 2 and 3 were combined in a flask set to total reflux and stirred and heated to 35°C under a nitrogen atmosphere. Feed 4 was then added in quarters with a hold of 30 minutes after each addition. After addition of Charge 4, the flask was rinsed with Charge 5 and held at 95°C for one hour. The mixture was then cooled to 70°C, and then Charge 6 was added over two hours while maintaining the reaction temperature below 100°C. After addition of Feed 6, the reactor was held at 105°C for one hour. Continue to maintain until there ...
Embodiment 2
[0179] Cationic Amine Functionalized Resinous Dispersions Prepared Using the DBGA Blocked Polyisocyanate Curing Agent of Example 1
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[0181]
[0182] 1 Bifunctional Bisphenol A / Epichlorohydrin Derived Liquid Epoxy Resin
[0183] 2 Available from DOW chemical company
[0184] 3 The reaction product of diethylenetriamine and methyl isobutyl ketone, prepared by combining diethylenetriamine and excess methyl isobutyl ketone in a reactor equipped with a mechanical stirrer, A temperature probe and condenser was attached to a Dean Stark trap filled with methyl isobutyl ketone and the mixture was heated to reflux. Water was separated from the MIBK in the Dean Stark trap and removed from the reaction. The theoretical solids content of the final product was 72.7% by weight.
[0185] 4 Prepared as in Example 1.
[0186] The procedure for preparing the cationic amine functionalized resinous dispersion was carried out as follows: Charges 1 to 4 were added to the react...
Embodiment 3
[0188] Synthesis of N-butylethanolamide blocking agent
[0189] N-butylethanolamide sealant was prepared according to the following procedure: 1,000.43 g of glycolide (commercially available from AK Scientific, Inc.) was added to a 3000-mL, 4-neck tank equipped with a stirrer, condenser, nitrogen inlet, and thermocouple. Round-bottomed flask. 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 the addition was complete, the reaction mixture was heated to 80°C for 4 hours until the MEQ amine was less than 0.2 as measured by titration using a Metrohm 751PGPD Titrino with 0.1 N perchloric acid in glacial acetic acid as the titrant. A yellowish liquid co...
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