Powder coatings or adhesives employing silanes or silane treated fillers
A technology for powder coatings and adhesives, applied in powder coatings, adhesives, coatings, etc., can solve the problems of difficult low molecular weight components, formation of tough films, easy flow, etc.
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Embodiment 1
[0095] Silyl carbamate compounds were prepared from the reaction of isocyanatopropyltrimethoxysilane with the polyol compounds listed in Table I. The reaction was carried out using a 2:1.05 mole ratio of isocyanatopropyltriethoxysilane:diol and 300-500 ppm dibutyltin dilaurate (DBTDL) catalyst at a total weight of about 30 grams. A 100 ml round bottom 3 neck flask was fitted with a magnetic stir bar and a thermometer on one side. The equipment includes a heating mantle with a calorimeter. Use TEFLON at the junction lubricant. The ingredients were transferred to a flask, including a catalyst charge of 300-500 ppm DBTDL. Under nitrogen, the flask was slowly heated until an exotherm occurred. Keep the maximum temperature at about 100°C to reduce the color of the final product. Using IR, the reaction was controlled by the disappearance of NCO to proceed to completion. The appearance and viscosity of the product were recorded, and if the product was a solid, the melting poi...
Embodiment 2
[0098] Preparation of Bis[3-(triethoxysilyl)propyl]-1,4-cyclohexanedimethyldicarbamate
[0099] Under nitrogen protection, 199.4 grams of molten cyclohexanedimethanol (purchased from Aldrich), 685.6 grams of SILQUEST A-1310 (3-isocyanatopropyltriethoxysilane, available from Witco Corp.) and 0.44 grams of DBTDL. With good mixing and a little heating, the contents of the flask exothermed to 146°C. The temperature of the reaction mixture was maintained at 90-110°C for 3 hours. As the reaction progressed, the infrared spectrum of the reaction mixture was measured at intervals. When the isocyanate is at 2272cm -1 When the absorption peak disappears substantially, the reaction is considered to be over. Upon cooling, a white solid was obtained. The melting point of this material was measured by DSC (differential scanning calorimetry) and was 82.6°C. product of 13 C and 29 Si NMR analysis confirmed the formation of bis[3-(triethoxysilyl)propyl]-1,4-cyclohexanedimethyldicarb...
Embodiment 3
[0101] Preparation of Bis[3-(trimethoxysilyl)propyl]-1,4-cyclohexanedimethyldicarbamate
[0102] SILQUEST will be purchased Y-5187 (3-isocyanatopropyltrimethoxysilane, available from Witco Corp.) was distilled and analyzed by GC to give a purity of 98.5%. Under nitrogen protection, 21.9 g of molten cyclohexanedimethanol and 0.0101 g (10 mL) of DBTDL were added to a 100 mL three-necked flask equipped with a magnetic stirrer, thermometer, reflux condenser, and addition funnel. The contents were heated to 50°C. With good stirring, distilled Y-5187 (3-isocyanatopropyltrimethoxysilane) was added dropwise. Upon initiation of the addition, an exotherm occurred and the temperature of the reaction mixture rose to 100°C. Remove the heat source and continue to add Y-5187 at a rate that keeps the internal temperature below 100°C. After the addition was complete, the reaction mixture was at 85°C. Hold for 1 hour. Infrared analysis showed no isocyanate. After cooling to room tempe...
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