Polyurethane foams made with blowing catalyst compositions containing primary hydroxyl groups and high ethylenediamine backbones
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example 1
Synthesis of N-[2-hydroxyethyl]-N,N′,N″,N′″,N′″pentamethyltriethylenetetramine
[0052] A sample of about 519 grams of commercially available triethylenetetramine (about 67 wt %) was charged into a one-liter stainless steel reactor equipped with a cooling and heating jacket, a stirrer, a syringe pump and FTIR. The amine was heated to about 50° C. and pressurized with approximately 50 psig nitrogen. Ethylene oxide (about 170 g) was slowly added to the mixture and the product was allowed to stir for approximately one hour after addition, until the reaction was finished. The product was collected (about 639 g) and distilled under vacuum (20 mm Hg) to remove any unreacted amine. The crude ethoxylated product was dissolved in isopropanol and placed in the reactor together with 5% palladium on a carbon catalyst. The reactor was pressurized with hydrogen and heated up to about 90° C. Formalin (37% formaldehyde in water) was slowly added while the hydrogen pressure was monitored. At the end o...
example 2
Synthesis of N-[2-hydroxypropyl]-N,N′,N″,N′″,N′″pentamethyltriethylenetetramine
[0053] A sample of about 500 grams of commercially available triethylenetetramine (about 67 wt %) was charged into a one-liter stainless steel reactor equipped with a cooling and heating jacket, a stirrer, a syringe pump and FTIR. The amine was heated to about 80° C. and propylene oxide (about 187 g) was slowly added to the mixture. The product was allowed to stir for approximately one hour after addition, until the reaction was completed. The product was collected and distilled under vacuum (20 mm Hg) to remove any unreacted amine. The product mixture was dissolved in methanol and placed in the reactor together with 5% palladium on carbon catalyst. The reactor was pressurize with hydrogen and heated up to about 90° C. Formalin (37% formaldehyde in water) was slowly added while the hydrogen pressure was monitored. At the end of the addition the reaction was kept at about 90° C. for approximately one hour...
example 3
Rate of Rise of Polyurethane Foams
[0054] Two foams were prepared. Foam A was prepared using the catalyst of Example 1 (a mixture comprising, in major part, N-[2-hydroxyethyl]-N,N′,N″,N′″,N′″pentamethyltriethylenetetramine) and Foam B was prepared using the catalyst of Example 2 (a mixture comprising, in major part, N-[2-hydroxypropyl]-N,N′,N″,N′″,N′″pentamethyltriethylenetetramine).
[0055] For each foam, the catalyst was added to about 192 g of the premix (described in Table 2) in a 32 oz (951 mL) paper cup. The formulation was mixed for about 10 seconds at about 6,000 RPM using an overhead stirrer fitted with a 2 inch (5.1 cm) diameter stirring paddle.
TABLE 2Premix Components (Example 3)ComponentPercent by WeightPolyol 150Polyol 250Water2.34Silicon surfactant0.75DABCO 33-LV ®0.25DABCO ® BL-110.10Crosslinker1.76
[0056] Toluene diisocyanate was added in an amount sufficient to produce a foam with an NCO index of approximately 100. The formulation was mixed well for about 6 seconds...
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