Trimethylolpropane → 50586-59-9

Participants

Reaction Conditions

Reaction Steps

Trimethylolpropane (Wako Pure Chemical Industries, Ltd., 200 g, hereinafter also referred to as “TMP”) and a 30% sodium hydroxide aqueous solution (3.62 g) were charged into a pressure-resistant reaction vessel equipped with a stirrer. The temperature of the reaction system was heated up to 100° C. with an oil bath. The pressure of the reaction system was reduced to 100 mmTorr for 1 hour with a vacuum pump while nitrogen was slowly bubbled into the reaction system, and thereby water (2.53 g) was distilled off. The pressure was further kept at 100 mmTorr for 1 hour with a vacuum pump. Then, the temperature inside the vessel was heated up to 130° C., and the inner pressure was adjusted to 0.5 MPa by nitrogen introduction. While the temperature inside the vessel was kept at 130° C.±2° C., ethylene oxide (1,969.9 g, 30-fold in mole relative to TMP) was added. Here, the inner pressure was controlled so as not to exceed 0.8 MPa. After the ethylene oxide addition, the inner temperature was kept at 130° C. for 1 hour to complete the reaction. The yield was found to be 99.7% from the masses before and after the reaction. As a result, the reaction provided a trimethylol propane ethylene oxide 29.9 mol adduct (hereinafter, also referred to as “TMP-30”).

Provenance & Evidence