Trimethylolpropane → 50586-59-9

Temperature

100 °C

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”).

1. additionwere charged into a pressure-resistant reaction vessel
2. customequipped with a stirrer
3. customwas slowly bubbled into the reaction system
4. distillationwater (2.53 g) was distilled off
5. waitThe pressure was further kept at 100 mmTorr for 1 hour with a vacuum pump
6. temperatureThen, the temperature inside the vessel was heated up to 130° C.
7. customwas kept at 130° C.±2° C.
8. additionethylene oxide (1,969.9 g, 30-fold in mole relative to TMP) was added
9. additionAfter the ethylene oxide addition
10. waitthe inner temperature was kept at 130° C. for 1 hour
11. customthe reaction
12. customafter the reaction

ORD record

ord-36e776614d0c4539a785804f1481d06d

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08476341B2