Biodiesel production is increasing tremendously. However the catalyst separation is still a big challenge, as widely used homogeneous catalysts, such as sodium methoxide, are difficult to separate and may produce soap that is detrimental to the product separation. This paper studies tuning catalyst and process for easy catalyst separation and improved reaction rate. Multibond metal alkoxides and ultrasonic pretreatment are employed as they can cooperate to produce nanoemulsions with large interfacial area. These emulsions have the potential to be separated easily. With aluminum isopropoxide or titanium isopropoxide as the catalyst and surfactant, transparent alcohol/oil emulsions can be formed in less than four minutes, and can significantly accelerate transesterification reaction. The micelle size was observed to be as low as 5.1 nm. Over aluminum isopropoxide, the yield in 2 hours at 150 degree Celsius increased to 20% in comparison with less than 2% without ultrasonic pretreatment. Over titanium isopropoxide, the yield in 2 hours at 150 degree Celsius increased to 64% in comparison with 48% without ultrasonic pretreatment. Although the active groups were reduced, partially polymerized titanium isopropoxide still showed good catalytic activity. Dimer of titanium isopropoxide had a yield of 45%, while cyclic tetramer of titanium isopropoxide seemingly had a yield of 32%. Apparent vapor pressure reduction was also observed, which could be at least 14% under normal initial gauge pressure (14 kPa) and 50% under an initial gauge pressure (550 kPa). The alcohol/soybean oil molar ratio was a main factor for apparent vapor pressure reduction.