1-Butanol → Dibutoxydibutylstannane

Participants

Reaction Conditions

Reaction Steps

A feed pump was used to start feeding the starting material 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane prepared in the same manner as in Example 12 from supply line 93 at 280 g/Hr and the reactant 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 94 at 1,330 g/Hr. The holding time in the reactor was 6 minutes. A pump was used to supply hexane (manufactured by Wako Pure Chemical Industries Ltd., Japan, dehydration grade) at 300 g/Hr from the organic solvent supply line 96 to the reactor lower portion 102, wherein accumulated reaction solution was circulated at 6,000 g/Hr by the circulation line 97 and the reboiler 98 while heating at a temperature of about 140° C. The liquid temperature inside the reactor was 140° C., and the pressure of the back pressure valve 106 was adjusted to 0.12 MPa-G. Continuous supply was continued in this state for 10 hours, after which the system reached a steady state. Low boiling point components flowed from the reactor upper portion 101 and through the low boiling point component recovery line 103 for liquefaction at the condenser 104, and were thereby recovered from the liquid-phase recovery line 108 at 1,088 g/Hr. Furthermore, from the reactor lower portion 102, a dibutyltin alkoxide-containing component was recovered at 821 g/Hr from the extraction line 109. Analysis of the recovered liquid showed that using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 54.0% dibutyl-di(butyloxy)tin and 46.0% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.013%. Meanwhile, the liquid recovered from the liquid-phase recovery line 108 was transparent and contained 2,500 ppm of moisture. The dehydration rate in the column reactor was 0.24 mol/Hr, which was greater than the value 0.00037 mol/Hr calculated from expression (16).

Provenance & Evidence