HRID1811607

反应详情

EQUATION

反应方程式

HRID 1811607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A carbon dioxide complex-containing mixture was produced using an apparatus as shown in FIG. 5. Approximately 1000 g of dibutyltin dimethoxide (made by Aldrich, USA) and approximately 7500 g of 1-propanol (made by Wako Pure Chemical Industries, Ltd., dehydrated grade) were fed via a transfer line 4 into a tank reactor 220 equipped with a stirrer, and the liquid mixture was heated to approximately 100° C., so as to produce dibutyltin dipropoxide. Methanol-containing 1-propanol produced from the reaction was recovered from a transfer line 6, and a dibutyltin dipropoxide-containing alkyltin alkoxide composition was transferred via a transfer line 5 into a thin film evaporator 130, where 1-propanol was evaporated off, and recovered via a condenser 132 and a transfer line 8. The alkyltin alkoxide composition was obtained from a lower portion of the thin film evaporator 130, this composition containing approximately 92 wt % of dibutyltin dipropoxide and approximately 7 wt % of 1,1,3,3-tetrabutyl-1,3-di(propyloxy)-distannoxane. The composition was cooled to approximately 95° C. using a cooler 131, and transferred into an upper portion of a carbon dioxide complex production apparatus 140 at a flow rate of approximately 1175 g/hr via a transfer line 7. A column reactor 240 of inside diameter 53.5 mm and effective length 2680 mm (packed length approximately 2000 mm) packed with a Dixon packing (made by Tokyo Tokushu Kanaami, Japan, size 6 mm) and equipped with a cooling jacket as shown in FIG. 7 was used as the carbon dioxide complex production apparatus 140. Gaseous carbon dioxide (made by Showa Tansan Co., Ltd., Japan, purity 99.99%, water content not more than 40 ppm) was supplied at normal pressure at approximately 200 g/hr via a transfer line 9 into a lower portion of the column reactor 240. The reaction temperature in the column reactor 240 was adjusted to approximately 100° C., and a carbon dioxide complex-containing mixture was produced. The mixture was a liquid, and was transferred out at normal pressure at a temperature of 100° C. via a transfer line 10, it being possible to carry out the transfer via the transfer line 10 without problems such as blockage of the line occurring. The mixture was sampled, and subjected to elemental analysis, whereupon the molar ratio between tin atoms, carbon dioxide, and OR groups in the mixture (Z:(CO2)x:(OR)y) was found to be such that x=0.25 and y=1.88.

WORKUP

后处理

  1. custom220 equipped with a stirrer