反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Behenic methyl esters are made from hydrogenated high erucic acid rapeseed oil. About 870 grams of hydrogenated high erucic acid rapeseed oil, about 174 grams of methanol, and about 12.2 grams of sodium methoxide solution (25% in methanol) are added to a spherical 3-liter glass reactor. The reactor has a heating mantle, thermometer, temperature controller, reflux condenser, variable speed agitator, vacuum take-off, and bottom outlet. The mixture is reacted at about 65° C. for approximately 1.5 hours,while refluxing the methanol. The agitation is stopped, and the glycerin isallowed to settle for about 30 minutes. The glycerin settles to the bottom of the reactor, and is removed through the bottom outlet. About 30 additional grams of methanol, and about 5.2 grams of sodium methoxide solution (25% in methanol) are added to the glass reactor, and the mixtureis reacted at about 65° C. for about 30 minutes. The agitation is stopped, the glycerin is settled for about 30 minutes, and removed throughthe bottom outlet. About 100 grams of water are added to the mixture, stirred, allowed to settle, and removed through the bottom outlet. The water-washing procedure is repeated two more times. The reflux condenser is removed, and vacuum is broken, and a fractionation column is added to the reactor. The reactor is heated to about 170°-200° C. under a vacuum of about 0.3-1.0 mm Hg. Approximately 50% of the first material to evaporate from the column is collected and discarded. The next40% (approximately) of the material to evaporate from the column is collected as product. This product is approximately 92% by weight methyl behenate.
WORKUP
后处理
- temperaturethermometer, temperature controller, reflux condenser
- customThe mixture is reacted at about 65° C. for approximately 1.5 hours
- customis removed through the bottom outlet
- additionAbout 30 additional grams of methanol, and about 5.2 grams of sodium methoxide solution (25% in methanol) are added to the glass reactor
- customthe mixtureis reacted at about 65° C. for about 30 minutes
- customremoved throughthe bottom outlet
- additionAbout 100 grams of water are added to the mixture
- customremoved through the bottom outlet
- washThe water-washing procedure
- customThe reflux condenser is removed
- additiona fractionation column is added to the reactor
- temperatureThe reactor is heated to about 170°-200° C. under a vacuum of about 0.3-1.0 mm Hg
- customApproximately 50% of the first material to evaporate from the column
- customis collected
- customThe next40% (approximately) of the material to evaporate from the column
- customis collected as product