摘要
研究以二氯甲烷为溶剂,三氯化磷、正丁醇为原料合成亚磷酸二正丁酯(T304)的技术,探讨了进料方式、原料比、反应时间、反应温度、溶剂用量与吹扫氮气流速对反应结果的影响,确定了优化的合成技术条件。结果表明,以二氯甲烷为反应溶剂,采用滴加正丁醇到PCl3与二氯甲烷混合液中的加料方式,反应物PCl3与C4H9OH的物质的量比为1.0∶3.0,反应温度为5～8,反应时间为100～120 min,副产物HCl采用氮气吹扫与真空泵抽真空相结合的排除方式,合成的T304产品收率达98.1%。31P核磁分析显示产物中亚磷酸二正丁酯的纯度超过99.0%。
The method for preparing dibutyl phosphite （T304） was improved using n -butanol and phosphorus trichloride as materials and dichloromethane as solvent. The influences of materials feeding mode, mole ratio, reaction time, reaction temperature, the amount of solvent and flow rate of nitrogen on the reaction were studied, and the optimal technology con- ditions were obtained. The results showed that, when dropping n - butanol into the mixture of PCI3 and dichloromethane, reacting under the optimal technology conditions, and adopting the combination method of nitrogen purging and vacuum pumping to exhaust the by - product of HCI, the yield of T304 arrives to 98.1%. The purity of dibutyl phosphite is more than 99% by 3, p NMR analysis.
出处
《润滑油》
CAS
2012年第5期39-42,46,共5页
Lubricating Oil
