小弟最近用到三乙胺,但是要求是干燥的,所以想在此请教如何干燥处理?
用KOH
如果对纯度要求不高,可以先用氢氧化钾或无水碳酸钾、4A分子筛、氢化钙、氢化铝锂等干燥,然后蒸馏即可。
如果对纯度要求很高,有三种方法。
1、加入乙酐,回流,再精馏。
2、加入苯甲酰氯或对甲苯磺酰氯回流,滤去不溶物,再精馏。
3、制成盐酸盐,用无水乙醇重结晶,再游离,氢氧化钾干燥。氮气保护下,加入少量金属钠精馏。
挺专业的,呵呵,长见识啊
了,确实够专业
ddddddddddddd
我记得好像使用氢化钙处理好重蒸的
Purification:
dried over CaSO4, LiAlH4, 4um sieves, CaH2, KOH, or K2CO3,
then distilled from BaO, sodium, P2O5 or CaH2.
Dried with CaSO4, LiAlH4, Linde type 4A molecular sieves, CaH2, KOH, or K2CO3, then distd, either alone or from BaO, sodium, P2O5 or CaH2. It has also been distd from zinc dust, under nitrogen. To remove traces of primary and secondary amines, triethylamine has been refluxed with acetic anhydride, benzoic anhydride, phthalic anhydride,
then distd, refluxed with CaH2 (ammonia-free) or KOH (or dried with activated alumina), and again distd. Another purification involved refluxing for 2h with p-toluenesulfonyl chloride, then distd. 够了吧!
用KOH
如果对纯度要求不高,可以先用氢氧化钾或无水碳酸钾、4A分子筛、氢化钙、氢化铝锂等干燥,然后蒸馏即可。
如果对纯度要求很高,有三种方法。
1、加入乙酐,回流,再精馏。
2、加入苯甲酰氯或对甲苯磺酰氯回流,滤去不溶物,再精馏。
3、制成盐酸盐,用无水乙醇重结晶,再游离,氢氧化钾干燥。氮气保护下,加入少量金属钠精馏。
挺专业的,呵呵,长见识啊
了,确实够专业
ddddddddddddd
我记得好像使用氢化钙处理好重蒸的
Purification:
dried over CaSO4, LiAlH4, 4um sieves, CaH2, KOH, or K2CO3,
then distilled from BaO, sodium, P2O5 or CaH2.
Dried with CaSO4, LiAlH4, Linde type 4A molecular sieves, CaH2, KOH, or K2CO3, then distd, either alone or from BaO, sodium, P2O5 or CaH2. It has also been distd from zinc dust, under nitrogen. To remove traces of primary and secondary amines, triethylamine has been refluxed with acetic anhydride, benzoic anhydride, phthalic anhydride,
then distd, refluxed with CaH2 (ammonia-free) or KOH (or dried with activated alumina), and again distd. Another purification involved refluxing for 2h with p-toluenesulfonyl chloride, then distd. 够了吧!