【作者】 孙崇鲁；

【导师】 黄克瀛；

【作者基本信息】 中南林业科技大学 ， 林产化学加工工程， 2007， 硕士

【摘要】 本课题对粉檀麝香(Phantolide)的合成工艺过程进行了研究,共分为三个部分：工业双戊烯液相催化脱氢制取对伞花烃的研究；以对伞花烃和含活性基团的五碳有机物为原料合成中间体1,1,2,3,3,6-六甲基茚满(HMI)的研究；HMI经过乙酰化反应合成粉檀麝香(Phantolide)的研究。对伞花烃的合成部分,以工业双戊烯为原料,通过液相脱氢反应来实现。对于此部分主要从催化剂的选择、催化剂的制备工艺对对伞花烃合成产率的影响及反应条件对合成产率的影响进行了研究。确定了最佳的催化剂制备工艺为浸渍时间4小时、浸渍温度80℃、钯的含量6%、浸渍的pH值为7.5、还原温度70℃、还原时间为1小时。最佳反应条件为反应温度为170-180℃、催化剂的用量为0.3%为宜、反应时间为3小时为宜。并且得出每次进行新的反应时,如果补充新的0.03%的催化剂就能够保持对伞花烃的得率基本不变达7次。在中间体HMI的合成部分,本课题分别以叔戊醇、2-甲基-2-丁烯为原料合成HMI的工艺进行了研究,然后利用GC-MS对两种原料合成HMI的主要副产物分别进行了分析。由叔戊醇合成HMI的反应中,通过单因素优化实验,确定较好的反应条件为：反应时间1.5小时左右,反应温度-10-0℃,反应中的浓硫酸的用量125g左右,对伞花烃和叔戊醇的摩尔比1：2。此时反应收率为40.89%。由2-甲基-2-丁烯合成HMI的反应中,通过单因素优化实验,确定较好的反应条件为：反应时间4小时,反应温度为：0℃,较佳溶剂为：对伞花烃,反应中的三氯化铝的用量为2.4g左右,对伞花烃的用量40.2g。此时反应收率为67.25%。通过对上述二种方法的比较研究可知,由于利用叔戊醇为原料时采用浓硫酸做催化剂,对设备腐蚀较大,利用2-甲基-2-丁烯为原料时采用三氯化铝做催化剂,比较适合工业上生产HMI。并且知道用2-甲基-2-丁烯合成HMI得率较高。在Phantolide的合成工艺研究部分,通过单因素试验,找到了反应收率最高的反应条件为：反应时间4小时,反应温度20℃,乙酰氯的用量8.5g左右,反应中的三氯化铝的用量20 g左右,此时反应收率可达88.92%。更多还原

【Abstract】 This thesis was mainly a detailed introduction of the process for preparing phantolide by three steps:first preparing p-cymene with liquid-phase catalytic dehydrogenation from industrial dipentene, then preparing 1,1,2,3,3,5-hexamethylindan(HMI)by using five-carbon-hydrocarbon containing active group and p-cymene as materials, at last preparing phantolide by acylation of HMI with chlori-acytyl.In the part of preparing p-cymene, the thesis did research on the preparing process of using industrial dipentene as the materials with liquid-phase catalytic dehydrogenation. For this part, the thesis mainly researced the choice of the catalyst, the effect to the yield of p-cymene by catalyst preparation craft and the reaction condition. We has determined the best catalyst preparation craft:dipping time was 4 hours, dipping temperature is 80℃, the content of Pd is 6%, the pH of dipping liquid is 7.5, the restoring temperature is 70℃, the restoring time is 1 hour.And we also has determined the best reaction condition:The reaction temperature is 170-180℃, the catalyst amount used is 0.3% for suitable, the reaction time is 3 hours for suitable. And we knew when each time carries on the new response, if supplemented the new 0.03% catalyst can maintain to the p-cymene yield invariablely 7 times.In the part of preparing HMI, the thesis did research on the preparing process of using Tertiary amyl alcohol,2-methyl-2-butene as the materials respectively. Then using GC-MS, the main outgrowths in each reaction systems were analyzed.In the part of Tertiary amyl alcohol producing HMI, through single-factor-experiments, the best reaction condition was found as:the keeping reaction time was about 1.5 hours; the reaction temperature was -10-0℃;the quantity of sulfuric acid was about 125g, the molar Ratio of p-cymene and Tertiary amyl alcohol is 1:2 and in such a condition the yield of reaction was 40.89%.In the part of using 2-methyl-2-butene as the material, through single-factor-experiments, the best condition was found:reaction time was 4 hours:reaction temperature was 0℃, the quantity of p-cymene was 21.998, the quantity of cyclo-hexane was 28.6g, the quantity of p-cymene is 40.2g and the yieldof reaction was 67.25%.Through mechanism analyzing on the process of producing HMI, it was known that because the sulfuric acid is more Spoile than the aluminum chloride. And also the yield to ben high when we used the 2-methyl-2-butene as materials. So it was suitable for producing HMI in industry production.In the part of producing Phantolide, through single-factor-Experiments, the highest yield of reaction condition was confirmed as:reaction time about 4 hours; reaction temperature about 20℃; the quantity of chlori-acytyl about 8.5g; the quantity of aluminum chloride 20g and the yield of reaction was as high as 88.92%.更多还原