CN1056488A - 合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺 - Google Patents
合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺 Download PDFInfo
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- CN1056488A CN1056488A CN 91103318 CN91103318A CN1056488A CN 1056488 A CN1056488 A CN 1056488A CN 91103318 CN91103318 CN 91103318 CN 91103318 A CN91103318 A CN 91103318A CN 1056488 A CN1056488 A CN 1056488A
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Abstract
本发明属于合成柳酸丁酯、柳酸异丁酯和柳酸异
戊酯的一种新工艺,该工艺的特征在于它采用了一种
普通市售的硼酸作催化剂,采用该催化剂所合成的柳
酸丁酯、柳酸异丁酯和柳酸异戊酯,其得率可在90~
95%之间。
Description
本发明属于合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺,涉及一种有机化合物的生产工艺方法。
柳酸丁酯、柳酸异丁酯和柳酸异戊酯是重要的系列合成香料化工原料,广泛用于化妆品和皂用香精中。目前,工业上生产柳酸丁酯、柳酸异丁酯和柳酸异戊酯的方法,基本是采用硫酸作催化剂,将柳酸和醇(丁醇、异丁醇或异戊醇)进行加热共沸脱水而成的。(参阅刘树文译、顾永康校的《香料化学》,第129页)。由于使用硫酸作催化剂,不仅对设备有严重腐蚀和三废污染环境的缺点贿对柳酸和醇均会产生破坏作用,影响产品香气质量。
本发明是采用普通市售硼酸作催化剂,其化学分子式是H3BO3,不需要作任何加工前处理,就可替代硫酸作催化剂,使得所需的柳酸丁酯、异丁酯和异戊酯的收得率可达90%-95%,产品含酯量均达99%以上。
下面以柳酸异戊酯的制备方法为例,将本发明详述如下:
在一个装有回流冷凝器、分水器和温度计的三口烧瓶中,加入柳酸138克,异戊醇170克及硼酸6克。将反应烧瓶置于一个带有自动温度控制器的电加热套中加热回流脱水,当分水器中分出的水分不再增加也就是水分出完时,除去电加热套,待反应物冷至室温后,将反应物进行洗涤,除去未反应的柳酸(可回收重复使用),即得到粗酯,将粗酯再进行减压分馏,得到所需产品柳酸异戊酯182克,其含酯量达99%以上;n20为1.5055;d25为1.048;柳酸异戊酯得率为95.8%。同样其他二种产品的实施例,试验数据列于下表:
本发明由于使用了硼酸替代硫酸,这样就避免了由于使用硫酸而引起对柳酸和醇产生破坏作用;而且在没有增加成本的基础上对设备腐蚀和三废污染环境等有很大的解决,故是目前合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯最为理想的酯化方法。
Claims (3)
1、一种合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯的新工艺,其特征在于它采用普通市售的硼酸作为合成的催化剂。该催化剂的化学成份为H3BO3。
2、根据权利要求1所述的新工艺,其特征为:在一个装有回流冷凝器、分水器和温度计的三口瓶中,加入柳酸和醇,以及权利要求1所述的催化剂,将烧瓶置于一个带有自动温度控制器的电加热套中加热,回流脱水,直至水分分离完毕为止,然后,除去电加热套,待反应物冷却到室温后,将反应物中未反应的柳酸洗去得到粗酯,再将粗酯进行减压分馏,即得所需柳酸酯制品。
3、根据权利要求2所述新工艺,其特征是在所述的在电加热套中加热的温度是120℃~170℃;回流脱水时间为5~10小时,所加入的酸和醇的克分子比为1∶1.2~3,催化剂加入量为柳酸加入量的1%-10%。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 91103318 CN1056488A (zh) | 1991-05-17 | 1991-05-17 | 合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺 |
Applications Claiming Priority (1)
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CN 91103318 CN1056488A (zh) | 1991-05-17 | 1991-05-17 | 合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺 |
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CN1056488A true CN1056488A (zh) | 1991-11-27 |
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CN 91103318 Pending CN1056488A (zh) | 1991-05-17 | 1991-05-17 | 合成柳酸丁酯、柳酸异丁酯和柳酸异戊酯新工艺 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000027953A1 (en) * | 1998-11-10 | 2000-05-18 | Shell International Research Maatschappij B.V. | Lubricity additive, process for preparing lubricity additives, and middle distillate fuel compositions containing the same |
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1991
- 1991-05-17 CN CN 91103318 patent/CN1056488A/zh active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000027953A1 (en) * | 1998-11-10 | 2000-05-18 | Shell International Research Maatschappij B.V. | Lubricity additive, process for preparing lubricity additives, and middle distillate fuel compositions containing the same |
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