CN104479861A - 一种萃取脂溶性物质的方法 - Google Patents
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Abstract
本发明涉及一种萃取脂溶性物质的方法。用三氯三氟乙烷作为溶剂，在密闭萃取器内、常压状态下，萃取经过前处理的植物种子、花朵、微生物发酵法培养的菌体、辣椒、油砂等，物料与溶剂的重量比为1：0.8～6，温度15～50℃、压力-0.01～0.1MPa，萃取时间为10～60min，萃取结束后，进行固液分离，再分别回收物料及液体内的溶剂，溶剂回收后重新使用。采用本发明，所用溶剂本身无毒、不燃烧；萃取效果好，出油率高；设备为常压设备，一次投资及运行成本低；萃取及浓缩分离溶剂的温度低，可实现低温保质萃取，推广应用前景较好。
Description
技术领域
本发明涉及一种萃取脂溶性物质的方法，具体的说是以三氯三氟乙烷为溶剂萃取油脂的方法。
背景技术
目前，植物种子、花朵等油脂的制取包括压榨法、萃取法。萃取法分为常温萃取、亚临界低温萃取、超临界二氧化碳萃取三种。超临界二氧化碳萃取系统压力高、设备投资大、运行成本高，一般企业无法接受；亚临界低温萃取投资、运行成本比超临界二氧化碳萃取低，但远比同等规模常温己烷萃取高得多，溶剂为易燃、易爆的丙烷、丁烷、甲醚等，且为压力容器、压力管道；常温己烷萃取为国内大多数油脂企业的首选，虽是常压设备，其投资、运行成本都低，但是所选的溶剂为易燃、易爆的己烷、戊烷、丙酮等。存在较大安全隐患。
三氯三氟乙烷无毒、不易燃烧、萃取油脂效果非常好，设备为常压容器，并能实现低温物理分离。以液态三氯三氟乙烷作为溶剂萃取油脂具备很好的发展前景。
CN85108457A公开了三氯三氟乙烷、乙醇、硝基甲烷和2-甲基戊烷或各种己烷的混合物的类似共沸混合物的组成，作为脱脂剂用于各种工业清洗，清洗固体表面油污，没有用于植物种子等油脂的萃取。
CN85108360A公开了三氯三氟乙烷、乙醇、丙酮、硝基甲烷和己烷的类似共沸混合物的组成，作为脱脂剂用于各种工业清洗，清洗固体表面油污，没有用于植物种子等油脂的萃取。
申请号87108260.8公开了三氯三氟乙烷与二氯二氟乙烷的共沸物或类共沸物的组成，作为脱脂剂用于各种工业清洗，清洗固体表面油污，没有用于植物种子等油脂的萃取。
申请号88104320.6公开了三氯三氟乙烷、甲醇、硝基甲烷和丙酮的共沸状组合物，作为脱脂剂用于各种工业清洗，清洗印刷线路板的助焊剂等，没有用于植物种子等油脂的萃取。
申请号881044803.8公开了三氯三氟乙烷、甲醇和1，2-二氯乙烯的共沸物或类似共沸物的混合物，作为脱脂剂用于各种工业清洗，清洗印刷线路板的助焊剂等，没有用于植物种子等油脂的萃取。
发明内容
本发明的目的在于提供一种萃取脂溶性物质的方法。
一种萃取脂溶性物质的方法，以三氯三氟乙烷作为溶剂，在密闭萃取器内、常压或微负压状态下，对植物种子、花朵、微生物发酵法培养的菌体、辣椒、油砂中的脂溶性物质进行萃取，其工艺条件为：
（1）预处理：将被萃取的物料进行预处理，植物种子经过压榨成饼或轧成0.25~0.3mm薄片；花朵经烘干、粉碎成40~60目，再造成φ3~5×15~35棒粒；辣椒经脱籽、烘干、粉碎成40~60目，再造成φ3~5×15~35棒粒；油砂粉碎成5~10目；
（2）萃取：把经过预处理的物料投入萃取器内，以三氯三氟乙烷作为溶剂，对物料进行萃取，物料与溶剂的重量比为1：0.8～6，萃取温度为15～50℃，压力-0.01～0.1MPa，萃取时间为10～60min；按照逆流萃取原理重复萃取2～8次，进行固液分离，收集萃取液；
（3）浓缩：对（2）中收集的萃取液进行过滤或沉降，去除其中的细小杂质，将萃取液分离为气相和浓缩物，将气相冷凝、液化、回收后重新使用，浓缩物即为所萃取的脂溶性物质。
采用本发明，所用溶剂本身无毒、不燃烧；萃取效果好，出油率高；设备为常压设备，一次投资及运行成本低；萃取及浓缩分离溶剂的温度低，可实现低温保质萃取，推广应用前景较好。
具体实施方式
下面具体说明实现本发明的工艺流程和实现方式：
（一）、工艺流程
（1）预处理：将被萃取的物料进行预处理，植物种子（如大豆、花生、菜籽、印楝等）经过压榨成饼或直接轧成0.25~0.3mm薄片；花朵（如万寿菊、除虫菊等）经烘干、粉碎成40~60目后再造成φ3~5×15~35棒粒；辣椒经脱籽、烘干、粉碎成40~60目后，再造成φ3~5×15~35棒粒；油砂粉碎成5~10目。
（2）萃取：把经过预处理的物料投入萃取器内，以三氯三氟乙烷作为溶剂，对物料进行萃取，物料与溶剂的重量比为1：0.8～6，萃取温度为15～50℃，压力-0.01～0.1MPa，萃取时间为10～60min；按照逆流萃取原理重复萃取2～8次，进行固液分离，收集萃取液。
（3）浓缩：对（2）中收集的萃取液进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热分离为气相和浓缩物，将气相溶剂冷凝、液化、回收后重新使用，浓缩物即为所萃取的毛油或脂溶性物质。
上述操作过程均是在密闭的条件下完成。
（二）、实现方式
下面用具体实施方式进一步说明本发明的方法：
实施例1：取根据上述工艺流程中步骤1制备的花生饼100㎏，置于萃取容器中，加入100㎏三氯三氟乙烷，萃取温度为40℃，萃取时间为60min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取2～8次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的花生油。
实施例2：取根据上述工艺流程中步骤1制备的大豆片100㎏，置于萃取容器中，加入100㎏三氯三氟乙烷，萃取温度为35℃，萃取时间为30min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取3～6次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收到溶剂周转罐；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的大豆油。
实施例3：取根据上述工艺流程中步骤1制备的除虫菊颗粒50㎏，置于萃取容器中，加入150㎏三氯三氟乙烷，萃取温度为40℃，萃取时间为60min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取2～8次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收到溶剂周转罐；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的除虫菊酯。
实施例4：取根据上述工艺流程中步骤1制备的辣椒颗粒100㎏，置于萃取容器中，加入300㎏三氯三氟乙烷，萃取温度为40℃，萃取时间为60min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取2～8次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收到溶剂周转罐；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的辣椒油。
实施例5：取根据上述工艺流程中步骤1制备的油砂颗粒100㎏，置于萃取容器中，加入100㎏三氯三氟乙烷，萃取温度为50℃，萃取时间为60min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取3～6次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收到溶剂周转罐；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的矿物油。
实施例6：取根据上述工艺流程中步骤1制备的微生物发酵法培养的菌体100㎏，置于萃取容器中，加入200㎏三氯三氟乙烷，萃取温度为15℃，萃取时间为60min；萃取结束后进行固液分离，对分离的固相按上述工艺条件重复萃取2～8次；对液相进行过滤或沉降，去除其中的细小杂质后注入分离器，在分离器内加热或减压分离为气相和浓缩物，将气相溶剂冷凝液化回收到溶剂周转罐；将浓缩物控制温度在20～50℃，常压或负压的条件下脱除溶剂，就得到了所萃取的微藻油。
根据本发明的方法，会有无数种萃取条件，仅用几个实施例很难概括所有萃取条件，但只要是符合本发明的技术原意的萃取条件和方法，均应列入本发明的保护范围。
Claims (2)
1.一种萃取脂溶性物质的方法，以三氯三氟乙烷作为溶剂，在密闭萃取器内、常压或微负压状态下，对植物种子、花朵、微生物发酵法培养的菌体、辣椒、油砂中的脂溶性物质进行萃取，其工艺条件为：
（1）预处理：将被萃取的物料进行预处理，植物种子经过压榨成饼或轧成0.25~0.3mm薄片；花朵经烘干、粉碎成40~60目，再造成φ3~5×15~35棒粒；辣椒经脱籽、烘干、粉碎成40~60目，再造成φ3~5×15~35棒粒；油砂粉碎成5~10目；
（2）萃取：把经过预处理的物料投入萃取器内，以三氯三氟乙烷作为溶剂，对物料进行萃取，物料与溶剂的重量比为1：0.8～6，萃取温度为15～50℃，压力-0.01～0.1MPa，萃取时间为10～60min；按照逆流萃取原理重复萃取2～8次，进行固液分离，收集萃取液；
（3）浓缩：对（2）中收集的萃取液进行过滤或沉降，去除其中的细小杂质，将萃取液分离为气相和浓缩物，将气相冷凝、液化、回收后重新使用，浓缩物即为所萃取的脂溶性物质。
2.根据权利要求1所述的一种萃取脂溶性物质的方法，其特征在于所述被萃取物料，植物种子包括大豆、花生、菜籽、印楝、葵花、蓖麻，花朵包括万寿菊、除虫菊、微生物发酵法培养的菌体DHA、ARA、辣椒、油砂，包括但不限于上述物料。
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