CN107774006A - 一种可控温的红外辅助提取与反应系统 - Google Patents
一种可控温的红外辅助提取与反应系统 Download PDFInfo
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Abstract
本发明属于混合物提取分离技术领域,涉及一种可控温的红外辅助提取与反应装置及其应用;该系统由红外光源、冷却控温机构、冷凝回流装置和反应容器构成;所述红外光源和所述冷却控温机构位于所述反应容器内部或外部,所述冷凝回流装置与所述反应容器相连接;所述反应物及溶剂位于所述反应容器内部。本发明利用红外线激励分子的振动、转动,从而加速了反应速率;控温机制确保了本发明可用于对温度敏感的反应。本发明与传统红外辅助提取装置相比,具有安全、适用范围广、反应效率高、反应过程可控性强和节能等优点。
Description
技术领域
本发明属于混合物提取分离技术领域,涉及一种可控温的红外辅助提取与反应系统及其应用。
背景技术
据资料显示,对于天然产物提取、药物分析和生产等领域,如何将目标成分快速、高效和安全地提取是工艺和方法研究的重点。目前,本领域采用的提取手段有溶剂提取、超声辅助提取、微波辅助提取和红外辅助提取;其中,所述溶剂提取是通过选择合适的溶剂,在常温或加热和条件下,将目标成分从基体中提取至溶剂中;通常采用该方法提取的耗时较长,可达数小时至数天,因而提取效率低下。所述超声辅助提取是利用介质(通常是溶剂)将高频机械波的能量传导至待提取物中,通过使其振动、破碎实现目标成分的溶出;然而,所述超声辅助提取会在工作过程中会产生人耳可闻的尖锐噪声,操作人员长期处于该环境下会对精神状态产生不利影响。所述微波辅助提取是利用微波能量激励电极性分析振动,从而增加分子的内能,加速目标物质的溶出,使用微波辅助提取的工作时间较短,通常在数分钟至数十分钟范围;然而,该方法不适用于非极性介质,且存在介质内加热不均匀的问题,局部的高温区会导致样品被分解、破坏;此外,由于微波辐射对人体有害,该方法的使用中还需严防微波能量的泄露,因而对设备的设计和使用提出了较高的要求,进而限制了该方法的通用性。所述红外辅助提取技术的原理是利用波长在1-50微米的红外线作用于样品及溶剂分子,使其通过吸收红外能量而提升内能,从而在分子层面加速目标物质向溶液的扩散;该方法的提取效率高,反应时间可从数小时缩短至几分钟;由于红外能量可高效地被样品及溶剂吸收,因而溶液体系的温度会迅速上升,若无有效的控温手段,则不可避免地造成样品中对温度敏感的目标成分被破坏,从而影响提取效率;对于一些酶解反应,由于酶极易被高温破坏,该反应通过使用传统的红外辅助提取装置几乎无法进行。
现有技术(中国专利CN101816842B)公开了一种红外辅助提取的系统和方法,其技术要点之一是通过红外线的辐照使样品升温并沸腾,从而完成提取过程。而大量的研究与试验实践表明,若干药品与食品中的有效成分对于温度较为敏感,在沸腾的温度条件下将会迅速分解;因此,对于该类物质的提取,上述专利公开的红外辅助提取装置与方法并不适用。
基于现有技术的现状,本发明针对现有技术的局限性,拟提供一种可控温的红外辅助提取与反应系统;该系统将显著扩展红外辅助提取技术的应用范围,有效解决温度敏感成分的提取或反应问题,并使得对红外辅助提取的热力学研究成为可能。
发明内容
本发明的目的在于克服现有技术的缺陷或不足,提供一种可控温的红外辅助提取与反应系统。
本发明的可控温的红外辅助提取与反应系统,其特征在于,主要由红外光源7、反应介质控温装置、冷凝回流装置1和反应容器6构成;所述红外光源7与反应介质控温装置位于所述反应容器6的内部或外部,所述冷凝回流装置1与所述反应容器6相连接;
本发明中,所述红外辅助提取技术利用波长在1-50微米的红外线能量可被大多数分子吸收的特性,通过红外辐照使分子的振动与转动加剧从而提升分子的内能,在分子水平上促进了目标成分的溶出或加快了反应速度;
所述的红外光源7的波长峰值为1-50微米;
本发明的一个实施例中,所述的红外光源可采用市售的红外灯泡,亦可针对容器形状订制红外灯管,其红外辐射峰值波长为1-50微米;
本发明中,所述反应介质控温装置包括热交换装置和搅拌装置;
更具体的,所述的反应介质控温装置由传热介质、冷却槽10、循环泵8、温度传感器4、温度控制器9和搅拌器2组成;所述传热介质通过循环泵8往复于冷却槽10与反应容器6内的传热介质管路3,将所述反应介质5的热量带走;所述循环泵8的启停由所述温度传感器4和温度控制器9控制,以恒定反应介质5的温度;为确保所述反应容器6内温度场的均匀性,可使用搅拌器2帮助混合处于不同温度的反应介质5;
本发明中,所述的反应介质5为液体,对于大多数应用场合,所述反应介质5可采用水;
本发明中,所述的反应介质控温装置的控温方式为致冷;
本发明中,所述的反应介质控温装置作用于反应介质的热传导媒介是液体或气体;
本发明中,所述的冷凝回流装置1,在设定温度不高时,可不启用;当设定温度较高,或反应介质5中有饱和蒸气压较高的物质时,可通过冷凝回流装置1帮助收集蒸汽,减少逸散及消除安全隐患;
本发明中,所述反应介质5(反应物及溶剂)置于所述反应容器6内部;
本发明利用红外线激励分子的振动、转动,从而加速了反应速率;控温机制确保了本发明可用于对温度敏感的反应。本发明与传统红外辅助提取装置相比,由于具有控温机制,从而使本发明具有安全、适用范围广、反应效率高、反应过程可控性强和节能等优点。
本发明所述系统充分考虑到现有红外辅助提取装置和方法的局限性,通过大量的理论分析和试验,提出了本发明所述可控温红外辅助提取与反应系统;本发明充分利用了红外辅助提取的快捷性,同时,通过控温机构又可任意调节反应体系的温度,使得原先无法通过现有红外辅助装置与方法进行的反应得以进行,不仅显著地扩展了红外辅助提取技术的适用物质范围,更由于可以精确控制反应体系的温度,从而可以进行红外辅助提取方法的热力学研究。本发明提供了研究红外线能量与物质反应机理的一种重要工具。
附图说明
图1为本发明的可控温的红外辅助提取与反应系统的系统示意图,
其中,1为冷凝回流装置,2为搅拌器,3为传热介质管路,4为温度传感器,5为反应介质,6为反应容器,7为红外光源,8为循环泵,9为温度控制器,10为冷却槽,11为电源接口。
图2为在不同提取温度下,丹参中丹酚酸B的提取率。
图3为在不同提取温度下,黄芩中黄芩素的提取率。
具体实施方式
实施例1:
如图1所示,本发明的可控温的红外辅助提取与反应系统中,所述反应容器6选取高硼硅玻璃或石英玻璃制备,要求容器材料耐高温,且对红外光有高的透过性;在所述反应容器6设有螺旋状的高硼硅玻璃或全氟乙丙稀的传热介质管路3,所述传热介质在管路内流过,完成与反应介质的热交换过程;所述传热介质管路3的选材既确保了红外线能有效透过管路,又可使换热过程能有效地进行;
对于小体积的反应容器,可将所述红外光源7置于反应容器6外;通常,所述红外光源7与所述反应容器6间维持一定距离,可设定为2厘米;所述红外光源7的功率视需要而定,一般为100-1000瓦;
所述冷却槽10的降温方式可采用冰块、压缩机或半导体制冷器;一般情况下,槽内储存的传热介质维持在1-2℃左右;
所述温度传感器4可采用铠装热电偶制备,直接插入于所述反应容器6内的反应介质5中,测量温度;
所述温度控制器9可采用PID(比例-积分-微分)温控器,通过调整合适的参数,可使所述反应介质5的温度稳定于设定温度;
所述反应容器6的顶部设有冷凝回流装置1,若所述反应介质5的温度较高,或其饱和蒸气压较高时,可开启回流,将蒸汽冷凝至液态,回流至反应容器6内;
所示搅拌器2可采用玻璃桨叶,使红外光源7发出的红外线能穿透桨叶,照射至所述反应介质5;
所述循环泵8可采用隔膜泵。
实施例2:丹参中丹酚酸B的控温红外辅助提取
丹参中丹酚酸B的控温红外辅助提取采用如图1所示的系统。
称取0.1g丹参粉末,在反应容器6内加入20ml去离子水作为提取溶剂,接通电源11,将温控器9设定为90℃,开启冷凝回流装置1,待温度稳定后加入丹参粉末开始反应并计时,反应8分钟后切断电源11,提取液定容、过滤,进样测定;色谱条件:岛津SPD-A紫外检测器;色谱柱:Diamonsil C18柱(5μm,150mm×4.6mm);流动相:乙腈-0.1%磷酸水溶液(22∶78);检测波长:286nm;柱温:25℃;流速:1.2mL·min-1;进样量:20μL;经计算,丹参中丹酚酸B的提取率为47.3mg/g。
提取温度对提取效果的影响如图2所示,图2为采用图1所示系统在40、60、80和90℃及不控温(图上100℃)条件下测得的丹参中丹酚酸B的提取率,分别为43.5、45.8、46.9、47.3和45.4mg/g。
结果如图2所示,当在不控温状态下进行红外辅助提取时,高温对丹酚酸B有明显的破坏作用,导致了丹参中丹酚酸B提取率的下降;试验结果表明了控温的必要性。
实施例3:黄芩中黄芩素的控温红外辅助提取
黄芩中黄芩素的控温红外辅助提取采用如图1所示的系统。
称取0.5g黄芩粉末,在反应容器6中加入10ml去离子水作为提取溶剂,接通电源11,将温控器9设定为50℃,开启冷凝回流装置1,待温度稳定后加入黄芩粉末开始反应并计时,反应60分钟后加入80ml的甲醇-盐酸(200∶1)至反应器6中,继续红外辐射20分钟后切断电源11,提取液定容、过滤,进样测定;色谱条件:安捷伦1200紫外检测器;Welch UltimateLP-C18(250×4.6mm,5μm)色谱柱;以甲醇(C)、0.4%磷酸溶液(B)为流动相,梯度洗脱:C:47%~47%,B:53%~53%(0~10min);C:47%~55%,B:53%~45%(10~30min);C:55%~60%,B:45%~40%(30~40min);C:40%~40%,B:60%~60%(40~50min);C:40%~53%,B:60%~47%(50~55min);C:53%~53%,B:47%~47%(55~60min);经计算,黄芩中黄芩素的提取率为139.6mg/g。
提取温度对提取效果的影响如图3所示,图3为采用如图1所述系统在20、30、40、50、60和70℃及不控温(图上100℃)条件下测得的黄芩中黄芩素的提取率,分别为126.8、136.6、138.5、139.6、117.7、80.6和47.7mg/g。
作为对照,利用水浴提取的方法在50℃、3小时条件下进行了提取,经计算,黄芩素的提取率为129.8mg/g。
所述黄芩中存在的黄芩酶能使黄芩苷分解为黄芩素等物质,然而黄芩酶的温度稳定性差,在高温下即被分解;在现有的红外辅助提取技术下,无法有效地完成黄芩中黄芩素的提取;通过应用本发明所述的控温红外辅助提取系统,不仅能使得该提取过程快速、高效地完成,更可将其作为研究提取过程动力学的有力工具。
需要指出的是,上述实施例仅为了说明本发明的技术构思与特点。本领域的技术人员可以根据本文说明,在本发明的范围内对本发明做出的各种修正和改变,这些修正和改变也纳入本发明的保护范围内。
Claims (8)
1.一种可控温的红外辅助提取与反应系统,其特征在于,主要由红外光源(7)、反应介质控温装置、冷凝回流装置(1)和反应容器(6)构成;所述红外光源(7)与所述反应介质控温装置位于所述反应容器(6)的内部或外部,所述冷凝回流装置(1)与所述反应容器(6)相连接。
2.按权利要求1所述的可控温的红外辅助提取与反应系统,其特征在于,所述反应介质控温装置由传热介质、冷却槽(10)、循环泵(8)、温度传感器(4)、温度控制器(9)和搅拌器(2)组成。
3.按权利要求2所述的可控温的红外辅助提取与反应系统,其特征在于,所述的反应介质控温装置作用于所述反应介质(5)的热传导媒介是液体或气体。
4.按权利要求2所述的可控温的红外辅助提取与反应系统,其特征在于,所述传热介质通过循环泵(8)往复于冷却槽(10)与反应容器(6)内的传热介质管路(3)。
5.按权利要求2所述的可控温的红外辅助提取与反应系统,其特征在于,所述循环泵(8)的启停由所述温度传感器(4)和温度控制器(9)控制,恒定所述反应介质(5)的温度。
6.按权利要求1或5任一所述的可控温的红外辅助提取与反应系统,其特征在于,所述反应介质(5)为液体。
7.按权利要求1或5任一所述的可控温的红外辅助提取与反应系统,其特征在于,所述的反应介质控温装置的控温方式为致冷。
8.按权利要求1所述的可控温的红外辅助提取与反应系统,其特征在于,所述红外光源(7)的波长峰值为1-50微米。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3970507A1 (en) * | 2020-09-17 | 2022-03-23 | HallStar Beauty and Personal Care Innovations Company | Extracting process of natural compounds assisted by infrared and infrasound |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4342200A (en) * | 1975-11-12 | 1982-08-03 | Daeco Fuels And Engineering Company | Combined engine cooling system and waste-heat driven heat pump |
CN101816842A (zh) * | 2010-01-20 | 2010-09-01 | 复旦大学 | 一种远红外辐射辅助提取系统 |
CN102023191A (zh) * | 2009-09-22 | 2011-04-20 | 复旦大学 | 一种从蔬果中提取抗坏血酸的方法 |
CN102133487A (zh) * | 2010-01-22 | 2011-07-27 | 复旦大学 | 一种红外提取与反应装置及其用途 |
CN203253194U (zh) * | 2013-05-21 | 2013-10-30 | 四川中方制药有限公司 | 一种自动控制温度的中药提取罐 |
CN203620290U (zh) * | 2013-12-17 | 2014-06-04 | 浙江华建尼龙有限公司 | 一种用于生产尼龙6切片的萃取塔 |
US20150157958A1 (en) * | 2013-12-06 | 2015-06-11 | Mazza Innovations, Ltd. | Pressurized low polarity water extraction apparatus and methods of use |
CN205007634U (zh) * | 2015-09-28 | 2016-02-03 | 河南智晶生物科技股份有限公司 | 双开关提取器 |
CN206424623U (zh) * | 2016-08-26 | 2017-08-22 | 段昊天 | 一种可控温的红外辅助提取与反应系统 |
-
2016
- 2016-08-26 CN CN201610747899.2A patent/CN107774006A/zh active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4342200A (en) * | 1975-11-12 | 1982-08-03 | Daeco Fuels And Engineering Company | Combined engine cooling system and waste-heat driven heat pump |
CN102023191A (zh) * | 2009-09-22 | 2011-04-20 | 复旦大学 | 一种从蔬果中提取抗坏血酸的方法 |
CN101816842A (zh) * | 2010-01-20 | 2010-09-01 | 复旦大学 | 一种远红外辐射辅助提取系统 |
CN102133487A (zh) * | 2010-01-22 | 2011-07-27 | 复旦大学 | 一种红外提取与反应装置及其用途 |
CN203253194U (zh) * | 2013-05-21 | 2013-10-30 | 四川中方制药有限公司 | 一种自动控制温度的中药提取罐 |
US20150157958A1 (en) * | 2013-12-06 | 2015-06-11 | Mazza Innovations, Ltd. | Pressurized low polarity water extraction apparatus and methods of use |
CN203620290U (zh) * | 2013-12-17 | 2014-06-04 | 浙江华建尼龙有限公司 | 一种用于生产尼龙6切片的萃取塔 |
CN205007634U (zh) * | 2015-09-28 | 2016-02-03 | 河南智晶生物科技股份有限公司 | 双开关提取器 |
CN206424623U (zh) * | 2016-08-26 | 2017-08-22 | 段昊天 | 一种可控温的红外辅助提取与反应系统 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3970507A1 (en) * | 2020-09-17 | 2022-03-23 | HallStar Beauty and Personal Care Innovations Company | Extracting process of natural compounds assisted by infrared and infrasound |
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