CN110015941B - Method for monitoring liquid holdup in process of preparing high-purity elemene - Google Patents
Method for monitoring liquid holdup in process of preparing high-purity elemene Download PDFInfo
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Abstract
The invention belongs to the technical field of separation and rectification of natural medicines, and discloses a method for monitoring liquid holdup in a process of preparing high-purity elemene. When the heating temperature and the vacuum degree of the column bottom are constant, the gas-liquid conversion frequency in the rectification column is increased, the gas which rises to the condenser part in unit time is decreased, and the liquid amount condensed by the condenser, namely the liquid holdup, is monitored, so that the fractionation effect in the rectification column can be judged. The liquid holdup range of high-quality products can be stably produced, the control range of the liquid holdup is determined, the liquid holdup is monitored in the production process, the liquid holdup is adjusted in time, and the purpose of stably producing the high-quality products is achieved.
Description
Technical Field
The invention belongs to the technical field of separation and rectification of natural medicines, and relates to a method for monitoring liquid holdup in a process of preparing high-purity elemene.
Background
In the last 70 th century, people found that zedoary turmeric oil extracted from Curcuma wenyujin had antiviral and antitumor effects; elemene is separated from zedoary turmeric oil in 90 years, and is considered to be an effective component for resisting tumors through research, the action mechanism of the elemene is that the elemene has strong affinity with tumor cells, the tumor cell membranes are damaged, the permeability of the tumor cell membranes is changed, the tumor cell interstitial leakage is caused, the tumor cell apoptosis is induced, and the elemene can be directly contacted with the tumor cells to better exert the curative effect of resisting the tumors. Therefore, it is important to industrialize the production of elemene and obtain high-purity elemene both economically and in terms of overcoming cancer and promoting human health.
Chinese patent 'an industrial production method of high-purity beta-elemene bulk drug' (publication No. CN 101402544A) discloses a method for preparing high-purity beta-elemene from natural plants containing beta-elemene, such as rhizoma Zedoariae, cymbopogon citratus, one day lily, etc., which can improve the production efficiency from starting materials to high-purity beta-elemene and reduce the production cost. The method comprises the steps of taking roots, stems, leaves, flowers and seeds of the natural plants as raw materials, extracting volatile oil by adopting different volatile oil extraction methods, rectifying the volatile oil by adopting a rectification method to obtain high-content beta-elemene, removing impurity components by sequentially adopting a macroporous adsorption resin separation method or a macroporous adsorption resin combined ethanol extraction method and a silver nitrate complexation extraction method, and finally carrying out reduced pressure distillation or rectification to obtain the beta-elemene with the content of 95-99.9%. The extract is obtained by extracting beta-elemene from Cymbopogon citratus, and is deficient in gamma-elemene and delta-elemene, and has poor therapeutic effect compared with extract obtained by extracting elemene from Curcumae rhizoma.
Chinese patent ZL200510049615.4 discloses a production process for extracting beta-elemene anticancer raw material medicine from common turmeric, which takes common turmeric rhizome as a raw material for extracting the beta-elemene, and obtains the anticancer raw material medicine through steam distillation, multi-row synchronous rectification and precise fractionation. The method solves the problem of low industrial production degree of the beta-elemene in the prior art, has more materials for one time, has large quantity of the beta-elemene anticancer raw material medicines for collecting, greatly shortens the extraction time, and is suitable for industrial production. The process adopts a method of synchronous rectification and precise fractionation, and as the zedoary turmeric oil obtained by steam distillation contains more components, when the zedoary turmeric oil is subjected to a multi-row synchronous rectification and precise fractionation method, key process parameters of the process are vacuum degree, reflux ratio and temperature, the vacuum degree, reflux ratio and temperature are not fixed values but are in a variable range under the influence of complex components of raw zedoary turmeric oil, and the stability of the quality of the produced product cannot be ensured through manual operation.
The existing vacuum distillation; the extraction equipment is divided into four main parts, namely a heating kettle, a fractionating column, a condenser and a vacuum system. The heating kettle mainly heats the mixture to gasify the mixture, the mixture ascends to the fractionating column, high-boiling-point steam in the fractionating column is liquefied when meeting cold, low-boiling-point steam continuously ascends, the high-boiling-point steam in the ascending steam is liquefied when meeting cold, the low-boiling-point steam continuously ascends, the liquefied low-boiling-point substances are partially gasified when meeting the steam newly entering the fractionating column, the steps are repeated, gas-liquid conversion is carried out in the fractionating column from bottom to top for many times, and finally the gas moving to the condenser part is gas with single component, so that the aim of rectifying and extracting the target fraction is fulfilled.
However, the prior rectification technology has no method for monitoring and controlling the liquid holdup to control the product quality.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for monitoring liquid holdup in the process of preparing high-purity elemene. The liquid holdup range of high-quality products can be stably produced, the control range of the liquid holdup is determined, the liquid holdup is monitored in the production process, the liquid holdup is adjusted in time, and the purpose of stably producing the high-quality products is achieved.
The above purpose of the invention is realized by the following technical scheme:
a method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. adding zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300-340 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 1000Pa until reflux appears, adjusting the temperature of the tower kettle to be 230-270 ℃ to carry out total reflux for 30-50 minutes, and then starting to receive fraction I, wherein the reflux ratio is controlled to be 4-6;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. total reflux is carried out for 50-60min;
D. c, starting to receive fraction III after the step C, and controlling the reflux ratio to be 4-5 until the fraction is obviously layered;
E. fraction four was initially received after step D: elemene with a reflux ratio of 5-6:1, preparing elemene.
Preferably, during the extraction of elemene, four fractions are separated from low boiling point to high boiling point.
Preferably, the liquid holding capacity of fraction one is controlled to be 4-11ml/min.
Preferably, fraction two does not control the liquid hold-up due to the presence of crystals.
Preferably, the liquid holding capacity of the fraction is controlled to be 2-7ml/min.
Preferably, the liquid content of the fraction IV is controlled to be 2.5-9ml/min.
And a receiving buffer valve is added at the lower receiver part of the condenser, volume scales are marked at the upper end of the valve, the time required for receiving a certain amount of products is recorded, and the liquid holdup is obtained through conversion. The fractionation effect is known through monitoring the liquid holdup in the whole vacuum distillation process, the heating temperature of the tower kettle is adjusted in time according to the change of the liquid holdup, the separation effect is controlled within the process requirement range, the one-time yield of elemene is improved, the product quality of elemene is stabilized, and the purity of elemene is improved.
The quality and purity of the rectification product are mainly determined by the gas-liquid conversion capacity in the fractionating column, and the more gas-liquid conversion times, the purer the components of the target product; the gas-liquid conversion times in the fractionating column in unit time can be judged by the liquid amount condensed by the condenser, namely the liquid holdup, and under the condition that the temperature and the vacuum degree of the tower kettle are not changed, the large liquid holdup indicates that the gas-liquid conversion times in unit time are small, the column efficiency is low, the separation effect is poor, and otherwise, the separation effect is good.
Compared with the prior art, the invention has the beneficial effects that:
the liquid holdup is controlled according to the component amount of each stage in the process of reduced pressure distillation, so that the purpose of stabilizing column effect is achieved, the liquid holdup in the production process is monitored in real time, the one-time finished product rate of elemene is improved, the product quality of elemene is stabilized, the elemene purity is improved, the average elemene content of the existing elemene extraction method is 80%, and the average elemene content can reach 87% by adopting the method.
Drawings
FIG. 1 is a schematic view of a fractionating column structure of a fractionating apparatus according to the present invention.
In the figure, 1 is a condenser, 2 is a buffer receiving valve, and 3 is a receiver.
Detailed Description
The present invention will be described in more detail below with reference to the accompanying drawings by way of specific embodiments. The following examples are illustrative only, not limiting, and are not intended to limit the scope of the invention. In the examples, unless otherwise specified, the experimental methods are all conventional methods; the test apparatus is commercially available unless otherwise specified. The instruments adopted in the invention are all manufactured by Dalian quartz glass instrument factories. The preparation methods employed in the examples can be carried out using the fractionation apparatus described in FIG. 1.
Example 1
A method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 500Pa until reflux appears, adjusting the temperature of the tower kettle to be 260 ℃ to carry out total reflux for 30 minutes, then starting to receive fraction I, controlling the liquid holdup of the fraction I to be 4mL/min, and controlling the reflux ratio to be 4;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III, controlling the liquid holding amount to be 2mL/min, and controlling the reflux ratio to be 5;
E. starting to receive fraction four after step D: elemene with a reflux ratio of 6:1, controlling the liquid holdup to be 2.5mL/min to prepare elemene.
Example 2
A method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 500Pa until reflux appears, adjusting the temperature of the tower kettle to be 260 ℃ to carry out total reflux for 30 minutes, then starting to receive fraction I, controlling the liquid holdup of the fraction I to be 7mL/min, and controlling the reflux ratio to be 4;
B. until crystallization occurs, starting to receive fraction two until the crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III after the step C, controlling the liquid holding amount to be 5mL/min, and controlling the reflux ratio to be 5;
E. starting to receive fraction four after step D: elemene with a reflux ratio of 6:1, controlling the liquid holdup at 6mL/min to obtain elemene.
Example 3
A method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 500Pa until reflux appears, adjusting the temperature of the tower kettle to be 260 ℃ to carry out total reflux for 30 minutes, then starting to receive fraction I, controlling the liquid holdup of the fraction I to be 11mL/min, and controlling the reflux ratio to be 4;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III after the step C, controlling the liquid holding amount to be 7mL/min, and controlling the reflux ratio to be 5;
E. starting to receive fraction four after step D: elemene with a reflux ratio of 6:1, controlling the liquid holdup to be 9mL/min to prepare elemene.
Example 4
A method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 340 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 1000Pa until reflux appears, adjusting the temperature of the tower kettle to be 230 ℃ to carry out total reflux for 50 minutes, then starting to receive fraction I, controlling the liquid holdup of the fraction I to be 11mL/min, and controlling the reflux ratio to be 6;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III, controlling the liquid holding amount to be 7mL/min, and controlling the reflux ratio to be 4;
E. starting to receive fraction four after step D: elemene with a reflux ratio of 5:1, controlling the liquid holdup to be 9mL/min to prepare elemene.
Example 5
A method for monitoring liquid holdup in the process of preparing high-purity elemene comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 340 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 1000Pa until reflux occurs, adjusting the temperature of the tower kettle to be 270 ℃, starting to receive a fraction I after full reflux is carried out for 50 minutes, controlling the liquid holdup of the fraction I to be 11mL/min, and controlling the reflux ratio to be 4;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III after the step C, controlling the liquid holding amount to be 7mL/min, and controlling the reflux ratio to be 5;
E. fraction four was initially received after step D: elemene with a reflux ratio of 5:1, controlling the liquid holdup to be 9mL/min to prepare elemene.
The traditional method comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 330 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 900Pa until reflux appears, adjusting the temperature of the tower kettle to be 230 ℃ and carrying out total reflux for 50 minutes, and then starting to receive fraction I, wherein the reflux ratio is controlled to be 3;
B. until crystallization appears, fraction II begins to be received until crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III after the step C, and controlling the reflux ratio to be 4;
E. starting to receive fraction four after step D: elemene with a reflux ratio of 5:1, preparing elemene.
Compared with the elemene prepared by 5 batches in the comparative example of the traditional method, the purity of the elemene prepared by the methods of the examples 1 to 5 is obviously improved, and the elemene is detailed in the following table:
while the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims; meanwhile, any equivalent changes, modifications and variations of the above embodiments according to the essential technology of the present invention are within the scope of the technical solution of the present invention.
Claims (2)
1. A method for monitoring liquid holdup in the process of preparing high-purity elemene is characterized in that elemene is divided into four fractions from low boiling point to high boiling point in the extraction process of elemene;
the method comprises the following specific steps:
A. adding zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300-340 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 1000Pa until reflux appears, adjusting the temperature of the tower kettle to be 230-270 ℃ to carry out total reflux for 30-50 minutes, and then starting to receive fraction I, wherein the reflux ratio is controlled to be 4-6:1;
B. until crystallization occurs, starting to receive fraction two until the crystallization disappears;
C. total reflux is carried out for 50-60min;
D. c, starting to receive fraction III after the step C, and controlling the reflux ratio to be 4-5:1 until the fraction is obviously layered;
E. starting to receive fraction four after step D: preparing elemene with reflux ratio of 5-6: 1;
monitoring the liquid volume (namely liquid holdup) condensed by the condenser, and adjusting the heating temperature of the tower kettle in time according to the change of the liquid holdup;
the liquid holding amount of the first fraction is controlled to be 4-11ml/min;
the liquid holding amount of the fraction III is controlled to be 2-7ml/min;
the liquid content of the fraction IV is controlled to be 2.5-9ml/min.
2. The method as claimed in claim 1, wherein the method comprises the following steps:
A. putting 3000 g of zedoary turmeric oil into a tower kettle of a reduced pressure precise fractionation device, setting the heating temperature of the tower kettle to be 300 ℃, adjusting a valve on a vacuum pipeline to control the vacuum degree to be below 500Pa until reflux occurs, adjusting the temperature of the tower kettle to be 260 ℃, performing total reflux for 30 minutes, then starting to receive a fraction I, controlling the liquid holdup of the fraction I to be 7mL/min, and controlling the reflux ratio to be 4:1;
B. until crystallization occurs, starting to receive fraction two until the crystallization disappears;
C. performing total reflux for 60min;
D. c, starting to receive fraction III after the step C, controlling the liquid holding amount to be 5mL/min, and controlling the reflux ratio to be 5:1 until the fraction is obviously layered;
E. fraction four was initially received after step D: the elemene is prepared by controlling the reflux ratio of elemene to be 6:1 and the liquid holding amount to be 6 mL/min.
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| CN101531563A (en) * | 2009-02-16 | 2009-09-16 | 沈阳万爱普利德医药科技有限公司 | Chemical complexing directional separation and purification method for preparing high-purity beta-elemene raw material medicament |
| CN105467965B (en) * | 2015-12-30 | 2018-02-23 | 大连德泽药业有限公司 | The automatic acceptance control method of elemene industrialized production |
| CN105477899B (en) * | 2015-12-30 | 2017-11-03 | 大连德泽药业有限公司 | The automatic receiving control device of elemene industrialized production |
| CN105797417B (en) * | 2016-04-29 | 2018-07-06 | 大连德泽药业有限公司 | Monitor fractionating device, method and system that temperature prepares high-purity fraction |
| CN205649874U (en) * | 2016-04-29 | 2016-10-19 | 大连德泽药业有限公司 | Fractional distillation apparatus and system of control temperature preparation high -purity fraction |
| CN106588615A (en) * | 2016-11-29 | 2017-04-26 | 大连德泽药业有限公司 | Application of Zedoary turmeric oil in preparation of camphor and isolation and extraction method of Zedoary turmeric oil |
| CN107389150A (en) * | 2017-08-17 | 2017-11-24 | 中国大唐集团科学技术研究院有限公司华中分公司 | A kind of wet method fume desulfurizing system absorption tower pallet liquid holdup monitoring method |
| CN208104255U (en) * | 2017-08-29 | 2018-11-16 | 湖北工程学院 | A kind of n-hexane purification system and chromatographically pure n-hexane production system |
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