CN101879380A - Energy-saving concentration process for extracting active ingredients of plants and concentration device thereof - Google Patents
Energy-saving concentration process for extracting active ingredients of plants and concentration device thereof Download PDFInfo
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- CN101879380A CN101879380A CN 201010209340 CN201010209340A CN101879380A CN 101879380 A CN101879380 A CN 101879380A CN 201010209340 CN201010209340 CN 201010209340 CN 201010209340 A CN201010209340 A CN 201010209340A CN 101879380 A CN101879380 A CN 101879380A
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Abstract
The invention discloses an energy-saving concentration process for extracting active ingredients of plants and a concentration device thereof. The process of the invention comprises the steps of solvent extraction, centrifugal separation, filtration and film concentration. The concentration device comprises an extraction device, a centrifugal separation device, a filtration device and a film concentration device which form a closed circulation system. By using a film centrifugal separation technology for replacing the evaporation method of the prior art for concentrating, the concentration device of the invention has the advantages of simple structure and high working efficiency; the active ingredients of plants are concentrated without being heated; compared with the prior art, the energy is saved by more than 90%; and simultaneously, oxidative degeneration and loss of the active ingredients are reduced, the extraction rate is higher, and the quality is better. In the invention, a closed process system of extraction, separation and concentration is formed, and a heat exchange device is arranged in the closed process system, thereby being favorable for improving the utilization rate of heat energy.
Description
Technical field:
The invention belongs to bio-separation extractive technique field, be specifically related to the active ingredients of plants extractive technique, more specifically relate to a kind of energy-efficient, can effectively prevent effective ingredient oxidative deformation in leaching process loss, based on the energy-saving concentration process and the enrichment facility thereof of the extraction active ingredients of plants of membrane separation technique.
Background technology:
The prior art that active ingredients of plants extracts is earlier plant to be positioned over extractor to heat extraction, is generally water extraction or alcohol extract one to secondary, and extract carries out reduction vaporization and obtains medicinal extract after centrifugal clarification or filtration.The water extraction and alcohol precipitation method of available technology adopting also needs ethanol evaporation to obtain medicinal extract, and this method is promptly adopted in the extraction of Chinese medicine Radix Isatidis effective ingredient.Having is that ethanol evaporation makes the water extract after adopting alcohol extracting again, goes up the resin adsorption column again and is adsorbed with effective constituent, and then with eluent ethanol elution effective ingredient, and evaporation of eluate obtains effective ingredient, and the extraction of notoginseng total saponin is exactly to adopt this method.In general, the plant extract process of prior art must adopt the evaporation and concentration operation, the technology that has even need evaporation and concentration nearly two, three times.The evaporating and concentrating process of prior art even if the reduction vaporization concentration technology still needs a large amount of steam, must consume a large amount of energy, also can discharge a large amount of greenhouse gases simultaneously.In the prior art, the ratio that the steam energy consumption accounts for the plant extract cost is also more and more higher, and many pharmacy and plant enterprise urgently wish to reduce energy consumption in the evaporation and concentration link, save production cost, and increase work efficiency.And prior art needs long-time heating, causes effective ingredient sex change even destroyed, greatly reduces extract quality and effect.For this reason, the inventor is through concentrating on studies, and developed a kind of energy-saving concentration process and enrichment facility thereof of the extraction active ingredients of plants based on membrane separation technique.
Summary of the invention:
First purpose of the present invention is to provide a kind of technology easy, energy-efficient, can effectively prevent effective ingredient oxidative deformation in leaching process loss, based on the energy-saving concentration process of the extraction active ingredients of plants of membrane separation technique.
Another object of the present invention is to provide a kind of enrichment facility of enforcement first purpose.
First purpose of the present invention is achieved in that and comprises solvent extraction, centrifugation, filtration, film enrichment process, specifically comprises following operation:
A, solvent extraction: raw material cooperates solvent to extract by extraction process, obtains extract;
B, centrifugation; Extract imports centrifugation in the centrifugal separation equipment, obtains clarifying extract;
C, filtration: will clarify extract and carry out micro-filtration or ultrafiltration, and remove impurity and insoluble matter and obtain clean extract;
D, film concentrate: clean extract concentrates by film condensing device, reclaims solvent simultaneously;
E, circulation are extracted and concentrated: recovered solvent is back to and replenishes the consumption of extracting solvent in the extraction element; Concentrate passes back into concentrated circulating tank and further concentrates until the concentration that reaches technological requirement.
Another object of the present invention is achieved in that and comprises extraction element, centrifugal separating device, filter and film condensing device that described extraction element is connected with centrifugal separating device technology; Described centrifugal separating device connects concentrated circulating tank, concentrate the liquid feeding side that the circulating tank outlet is provided with choke valve and connects filter by force (forcing) pump, filter see through the liquid feeding side of liquid side by force (forcing) pump connecting film enrichment facility, the concentrate side of film condensing device connects concentrated circulating tank inlet by choke valve, the liquid side that sees through of film condensing device connects the solvent recovery jar, and the solvent recovery jar connects extraction element.
The evaporation that the present invention adopts membrane separation technique to substitute prior art concentrates, and the extraction of finishing under the normal temperature state active ingredients of plants concentrates, and is energy-conservation more than 90%, reduced effective ingredient oxidative deformation and loss simultaneously, and recovery rate is higher, and quality is better.Enrichment facility technological process of the present invention is easy, and filtering-condensing apparatus forms the closed process system that circulation concentrates the loop and extraction, the common formation of separator can be extracted continuously, concentrate.The heat-exchange device of apparatus of the present invention helps making full use of of thermal source.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Fig. 2 is apparatus of the present invention structural relation schematic diagram;
Fig. 3 is that another example structure of apparatus of the present invention concerns schematic diagram.
Among the figure: the 1-extraction element, the 2-centrifugal separating device, 3-transfer jar, the 4-heat-exchange device, 5-concentrates circulating tank, 6-filter, 7-film condensing device, 8-solvent recovery jar, 9-force (forcing) pump, 10-control valve.
Specific embodiments:
The present invention is further illustrated below in conjunction with drawings and Examples, but never in any form the present invention is limited, and any conversion based on training centre of the present invention is done all falls into protection scope of the present invention.
As shown in Figure 1, the present invention extracts the energy-saving concentration process of active ingredients of plants: comprise solvent extraction, centrifugation, filtration, film enrichment process, specifically comprise following operation:
A, solvent extraction: raw material cooperates solvent to extract by extraction process, obtains extract;
B, centrifugation: extract imports centrifugation in the centrifugal separation equipment, obtains clarifying extract;
C, filtration: will clarify extract and carry out micro-filtration or ultrafiltration, and remove impurity and insoluble matter and obtain clean extract;
D, film concentrate: clean extract concentrates by film condensing device, reclaims solvent simultaneously;
E, circulation are extracted and concentrated: recovered solvent is back to and replenishes the consumption of extracting solvent in the extraction element; Concentrate passes back into concentrated circulating tank and further concentrates until the concentration that reaches technological requirement.
Described solvent is any one in water, methyl alcohol, ethanol, benzinum, the acetone, uses the solvent extraction of other types not influence technology purpose realization of the present invention.
Described clarification extract carries out membrane filtration again after the heat exchange operation is reduced to normal temperature.
Described recovery solvent heats up through the heat exchange operation and is back in the extraction element after extracting temperature.
Fig. 2 shows the structural relation of enrichment facility of the present invention, comprises extraction element 1, centrifugal separating device 2, filter 6 and film condensing device 7, and described extraction element 1 is connected with centrifugal separating device 2 technologies; Described centrifugal separating device 2 connects concentrated circulating tank 5, concentrate the liquid feeding side that circulating tank 5 outlets are provided with choke valve 10 and connect filter 6 by force (forcing) pump 9, filter 6 see through the liquid feeding side of liquid side by force (forcing) pump 9 connecting film enrichment facilities 7, the concentrate side of film condensing device 7 connects concentrated circulating tank 5 inlets by choke valve 10, the liquid side that sees through of film condensing device 7 connects solvent recovery jar 8, and solvent recovery jar 8 connects extraction element 1.
Fig. 3 shows the another kind of embodiment of enrichment facility of the present invention, and setting gradually also between described centrifugal separating device 2 and the concentrated circulating tank 5, technology connects transfer jar 3 and heat-exchange device 4.
Described solvent recovery jar 8 connects extraction element 1 by pipeline through heat-exchange device 4.
Described filter 6 is micro-filtration or milipore filter device.
Described centrifugal separating device 2 is a kind of in perforated wall centrifuge, sedimentation-type centrifuge, the tube centrifuge.
Described film condensing device 7 is anti-seepage membrane and/or NF membrane device.
Operation principle of the present invention:
The present invention adopts membrane separation technique to substitute the evaporation and concentration of prior art, concentrated circulating tank 5, filter 6 and film condensing device 7 have formed independent concentrated closed circuit, and cooperate common formation to extract, separate, concentrate the closed process system that reaches solvent recovery with solvent recovery jar 8, extraction element 1, centrifugal separating device 2.Increase heat-exchange device 4 simultaneously, realized under heated state not the concentrating of effective ingredient reduced the use of steam, saved the energy in a large number, reduced the discharging of greenhouse gases.
Present embodiment is that Radix Isatidis is extracted the pilot plant test that concentrates, from extraction element 1, get the 200kg crude extract, after sedimentation centrifuge is centrifugal, obtain clarified solution, clarified solution is cooled to 35 ℃ enters concentrated circulating tank 5, from clarified solution being pumped into micro-filtration (aperture is 2 μ m), see through liquid and enter film condensing device, circulation concentrates 20 minutes, obtains concentrate and aqueous solvent (seeing through liquid).Concrete analysis the results are shown in following table.
Concentrated effect is analyzed:
| Project | Material liquid | Concentrate | See through liquid | Enrichment factor |
| Testing result | ??200kg | ??39kg | ??161 | ??80.5％ |
See through the liquid analysis result:
| Analysis project | Colourity | Turbidity | The existing thing of naked eyes | ??TDS | Electrical conductivity | Hardness | ??COD |
| Testing result | ?＜1 | ?＜0.1 | Do not have | ?36mg/L | ??47μs.cm -1 | ??＜10mg/L | ??8mg/L |
After the concentrate drying in the dried cream indigo red content be 8.20 μ g/g, and be 5.8 μ g/g with conventional method of evaporating content.Result of the test explanation: adopt the separation of membrane separation technique to concentrate, can one the step with the crude extract dehydration by evaporation more than 80%, recycle-water does not contain effective ingredient, can directly be back to extraction element 1 and make the extraction solvent, concentrate after drying, effective component content is significantly improved.
Present embodiment is that the extract to notoginseng total saponin ethanol chromatographic column wash-out carries out the test that the film centrifugation concentrates, get notoginseng total saponin ethanol extract 20L, sending into apparatus of the present invention carries out the film centrifugation by technology of the present invention and concentrates, circulate after 25 minutes, obtain concentrate and alcohol solvent (seeing through liquid), concrete analysis result such as following table.
Characteristics of the present invention:
1, simple in structure, technological process is easy, and the working time is short, and efficient is high;
2, do not concentrate under the heated condition, energy-conserving and environment-protective, energy-conservation more than 90% than prior art;
3, do not heat concentratedly, reduced the effective ingredient oxidative deformation and the loss that cause because of evaporation and concentration, the effective ingredient recovery rate is high, quality better.
Claims (9)
1. energy-saving concentration process that extracts active ingredients of plants is characterized in that: comprise solvent extraction, centrifugation, filtration, film enrichment process, specifically comprise following operation:
A, solvent extraction: raw material cooperates solvent to extract by extraction process, obtains extract;
B, centrifugation; Extract imports centrifugation in the centrifugal separation equipment, obtains clarifying extract;
C, filtration: will clarify extract and carry out micro-filtration or ultrafiltration, and remove impurity and insoluble matter and obtain clean extract;
D, film concentrate: clean extract concentrates by film condensing device, reclaims solvent simultaneously;
E, circulation are extracted and concentrated: recovered solvent is back to and replenishes the consumption of extracting solvent in the extraction element; Concentrate passes back into concentrated circulating tank and further concentrates until the concentration that reaches technological requirement.
2. the energy-saving concentration process of extraction active ingredients of plants as claimed in claim 1 is characterized in that: described clarification extract carries out membrane filtration again after the heat exchange operation is reduced to normal temperature.
3. the energy-saving concentration process of extraction active ingredients of plants as claimed in claim 1 is characterized in that: described recovery solvent heats up through the heat exchange operation and is back in the extraction element after extracting temperature.
4. enrichment facility of realizing the described technology of claim 1, comprise extraction element (1), centrifugal separating device (2), filter (6) and film condensing device (7), described extraction element (1) is connected with centrifugal separating device (2) technology, it is characterized in that: described centrifugal separating device (2) connects concentrated circulating tank (5), concentrate the liquid feeding side that circulating tank (5) outlet is provided with choke valve (10) and connects filter (6) by force (forcing) pump (9), filter (6) see through the liquid feeding side of liquid side by force (forcing) pump (9) connecting film enrichment facility (7), the concentrate side of film condensing device (7) connects concentrated circulating tank (5) inlet by choke valve (10), the liquid side that sees through of film condensing device (7) connects solvent recovery jar (8), and solvent recovery jar (8) connects extraction element (1).
5. enrichment facility as claimed in claim 4 is characterized in that: set gradually between described centrifugal separating device (2) and the concentrated circulating tank (5) and technology connects transfer jar (3) and heat-exchange device (4).
6. enrichment facility as claimed in claim 4 is characterized in that: described solvent recovery jar (8) connects extraction element (1) by pipeline through heat-exchange device (4).
7. enrichment facility as claimed in claim 4 is characterized in that: described filter (6) is micro-filtration or milipore filter device.
8. enrichment facility as claimed in claim 4 is characterized in that: described centrifugal separating device (2) is any one in perforated wall centrifuge, sedimentation-type centrifuge, the tube centrifuge.
9. enrichment facility as claimed in claim 4 is characterized in that: described film condensing device (7) is anti-seepage membrane and/or NF membrane device.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102198049A (en) * | 2011-05-10 | 2011-09-28 | 浙江中医药大学 | Traditional Chinese medicine preparation method and device |
| CN102600634A (en) * | 2011-01-25 | 2012-07-25 | 福建中烟工业有限责任公司 | Improved hot-reflux extraction and concentration equipment |
| CN103127741A (en) * | 2013-02-20 | 2013-06-05 | 中国科学院过程工程研究所 | Method for enhancing natural product solvent extraction through membrane separation process |
| CN103585344A (en) * | 2013-11-22 | 2014-02-19 | 无锡合众信息科技有限公司 | Extracting device for total lignans of schisandra chinensis |
| CN104027429A (en) * | 2014-06-03 | 2014-09-10 | 江口县苗药生物科技有限公司 | Integrated rhynchophylla total alkali extraction device |
| CN104162289A (en) * | 2014-08-10 | 2014-11-26 | 胡刘满 | Equipment for rapidly extracting total flavones of rhododendra |
| CN104174183A (en) * | 2014-08-10 | 2014-12-03 | 胡刘满 | System for extracting flavone in stems and leaves of plants |
| CN104971514A (en) * | 2014-08-10 | 2015-10-14 | 胡刘满 | Device for extracting total flavones of rhododendra |
| CN103232553B (en) * | 2013-05-06 | 2015-11-25 | 陕西理工学院 | A kind of semi continuous extracts the apparatus and method of polyporusum bellatus |
| CN105153736A (en) * | 2014-08-10 | 2015-12-16 | 王选明 | Energy-efficient equipment for extracting plant pigments |
| CN105170044A (en) * | 2014-08-10 | 2015-12-23 | 胡刘满 | Energy saving apparatus for extracting plant flavones |
| CN106967032A (en) * | 2014-08-10 | 2017-07-21 | 葛云龙 | To the equipment and its method of work of the rapid extraction of flavones in plant stem-leaf |
| CN110279725A (en) * | 2019-05-24 | 2019-09-27 | 广东青云山药业有限公司 | A kind of Rhizoma Drynariae extract and preparation method thereof |
| CN111495192A (en) * | 2020-06-09 | 2020-08-07 | 云南中烟再造烟叶有限责任公司 | Concentration method for extracting nicotine condensate by steam distillation |
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| US20060263454A1 (en) * | 2005-05-20 | 2006-11-23 | Kao Corporation | Production process of purified green tea extract |
| CN101525326A (en) * | 2008-03-06 | 2009-09-09 | 陕西嘉禾植物化工有限责任公司 | Method for extracting anthocyanin |
| CN101555293A (en) * | 2009-05-05 | 2009-10-14 | 西藏奇正原生态健康品有限公司 | Method for extracting beta- glucosans from bran of corn |
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| CN102600634A (en) * | 2011-01-25 | 2012-07-25 | 福建中烟工业有限责任公司 | Improved hot-reflux extraction and concentration equipment |
| CN102600634B (en) * | 2011-01-25 | 2015-01-21 | 福建中烟工业有限责任公司 | Improved hot-reflux extraction and concentration equipment |
| CN102198049A (en) * | 2011-05-10 | 2011-09-28 | 浙江中医药大学 | Traditional Chinese medicine preparation method and device |
| CN103127741A (en) * | 2013-02-20 | 2013-06-05 | 中国科学院过程工程研究所 | Method for enhancing natural product solvent extraction through membrane separation process |
| CN103232553B (en) * | 2013-05-06 | 2015-11-25 | 陕西理工学院 | A kind of semi continuous extracts the apparatus and method of polyporusum bellatus |
| CN103585344A (en) * | 2013-11-22 | 2014-02-19 | 无锡合众信息科技有限公司 | Extracting device for total lignans of schisandra chinensis |
| CN104027429A (en) * | 2014-06-03 | 2014-09-10 | 江口县苗药生物科技有限公司 | Integrated rhynchophylla total alkali extraction device |
| CN104027429B (en) * | 2014-06-03 | 2016-07-06 | 江口县苗药生物科技有限公司 | A kind of integration Rhomotoxine extraction element |
| CN105153736A (en) * | 2014-08-10 | 2015-12-16 | 王选明 | Energy-efficient equipment for extracting plant pigments |
| CN104971514A (en) * | 2014-08-10 | 2015-10-14 | 胡刘满 | Device for extracting total flavones of rhododendra |
| CN104174183A (en) * | 2014-08-10 | 2014-12-03 | 胡刘满 | System for extracting flavone in stems and leaves of plants |
| CN105170044A (en) * | 2014-08-10 | 2015-12-23 | 胡刘满 | Energy saving apparatus for extracting plant flavones |
| CN104162289A (en) * | 2014-08-10 | 2014-11-26 | 胡刘满 | Equipment for rapidly extracting total flavones of rhododendra |
| CN106243160A (en) * | 2014-08-10 | 2016-12-21 | 胡刘满 | A kind of energy-saving equipment extracted for plant flavone |
| CN106967032A (en) * | 2014-08-10 | 2017-07-21 | 葛云龙 | To the equipment and its method of work of the rapid extraction of flavones in plant stem-leaf |
| CN106243160B (en) * | 2014-08-10 | 2018-10-19 | 山东国和堂制药有限公司 | A kind of energy-saving equipment for plant flavone extraction |
| CN105153736B (en) * | 2014-08-10 | 2019-04-12 | 河北瑞龙生物科技有限公司 | Extract the energy-saving equipment of phytochrome |
| CN106967032B (en) * | 2014-08-10 | 2019-12-20 | 丁雪强 | Equipment for rapidly extracting flavone from plant stems and leaves and working method thereof |
| CN106967032B8 (en) * | 2014-08-10 | 2020-01-14 | 广东香龙香料有限公司 | Equipment for rapidly extracting flavone from plant stems and leaves and working method thereof |
| CN110279725A (en) * | 2019-05-24 | 2019-09-27 | 广东青云山药业有限公司 | A kind of Rhizoma Drynariae extract and preparation method thereof |
| CN111495192A (en) * | 2020-06-09 | 2020-08-07 | 云南中烟再造烟叶有限责任公司 | Concentration method for extracting nicotine condensate by steam distillation |
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