CN103349849B - Multifunctional continuous phase transition extraction device - Google Patents
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Abstract
A multifunctional continuous phase transition extraction device comprises an extraction system, an analysis system and a solvent reclaiming system, wherein the extraction system comprises a first heat exchanger (8I), a extraction tank (1); the analysis system comprises a second heat exchanger (8II) and a first analysis tank (2I), a second analysis tank (2II), a first purifying pillar (3I), and a second purifying pillar (3II); the solvent reclaiming system comprises a first condenser (4I), a second condenser (4II), a first solvent tank (5I), and a second solvent tank (5II). According to the device, two paths of extraction circuits are formed. During the whole extraction process, the phase transition process of an extracting agent is instant and continuous; the extracting agent can be subjected to continuous phase transition and can be recycled, so that target objects can be extracted to the utmost extent, and accordingly, the efficiency is very high and the solvent consumption is small. Moreover, the whole process is performed in a sealed and low-pressure environment, the function is complete, and the purposes of safety and reliability are achieved. Therefore, the device is suitable for extraction of most natural products.
Description
Technical field
The present invention relates to extraction and separation technology field, is the new equipment of a kind of multi-functional continuous phase transistion abstraction technique aspect extract and separate.
Background technology
The general method adopting of natural products extraction at present has solvent extraction method, refluxing extraction, supercritical carbon dioxide extracting, subcritical abstraction etc.The problems such as solvent extraction method, because its cost is simple compared with low, equipment, applied range is widely used, but exists extraction efficiency low, has extracted and has filtered inconvenience, and solvent recovery is not convenient.Refluxing extraction, the Chinese patent that is CN1454694A as publication number discloses a kind of hot reflux high pressure extraction-vacuum concentration process, this technology can extract, filters, concentratedly complete simultaneously, but what this extraction element adopted is spray design, pressure is the highest also can only reach 0.1MPa, the solvent using limits to some extent, and efficiency does not obtain great raising.Supercritical extraction technique, the Chinese patent that is CN201799133U as publication number discloses a kind of supercritical CO
2fluid extraction device, this technology environmental protection, solvent is cheaply easy to get, and substance is better separated, but it also has very large shortcoming: one, only nonpolar material is had to good effect of extracting, but poor to the extraction effect of polar substances; Two, must under the super-pressure state more than 20MPa, just can extract, high pressure limit the amplification of volume of equipment; Three, its device fabrication cost and maintenance cost are too high, and these factors have all limited the development of this technology, thereby can not get extensive use.Subcritical abstraction technology, the Chinese patent that is CN101642632A as publication number discloses a kind of subcritical fluid extraction device and method of active ingredient of natural product, this technical equipment device extraction temperature and pressure are lower, can be different according to extracted object, select flexibly different subcritical abstraction media, but exist extraction time long, extractant demand is large, can not break away from the problem of conventional solvent extraction batch (-type) operation.Publication number is that the Chinese patent of CN102258882A discloses on the original base of the Chinese patent " a kind of subcritical fluid extraction device of active ingredient of natural product and method " that " a kind of device that utilizes subcritical fluids dynamic extraction " is CN101642632A at publication number and improves, changed the problem of conventional solvent extraction batch (-type) operation, but only have equally nonpolar material is had to good effect of extracting, and poor to the extraction effect of polar substances.Present stage is badly in need of a kind of polarity and apolar substance being had to fine extraction effect, and extraction efficiency is high, that cost is low, the extraction equipment of energy industrialization.
Summary of the invention
The object of the present invention is to provide a kind of device of multi-functional continuous phase transistion extraction, its solvent extraction applied range, overcritical dynamic extraction safe, continuous, equipment cost and operating cost are all low than supercritical extraction unit, and can realize industrialization, can realize the comprehensive efficient extraction of natural products.
For achieving the above object, technical scheme of the present invention is: a kind of multi-functional continuous phase transistion extraction equipment, comprise extracting system, resolution system, solvent recovering system, described extracting system comprises First Heat Exchanger and extractor, First Heat Exchanger and extractor are connected in series by connecting pipe, connecting pipe is provided with valve, described resolution system comprises the second heat exchanger, first resolves tank, second resolves tank, the first decontaminating column and the second decontaminating column, the second heat exchanger and first resolves that tank is parallel with one another to be connected with extractor, second resolves tank is connected with the second heat exchanger, the first decontaminating column and first is resolved tank and is connected, the second decontaminating column and second is resolved tank and is connected, on the second heat exchanger and the tank connected pipeline of extraction, be provided with the first pressure control valve, at the first parsing tank and second, resolve pot bottom and be provided with the first bottom valve and the second bottom valve, on the first parsing tank and the tank connected pipeline of extraction, be provided with the second pressure control valve, described solution recovery system comprises the first condenser, the second condenser, the first solvent tank, the second solvent tank, the first solvent tank and the second solvent tank are parallel with one another to be communicated with First Heat Exchanger, on the pipeline being connected with First Heat Exchanger with the second solvent tank at the first solvent tank, be provided with high-pressure pump, the first condenser is communicated with the first solvent tank, the second condenser is communicated with the second solvent tank, is respectively equipped with the first valve and the second valve at the first solvent tank with the second solvent tank with high-pressure pump on the pipeline being connected.
On described the second solvent tank, liquid-ring vacuum pump is installed, so that use the higher solvent extraction of boiling point.
Described extractor can serial or parallel connection arranges a plurality ofly, and extractor is provided with chuck heating.
Described first resolves tank and second resolves tank and can be arranged in parallel a plurality ofly, and first resolves tank and second resolves tank and be provided with and in chuck heating arrangement or chamber, be provided with heating tube or heat for outer circulation type.
Described the first decontaminating column and the second decontaminating column can be in parallel or series connection arrange a plurality ofly, the first decontaminating column and the second decontaminating column top are respectively equipped with first emptying valve and second emptying valve.
Described the first condenser, the second condenser can in series or in parallel with each otherly arrange a plurality of, and the first solvent tank, the second solvent tank can in series or in parallel with each otherly arrange a plurality of.
Described the first decontaminating column and the second decontaminating column top are provided with packing layer, and packing layer is stainless steel cloth, and bottom is that cavity is established sight glass.
Described extractor, first is resolved on tank, the second parsing tank, the first solvent tank and the second solvent tank and is respectively arranged with pressure vacuum meter.
The present invention is the novel dynamic extraction equipment that a kind of function is complete, efficiency is high, can form two extraction loops: the one, for solvent under normal temperature and pressure, be liquid loop, the 2nd, the loop that is gaseous state for solvent under normal temperature and pressure, in extraction process, solvent constantly circulates in loop.Material is packed into after the extractor of continuous phase transistion extraction equipment, under all the time lower than the critical pressure of extractant and the condition of critical-temperature, to extractant, pressurize, with the certain flow rate extractor of flowing through from the bottom up, after extraction, enter and resolve in tank, by heating, decompression makes extractant become mutually gas, again by immediately cooling, pressurization becomes the liquid extractor of flowing through, material is extracted again, in whole extraction process, extractant by liquid state, to gaseous state, to liquid phase transition process, be instant again, continuous, extractant is to carry out continuous phase transistion, recycle, the material of extraction is kept at resolves in tank, after having extracted, emit collection.Solvent can be the low polar solvents such as propane, normal butane, liquefied petroleum gas, can be also Semi-polarity, the high polar solvents such as acetone, ethyl acetate, ethanol, methyl alcohol, water; The solvent that enters extractor due to any moment is all pure, therefore can extract to greatest extent object, very efficient.
The present invention has following technique effect:
1, in whole extraction process, extractant by liquid state, to gaseous state, to liquid phase transition process, be instant, continuous again, extractant carries out continuous phase transistion, recycles, but is pure, the material of extraction is kept at resolves in tank, after having extracted, emits collection.
2, in the process of extraction, can realize fast solvent recovery, so it is few to process the solvent use amount that extracts mode than other in equal material situation, under equal extractor volume, material treating capacity is large compared with other extraction mode.
3, can use the solvent of the various polarity such as propane, normal butane, liquefied petroleum gas, acetone, ethyl acetate, ethanol, methyl alcohol, water.
4, whole service process is all carried out under the environment of, low pressure airtight at one, safe and reliable.
5, be applicable to the extraction of most of natural products, function is complete, and efficiency is high, breaks away from traditional batch (-type) operation.
Accompanying drawing explanation
Fig. 1 is system structure of device schematic diagram of the present invention.
The specific embodiment
As shown in Figure 1, multi-functional continuous phase transistion extracting system device, comprises extracting system, resolution system, solvent recovering system.
Extracting system is comprised of First Heat Exchanger 8 I and extractor 1, and First Heat Exchanger 8 I and extractor 1 are connected in series by connecting pipe, and connecting pipe is provided with valve V1.
Resolution system is by the second heat exchanger 8 II, first resolves tank 2 I, second resolves tank 2 II, the first decontaminating column 3 I and the second decontaminating column 3 II form, the second heat exchanger 8 II and first resolve that tank 2 I are parallel with one another to be connected with extractor 1, second resolves tank 2 II is connected with the second heat exchanger 8 II, the first decontaminating column 3 I and first are resolved tank 2 I and are connected, the second decontaminating column 3 II and second are resolved tank 2 II and are connected, the first decontaminating column 3 I and the second decontaminating column 3 II tops are respectively equipped with first emptying valve V01 and second emptying valve V02, on the pipeline being connected with extractor 1 in the second heat exchanger 8 II, be provided with the second pressure control valve V22, on the pipeline being connected with extractor 1 in the first parsing tank 2 I, be provided with the first pressure control valve V21, first resolves tank 2 I and second resolves tank 2 II and is provided with and in chuck heating arrangement or chamber, is provided with heating tube or heats for outer circulation type.In the first parsing tank 2 I and second, resolve tank 2 II bottoms and be provided with the first bottom valve V31 and the second low V32.
Solution recovery system is by the first condenser 4 I, the second condenser 4 II, the first solvent tank 5 I, the second solvent tank 5 II form, the first solvent tank 5 I and the second solvent tank 5 II are parallel with one another to be communicated with First Heat Exchanger 8 I, on the pipeline being connected with First Heat Exchanger 8 I with the second solvent tank 5 II in the first solvent tank 5 I, be provided with high-pressure pump 7, the first condenser 4 I are communicated with the first solvent tank 5 I, the second cool condenser 4 II are communicated with the second solvent tank 5 II, in the second solvent tank 5 II, be connected with liquid-ring vacuum pump 6, on the pipeline being connected with high-pressure pump 7 with the second solvent tank 5 II in the first solvent tank 5 I, be respectively equipped with the first valve V41 and the second valve V42.At extractor 1, first, resolve in tank 2 I, the second parsing tank 2 II, the first solvent tank 5 I and the second solvent tank 5 II and be respectively arranged with pressure vacuum meter P11, P21, P22, P31, P32.
For raising the efficiency, extractor 1 can arrange more than two by serial or parallel connection, and first resolves tank 2 I and second resolves tank 2 II and can be arranged in parallel more than two, the first decontaminating column 3 I and the second decontaminating column 3 II can be in parallel or series connection arrange more than two.
The first decontaminating column 3 I and the second decontaminating column 3 II tops are provided with packing layer, and filler is stainless steel cloth, and bottom is that cavity is established sight glass.Solvent becomes gaseous state at parsing tank and enters into decontaminating column, and the drop that can congeal into after the part object that solvent may be carried secretly contacts with packing layer flows back to resolves tank 2 I and resolves in tank 2 II.
Said system can form two extraction loops, and the one, for solvent under normal temperature and pressure, be liquid loop, the 2nd, the loop that is gaseous state for solvent under normal temperature and pressure, in extraction process, solvent constantly circulates in loop.As shown in Figure 1, the solvent through high-pressure pump 7, enters heat exchanger 8 I and is heated to certain temperature, then enters 1 pair of material of extractor extract by valve V1.The solvent that enters extractor 1 due to any moment is all pure, therefore the solvability of the penetrating power of material and object is arrived at utmost.Solution process pressure-control valve V21 after extraction or heat exchanger 8 II, pressure-control valve V22 enter and resolve tank 2 I or resolve tank 2 II and resolve.The object parsing is discharged from the first bottom valve V31 or the second low V32; Gaseous solvent after parsing purifies through decontaminating column 3 I or decontaminating column 3 II, then enters condenser 4 I or condenser 4 II condensations.Condensed solvent is got back to after holding vessel 5 I or the of short duration storage of holding vessel 5 II, enters high-pressure pump 7 again go to next circulation through valve V41 or valve V42.
The present invention can first pass through path 1: extractor 1, the first pressure-control valve V21, first are resolved tank 2 I, the first decontaminating column 3 I, the first condenser 4 I, the first solvent tank 5 I, the first valve V41, high-pressure pump 7, First Heat Exchanger 8 I, to material with under normal temperature and pressure for the solvent of gaseous state extracts; After having extracted, can be switched to path 2: extractor 1, First Heat Exchanger 8 II, the second pressure-control valve V22, second are resolved tank 2 II, the second decontaminating column 3 II, the second condenser 4 II, the second solvent tank 5 II, the second valve V42, high-pressure pump 7, heat exchanger 8 I at once, to material with extracting for liquid solvent under normal temperature and pressure.On a covering device, carry out omnibearing extraction, for the extract and separate of natural products is provided convenience.
Below by specific embodiment, the present invention is further elaborated, but be not limited to this specific examples.
Embodiment 1:
(1) camellia oil fruit (through being crushed to 20 orders, dry and make moisture≤5%) takes 7KG, directly puts into extractor 1, by high-pressure pump 7 pressurizations, make normal butane through heat exchanger 8 I, enter into extractor 1 and extract, its extraction temperature is 45 ℃, and extracting pressure is 0.5MPa; Solvent through extractor 1 enters and resolves tank 2 I with oil, is resolving tank 2 I parsings, and resolving tank 2 I temperature is 55 ℃, and pressure is 0.25MPa; Whole extraction time is 50min, at the first bottom valve V31 that resolves tank 2 I, obtains 1.94KG product, and empirical tests recovery rate is 99.3%.
(2) after grease has extracted, be switched to path extractor 1, heat exchanger 8 II, the second pressure-control valve V22, the second parsing tank 2 II, the second decontaminating column 3 II, the second condenser 4 II, the second solvent tank 5 II, the second valve V42, high-pressure pump 7, heat exchanger 8 I, with methyl alcohol, extract, extraction temperature is 55 ℃, and extracting pressure is 0.1MPa, and resolution temperature is 65 ℃, resolving pressure is-0.08MPa, extraction time is 90min, empirical tests, and the Tea Saponin in material is removed substantially.
Embodiment 2:
(1) castor bean takes 10KG, first pass through hydraulic pressure, extrude the oil of 3KG, the dregs of rice, again through being crushed to 20 orders, are dried and are made moisture≤5%, directly put into extractor 1, by high-pressure pump 7 pressurizations, make normal butane through changing First Heat Exchanger 8 I, enter into extractor 1 and extract, its extraction temperature is 80 ℃, and extracting pressure is 1.0MPa; Solvent through extractor 1 enters the first parsing tank 2 I with oil, in the first parsing tank 2 I, resolves, and resolution temperature is 60 ℃, pressure is 0.3MPa, whole extraction time is 150min, at the first bottom valve V31 of the first parsing tank 2 I, obtains 1.97KG product, and empirical tests recovery rate is 98.5%.
(2) after grease has extracted, be switched to path extractor 1, the second heat exchanger 8 II, the second pressure-control valve V22, the second parsing tank 2 II, the second decontaminating column 3 II, the second condenser 4 II, the second solvent tank 5 II, the second valve V42, high-pressure pump 7, heat exchanger 8 I, with methyl alcohol, extract, extraction temperature is 90 ℃, extracting pressure is 0.6MPa, resolution temperature is 65 ℃, resolving pressure is-0.08MPa, extraction time is 120min, empirical tests, the ricin (WA) in material (recinine, ricin, allergen, agglutinin) is removed substantially.
Embodiment 3:
(1) the fermented soya bean (through being crushed to 40 orders, dry make moisture≤10%) of soy sauce takes 7KG, directly puts into extractor 1, by high-pressure pump 7 pressurizations, make propane through heat exchanger 8 I, enter into extractor 1 and extract, its extraction temperature is 45 ℃, and extracting pressure is 1.2MPa; Solvent through extractor 1 enters the first parsing tank 2 I with oil, in the first parsing tank 2 I, resolves, and resolution temperature is 60 ℃, pressure is 0.35MPa, whole extraction time is 65min, at the first bottom valve V31 of the first parsing tank 2 I, obtains 2.02KG product, and empirical tests recovery rate is 99%.
(2) after grease has extracted, be switched to path extractor 1, the second heat exchanger 8 II, the second pressure-control valve V22, the second parsing tank 2 II, the second decontaminating column 3 II, the second condenser 4 II, second day solvent tank 5 II, the second valve V42, high-pressure pump 7, heat exchanger 8 I, with ethanol, extract, extraction temperature is 60 ℃, extracting pressure is 0.1MPa, resolution temperature is 70 ℃, resolving pressure is-0.08MPa, extraction time is 120min, the second bottom valve V32 in the second parsing tank 2 II obtains 9.0g product, and empirical tests recovery rate is 94.7%.
Claims (10)
1. a multi-functional continuous phase transistion extraction equipment, comprise extracting system, resolution system, solvent recovering system, described extracting system comprises First Heat Exchanger (8 I) and extractor (1), First Heat Exchanger (8 I) and extractor (1) are connected in series by connecting pipe, and connecting pipe is provided with valve (V1), described resolution system comprises the second heat exchanger (8 II), first resolves tank (2 I), second resolves tank (2 II), the first decontaminating column (3I) and the second decontaminating column (3 II), the second heat exchanger (8 II) and first resolves that tank (2 I) is parallel with one another to be connected with extractor (1), second resolves tank (2 II) is connected with the second heat exchanger (8 II), the first decontaminating column (3 I) and first is resolved tank (2 I) and is connected, the second decontaminating column (3 II) and second is resolved tank (2 II) and is connected, on the pipeline being connected with extractor (1) at the second heat exchanger (8 II), be provided with the first pressure control valve (V22), at the first parsing tank (2 I) and second, resolve tank (2 II) bottom and be provided with the first bottom valve (V31) and the second bottom valve (V32), on the pipeline being connected with extractor (1) at the first parsing tank (2 I), be provided with the second pressure control valve (V21), described solution recovery system comprises the first condenser (4 I), the second condenser (4 II), the first solvent tank (5 I), the second solvent tank (5 II), the first solvent tank (5 I) and the second solvent tank (5 II) are parallel with one another to be communicated with First Heat Exchanger (8 I), on the pipeline being connected with First Heat Exchanger (8 I) with the second solvent tank (5 II) at the first solvent tank (5 I), be provided with high-pressure pump (7), the first condenser (4 I) is communicated with the first solvent tank (5 I), the second condenser (4 II) is communicated with the second solvent tank (5 II), on the pipeline being connected with high-pressure pump (7) with the second solvent tank (5 II) at the first solvent tank (5 I), be respectively equipped with the first valve (V41) and the second valve (V42).
2. multi-functional continuous phase transistion extraction equipment according to claim 1, is characterized in that, on the second solvent tank (5 II), liquid-ring vacuum pump (6) is installed.
3. multi-functional continuous phase transistion extraction equipment according to claim 1, is characterized in that, described extractor (1) serial or parallel connection arranges a plurality of, and extractor (1) is provided with chuck heating.
4. multi-functional continuous phase transistion extraction equipment according to claim 1, is characterized in that, described the first parsing tank (2 I) and second is resolved tank (2 II) and can be arranged in parallel a plurality of.
5. according to the multi-functional continuous phase transistion extraction equipment described in claim 1 or 4, it is characterized in that, first resolves tank (2 I) and second resolves tank (2 II) and is provided with and in chuck heating arrangement or chamber, is provided with heating tube or is that outer circulation type heats.
6. multi-functional continuous phase transistion extraction equipment according to claim 1, is characterized in that, the first described decontaminating column (3 I) and the second decontaminating column (3 II) can be in parallel or series connection arrange a plurality of.
7. according to the multi-functional continuous phase transistion extraction equipment described in claim 1 or 6, it is characterized in that, the first decontaminating column (3 I) and the second decontaminating column (3 II) top are equipped with exhaust-valve (V01) and (V02).
8. multi-functional continuous phase transistion extraction equipment according to claim 1, it is characterized in that, described the first condenser (4 I), the second condenser (4 II) can in series or in parallel with each otherly arrange a plurality of, and the first solvent tank (5 I), the second solvent tank (5 II) can in series or in parallel with each otherly arrange a plurality of.
9. multi-functional continuous phase transistion extraction equipment according to claim 1, is characterized in that, the first described decontaminating column (3 I) and the second decontaminating column (3 II) top are provided with packing layer, and packing layer is stainless steel cloth, and bottom is that cavity is established sight glass.
10. multi-functional continuous phase transistion extraction equipment according to claim 1, it is characterized in that, described extractor 1, first is resolved on tank (2 I), the second parsing tank (2 II), the first solvent tank (5 I) and the second solvent tank (5 II) and is respectively arranged with pressure vacuum meter (P11), (P21), (P22), (P31), (P32).
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| CN201310306553.5A CN103349849B (en) | 2013-07-22 | 2013-07-22 | Multifunctional continuous phase transition extraction device |
| US14/902,908 US10016700B2 (en) | 2013-07-22 | 2014-07-11 | Multifunctional continuous phase transition extraction apparatus |
| PCT/CN2014/082107 WO2015010551A1 (en) | 2013-07-22 | 2014-07-11 | Multifunctional continuous phase transition extraction apparatus |
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| CN201310306553.5A CN103349849B (en) | 2013-07-22 | 2013-07-22 | Multifunctional continuous phase transition extraction device |
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| CN103349849B true CN103349849B (en) | 2014-09-03 |
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| WO2015010551A1 (en) * | 2013-07-22 | 2015-01-29 | Cao Yong | Multifunctional continuous phase transition extraction apparatus |
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| CN103772274A (en) * | 2014-02-24 | 2014-05-07 | 曹庸 | Method for removing ricinine in castor pulp by continuous phase-change extraction |
| CN103766599B (en) * | 2014-02-24 | 2016-04-20 | 曹庸 | The method of agglutinin in Castor seed Meal is removed in a kind of continuous phase transistion extraction |
| CN103766598B (en) * | 2014-02-24 | 2016-04-20 | 曹庸 | The method of ricin in Castor seed Meal is removed in a kind of continuous phase transistion extraction |
| CN104289007A (en) * | 2014-09-24 | 2015-01-21 | 华南农业大学 | Continuous phase change-based method for extracting tea polyphenol |
| CN104560379A (en) * | 2014-11-26 | 2015-04-29 | 浙江康莱特药业有限公司 | Coix seed oil and extraction process thereof |
| CN105477902A (en) * | 2015-12-23 | 2016-04-13 | 江苏七O七天然制药有限公司 | Extracting separating device by utilization of impregnation method |
| CN105950279A (en) * | 2016-06-12 | 2016-09-21 | 中国农业科学院油料作物研究所 | Method and system for extracting grease from oil |
| CN106146681B (en) * | 2016-07-15 | 2018-09-11 | 东莞市民益生物科技有限公司 | A kind of method of low temperature continuous phase transistion extraction sea grass polysaccharide |
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| CN109096353A (en) * | 2018-08-08 | 2018-12-28 | 曹庸 | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit |
| CN110201417B (en) * | 2019-06-26 | 2021-05-07 | 晨光生物科技集团股份有限公司 | Leacher and control method thereof |
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