CN103349849A - Multifunctional continuous phase transition extraction device - Google Patents
Multifunctional continuous phase transition extraction device Download PDFInfo
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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 the 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 that adopts of at present natural products extraction has solvent extraction method, refluxing extraction, supercritical carbon dioxide extracting, subcritical abstraction etc.Solvent extraction method,, equipment lower because of its cost is simple, applied range is widely used, but exists extraction efficiency low, has extracted filter inconvenient, the problem such as solvent recovery is not convenient.Refluxing extraction, be that the Chinese patent of CN1454694A discloses a kind of hot reflux high pressure extraction-vacuum concentration process such as publication number, this technology can be extracted, filters, concentrate and finish simultaneously, but what this extraction element adopted is the spray design, pressure is the highest also can only to reach 0.1MPa, the solvent that uses limits to some extent, and efficient does not obtain great raising.Supercritical extraction technique is that the Chinese patent of CN201799133U discloses a kind of supercritical CO such as publication number
2The fluid extraction device, this technology environmental protection, solvent cheaply is easy to get, and substance better separates, but it also has very large shortcoming: one, only nonpolar material there is preferably effect of extracting, but relatively poor to the extraction effect of polar substances; Two, must under the super-pressure state more than the 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, be subcritical fluid extraction device and the method that the Chinese patent of CN101642632A discloses a kind of active ingredient of natural product such as publication number, this technical equipment device extraction temperature and pressure are lower, can be different according to extracted object, the subcritical abstraction medium that flexible choice is different, but exist extraction time long, the extractant demand is large, can not break away from the problem of conventional solvent extraction batch (-type) operation.Publication number is that to disclose " a kind of device that utilizes the subcritical fluids dynamic extraction " be that the original base of the Chinese patent " a kind of subcritical fluid extraction device of active ingredient of natural product and method " of CN101642632A is improved at publication number to the Chinese patent of CN102258882A, changed the problem of conventional solvent extraction batch (-type) operation, but only have equally nonpolar material is had preferably effect of extracting, and relatively poor to the extraction effect of polar substances.Present stage is badly in need of a kind of polarity and apolar substance being had 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 resolves with being connected 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, be provided with the first pressure control valve at the second heat exchanger and the tank connected pipeline of extraction, resolve pot bottom at the first parsing tank and second and be provided with the first bottom valve and the second bottom valve, resolve tank first and be provided with the second pressure control valve with the tank connected pipeline of extraction; 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, the first solvent tank be connected the pipeline that solvent tank is connected with First Heat Exchanger and 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, the first solvent tank be connected the pipeline that solvent tank is connected with high-pressure pump and be respectively equipped with the first valve and the second valve.
On described the second solvent tank liquid-ring vacuum pump is installed, so that use the higher solvent extraction of boiling point.
It is a plurality of that but described extractor serial or parallel connection arranges, and extractor is provided with the 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 be provided with heating tube in chuck heating arrangement or the chamber 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 the 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, efficient is high, can form two extraction loops: the one, be liquid loop for solvent under the normal temperature and pressure, the 2nd, be the loop of gaseous state for solvent under the normal temperature and pressure, solvent constantly circulates in the loop in extraction process.Material is packed into behind the extractor of continuous phase transistion extraction equipment, under the condition of the critical pressure that is lower than all the time extractant and critical-temperature, pressurize to extractant, with the certain flow rate extractor of flowing through from the bottom up, after the extraction, enter and resolve in the tank, by heating, decompression makes extractant become mutually gas, again by instant cooling, pressurization becomes the liquid extractor of flowing through, and material is extracted again, in the whole extraction process, extractant be instant to liquid phase transition process again by liquid state to gaseous state, continuous, extractant is to carry out continuous phase transistion, recycle, the material of extraction is kept at resolves in the tank, emits collection after having extracted.Solvent can be the low polar solvents such as propane, normal butane, liquefied petroleum gas, also can be Semi-polarity, the high polar solvents such as acetone, ethyl acetate, ethanol, methyl alcohol, water; Because it all is pure that any moment enters the solvent of extractor, therefore can extract to greatest extent object, very efficient.
The present invention has following technique effect:
1, in the whole extraction process, extractant be instant, continuous to liquid phase transition process again by liquid state to gaseous state, extractant carries out continuous phase transistion, recycles, but is pure, the material of extraction is kept at resolves in the tank, emits collection after having extracted.
2, can realize fast solvent recovery in the process of extraction, lack than the solvent use amount of other extraction mode so process in the equal material situation, under equal extractor volume, the material treating capacity is large than 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, and is safe and reliable.
5, be applicable to the extraction of most of natural products, function is complete, and efficient is high, breaks away from traditional batch (-type) operation.
Description of drawings
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 resolve with being connected 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, the pipeline that is connected with extractor 1 in the second heat exchanger 8 II is provided with the second pressure control valve V22, resolve the pipeline that tank 2 I are connected with extractor 1 first and be provided with the first pressure control valve V21, first resolves tank 2 I and the second parsing tank 2 II is provided with and is provided with heating tube in chuck heating arrangement or the chamber or is that outer circulation type heats.Resolve tank 2 II bottom in the first parsing tank 2 I and second and be provided with the first bottom valve V31 and the second low V32.
The 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, the first solvent tank 5 I be connected solvent tank 5 II and be provided with high-pressure pump 7 with the pipeline that First Heat Exchanger 8 I are connected, 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, be connected with liquid-ring vacuum pump 6 in the second solvent tank 5 II, the first solvent tank 5 I be connected the pipeline that solvent tank 5 II are connected with high-pressure pump 7 and be respectively equipped with the first valve V41 and the second valve V42.Resolve tank 2 I, the second parsing tank 2 II, the first solvent tank 5 I and the second solvent tank 5 II at extractor 1, first 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 the bottom is that cavity is established sight glass.Solvent becomes gaseous state and enters into decontaminating column resolving tank, and the part object that solvent may be carried secretly and the drop that can congeal into after packing layer contact flow back to resolves in tank 2 I and parsing tank 2 II.
Said system can form two extraction loops, and the one, be liquid loop for solvent under the normal temperature and pressure, the 2nd, be the loop of gaseous state for solvent under the normal temperature and pressure, solvent constantly circulates in the loop in extraction process.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 by valve V1 and extracts.Because it all is pure that any moment enters the solvent of extractor 1, therefore the penetrating power of material and the solvability of object are arrived at utmost.Solution process pressure-control valve V21 after the extraction or heat exchanger 8 II, pressure-control valve V22 enter parsing tank 2 I or resolve tank 2 II and resolve.The object that parses is discharged from the first bottom valve V31 or the second low V32; Gaseous solvent after the parsing purifies through decontaminating column 3 I or decontaminating column 3 II, then enters condenser 4 I or condenser 4 II condensations.After condensed solvent is got back to holding vessel 5 I or the of short duration storage of holding vessel 5 II, enter high-pressure pump 7 through valve V41 or valve V42 again and go to next circulation.
The present invention can pass through first 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 extracting for the solvent of gaseous state under the normal temperature and pressure; Can switch to path 2 after having extracted: extractor 1, First Heat Exchanger 8 II, the second pressure-control valve V22, second resolve 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, and material is extracted with the solvent for liquid state under the normal temperature and pressure.Carry out omnibearing extraction at a covering device, for the extract and separate of natural products is provided convenience.
Below the present invention is further elaborated by specific embodiment, but be not limited to this specific examples.
Embodiment 1:
(1) camellia oil fruit (through being crushed to 20 orders, oven dry makes moisture≤5%) takes by weighing 7KG, directly puts into extractor 1, make normal butane through heat exchanger 8 I by high-pressure pump 7 pressurizations, enter into extractor 1 and extract, its extraction temperature is 45 ℃, and extracting pressure is 0.5MPa; Solvent through extractor 1 enters parsing tank 2 I with oil, is resolving the parsing of tank 2 I, and resolving tank 2 I temperature is 55 ℃, and pressure is 0.25MPa; Whole extraction time is 50min, obtains the 1.94KG product at the first bottom valve V31 that resolves tank 2 I, and the empirical tests recovery rate is 99.3%.
(2) after grease has extracted, switch 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, extract with methyl alcohol, 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 the material is removed substantially.
Embodiment 2:
(1) castor bean takes by weighing 10KG, pass through first hydraulic pressure, extrude the oil of 3KG, through being crushed to 20 orders, oven dry makes moisture≤5% to the dregs of rice, directly puts into extractor 1 again, make normal butane through changing First Heat Exchanger 8 I by high-pressure pump 7 pressurizations, 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, resolves in tank 2 I first and resolves, and resolution temperature is 60 ℃, pressure is 0.3MPa, whole extraction time is 150min, obtains the 1.97KG product at the first the first bottom valve V31 that resolves tank 2 I, and the empirical tests recovery rate is 98.5%.
(2) after grease has extracted, switch 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, extract with methyl alcohol, 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 the material (recinine, ricin, allergen, agglutinin) is basic to be removed.
Embodiment 3:
(1) the fermented soya bean (through being crushed to 40 orders, oven dry makes moisture≤10%) of soy sauce takes by weighing 7KG, directly puts into extractor 1, make propane through heat exchanger 8 I by high-pressure pump 7 pressurizations, 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, resolves in tank 2 I first and resolves, and resolution temperature is 60 ℃, pressure is 0.35MPa, whole extraction time is 65min, obtains the 2.02KG product at the first the first bottom valve V31 that resolves tank 2 I, and the empirical tests recovery rate is 99%.
(2) after grease has extracted, switch 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, extract with ethanol, extraction temperature is 60 ℃, extracting pressure is 0.1MPa, resolution temperature is 70 ℃, resolving pressure is-0.08MPa, extraction time is 120min, obtain the 9.0g product at the second the second bottom valve V32 that resolves tank 2 II, the empirical tests recovery rate is 94.7%.
Claims (10)
1. 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) resolves with being connected 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, the pipeline that is connected with extractor (1) at the second heat exchanger (8 II) is provided with the first pressure control valve (V22), resolve tank (2 II) bottom at the first parsing tank (2 I) and second and be provided with the first bottom valve (V31) and the second bottom valve (V32), the pipeline that is connected with extractor (1) at the first parsing tank (2 I) is 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), the first solvent tank (5 I) be connected solvent tank (5 II) and be provided with high-pressure pump (7) with the pipeline that First Heat Exchanger (8 I) is connected, 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), the first solvent tank (5 I) be connected the pipeline that solvent tank (5 II) is connected with high-pressure pump (7) and 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, at 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 the 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 claim 1 or 4 described multi-functional continuous phase transistion extraction equipments, it is characterized in that, first resolves tank (2 I) and second resolves tank (2 II) and is provided with and is provided with heating tube in chuck heating arrangement or the chamber or is that outer circulation type heats.
6. multi-functional continuous phase transistion extraction equipment according to claim 1 is characterized in that, described the first 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 claim 1 or 6 described multi-functional continuous phase transistion extraction equipments, 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, described the first 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 the 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 |
| PCT/CN2014/082107 WO2015010551A1 (en) | 2013-07-22 | 2014-07-11 | Multifunctional continuous phase transition extraction apparatus |
| US14/902,908 US10016700B2 (en) | 2013-07-22 | 2014-07-11 | Multifunctional continuous phase transition extraction apparatus |
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