CN102240464A - Method for dynamic extraction by utilizing subcritical fluid - Google Patents
Method for dynamic extraction by utilizing subcritical fluid Download PDFInfo
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- CN102240464A CN102240464A CN2011100975224A CN201110097522A CN102240464A CN 102240464 A CN102240464 A CN 102240464A CN 2011100975224 A CN2011100975224 A CN 2011100975224A CN 201110097522 A CN201110097522 A CN 201110097522A CN 102240464 A CN102240464 A CN 102240464A
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Abstract
The invention discloses a method for dynamic extraction by utilizing subcritical fluid. In the method, a solvent which is in the gaseous state at normal temperature is subjected to dissolution, separation, condensate storage, recycling and the like continuously in a loop in the subcritical state to be circulated continuously until the extraction is finished. In the novel dynamic extraction, the solvent entering an extraction kettle at each time point is the highest in purity, so the concentration difference of the solvent and an extracted substance is the largest, and the efficiency is the highest. In the method, the treatment quantity of materials under the same volume of the extraction kettle is greater than that of other extraction methods; the solvent is used circularly, the integral process is performed at normal temperature under low pressure and is safe and reliable, the investment of equipment is saved, and the economic benefit is high. The method is particularly suitable for separating, purifying and refining natural plants, and particularly can replace the conventional solvent extraction method in low-additional value products.
Description
Technical field
The present invention relates to chemical separating, mass transfer exchange field, is a kind of new technology of utilizing subcritical fluids dynamic extraction technology to be applied in chemical separating, purification, refining aspect.
Background technology
The separation of present most grease and natural products is purified and is all adopted solvent extraction, the extensive use because his operating cost is low.Also have the expert to propose to extract with subcritical in recent years, this technology also has to a certain extent raising in the quality of product and efficient.Subcritical fluid extraction device and method as patent of invention CN 101642632A active ingredient of natural product: the method for this invention is, device is made of control system part and leaching components of system as directed, wherein leaches components of system as directed by extractor, evaporator, surge tank, condenser, dissolving tank, ultrasonic generating means, vavuum pump, spark arrester, compressor, heat-exchanger pump, boiler constitutes: described control system partly comprises extraction temperature control, extraction time control, the control of leaching number of times, expect molten than control, the control of precipitation adjustment, the control of precipitation pressure feedback, the electrical equipment control of device, and over-temp and over-pressure closes leakage alarm.This patent of invention has been taked subcritical technology to step widely from the quality of product and efficient to go a step further.But this invention is just carried out extract and separate with the subcritical fluids replace solvents on original technology, stirs the immersion way extraction owing to still adopt, and effect of extracting has much room for improvement, and does not change the intermittently operated function of former dissolution extraction, and efficient is lower.
Summary of the invention
Problem at above-mentioned prior art existence, the purpose of this invention is to provide a kind of method of utilizing the subcritical fluids dynamic extraction, it can solve the intermittently operated of solvent extraction and subcritical extraction method, realizes the dynamic subcritical fluids dynamic extraction of circulation continuously.
The object of the present invention is achieved like this: a kind of method of utilizing the subcritical fluids dynamic extraction, it is characterized in that: adopting normal temperature is that the solvent of gas is under subcritical state, constantly circulation in dissolving, separation, condensation storage, solvent recirculation step continuously finishes up to extraction.
In the described dissolving step, subcritical solvent is treated the extraction material and is dissolved, and pressure limit is 0.5-2MPa, and temperature is 10-60 ℃.
In the described separating step, solvent separates with object, and pressure limit is 0.1-1MPa, and temperature is 10-80 ℃.
Described solvent is selected from propane, butane, high-purity iso-butane, 1,1,1, one or more mixing in 2-HFC-134a, dimethyl ether, liquefied petroleum gas or the sulfur hexafluoride.
Described solvent recirculation step is to make solvent become subcritical state once more by the heating of boosting.
The present invention is a kind of effectively novel dynamic extraction, because the solvent that enters on each time point in the extraction kettle all is that purity is the highest, therefore in the solvent and the extract concentration difference maximum of extraction process, the mass transfer exchange coefficient can reach maximum, so efficient is very high.The material treating capacity of the present invention under equal extraction kettle volume is greater than other extracting process, and solvent recycles, and whole process is carried out under normal temperature, low pressure, and is safe and reliable, and under the situation of same treating capacity low equipment investment, the economic benefit height.Particularly suitable of the present invention is purified and refining in the separation of natural plants, because the efficient of this method is very high, can replace traditional solvent-extracted method in low value-added product.
Description of drawings
Fig. 1 is the schematic diagram of apparatus system of the present invention.
The specific embodiment
The present invention is a kind of method of utilizing the subcritical fluids dynamic extraction, adopt normal temperature be the solvent of gas under subcritical state, constantly circulation in dissolving, separation, condensation storage, solvent recirculation step continuously finishes up to extraction.In the described dissolving step, pressure limit is 0.5-2MPa, and temperature is 10-60 ℃, and is preferred, and pressure limit is 0.8-1.5MPa, and temperature is 20-50 ℃, according to the solvent of selecting for use be extracted material adjustment.In the described separating step, pressure limit is 0.1-1MPa, and temperature is 10-80 ℃, and preferred, pressure limit is 0.2-0.8MPa, and temperature is 20-70 ℃, adjusts according to solvent of selecting for use and the solute that is extracted.Described solvent is selected from propane, butane, high-purity iso-butane (R600a), 1,1,1, one or more mixing in 2-HFC-134a (r134a), dimethyl ether (DME), liquefied petroleum gas (LPG) or the sulfur hexafluoride.The present invention can select different solvents according to being extracted the object difference, and most preferred, solvent is selected safety for use, the r134a of nontoxic, environmental protection.Described solvent recirculation step is to make solvent become subcritical state once more by the heating of boosting.
Realize that the above-mentioned apparatus system of subcritical fluids dynamic extraction method that utilizes comprises: extraction kettle 1 is used to be installed in wait to extract material and treat the extraction material by subcritical solvent and dissolves; Separating still 2 is used for object is separated with solvent; The condenser 3 that the solvent condensation that separating still 2 is evaporated is got off; The holding vessel 4 that the solvent that condensation is got off is kept in; Keep the power of whole system dynamic equilibrium and the force (forcing) pump 5 that solvent is pressurizeed; The solvent that condensation is got off heats the heater 6 that makes solvent become subcritical state once more; Above-mentioned extraction kettle, separating still, condenser, holding vessel, force (forcing) pump, heater connect successively and form a loop, and solvent constantly circulates in the loop in extraction process.Extraction kettle 1 can for more than 1 or 2 and or series connection, separating still 2 can be series connection more than 1 or 2, thereby further raises the efficiency.The solvent input port of extraction kettle is positioned at the bottom, and delivery outlet is positioned at top, and the subcritical solvent that purity is the highest enters from extraction kettle 1 bottom, and the material to be extracted of flowing through flows out from the top delivery outlet behind the solubilized target thing.The first half of separating still 2 is provided with packing filter, and Lower Half is a cavity, and the solvent input port is positioned at Lower Half, and delivery outlet is positioned at the first half.Packing filter can be selected stainless steel cloth filler, stainless steel ring, pottery, conjugate ring etc. for use.The solvent that is dissolved with object flows into the Lower Half cavity of separating still 2, under certain temperature and pressure, liquid object is stayed separating still 2 Lower Halves, the gaseous state solvent then flows out from delivery outlet through packing filter, thus the part object that the gaseous state solvent may be carried secretly with cohesion can take place after packing filter contacts drips back again in the separating still 2.Be respectively arranged with Pressure gauge P1, P2, P3 on extraction kettle 1, separating still 2, the holding vessel 4, with the monitor force scope.Extraction kettle is provided with the temperature that the chuck heating arrangement guarantees extraction kettle.
As shown in Figure 1: through the solvent of force (forcing) pump 5 pressurizations, enter heater 6 heating by valve V1, the solvent fluid becomes subcritical fluids, enters 1 pair of material of extraction kettle and dissolves.Owing to enter subcritical fluids in the extraction kettle 1 on each time point all is totally not have extract to pollute, so mass transfer velocity is fast, the permeability and the solvability of low pole in the natural products and apolar substance is significantly improved.The solute of the high concentration after the extraction enters separating still 2 through pressure-reducing valve V2 to be separated.The object of separating is discharged from valve V3, separate after resolving solvent fluid (or gaseous fluid) then through valve V4 enter return holding vessel 4 of short duration storages after condenser 3 condensations after, at once in valve V5 enters next time cycling extraction.Gas cylinder 7 is the solvents that are used for replenishment system, inserts by valve V6 between the condenser 3 and holding vessel 4 in above-mentioned loop.
Method of the present invention is by the continuous cycling extraction of solvent, solvent purity when each time point is seen the subcritical abstraction that enters extraction kettle all is the highest, therefore its efficient than the subcritical extraction method that soaks is much higher, and whole process is that continuous circulation is constantly carried out finishing up to extraction, have suffered in the journey wait of need not solvent soaking, solute shifts, evaporating course separately, therefore need not to control soak time, soaks number of times, the molten technological parameter such as compare of material.The big floor space of the equipment volume of traditional solvent extraction and subcritical abstraction method is big, invests also greatly, and this method obviously is better than traditional solvent extraction, subcritical abstraction method, can also reach energy saving purposes.
Below the present invention is further elaborated by specific embodiment, but the present invention is not limited to this specific examples.The 3X10L subcritical fluids dynamic extraction device that device is provided by the great upright bio tech ltd transformation in Guangzhou, solvent is r134a.
(1) the manioca fruit (about 10 orders after crushed sieve) of Guangxi plantation is weighed 25Kg, directly put in the extraction kettle 1, adding pressure handle solvent fluid by force (forcing) pump 5 makes the solvent fluid become subcritical fluids through heater 6, entering into extraction kettle 1 from extraction kettle 1 bottom extracts, its extracting pressure is 1MPa, 30 ℃ of extraction temperature.
(2) the oil-containing solute fluid that is dissolved out through extraction kettle 1 enters in the separating still 2, separates parsing for 2 li at separating still.Separating still 2 pressure 0.2MPa, 45 ℃ of temperature; In whole subcritical fluid extraction process about 35 minutes, obtain 6Kg target extract at separating still bottom valve V3.The oily recovery rate of manioca fruit is 24%.
(1) the manioca fruit (about 20 orders after crushed sieve) of Guangxi plantation is weighed 25Kg, directly put in the extraction kettle 1, adding pressure handle solvent fluid by force (forcing) pump 5 makes the solvent fluid become subcritical fluids through heater 6 to enter into extraction kettle 1 from extraction kettle 1 bottom and extract, its extracting pressure is 1.5MPa, 30 ℃ of extraction temperature.
(2) the oil-containing solute fluid that is dissolved out through extraction kettle 1 enters in the separating still 2, separates parsing for 2 li at separating still.Separating still 2 pressure 0.2MPa, 45 ℃ of temperature; In whole subcritical fluid extraction process about 45 minutes, V3 obtained the 7.2Kg target product in the separating still bottom valve.The oily recovery rate of manioca fruit is 28.8%.
(1) the manioca fruit (about 20 orders after crushed sieve) of Guangxi plantation is weighed 25Kg, directly put in the extraction kettle 1, adding pressure handle solvent fluid by force (forcing) pump 5 makes the solvent fluid become subcritical fluids through heater 6 to enter into extraction kettle 1 from extraction kettle 1 bottom and extract, its extracting pressure is 1.2MPa, 30 ℃ of extraction temperature.
(2) the oil-containing solute fluid that is dissolved out through extraction kettle 1 enters in the separating still 2, separates parsing for 2 li at separating still.Separating still 2 pressure 0.2MPa, 45 ℃ of temperature; In whole subcritical fluid extraction process about 60 minutes, V3 obtained the 7.8Kg target product in the separating still bottom valve.The oily recovery rate of manioca fruit is 31.2%.
Claims (5)
1. method of utilizing the subcritical fluids dynamic extraction is characterized in that: adopt normal temperature be the solvent of gas under subcritical state, constantly circulation in dissolving, separation, condensation storage, solvent recirculation step continuously finishes up to extraction.
2. the method for utilizing the subcritical fluids dynamic extraction according to claim 1 is characterized in that: in the described dissolving step, subcritical solvent is treated the extraction material and is dissolved, and pressure limit is 0.5-2MPa, and temperature is 10-60 ℃.
3. the method for utilizing the subcritical fluids dynamic extraction according to claim 1 is characterized in that: in the described separating step, solvent separates with object, and pressure limit is 0.1-1MPa, and temperature is 10-80 ℃.
4. the method for utilizing the subcritical fluids dynamic extraction according to claim 1, it is characterized in that: described solvent is selected from propane, butane, high-purity iso-butane, 1,1,1, one or more mixing in 2-HFC-134a, dimethyl ether, liquefied petroleum gas or the sulfur hexafluoride.
5. the method for utilizing the subcritical fluids dynamic extraction according to claim 1 is characterized in that: described solvent recirculation step is to make solvent become subcritical state once more by the heating of boosting.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102258882A (en) * | 2011-06-17 | 2011-11-30 | 广州市浩立生物科技有限公司 | Device for dynamic extraction by utilizing subcritical fluid |
| CN102533436A (en) * | 2012-02-15 | 2012-07-04 | 明强（福建）生物萃取科技有限公司 | Method for processing health-care camellia oil |
| CN103146486A (en) * | 2013-03-25 | 2013-06-12 | 广州绿萃生物科技有限公司 | Continuous phase-changed extraction method for orange peel oil |
| CN103173279A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change tea oil extraction method |
| CN103173280A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103834467A (en) * | 2013-03-25 | 2014-06-04 | 广州绿萃生物科技有限公司 | Method for extracting fructus perillae oil through continuous phase transition |
| CN107267185A (en) * | 2017-06-06 | 2017-10-20 | 南通瑞特科研仪器有限公司 | A kind of device and method of subcritical abstraction oily waste |
| CN107828507A (en) * | 2017-11-01 | 2018-03-23 | 广州市浩立生物科技有限公司 | A kind of camellia seed oil refinement method and equipment |
| TWI650167B (en) * | 2017-11-30 | 2019-02-11 | 財團法人金屬工業研究發展中心 | Extraction method and device |
| CN110022956A (en) * | 2016-11-26 | 2019-07-16 | 乔治·斯特彻夫 | Portable extraction equipment |
| CN110527588A (en) * | 2019-09-27 | 2019-12-03 | 山东兴泉油脂有限公司 | A kind of sub-critical extraction method of corn oil |
| CN111939591A (en) * | 2019-08-02 | 2020-11-17 | 三益创价生物科技(深圳)有限公司 | Method for extracting composition rich in cinnamaldehyde from cinnamon |
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| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102258882A (en) * | 2011-06-17 | 2011-11-30 | 广州市浩立生物科技有限公司 | Device for dynamic extraction by utilizing subcritical fluid |
| CN102533436A (en) * | 2012-02-15 | 2012-07-04 | 明强（福建）生物萃取科技有限公司 | Method for processing health-care camellia oil |
| CN103173280B (en) * | 2013-03-06 | 2015-03-18 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103173279A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change tea oil extraction method |
| CN103173280A (en) * | 2013-03-06 | 2013-06-26 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103834467B (en) * | 2013-03-25 | 2016-03-09 | 广州绿萃生物科技有限公司 | A kind of method of continuous phase transistion extraction perilla oil |
| CN103834467A (en) * | 2013-03-25 | 2014-06-04 | 广州绿萃生物科技有限公司 | Method for extracting fructus perillae oil through continuous phase transition |
| CN103146486B (en) * | 2013-03-25 | 2014-04-16 | 广州绿萃生物科技有限公司 | Continuous phase-changed extraction method for orange peel oil |
| CN103146486A (en) * | 2013-03-25 | 2013-06-12 | 广州绿萃生物科技有限公司 | Continuous phase-changed extraction method for orange peel oil |
| CN110022956A (en) * | 2016-11-26 | 2019-07-16 | 乔治·斯特彻夫 | Portable extraction equipment |
| CN107267185A (en) * | 2017-06-06 | 2017-10-20 | 南通瑞特科研仪器有限公司 | A kind of device and method of subcritical abstraction oily waste |
| CN107828507A (en) * | 2017-11-01 | 2018-03-23 | 广州市浩立生物科技有限公司 | A kind of camellia seed oil refinement method and equipment |
| TWI650167B (en) * | 2017-11-30 | 2019-02-11 | 財團法人金屬工業研究發展中心 | Extraction method and device |
| CN111939591A (en) * | 2019-08-02 | 2020-11-17 | 三益创价生物科技(深圳)有限公司 | Method for extracting composition rich in cinnamaldehyde from cinnamon |
| CN110527588A (en) * | 2019-09-27 | 2019-12-03 | 山东兴泉油脂有限公司 | A kind of sub-critical extraction method of corn oil |
| CN110527588B (en) * | 2019-09-27 | 2022-04-15 | 山东兴泉油脂有限公司 | Subcritical extraction method of corn oil |
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