CN101239251A - Liquid-liquid extractor, split-phase adapter and liquid-liquid extracting method - Google Patents
Liquid-liquid extractor, split-phase adapter and liquid-liquid extracting method Download PDFInfo
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- CN101239251A CN101239251A CNA2008101021832A CN200810102183A CN101239251A CN 101239251 A CN101239251 A CN 101239251A CN A2008101021832 A CNA2008101021832 A CN A2008101021832A CN 200810102183 A CN200810102183 A CN 200810102183A CN 101239251 A CN101239251 A CN 101239251A
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Abstract
The present invention provides a liquid-liquid extraction device, and a phase splitting commutator and a liquid-liquid extraction method. The device is composed of an extraction container, a phase splitting commutator and a separating container, combined a seal structure. Wherein, the phase splitting commutator only allows liquid flow to separating container in single direction from the extraction container. Using the device for liquid-liquid extraction does not need liquid transfer tool, the operating step is simple, the extraction yield and the precision of the extracted object are higher.
Description
Technical field
The present invention relates to a kind of liquid-liquid extractor, used split-phase adapter and liquid-liquid extraction method.
Background technology
Liquid-liquid extraction method, be solvent extraction again, be the difference of utilizing different component in the sample to be distributed in solubility in two kinds of immiscible solvents or the distribution ratio purpose that reaches separation, extraction or purifying, be widely used in many fields such as environment, food, chemical, medicine, agricultural, technological process.At present, aspect separating and concentrating trace half volatile and some fixedness organic matter in various fluid samples or the suspension sample, liquid-liquid extraction method remains a kind of strong, sample treatment technology that other solvent-free abstraction techniques can not substitute fully.
The liquid-liquid extraction of conventional method needs multiple utensils such as separatory funnel, pipette, liquid-transfering gun, beaker, centrifuge tube.When the extractant consumption more for a long time, usually adopt separatory funnel to extract, fluid sample and extractant are added separatory funnel, through jolting or repeatedly the reversing sample and extractant are fully mixed, behind the standing demix, the valve of manual adjustments separatory funnel separates heavy phase solution to another container, and whether this heavy phase solution separation process is separated fully by people's visual determination fully; When extractant and sample size after a little while, small volume containers such as normal use centrifuge tube extract, sample and extractant are added wherein, make sample and extractant fully mix, leave standstill or centrifugal through vibration or jolting, after treating the two phase liquid layering, use instruments such as pipette or liquid-transfering gun to shift extraction solution and to another container, do further processing, the process need manual operation of shifting, whether fully often relevantly shift with operator's qualification, when shifting volatile, low viscous solution, the situation that liquid drips from transfer tool also often takes place.
When big or sample contained surfactant or fat when fluid sample viscosity, emulsion easily took place in liquid-liquid extraction.The appearance of emulsion can reduce the recovery rate of solute.Yet the breaking method that changes ionic strength or pH value can increase extra operating procedure, also can bring extra impurity into; Adopt centrifugal breaking method to be easy to generate the emulsion phenomenon again.
Use in the process of separatory funnel extraction, also otherwise the time piston " venting " of outwarding winding, in order to avoid the increase of funnel internal pressure is gone out liquid; Centrifuge tube also needs to unclamp stopper " venting " when vibration or jolting.Error in the operating process can cause solution loss, makes the inaccurate even the failure of an experiment of experimental data.
Summary of the invention
The technical problem to be solved in the present invention can be finished the operation that needs some containers and move the liquid instrument originally for a kind of liquid-liquid extractor and used split-phase adapter that need not transfer tool is provided in this device.The present invention also provides a kind of liquid-liquid extraction method of using said apparatus, and operating procedure is simple, and the recovery rate and the precision of extract are higher.
For this reason, the invention provides a kind of liquid-liquid extractor, used split-phase adapter and liquid-liquid extraction method.This device is made up of three parts, comprises extraction container, split-phase adapter and liquid separatnig container.This three part can be formed a closed structure.Wherein, the amount of capacity of extraction container is by the cumulative volume decision of sample solution and extractant, the amount of capacity of liquid separatnig container is determined by the adding volume than the heavy-fluid body in sample solution, the extractant, can be equipped with the extraction container and the liquid separatnig container of suitable capacity as required, this two vessel surface also can mark scale as required.Adopt one-way valve structures or valve road, small-bore structure in the split-phase adapter, the liquid way flow that only allows extraction container is to liquid separatnig container, and do not allow adverse current.When separating two phase liquid, inverted device, make extraction container last, liquid separatnig container is following, heavy phase solution can enter liquid separatnig container by one-way valve structures or valve road, small-bore structure, after whole device transfers upright state to, the solution that enters liquid separatnig container can adverse current to extraction container, thereby separate two phase liquid.The liquid-liquid extraction method of this device is: add sample and extractant in extraction container, behind the tight connection split-phase adapter, through vibration, after jolting or stirring make sample and extractant fully mix, tightly connect liquid separatnig container again, device is air-tight state, inverted device, through leaving standstill or centrifugal, under gravity or action of centrifugal force in the liquid layering heavy phase solution by separatory to liquid separatnig container, after heavy phase solution is full of liquid separatnig container, the device of becoming a full member, irreversible the flowing to of heavy phase solution in the liquid separatnig container into extraction container, thereby the light phase solution of heavy phase locate respectively with two containers in, realize that two phase liquid separates, required extraction solution.
When using this device to extract, two phase liquid layering and separation process are finished in obturator, do not have solution loss, so can improve recovery of extraction; Do not use the solution transfer tool, reduced operating procedure, saved the operating time, good reproducibility.The one-way valve structures of split-phase adapter or valve road, small-bore structure make that the two phase liquid contact-making surface after separating is little, and extraction solution separates fully.If emulsion has taken place two phase liquid, owing to the existence of one-way valve structures or valve road, small-bore structure, the two phase liquid contact-making surface is little behind centrifugal breakdown of emulsion, after whole device transfers upright state to, two phase liquid separates fully, thereby has prevented the generation of emulsion, has improved the recovery of extraction of solute.In addition, the gas that volatilizees when one-way valve structures or valve road, small-bore structure also can allow the two phase liquid mixing overflows, and needs the problem of " venting " when therefore having solved extraction.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is the decomposing schematic representation of this device.
Fig. 2 is the combination schematic diagram of this device.
Fig. 3 is the generalized section of split-phase adapter in this device.
Fig. 4 A and Fig. 4 B are split-phase adapter vertical view in this device.
The specific embodiment
Fig. 1 is the decomposing schematic representation of this device, and this liquid-liquid extractor comprises extraction container 3, split- phase adapter 2 and 1 three parts of liquid separatnig container.3 is extraction container, and sample and extractant are finished extraction process therein; 2 is split-phase adapter, and this split-phase adapter 2 can tightly be connected with 3 liang of containers of liquid separatnig container 1 and extraction container, as shown in Figure 2, when the three makes up, can make whole container airtight, no liquid spills, and two phase liquid is finished the separatory process by the check valve spline structure in the split-phase adapter 2; 1 is liquid separatnig container, and the heavy phase solution of separation is stored in this.This schematic diagram only is a kind of in the embodiment of the present invention, be not limited thereto, the amount of capacity of its liquid separatnig container 1 and extraction container 3 is by the consumption decision of required sample and extractant, and liquid separatnig container 1 and extraction container 3 can be test tube, centrifuge tube, flask or conical flask etc.Split-phase adapter 2 connects up and down, and the joint geometry of two containers can be cylindrical shape or conoid shape, the connected mode that adopts among the figure is that split-phase adapter 2 two ends are inserted liquid separatnig container 1 and extraction container 3 inside respectively, this only is a kind of in the connected mode, in addition, also can select for use screw socket, bayonet socket, ground, sealing ring and liquid separatnig container 1 and extraction container 3 insert split-phase adapters 2 inside etc. other can be airtight connected mode.
The present invention is in order to realize that solution is from the one-way flow of extraction container 3 to liquid separatnig container 1, in split-phase adapter 2, designed the check valve spline structure, Fig. 3 is the generalized section of split-phase adapter 2, can tightly connect extraction container 3 below the split-phase adapter 2, can tightly connect liquid separatnig container 1 above.Showed a kind of in the split-phase adapter 2 inner check valve spline structure embodiments among Fig. 3: valve road 5 end openings big conoid shape for little down, spool 6 is a spherical body, the slightly larger in diameter of spool 6 is in valve road end opening, liquid above spool 6 can stop during at valve road 5 end openings flows down position promptly shown in Figure 3.Fig. 4 A and Fig. 4 B are the vertical view of split-phase adapter 2, so that two kinds of embodiments of retaining 4 to be shown in the check valve spline structure, promptly have duct or vertical slots in the middle of valve road 5 shelves suitable for reading 4.When device was inverted, spool 6 slided into retaining 4 one side in the practical application, and liquid can flow in the liquid separatnig container 1 through duct or the vertical slot in the retaining 4, become a full member behind the device, spool 6 is fallen position shown in Fig. 3, top solution is enclosed within the liquid separatnig container 1, thereby has realized the one-way flow of solution.In addition, when the 5 end opening apertures, valve road of used one-way valve structures enough hour, can there be spool 6 and retaining 4 yet, be valve road, small-bore structure, because of when device is inverted, heavy phase solution can be pressed in the liquid separatnig container 1 by self and light phase solution gravity sum, after becoming a full member, because the aperture of valve road end opening is enough little,, thereby can reach the effect that the device of becoming a full member equally can adverse current to such an extent as to the surface tension of this place's liquid can overcome the gravity of himself.The pore size in this valve road, small-bore is relevant with the amount and the class of liquids of heavy phase solution.But the embodiment of this check valve spline structure is not limited thereto, and other structures that can realize the solution one-way flow also can be applicable to this.
When using this device extraction solution, fluid sample and extractant are added in the extraction container 3, the tight split-phase adapter 2 that connects, vibration or jolting or stir with magnetic stick, make the solute in the sample finish phase transfer, but evaporate this moment the gas jack-up spool 6 that produces or the aperture by valve road, small-bore enter surrounding air, have removed the step of " venting " from.After extraction is finished, tightly connect liquid separatnig container 1 again, single unit system is airtight, inverted device, be that liquid separatnig container 1 is following, extraction container 3 is last, leave standstill then or centrifugal, two phase liquid is finished layering under gravity or centrifugal action, and promptly heavy phase solution flows in the liquid separatnig container 1 by check valve in the split-phase adapter 2 or valve roads, small-bore, after heavy phase solution is full of liquid separatnig container 1, the separatory process is finished, and device is become a full member, and promptly extraction container 3 is following, liquid separatnig container 1 is last, as shown in Figure 2, because the heavy phase solution in the liquid separatnig container 1 can not adverse current, and light phase solution is still in extraction container 3, two phase liquid is among the different vessels respectively, thereby finishes the separation of two phase liquid.The capacity of selected liquid separatnig container 1 should be suitable with the volume of heavy phase solution, all separate for guaranteeing the sample solution after the extraction, do not pollute required extraction solution, when the sample solution phase time of attaching most importance to, the cavity volume that the liquid separatnig container of selecting 1 and spool 6 are formed should be slightly larger than the sample solution volume of adding, makes the two phase liquid layering interfaces be in a side by liquid separatnig container 1; When the extraction solution phase time of attaching most importance to, the liquid separatnig container 1 that should make selection is slightly less than the volume that adds extractant with the cavity volume that spool 6 is formed, and makes the two phase liquid layering interfaces be in a side by extraction container 3.Thereby guaranteed not contain in the extraction solution sample solution.
Claims (10)
1. liquid-liquid extractor, it is characterized by: form by extraction container, split-phase adapter and three parts of liquid separatnig container, wherein, a joint of split-phase adapter can tightly be connected with extraction container, another joint can tightly be connected with liquid separatnig container, three part one-tenth one closed structures capable of being combined.
2. liquid-liquid extractor according to claim 1, it is characterized by: extraction container and liquid separatnig container can be test tube, centrifuge tube, flask or conical flask.
3. liquid-liquid extractor according to claim 1, it is characterized by: extraction container and liquid separatnig container, its surface can mark scale.
4. liquid-liquid extractor according to claim 1, it is characterized by: extraction container and liquid separatnig container, its amount of capacity can be according to using needs to determine.
5. liquid-liquid extractor according to claim 1 is characterized by: described split-phase adapter only allow liquid by the extraction container way flow to liquid separatnig container.
6. liquid-liquid extractor according to claim 1, it is characterized by: described split-phase adapter can adopt one-way valve structures or valve road, small-bore structure to realize the liquid one-way flow.
7. the split-phase adapter of a liquid-liquid extractor is characterized by: can tightly connect liquid separatnig container and extraction container up and down, and only allow liquid by the extraction container way flow to liquid separatnig container.
8. as the split-phase adapter of liquid-liquid extractor as described in the claim 7, it is characterized by: connecting up and down, the joint of container can be cylindrical shape or conoid shape.
9. as the split-phase adapter of liquid-liquid extractor as described in the claim 7, it is characterized by: can adopt one-way valve structures or valve road, small-bore structure to realize the liquid one-way flow.
10. liquid-liquid extraction method, it is characterized by: add sample and extractant in the extraction container, tightly connect split-phase adapter, after treating sample and extractant fully mixing, the tight liquid separatnig container that connects, device is air-tight state, inverted device, under gravity or action of centrifugal force in the liquid layering heavy phase solution by separatory to liquid separatnig container, the device of becoming a full member, liquid in the liquid separatnig container can not adverse current, thereby separates two phase liquid, required extraction solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101021832A CN101239251A (en) | 2008-03-19 | 2008-03-19 | Liquid-liquid extractor, split-phase adapter and liquid-liquid extracting method |
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| CNA2008101021832A CN101239251A (en) | 2008-03-19 | 2008-03-19 | Liquid-liquid extractor, split-phase adapter and liquid-liquid extracting method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI400117B (en) * | 2011-01-26 | 2013-07-01 | Univ Nat Formosa | A liquid phase extraction apparatus, and a sample pretreatment method using the liquid phase extraction apparatus |
| CN105738185A (en) * | 2016-01-28 | 2016-07-06 | 润科生物工程（福建）有限公司 | Extraction device and applications thereof to extraction, oil extraction and measurement for oil content of microbial cell |
| CN112770824A (en) * | 2018-11-29 | 2021-05-07 | 美利凯公司 | Liquid-liquid mass transfer process and apparatus |
| CN112755584A (en) * | 2020-12-15 | 2021-05-07 | 鲁南制药集团股份有限公司 | High-efficient extraction centrifugal device |
| CN113648677A (en) * | 2021-07-08 | 2021-11-16 | 暨南大学 | Extraction device and method and application thereof |
-
2008
- 2008-03-19 CN CNA2008101021832A patent/CN101239251A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI400117B (en) * | 2011-01-26 | 2013-07-01 | Univ Nat Formosa | A liquid phase extraction apparatus, and a sample pretreatment method using the liquid phase extraction apparatus |
| CN105738185A (en) * | 2016-01-28 | 2016-07-06 | 润科生物工程（福建）有限公司 | Extraction device and applications thereof to extraction, oil extraction and measurement for oil content of microbial cell |
| CN112770824A (en) * | 2018-11-29 | 2021-05-07 | 美利凯公司 | Liquid-liquid mass transfer process and apparatus |
| CN112770824B (en) * | 2018-11-29 | 2023-07-11 | 美利凯公司 | Liquid-liquid mass transfer process and apparatus |
| CN112755584A (en) * | 2020-12-15 | 2021-05-07 | 鲁南制药集团股份有限公司 | High-efficient extraction centrifugal device |
| CN113648677A (en) * | 2021-07-08 | 2021-11-16 | 暨南大学 | Extraction device and method and application thereof |
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Open date: 20080813 |