CN108854153A - Film emulsification and extraction device and film emulsification and extraction method - Google Patents
Film emulsification and extraction device and film emulsification and extraction method Download PDFInfo
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- CN108854153A CN108854153A CN201810862913.2A CN201810862913A CN108854153A CN 108854153 A CN108854153 A CN 108854153A CN 201810862913 A CN201810862913 A CN 201810862913A CN 108854153 A CN108854153 A CN 108854153A
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- extraction
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- clarifying basin
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- film emulsification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0415—Solvent extraction of solutions which are liquid in combination with membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
Abstract
The present invention provides a kind of film emulsification and extraction devices, including：Liquid storage clarifying basin；The lower part of the liquid storage clarifying basin is provided with water phase outlet；The top of the liquid storage clarifying basin is provided with perforated membrane；Circulating pump；One end water phase outlet of the circulating pump is connected；The other end is connected with the perforated membrane；The area of section of liquid storage clarifying basin lower part is greater than the area of section on top.Compared with prior art, the present invention utilizes the peptizaiton of film, is sufficiently mixed continuous phase with dispersed phase, extraction and clarifying process is quickly and efficiently completed, to improve extraction efficiency and extraction rate；And the film emulsification and extraction device have the advantages that easy processing, rapidly and efficiently, low energy consumption, recyclable operation, occupied area is small, mutually separates fast, compact, efficient, safety, economy, laboratory and industrial application suitable for different scales are adaptable.
Description
Technical field
The invention belongs to separator technical field more particularly to a kind of film emulsification and extraction device and film emulsification and extraction sides
Method.
Background technique
Solid Phase Extraction and solvent extraction are most common methods when extracting target component from solution.
Solid Phase Extraction is adsorbent and ion exchange resin etc. to be absorbed method of the solid-filling of target component in column,
Device is simple, the simple operations that aqueous solution is sent into column only can be recycled target component by pump etc., but recycling capacity is small, and
It cannot quickly handle, be unsuitable for largely handling the solution containing high concentration target component.
Solvent extraction is that the target component that will be dissolved in the water extracts organic solvent unmixing with water (oil etc.)
Method, it is extracted using target component with distribution (distribution of the liquid liquid) attribute for having more compatibility one of in two kinds of liquid
It takes.Different from Solid Phase Extraction, it is big that capacity is recycled in solvent extraction, processing quickly, be suitable for a large amount of processing containing high concentration target at
The aqueous solution divided.But in solvent extraction, after water phase and oily phase " mixing ", the opposite behaviour of two-phase " separation " will be carried out at once
Make, it is therefore desirable to which special equipment, the device is complicated for operation, requires to proficiency.And industrialized extraction equipment, often
The extractant for needing higher concentration will lead to the generation of third phase since extractant concentration is higher in some cases.
Mixer-settler is quickly stirred by agitating paddle as the most common industrial equipment in extraction field and realizes water phase and oil
The mixing of phase forms emulsified state, separates water phase and oily phase under gravity, extraction efficiency is high, and treating capacity is big, but phase
Separation process needs special clarifying chamber, and the time is longer and takes up a large area.
Pulse extraction column mixes water phase and oily phase by the vibration of impulse generator, can be realized faster solvent extraction
It takes, but two-phase mixtures are insufficient, need to increase tower height, need bigger space.
Water phase is mutually sufficiently mixed with oil until emulsified state, then passes through centrifugal force by centrifugal extractor by mechanical stirring
It is rapidly separated two-phase.But apparatus structure is complicated, needs stronger centrifugal force and carries out mechanical stirring, energy consumption is higher, operation
Cost is big.And to prevent degradation problem caused by solid component accumulation from occurring, need repairing cost, limits centrifugation
The application of extractor.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing one kind quickly can mutually separate recyclable film emulsification
Extraction equipment and film emulsification and extraction method.
The present invention provides a kind of film emulsification and extraction devices, including：
Liquid storage clarifying basin；The lower part of the liquid storage clarifying basin is provided with water phase outlet；The top of the liquid storage clarifying basin is set
It is equipped with perforated membrane；
Circulating pump；One end water phase outlet of the circulating pump is connected；The other end is connected with the perforated membrane；
The area of section of liquid storage clarifying basin lower part is greater than the area of section on top.
Preferably, the ratio of the maximum cross-section area of the liquid storage clarifying basin and minimum cross-sectional area is more than or equal to 1.1：1.
Preferably, the ratio of the maximum cross-section area of the liquid storage clarifying basin and minimum cross-sectional area is (1.5~10)：1.
Preferably, the perforated membrane is cylindrical film；One end that the perforated membrane is not connected with circulating pump is enclosed construction.
Preferably, the aperture of the perforated membrane is 1~50 μm.
It preferably, further include triple valve；The water phase outlet is connected by triple valve with the circulating pump.
The present invention also provides a kind of film emulsification and extraction methods, including：
Using above-mentioned film emulsification and extraction device,
Water phase to be extracted and organic phase are sequentially added in liquid storage clarifying basin, make perforated membrane infiltration in organic phase；It is described
Organic phase includes diluent and extractant；
Circulating pump is opened, water phase to be extracted enters organic phase through circulating pump, perforated membrane, forms lotion；
After circulation terminates, under the effect of gravity, organic phase is separated from the water, obtains organic phase extracted.
Preferably, the flow velocity of the circulating pump is 40~1000ml/min.
The present invention provides a kind of film emulsification and extraction devices, including：Liquid storage clarifying basin；The lower part of the liquid storage clarifying basin is set
It is equipped with water phase outlet；The top of the liquid storage clarifying basin is provided with perforated membrane；Circulating pump；One end water phase of the circulating pump exports
It is connected；The other end is connected with the perforated membrane；The area of section of liquid storage clarifying basin lower part is greater than the section face on top
Product.Compared with prior art, the present invention passes through circulating pump and perforated membrane for the water phase and organic phase to be extracted in liquid storage clarifying basin
It is connected, forms closed cycle, provides pressure for the flowing of continuous phase, while for film emulsion process, lotion stream is formed, when it
By in place of Transformed area, lotion rapidly disappears, and separates water phase with organic phase by gravity, made using the dispersion of film
With, be sufficiently mixed continuous phase with dispersed phase, quickly and efficiently complete extraction and clarifying process, to improve extraction efficiency and extraction
Take rate；And the film emulsification and extraction device have easy processing, rapidly and efficiently, low energy consumption, recyclable operation, occupied area are small,
Fast advantage is mutually separated, compact, efficient, safety, economy, laboratory and industrial application suitable for different scales are adaptable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of film emulsifier unit provided by the invention；
Fig. 2 is the structural schematic diagram of film emulsifier unit provided by the invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of film emulsification and extraction devices, including：
Liquid storage clarifying basin；The lower part of the liquid storage clarifying basin is provided with water phase outlet；The top of the liquid storage clarifying basin is set
It is equipped with perforated membrane；
Circulating pump；One end water phase outlet of the circulating pump is connected；The other end is connected with the perforated membrane；
The area of section of liquid storage clarifying basin lower part is greater than the area of section on top.
Referring to Fig. 1 and Fig. 2, Fig. 1 is the structural schematic diagram of film emulsification and extraction device provided by the invention, wherein 1 is porous
Film, 2 be liquid storage clarifying basin, and 3 export for water phase, and 4 be triple valve, and 5 be circulating pump, and 6 be connecting pipe.
Film emulsification and extraction device provided by the invention includes liquid storage clarifying basin, and the area of section of its underpart is greater than cutting for top
Face area.Liquid storage clarifying basin is water phase to be extracted and organic phase integral pool, wherein the maximum cross-section area at water phase to be extracted is big
In the maximum cross-section area of organic phase.In the present invention on the one hand liquid storage clarifying basin is used for storage solutions, and as extraction process
The primary structure of progress, on the other hand the variation of its cross section is for the quick separating between different phases.The liquid storage clarifying basin
Preferably cylindrical body；The maximum cross-section area of the liquid storage clarifying basin and the ratio of minimum cross-sectional area are more than or equal to 1.1：1, more
Preferably (1.5~20)：1, it is further preferably (1.5~10)：1, most preferably (2~6)：1.The variation of sectional area is to increase
The interfacial tension of lotion can be clarified at changes of section, and convenient for separating, in industrial application, cross-sectional area reaches 6：1 with
On, the variation of caused interfacial tension can be very big, is able to satisfy the separation requirement of most extraction systems.
The lower part of the liquid storage clarifying basin is provided with water phase outlet, is connected with circulating pump, is used to form mobile phase,
Film emulsifies the channel that continuous phase is used in emulsion process, and extraction process is used for the separation of raffinate after the completion of carrying out.In the present invention
In, the water phase outlet of the liquid storage clarifying basin is preferably connected by triple valve with circulating pump.Triple valve can be used for extraction cycle
Channel switch, be also used for after the completion of extraction, collect the switch of water phase and organic phase.
The top of the liquid storage clarifying basin is provided with perforated membrane；The circulating pump is connected with perforated membrane.The perforated membrane
For perforated membrane well known to those skilled in the art, special limitation is had no, is preferably cylindrical film in the present invention；The cylindricality
Film be preferably it is open at one end closed at one end, i.e., the one end being connected with circulating pump be opening the other end closing；The hole of the perforated membrane
Diameter is preferably 1~50 μm, and it is further preferably 1~20 μm, most preferably 1~10 that more preferably 1~40 μm, which be further preferably 1~30 μm,
μm；The length of the perforated membrane is preferably less than the height for being equal to organic phase.It is extracted using porous membrane emulsification, may make and be dispersed into
The drop size of organic phase is smaller, and drop size is usually tens to one hundred micron；And in traditional stirring and emulsifying extraction side
In formula, drop is usually several hundred microns, and the size of drop is smaller, and specific surface area is bigger, so that mass transfer area is increased, so that
The extraction efficiency of the device is higher if other conditions are the same.In the identical situation of other parameters, porous membrane aperture
Smaller, extraction efficiency is higher, but the efficiency after its balance is that equally, reaching the time relationship that balance needs is that membrane aperture is got over
Small, equilibration time is shorter.
In the present invention, preferably pass through between the water phase outlet of the liquid storage clarifying basin, triple valve, circulating pump and perforated membrane
Connecting pipe is connected, and forms closed cycle, becomes access, and keep the flow between each component identical, and then make to extract
Process, which is stablized, to be carried out, and circulating pump is adjustable commutating speed, flow direction provides pressure for the flowing of continuous phase, while for film emulsion process,
To form lotion stream.Film emulsification and extraction device provided by the invention can also can be completed not by adjusting flow velocity and extraction time
It with the extraction process of cycle-index, and extracts completion and turns on the switch later, the collection respectively of water phase and organic phase can be completed.
According to the present invention, when the film emulsification and extraction device works in a manner of vertical, i.e. water phase under, organic phase upper,
It completes to separate two-phase by gravity later in order to extract, cooperates triple valve, collect the water phase after the completion of extraction respectively
And organic phase.
Water phase to be extracted in liquid storage clarifying basin is connected by the present invention by circulating pump and perforated membrane with organic phase, is formed
Closed cycle provides pressure for the flowing of continuous phase, while for film emulsion process, lotion stream is formed, when it becomes by section
Alternatively locate, lotion rapidly disappears, and separates water phase with organic phase by gravity, using the peptizaiton of film, makes continuous
It is mutually sufficiently mixed with dispersed phase, extraction and clarifying process is quickly and efficiently completed, to improve extraction efficiency and extraction rate；And
And the film emulsification and extraction device have easy processing, rapidly and efficiently, low energy consumption, recyclable operation, occupied area are small, mutually separation is fast
Advantage, compact, efficient, safety, economy, laboratory and industrial application suitable for different scales are adaptable, can be used for petroleum
The separator in the fields such as chemical industry, Industrial Wastewater Treatment, hydrometallurgy and pharmaceuticals industry.
Film emulsification and extraction device provided by the invention is shown in Table 1 compared with the parameter of traditional extraction device.
The parameter comparison result of table 1 film emulsification and extraction device and traditional extraction device
| Equipment | Hybrid mode | Cost | Mixing efficiency | Separating capacity | Treating capacity |
| Mixer-settler | Stirring | It is higher | It is high | Generally | Greatly |
| Pulse extraction column | Vibration | It is high | Generally | It is high | Greatly |
| Centrifugal extractor | Stirring | It is high | It is high | It is high | Generally |
| Film emulsification and extraction device | Film emulsification | It is low | It is high | It is high | Greatly |
The present invention also provides a kind of film emulsification and extraction methods, using above-mentioned film emulsification and extraction device, by water to be extracted
It is mutually sequentially added in liquid storage clarifying basin with organic phase, makes perforated membrane infiltration in organic phase；The organic phase include diluent with
Extractant；Circulating pump is opened, water phase to be extracted enters organic phase through circulating pump, perforated membrane, forms lotion；After circulation terminates, exist
Under gravity, organic phase is separated from the water, obtains organic phase extracted.
Wherein, the film emulsification and extraction device is same as above, and details are not described herein.
Water phase to be extracted and organic phase are sequentially added in liquid storage clarifying basin, water phase to be extracted under, organic phase upper, and
The maximum cross-section area of water phase to be extracted is greater than the maximum cross-section area of organic phase；The organic phase includes diluent and extraction
Agent；The diluent is organic solvent well known to those skilled in the art, has no special limitation；The extractant is this
Extractant known to the technical staff of field can be selected according to substance to be extracted, have no special limitation.
Circulating pump is opened, water phase to be extracted enters organic phase through circulating pump, perforated membrane, under the peptizaiton of film, and has
Machine is mutually thoroughly mixed to form lotion；The flow velocity of the circulating pump is preferably 40~1000ml/min, more preferably 40~500ml/
Min, is further preferably 40~200ml/min, and most preferably 40~120ml/min can be determined as needed.
Lotion rapidly disappears at the cross section variation of liquid storage clarifying basin.
After circulation terminates, under the effect of gravity, organic phase is separated from the water, preferably adjustment triple valve, obtains extracted
Organic phase.
The flow velocity of the adjustable mobile phase of device provided by the invention, replaces the clarification liquid storage tank of different capabilities, and not
The perforated membrane of same specification is to meet the needs of production application.
For different industrial requirements, the perforated membrane of different pore size, different materials may be selected.Liquid storage clarifying basin is divided to upper and lower two
Part, but it is an entirety, the cross section of lower part will be greater than upper partial cross sectional as far as possible, so that lotion is divided as early as possible
From material is selected according to actual needs.For the treating capacity in concrete application, the pump of different size may be selected.
In order to further illustrate the present invention, with reference to embodiments to a kind of film emulsification and extraction device provided by the invention and
Film emulsification and extraction method is described in detail.
Reagent used in following embodiment is commercially available.
Use film emulsification and extraction device shown in FIG. 1.
Perforated membrane 1 is fixedly connected by pipeline, and is immersed in organic phase；The aperture of perforated membrane is 1 μm；
Organic phase and water phase are in liquid storage clarifying basin, and in extraction process, lotion can become in the cross section of liquid storage clarifying basin
It disappears at change；The ratio between the maximum cross-section area and smallest cross-section area of the liquid storage clarifying basin are 2：1；
The outlet 3 of liquid storage clarifying basin 2 and triple valve 4 are connected by connecting pipe 6；
Triple valve 4 is connected by connecting pipe 6 and circulating pump 5, to complete the smooth flow of mobile phase；The flow velocity of circulation is
120ml/min；
Circulating pump 5 is connected with perforated membrane 1 again by connecting pipe 6, forms a closed circuit.
Embodiment 1
To the Fe of 1000ppm in hydrochloric acid system3+It is extracted, organic phase is kerosene and di-(2-ethylhexyl)phosphoric acid
Ester.
2 embodiment of table, 1 extraction results
Table 2 statistics indicate that, which can quickly and efficiently carry out solvent extraction, and device design is simple, cheap,
Easy to operate, occupied area is small, and low energy consumption.Specification is adjusted, it can be achieved that hundred milliliters for the treatment of capacities even higher to hectolitre, have
Very extensive prospects for commercial application.
Embodiment 2
To the Pd of 100ppb~1000ppm in hydrochloric acid system2+It is extracted, organic phase is toluene and Cyphos IL
101 ion liquid abstraction agent.
3 embodiment of table, 2 extraction results
| Experimental group | Concentration before extracting | Concentration after extraction | Extraction efficiency % |
| 1 | 100ppb | 0.475ppb | >99 |
| 2 | 10ppm | 1.279ppb | >99 |
| 3 | 100ppm | 0.062ppm | >99 |
| 4 | 1000ppm | 0.085ppm | >99 |
Table 3 shows that the device is capable of handling the solution of various concentration metal ion, and extraction efficiency is high, and the reality
Testing is carried out under lower extractant and object molar ratio to be extracted, this for the solution for handling high concentration object to be extracted,
The use for reducing extractant can reduce extractant concentration, this is conducive to a possibility that reducing third phase formation, and is conducive to
The mutually quick progress of separation.This feature is also advantageous to industrial application.
Embodiment 3
The U of 50ppm (VI) is extracted in nitric acid system, organic phase is hexamethylene and Cyphos IL104 ionic liquid
Body extractant, extractant used are only 1.25 times of theoretical value, and final extraction efficiency has reached 98%.More than this example combines
Example may indicate that the metal extraction under the device difference system, and the usage amount of extractant is small.
Embodiment 4
100ppmPd (II) is extracted respectively using film emulsification and extraction device provided by the invention and stirring extraction, uses Cyphos
IL101 extractant, flow velocity 120mL/min, the aperture using perforated membrane are 1 micron.Extraction results are shown in Table 4.
4 extraction results of table
| 1min | 2min | 3min | 4min | 5min | 6min | |
| Film emulsification and extraction device (efficiency) | 71.58% | 84.62% | 93.07% | 96.61% | 97.58% | 97.62% |
| Stirring extraction (efficiency) | 66.74% | 75.31% | 81.06% | 85.48% | 89.37% | 91.33% |
Claims (8)
1. a kind of film emulsification and extraction device, which is characterized in that including：
Liquid storage clarifying basin；The lower part of the liquid storage clarifying basin is provided with water phase outlet；The top of the liquid storage clarifying basin is provided with
Perforated membrane；
Circulating pump；One end water phase outlet of the circulating pump is connected；The other end is connected with the perforated membrane；
The area of section of liquid storage clarifying basin lower part is greater than the area of section on top.
2. film emulsification and extraction device according to claim 1, which is characterized in that the maximum cross-section face of the liquid storage clarifying basin
The long-pending ratio with minimum cross-sectional area is more than or equal to 1.1：1.
3. film emulsification and extraction device according to claim 1, which is characterized in that the maximum cross-section face of the liquid storage clarifying basin
The long-pending ratio with minimum cross-sectional area is (1.5~10)：1.
4. film emulsification and extraction device according to claim 1, which is characterized in that the perforated membrane is cylindrical film；It is described more
One end that pore membrane is not connected with circulating pump is enclosed construction.
5. film emulsification and extraction device according to claim 1, which is characterized in that the aperture of the perforated membrane is 1~50 μm.
6. film emulsification and extraction device according to claim 1, which is characterized in that further include triple valve；The water phase outlet
It is connected by triple valve with the circulating pump.
7. a kind of film emulsification and extraction method, which is characterized in that including：
Using film emulsification and extraction device described in claim 1~6 any one,
Water phase to be extracted and organic phase are sequentially added in liquid storage clarifying basin, make perforated membrane infiltration in organic phase；It is described organic
It mutually include diluent and extractant；
Circulating pump is opened, water phase to be extracted enters organic phase through circulating pump, perforated membrane, forms lotion；
After circulation terminates, under the effect of gravity, organic phase is separated from the water, obtains organic phase extracted.
8. film emulsification and extraction method according to claim 7, which is characterized in that the flow velocity of the circulating pump be 40~
1000ml/min。
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| CN201810862913.2A CN108854153B (en) | 2018-08-01 | 2018-08-01 | Film emulsification and extraction device and film emulsification and extraction method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111672157A (en) * | 2020-06-28 | 2020-09-18 | 郑州铁路职业技术学院 | Method for realizing rapid extraction of organic compound |
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| CN107080972A (en) * | 2017-06-20 | 2017-08-22 | 中国科学院青岛生物能源与过程研究所 | A kind of method for improving membrane extraction efficiency |
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| JP2007125535A (en) * | 2005-11-01 | 2007-05-24 | Kiyomoto Iron & Machinery Works Co Ltd | Emulsification process and emulsification apparatus |
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