CN1182905C - Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device - Google Patents
Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device Download PDFInfo
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- CN1182905C CN1182905C CNB021212104A CN02121210A CN1182905C CN 1182905 C CN1182905 C CN 1182905C CN B021212104 A CNB021212104 A CN B021212104A CN 02121210 A CN02121210 A CN 02121210A CN 1182905 C CN1182905 C CN 1182905C
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Abstract
The present invention relates to a liquid-liquid-liquid triphase horizontal and continuous lifting and stirring extraction device which comprises a horizontal reactor, wherein both ends of the horizontal reactor are respectively provided with a baffle plate box filled with material; an upper shaft and a lower shaft are arranged in parallel by transversely penetrating through the end walls of both sides and the baffle plate boxes; an upper baffle plate and a lower baffle plate are respectively and vertically arranged on two shafts of the baffle plate boxes in the reactor in parallel and at intervals; a circular-arc lifting barrel is horizontally arranged between the baffle plates; a light-phase outlet, an intermediate-phase inlet and a heavy-phase outlet are orderly arranged on the end walls of one side of the reactor from top to bottom; the intermediate-phase inlet is positioned between the upper shaft and the lower shaft; a light-phase inlet, an intermediate-phase outlet and a heavy-phase inlet are orderly arranged on the end walls of the other side of the reactor from top to bottom; the intermediate-phase outlet is positioned between the upper shaft and the lower shaft; the shaft ends of the two shafts are respectively provided with driving wheels driven by a motor. The utility model has the advantages of simple structure, low energy consumption, flexible operation, easy regulation, emulsification prevention and back mixing reduction, and the device is suitable for separation and purification of biochemical products with a high added value from the fermentation liquor of biologic products.
Description
Invention field
The invention belongs to the liquid-liquid-liquid three phase continuous extraction device, be particularly related to a kind of liquid-liquid-liquid three-phase (heavy phase, middle phase, light phase) horizontal continuous lifting stirring extraction device that is used for from COMPLEX MIXED system separate targets product, be specially adapted to use the three-phase one-step method from the biological product zymotic fluid, to separate the biogenetic products of purification high added value.
Background technology
Solvent extraction is as the existing history that goes up a century of a kind of traditional separation purification means, and it is widely used in fields such as oil, chemical industry, pharmacy, metallurgy, environmental protection and bioengineering.But along with the continuous development, particularly bioengineering of process industrial and the develop rapidly of biochemical pharmacy industry, traditional solvent extraction technology and equipment can not adapt to industrial requirement far away.The separation of carrying out the biofermentation product with traditional liquid-liquid two-phase solvent extraction process and equipment exists that technology is loaded down with trivial details, process is complicated, cause drawbacks such as emulsification easily.
For this reason, domestic and international many scholars have carried out new liquid-phase extraction Study on Technology work, and have obtained some progress.The novel penicillin g extract technology of developing as people such as Chen Ji, be triphase one-step extraction process to purify penicillin (Chinese invention patent CN00107655.8), this method can overcome the defective that exists in the prior art effectively, the three-phase that utilizes organic solvent and double-aqueous phase system to form is jointly once finished extraction and the purifying to complex mixture, the orientation of finishing target product and accessory substance that acts synergistically between the three-phase is separated, in single extraction, finish organic facies/water, and the synergic solvent extraction assigning process between the aqueous two-phase, can obviously improve the extraction quality, simplify production technology.He has also invented a kind of serial self-suction type multi-channel phase dispersing extractor (Chinese invention patent CN00107700.7) that uses with this process matching simultaneously.But this invention does not have material import and export device, can only be used for batch process, and treating capacity is little, can not adapt to industrial quantity-produced requirement.In addition, people such as Tan Xiandong has developed a kind of liquid-liquid-liquid three phase continuous extraction vibrating sieve plate tower (Chinese invention patent CN02106742.2).Though the invention of this equipment is industrially carried out extensive liquid-liquid-liquid three phase continuous extraction feasible scheme is provided for being implemented in, the part but this equipment still comes with some shortcomings, lower as mass-transfer efficiency and extraction efficiency, two-stage liquid-liquid extraction process is cascaded the continuous extraction of inreal realization liquid-liquid-liquid three-phase original position because this equipment is actually.And existing experimental result shows that the efficient of liquid-liquid-liquid three-phase original position extraction can reach more than 80%, is higher than the efficient (extraction efficiency only is 62%) of two-stage liquid-liquid extraction cascade process far away.Therefore, develop and to carry out quantity-produced liquid-liquid-liquid three-phase original position extraction equipment and have crucial meaning.
Summary of the invention
The objective of the invention is to overcome the defective of above-mentioned technology, and provide a kind of adapt to industrial continuously, the liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device of High-efficient Production.
Embodiment of the present invention are as follows:
Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device provided by the invention is characterized in that, this device comprises:
One horizontal reactor 1, the longitudinal cross-section of this horizontal reactor 1 are that the upper and lower part is divided into semicircle, and mid portion is the racetrack cross section of straight line; The top of this horizontal reactor 1 is provided with a steam vent 81, and the bottom is provided with an outage 8; A vertical hollow division board case 14 is installed at two ends respectively in the horizontal reactor 1, and this vertical porous division board case 14 contacts with horizontal reactor 1 inwall, in this vertical porous division board case 14 filler 11 is housed, and its plate tank wall is provided with through hole; Cross axle 5 and one lower shaft 9 in horizontal reactor 1 both sides end wall and the two vertical hollow division board case 14 parallel installations one, collar plate shape overhead gage 2 and the collar plate shape lower baffle plate 13 that vertical parallel interval is placed is installed respectively on the diaxon in the horizontal reactor 1 between the vertical hollow division board case 14, and level is installed circular-arc lifting bucket 3 between the baffle plate; Be provided with light phase export 18, middle phase import 16 and heavy out 15 from the top down successively on the horizontal reactor 1 one side walls, middle phase import 16 is between last axle 5 and lower shaft 9; Be provided with light phase import 4, centre on the opposite side end wall from the top down successively and export 7 and heavy phase import 10 mutually, the centre exports 7 mutually between last axle 5 and lower shaft 9; The direction of rotation of described upward axle 5 and lower shaft 9 or identical; The rotating speed of described upward axle 5 and lower shaft 9 is identical or different; The described axle 5 and lower shaft 9 and sidewall joint, horizontal reactor 1 two ends gone up is equipped with axle envelope 17; Liquid level gauge 19 and following liquid level gauge 20 are installed on the described horizontal reactor 1 one side sidewalls; The described axle head of going up axle 5 and lower shaft 9 installs one respectively by motor-driven drive 6.
Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device provided by the invention has following characteristics:
1, the present invention both can be made into small test device (diameter is about 0.1～0.15m, long 1m), also can be made into large industry equipment (diameter is about 2m, long 8m) and was used for large-scale industrial production;
2, be applicable to that white density differs very little, interfacial tension is low, is very easy to produce the system of emulsification;
3, owing to the shaft horizontal positioned, the unlikely generation axial circulating current of the variation of two-phase density contrast in the extraction process, thereby can reduce back-mixing;
If 4, stop suddenly in the running, can not destroy the inter-stage CONCENTRATION DISTRIBUTION, recover steady state operation when going into operation again easily;
5, be applicable to and handle solids-laden system and separate the many and little occasion for the treatment of capacity of progression that theoretical stage can reach eight grades;
6, three alternate cross-flow contacts have improved mass tranfer coefficient; Three phase extraction carries out in position, has improved extraction efficiency;
7, simple in structure, energy consumption is low;
8, body good leak tightness;
9, two horizontal lifting stirring extractors are carried out vertically overlapping, improved space availability ratio, saved floor space;
10. the rotating speed of axle 5 and axle 9 can be regulated respectively, thereby is applicable to the system that rate determining step is different;
11. inserted mass filler in the porous division board, when liquid was flowed through this plate, collision opportunity increased between drop, easier mutual gathering, phase-splitting, and can reduce the volume of settling section greatly.
Description of drawings
Accompanying drawing 1 is a structural representation of the present invention;
Accompanying drawing 2 is the right plate structural representation of horizontal reactor 1;
Accompanying drawing 3 is the left plate structural representation of horizontal reactor 1;
Accompanying drawing 4 is the E-E cutaway view of Fig. 1;
Accompanying drawing 5 is the circular-arc structural representation that promotes bucket 3
Accompanying drawing 6 is each fluid flow state figure in the three-phase in the running of the present invention;
Wherein:
Clarification phase-separating section Q1, Q2 three phase mixture H drives 6
Reactor 1 upper guard-plate 2 under shields 13
14 envelopes 17 of circular-arc lifting bucket 3 porous division board casees
Export 7 top liquid level gauges 19 mutually in the middle of the light phase import 4
Heavy phase import 10 gently with the interface 21 of centre between mutually
Heavy phase and middle interface, interface 22 between mutually
Steam vent 81 outages 8
Heavy out 15 butyl acetates (light phase)
Penicillin fermentation filtrate (heavy phase) the polyethylene glycol aqueous solution (middle phase)
Embodiment
As seen from the figure, liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device provided by the invention is characterized in that, this device comprises:
One horizontal reactor 1, the longitudinal cross-section of this horizontal reactor 1 are that the upper and lower part is divided into semicircle, and mid portion is the racetrack cross section of straight line; The top of this horizontal reactor 1 is provided with a steam vent 81, and the bottom is provided with an outage 8; A vertical hollow division board case 14 is installed at two ends respectively in the horizontal reactor 1, and this vertical porous division board case 14 contacts with horizontal reactor 1 inwall, in this vertical porous division board case 14 filler 11 is housed, and its plate tank wall is provided with through hole; Cross axle 5 and one lower shaft 9 in horizontal reactor 1 both sides end wall and the two vertical hollow division board case 14 parallel installations one, collar plate shape overhead gage 2 and the collar plate shape lower baffle plate 13 that vertical parallel interval is placed is installed respectively on the vertical hollow diaxon between high plate case 14 in the horizontal reactor 1, and level is installed circular-arc lifting bucket 3 between the baffle plate; Be provided with light phase export 18, middle phase import 16 and heavy out 15 from the top down successively on the horizontal reactor 1 one side walls, middle phase import 16 is between last axle 5 and lower shaft 9; Be provided with light phase import 4, centre on the opposite side end wall from the top down successively and export 7 and heavy phase import 10 mutually, the centre exports 7 mutually between last axle 5 and lower shaft 9; The direction of rotation of described upward axle 5 and lower shaft 9 or identical; The rotating speed of described upward axle 5 and lower shaft 9 is identical or different; The described axle 5 and lower shaft 9 and sidewall joint, horizontal reactor 1 two ends gone up is equipped with axle envelope 17; Liquid level gauge 19 and following liquid level gauge 20 are installed on the described horizontal reactor 1 one side sidewalls; The described axle head of going up axle 5 and lower shaft 9 installs one respectively by motor-driven drive 6.
Now sending out filtrate pure with triphase one-step extraction process to purify penicillin is example, briefly introduces the design feature and the operating conditions of device provided by the invention:
In triphase one-step extraction process to purify penicillin ferment filtrate process, heavy phase is a penicillin fermentation filtrate, and the centre is the polyethylene glycol aqueous solution mutually, gently is butyl acetate mutually.Except opening steam vent 81 and heavy phase import 10, other each import and export are all closed in advance on the horizontal reactor 1 inject liquid in horizontal reactor 1 before.Penicillin fermentation filtrate (heavy phase) enters horizontal reactor 1 from heavy phase import 10 earlier, arrives liquid level 22 up to it, opens heavy out 15, makes heavy phase keep flow regime; Then, phase import 16 allows the polyethylene glycol aqueous solution (middle phase) enter horizontal reactor 1 thus in the middle of opening, and after it arrives liquid level 21, exports 7 mutually in the middle of opening, and keeps flow regime in the middle of making mutually; And make middle phase liquid and heavy phase liquid be counter current contacting; At last, butyl acetate (light phase) phase import 4 on the lenient side flows into horizontal reactors 1, up to its with horizontal reactor 1 in remaining air drain, be full of whole horizontal reactor 1.At this time close steam vent 81 and open light phase export 18, make the continuous-flow of light phase liquid.So far, each phase liquid all carries out continuous-flow by horizontal reactor 1.In running, can regulate by separator-pump (heavy out control), control interface 22 (being heavy phase and middle interface between mutually), by pump-separator (light phase export control) adjusting, control interface 21 (promptly light and centre mutually between interface).
The axle (promptly going up axle 5 and lower shaft 9) of two levels is arranged in this device, drive respectively, slowly rotate by two motors.In three phase mixtures (H), vertical separately upper guard-plate 2 and the under shield 13 of being equipped with on last axle 5 and the lower shaft 9, a plurality of circular-arc lifting buckets 3 are housed between every adjacent screen, and opening is towards direction of rotation, and upper guard-plate 2 and under shield 13 form the annular gap with the equipment outer wall.
In three phase mixtures (H), when lower shaft 9 drives under shield 13 above it and rotates, interface 22 upper areas, phase (PEG) liquid in the middle of the circular-arc lifting bucket 3 that one end has drenched heavy phase has been ladled out, the other end circular-arc promotes the heavy phase (H that bucket 3 has been ladled out during the rotation of 22 lower areas at the interface simultaneously
2O) liquid drenches into middle phase (PEG) with the form of drop (decentralized photo).22 lower areas at the interface, the circular-arc lifting bucket 3 of disk one end has been ladled out heavy phase (H
2O), after the circular-arc lifting bucket 3 middle phases (PEG) of having been ladled out when interface 22 upper areas rotate of the other end enter heavy phase as decentralized photo simultaneously, and upwards elegant with the drop form, two-phase is mixed in this way, mass transfer.
In like manner, in three phase mixtures (H), when last upper guard-plate 2 that drives above it rotates, 21 upper areas at the interface, circular-arc liftings of phase bucket 3 had been ladled out light phase (BA) liquid in the middle of one end had drenched, and the other end circular-arc promotes barrels 3 middle phase (PEG) liquid of having been ladled out during the rotation of 21 lower areas at the interface and drench into light phase with the form of drop (decentralized photo) simultaneously.21 lower areas at the interface, phase (PEG) in the middle of the circular-arc lifting bucket 3 of upper guard-plate 2 one ends has been ladled out, simultaneously circular-arc liftings bucket 3 light phase (BA) liquid of when interface 21 upper areas rotate, having been ladled out of the other end enter as decentralized photo the centre mutually after, and upwards elegant with the drop form, two-phase is mixed in this way, mass transfer.
Subsequently, heavy phase (H
2O) enter clarification phase-separating section Q1 with the light porous division board 14 of (BA) liquid through filling filler mutually, and after this clarification, phase-splitting device for transferring; The porous division board 14 of middle phase (PEG) liquid through filling filler enters clarification phase-separating section Q2, and after this clarification, phase-splitting device for transferring.
By said process the extraction of liquid-liquid-liquid three-phase original position is carried out continuously, impurity such as foreign protein, mycelia, pigment are extracted into the water-soluble liquid phase of polyethylene glycol (middle phase) together and export 7 mutually from the centre and discharge; Penicillin fermentation filtrate (heavy phase) after the raffinate is discharged from the heavy out 15 that is positioned at device bottom; Penicillin is then come together to go in the butyl acetate continuously, and the light phase export 18 through being positioned at the equipment top is discharged, thereby has finished whole liquid-liquid-liquid three phase continuous extraction process.In actual production process, material into and out of all being continuously to carry out.
The horizontal reactor of this equipment, baffle plate, circular arc promote parts such as bucket, porous division board, axle and all can adopt the metal material manufacturing.If use this equipment, then should adopt the stainless steel that meets the GMP standard at pharmaceutical industry.Device bottom should be provided with support, and each liquid phase import and export place reserves flange-interface, drives so that fix, pacify installation and dismantling.
In sum, liquid-liquid-liquid three-phase continuous horizontal type lifting stirring extractor involved in the present invention has been realized the extraction of liquid-liquid-liquid three-phase continuous in-situ first.Have reduce back-mixing, theoretical stage height, extraction efficiency height, simple in structure, easy amplification, continuously-running, energy consumption low, take up an area of advantages such as economizing, be easy to recover steady state operation, be applicable to contain the solid matter and the easy biogenetic products extraction separation process of emulsification.The present invention provides the reliable device support for triphase one-step extraction process to purify penicillin and other liquid-liquid-liquid three phase extraction technology in industrial large-scale application, greatly reduce the expense in the Related product purifies and separates process, can effectively solve puzzlement industry " bottleneck " problem for many years, be of great immediate significance.
Claims (7)
1, a kind of horizontal continuous lifting stirring extraction device of three kinds of different densities liquid phases is characterized in that, this device comprises:
One horizontal reactor (1), the longitudinal cross-section of this horizontal reactor (1) are that the upper and lower part is divided into semicircle, and mid portion is the racetrack cross section of straight line; The top of this horizontal reactor (1) is provided with a steam vent (81), and the bottom is provided with an outage (8); A vertical hollow division board case (14) is installed at the interior two ends of horizontal reactor (1) respectively, this vertical porous division board case (14) contacts with horizontal reactor (1) inwall, in this vertical porous division board case (14) filler (11) is housed, its plate tank wall is provided with through hole; Cross axle (5) and a lower shaft (9) in horizontal reactor (1) both sides end wall and the parallel installation one of two vertical hollow division board casees (14), collar plate shape overhead gage (2) and the collar plate shape lower baffle plate (13) that vertical parallel interval is placed is installed respectively on the diaxon in the horizontal reactor (1) between the vertical hollow division board case (14), and level is installed circular-arc lifting bucket (3) between the baffle plate; Be provided with light phase export (18), middle phase import (16) and heavy out (15) on horizontal reactor (1) the one side wall from the top down successively, middle phase import (16) is positioned between axle (5) and the lower shaft (9); Be provided with light phase import (4) on the opposite side end wall from the top down successively, the centre exports (7) and heavy phase import (10) mutually, the centre exports (7) mutually and is positioned between axle (5) and the lower shaft (9).
2, by the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 1, it is characterized in that the direction of rotation of described upward axle (5) and lower shaft (9) or identical.
By the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 1, it is characterized in that 3, the rotating speed of described upward axle (5) and lower shaft (9) is identical or different.
By the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 2, it is characterized in that 4, the rotating speed of described upward axle (5) and lower shaft (9) is identical or different.
By the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 1, it is characterized in that 5, the described axle (5) and lower shaft (9) and sidewall joint, horizontal reactor (1) two ends gone up is equipped with axle envelope (17).
6, by the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 1, it is characterized in that, on described horizontal reactor (1) the one side sidewall liquid level gauge (19) and following liquid level gauge (20) are installed.
By the horizontal continuous lifting stirring extraction device of the described three kinds of different densities liquid phases of claim 1, it is characterized in that 7, the described axle head of going up axle (5) and lower shaft (9) installs one respectively by motor-driven drive (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021212104A CN1182905C (en) | 2002-06-10 | 2002-06-10 | Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021212104A CN1182905C (en) | 2002-06-10 | 2002-06-10 | Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1463782A CN1463782A (en) | 2003-12-31 |
| CN1182905C true CN1182905C (en) | 2005-01-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021212104A Expired - Fee Related CN1182905C (en) | 2002-06-10 | 2002-06-10 | Liquid-liquid-liquid triphase horizontal continuous lifting stirring extraction device |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233199B (en) * | 2010-04-30 | 2013-12-11 | 中国科学院过程工程研究所 | Three-phase solvent gas assisted extraction subsection-inlet back-mixing controllable continuous extraction device |
| CN102091436B (en) * | 2011-01-19 | 2015-05-06 | 中国科学院过程工程研究所 | Liquid-liquid-liquid triple-phase continuous counter-current extraction device and use method thereof |
| CN102380227B (en) * | 2011-11-14 | 2014-09-24 | 中国科学院过程工程研究所 | Extremely low concentration extraction method |
| CN112494988B (en) * | 2020-12-11 | 2023-12-19 | 浙江工业大学 | Horizontal liquid-liquid extraction device and application method thereof |
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