CN102430264B - Low rotating speed self-priming extraction equipment - Google Patents

Low rotating speed self-priming extraction equipment Download PDF

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Publication number
CN102430264B
CN102430264B CN201110280248.4A CN201110280248A CN102430264B CN 102430264 B CN102430264 B CN 102430264B CN 201110280248 A CN201110280248 A CN 201110280248A CN 102430264 B CN102430264 B CN 102430264B
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rotating shaft
hollow
liquid phase
extraction equipment
phase
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CN201110280248.4A
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CN102430264A (en
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杨良嵘
黄寅斌
邢慧芳
黄焜
刘会洲
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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Abstract

The invention relates to a low rotating speed self-priming extraction equipment, characterized in that: a hollow rotating shaft and a liquid phase diffuser fixed on the hollow rotating shaft are arranged in an extraction tank of the extraction equipment, wherein, the shaft wall of the hollow rotating shaft is provided with a feed inlet, the rotating shaft is connected with a motor, the liquid phase diffuser comprises two or more single channel simple liquid phase diffusers in series, each simple liquid phase diffuser is provided with a feed inlet, a hollow rotating shaft, and a hollow rotary drum which are communicated with each other, but each simple diffuser are not communicated through the hollow rotating shaft, and a channel exit of the last N-1 level simple diffuser is provided with a downward-facing outer cover. The extraction equipment is suitable for a large-phase ratio easy-emulsification system. According to the invention, by concatenating at least two self-priming phase-dispersed stirrers into a whole and uniformly dispersing a light phase in a heavy phase, the operation can be continuously carried out under the condition of distinct two-phase interface, thus the emulsification phenomenon is avoided, the advantages of small equipment investment, easy operation, low rotating speed of the motor, low power consumption, and small shearing force to solution are achieved. The invention is beneficial to keep the activity of biomacromolecules.

Description

A kind of low rotating speed self-priming extraction equipment
Technical field
The present invention relates to liquid-liquid two-phase solvent extraction equipment in a kind of medicine, metallurgy or biochemical field, be specifically related to a kind of low rotating speed self-priming extraction equipment, particularly in a kind of continuous extraction apparatus of large phase ratio easy emulsifying system.
Background technology
Solvent extraction is a kind of efficient separation and extraction technology, is 21 century one of the most promising green chemical industry developing direction.An important branch as chemical separating subject, abstraction technique can be selected suitable extraction system and flow process according to separate object and technological requirement, there is selective height, good separating effect, the feature such as easy operating and strong adaptability, thereby be widely used in the fields such as hydrometallurgy, petrochemical industry, atomic energy chemical industry, medicine, environmental protection, bioengineering and fabrication of new materials.But when extraction application is during in these fields, emulsion is distinct issues relatively in extraction process.
Because living things system is all very responsive to soda acid, organic solvent and mechanical shear stress etc., adopt the violent extraction mode of mixing of common paddle to be easy to cause inactivation and decomposition.In the separation and purification of biological product, emulsion is more outstanding.Such as: in antibiotic zymotic fluid, contain a large amount of protein and sugar etc., in organic solvent extraction process, protein molecule is easy to sex change.If adopt common agitating mode to mix, speed is too low can not complete extraction process, and the protein of a large amount of sex change can be adsorbed in high speed shear destruction generation a large amount of size of grains interface, form even protein cross structure of firm interfacial film, make emulsion become highly stable.The formation of emulsion is very unfavorable for extraction process, and emulsification causes the useless zymotic fluid of raffinate to carry solvent secretly, reduces product yield, meanwhile, carries zymotic fluid secretly and also to recycling, cause difficulty in organic phase.
Solvent extraction is the extracting penicillin history of existing more than 50 years from zymotic fluid, but extraction process does not have to change substantially: extraction equipment used adopts drum-type centrifugal extractor and decanter at present mostly, extractant used is mainly acetic acid fourth (penta) ester, methylisobutylketone etc.Extracting operation condition is: pH is 1.8~2.2, organic phase and water volume ratio O/A=1/2, and back extraction pH is 6.7~7.2, compares O/A=2/1.In extraction process, there are following two features: (1) penicillin destructible, relatively stable in pH 4~8 scopes, at pH < 4 or pH > 8, all easily decompose.At 2.0,10 ℃ of pH, the half-life of penicillin is 1.3 hours, and extraction will complete within very short time.In addition, what in two-phase, mix use is that oar formula stirs, and required rotating speed is higher, and this is destroyed the biologically active of penicillin.(2) owing to containing a large amount of protein, organic pigment and other biological byproduct in zymotic fluid, so emulsification is serious in extraction process.
CN 1047293A discloses a kind of composition and extracting process of extracting penicillin, described extracting process adds neutral phosphor (phosphine) class or sulfoxide compound in butyl acetate, make itself and butyl acetate form mixed extractant solvent penicillin, can make operating condition bring up to 3.0~3.5 from pH 1.8~2.2, yield has improved 3%.But this technique does not change on extraction equipment, and the effect that causes the method to obtain is in actual applications not fairly obvious.
At present, for solving the emulsification problem of mixed solvent, the efficient centrifugal extractor of industrial employing carries out Centrifugical extraction.But the defect of centrifugal extraction method is that equipment investment is larger, adopts centrifugal extraction method to be also difficult to emulsification to eliminate, and in technical process, must use demulsifier.Take North China Pharmaceutical Factory as example, and in annual penicillin production technique, the demulsifier consumption needing just reaches more than 1,000,000 yuan.
< < Liquid-liquid Extraction Processes and equipment > > (Atomic Energy Press, 1993, Fei Weiyang etc.) book is pointed out: when carrying out the selection of extraction equipment, the extraction of difficult clarification system is generally used centrifugal extractor and barrel formula extractor of drenching with rain.Centrifugal extractor is to carry out two-phase fully to mix fast, and utilize centrifugal force to replace the extraction equipment of the quick phase-splitting of gravity, though can solve the problem of phase-splitting difficulty, but shortcoming is complex structure, manufacture, operation and maintenance costs is higher, due to rapid stirring, shearing force causes more serious emulsion compared with great Yi in addition.Rain type extractor is a kind of horizontal successive extractor, the material that is applicable to process conventionally easily emulsification and contains solid particle, but that shortcoming is rotating speed is slow, mass transfer rate is low, lower than loading.
CN 1310034A discloses a kind of light phase or heavy phase is disperseed low-shearing force self-sucking stirring extraction device and method of operating, described self-priming stirring extraction device comprises motor, axle sleeve, agitator, mixing channel and baffle plate, described agitator is in mixing channel, this agitator is self-absorbing type stirrer, self-absorbing type stirrer is thinner circular shaft disperseing the epimere of light phase time rotating shaft, and hypomere is the circular shaft with cavity; On the circular shaft above or below rotating disk, have one or more apertures that communicate with top or the top of cavity, the lower end of rotating shaft connects the rotary drum of hollow, and the cavity of rotating shaft communicates with the cavity of rotary drum; On rotary drum, have the aperture communicating with cavity; The rotating disk that is positioned at rotating shaft middle part is comprised of upper disk, lower disk and blade, or be one or more disks compositions, and wherein said blade be take rotating shaft and as the center of circle, is uniformly distributed in rotating shaft surrounding and is vertically connected between upper and lower disk; The epimere of described self-absorbing type stirrer in mixing channel rotating shaft when disperseing heavy phase is thinner circular shaft, the circular shaft that the hypomere of rotating shaft is hollow open, and the rotary drum of hollow is positioned at the middle part of rotating shaft; The cavity of rotating shaft and the cavity of rotary drum are connected by the aperture in rotating shaft; Aperture can be opened top or the top that is positioned at cavity in rotating shaft; On rotary drum, have the aperture communicating with cavity; Rotating disk is positioned at the bottom of rotating shaft, and rotating disk is comprised of upper disk, lower disk and blade, or is that one or more disks form, and wherein said blade be take rotating shaft and as the center of circle, is uniformly distributed in rotating shaft surrounding and is vertically connected between upper and lower disk.Described apparatus and method are specially adapted in Research Advances in Reversed Micellar Extraction process mutually light or heavy phase and disperse low-shearing force self-sucking to stir extraction, and it,, keeping two-phase interface clearly in situation, can carry out intermittence and continued operation.But this device still can not be in low energy consumption, under the condition of low equal shearing force and maintenance large biological molecule activity, realize extraction.
CN 1324683A discloses a kind of serial self-suction type multi-channel phase dispersing extractor, described extraction equipment comprises motor, agitator, reactor, agitator is that self-absorption multichannel disperses agitator mutually, the motor that this self-absorption multichannel disperses mutually agitator to comprise hollow rotating shaft and is connected with hollow rotating shaft and drives hollow rotating shaft to rotate, hollow rotating shaft axial wall is provided with charging aperture, the bottom of hollow rotating shaft or middle part are fixedly connected with the liquid phase disperser that sidewall is provided with discharging opening, liquid phase disperser is a hollow cylinder, on liquid phase disperser, fixedly mount one, the uncovered sleeve making progress that two or more are concentric with hollow rotating shaft, or below liquid phase disperser, fixedly mount one, the uncovered downward sleeve that two or more are concentric with hollow rotating shaft, two self-absorption multichannels disperse agitator to be connected into one mutually.This device can carry out delivery type and gently be scattered in mutually the process of heavy phase in three-phase, can solve the phase-splitting difficult problem that the emulsification of three-phase one-step method causes.But this device is when disperseing mutually, can not be in low equal shearing force, low energy consumption, keeps realizing extraction under the active constant condition of biological substance.
Therefore how developing a kind of low rotating speed self-priming extraction equipment, effectively to solve the difficult problem that is separated in mixed extractant solvent (such as the extraction of penicillin) technique, and effectively avoid emulsion, is the difficult problem that affiliated technical field faces.
Summary of the invention
One of object of the present invention is to provide a kind of low rotating speed self-priming extraction equipment, can effectively solve the difficult problem that is separated in mixed extractant solvent (such as the extraction of penicillin) technique, can effectively avoid emulsion, significantly reduce energy consumption, reduce to stir shearing force, keep large biological molecule biologically active, and this equipment investment is little, easy to operate, be applicable to the extraction system that easily emulsification is compared greatly such as biochemical industry, pharmaceuticals industry, hydrometallurgy, oil prodution industry, food industry.
Low rotating speed self-priming extraction equipment of the present invention, install in its extractor on axial wall with the hollow rotating shaft of charging aperture and be fixed on the series connection liquid phase disperser on hollow rotating shaft, rotating shaft is connected with motor, channel exit in simple liquid phase disperser is provided with direction outer cover down, described liquid phase disperser is in series by 2 above simple liquid phase disperser, and each simple disperser all has charging aperture, hollow rotating shaft, hollow rotary drum and discharging opening.But between each simple disperser, by hollow rotating shaft, do not communicate, at the channel exit of the simple liquid phase disperser of upper N-1 level, be provided with direction outer cover down, discharging opening and the extractor of hollow rotary drum are connected.
Preferably, on hollow rotary drum, there are a row, two rows or more than three rows (containing three, arrange) discharging opening that diameter is identical, position is relative, be evenly distributed.
Preferably, series connection liquid phase disperser is comprised of the simple liquid phase disperser of single channel, two passages or triple channel above (containing triple channel).
Preferably, the lower edge of outer cover 7 is higher than the charging aperture 3 of next stage, and the lower edge of outer cover 7 is preferably lower than the lower edge of the charging aperture 3 of next stage.
" simply " liquid phase disperser of the present invention or " simply " disperser, mean existing liquid phase disperser or disperser, because of its structure simple with respect to " liquid phase disperser " of the present invention and " disperser ", therefore the present invention is called " simply " by " liquid phase disperser " of prior art and " disperser ", i.e. single-stage " liquid phase disperser " and " disperser ".
Low speed self-priming extraction equipment is in extraction process, oil phase feed liquid enters into the hollow rotating shaft 4 of simple liquid phase disperser from charging aperture 3, under the suction function producing at hollow rotary drum 5 centers of rotation, oil phase feed liquid constantly declines, and the increase along with rotating speed, the negative pressure producing increases, and the degree of depth that oil phase feed liquid declines also increases thereupon.When rotating speed increase makes pressure reach certain value, the oil phase feed liquid in hollow rotating shaft 4 enters into the hollow rotary drum 5 of the first order, and meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 of the first order enters into water from first order discharging opening 6; The oil droplet of water coalescence under the stopping of first order outer cover 7 is oil phase, from the charging aperture of second level liquid phase disperser, enter hollow rotating shaft, under the suction function producing at hollow rotary drum 5 centers, the second level of rotation, feed liquid in hollow rotating shaft enters into the hollow rotary drum 5 in the second level, meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 in the second level enters into water from second level discharging opening 6; The oil droplet of water under the stopping of second level outer cover 7 again coalescence be oil phase, from the charging aperture of third level liquid phase disperser, enter hollow rotating shaft, under the suction function producing at the hollow rotary drum of the third level 5 centers of rotation, oil phase feed liquid in hollow rotating shaft 4 enters into the hollow rotary drum 5 of the third level, meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 of the third level enters into water from third level discharging opening 6.Take this principle as basis, can carry out the self-priming extracting operation of N (N > 3) level.
Useful technique effect of the present invention is that extraction equipment of the present invention is specially adapted to compare greatly, easy emulsifying system.Three self-priming agitators that disperse are mutually conspired to create to one, to gently be evenly dispersed in mutually in the process of heavy phase, can be in two-phase interface continued operation in situation clearly, avoided emulsion, equipment investment is little, easy to operate, motor speed requires low, power consumption is low, little to the shearing force of solution, is conducive to keep the activity of large biological molecule.
Accompanying drawing explanation
Fig. 1 single-stage and self-priming extraction equipment
Fig. 2 single-stage and self-priming extraction equipment extraction schematic diagram
Fig. 3 low rotating speed self-priming extraction equipment
Fig. 4 low rotating speed self-priming extraction equipment extraction schematic diagram
The specific embodiment
In the present invention, Reference numeral is expressed as follows:
Hollow rotary drum 6 discharging opening 7 outer covers of 1 rotating shaft 2 axial wall 3 charging aperture 4 hollow rotating shaft 5
The single-stage and self-priming extraction equipment of prior art, as shown in Figure 1, it comprises the rotating shaft 1 being connected with motor to its structure, rotating shaft 1 is connected with hollow rotating shaft 4, the top of hollow rotating shaft 4 has charging aperture 3, and end connects hollow rotary drum 5, and the sidewall of hollow rotary drum 5 has discharging opening 6.
Described single-stage and self-priming extraction equipment in use, as shown in Figure 2, in extraction process, oil phase feed liquid enters into the hollow rotating shaft 4 of single-stage liquid phase disperser from charging aperture 3, under the suction function producing at hollow rotary drum 5 centers of rotation, oil phase feed liquid constantly declines, and along with the increase of rotating speed, the negative pressure producing increases, and the degree of depth that oil phase feed liquid declines also increases thereupon.When rotating speed increase makes pressure reach certain value, the oil phase feed liquid in hollow rotating shaft 4 enters into hollow rotary drum 5, and meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 of the first order enters into water from discharging opening 6, forms oil droplet.Under the buoyancy that the oil droplet of water forms at density contrast, from the bottom of water rising, in floating-upward process, oil droplet constantly contacts with water, thereby the extracting substance containing in water is extracted into oil phase, forms pregnant solution.Described oil droplet arrives the top of water, forms oil phase layer.Oil phase in described oil phase layer, under the suction function producing at hollow rotary drum 5 centers of rotation, the charging aperture 3 by it from hollow rotating shaft 4 sucks, thereby forms circulation.
Low rotating speed self-priming extraction equipment of the present invention, as shown in Figure 3, described extraction equipment comprises at least 2 grades of single-stage liquid phase disperser, preferably includes 2~6 grades of single-stage liquid phase disperser, more preferably comprises 2 grades, 3 grades or 4 grades of single-stage liquid phase disperser.Accompanying drawing 3 of the present invention be take 3 grades of single-stage liquid phase disperser and is described as example.
Described every grade of single-stage liquid phase disperser includes hollow rotating shaft 4 and hollow rotary drum 5, on the top axial wall 2 of described hollow rotating shaft 4, has charging aperture 3, and hollow rotating shaft 4 ends are communicated with hollow rotary drum 5, and the sidewall of hollow rotary drum 5 has discharging opening 6.The hollow rotating shaft 4 of the single-stage liquid phase disperser of extractor topmost one-level is connected with rotating shaft 1, and rotating shaft 1 is connected with motor (not shown).Motor drive shaft 1 is rotated, thereby drive first order hollow rotating shaft 4 to rotate and then drive rotary drum 5 to rotate, all the other hollow rotating shafts at different levels 4 are all connected with the hollow rotary drum 5 of upper level, thereby rotated by its drive, but between each single-stage disperser, by physics, do not communicate, between each single-stage disperser only by outside water together with.
The channel exit of every grade of liquid phase disperser is provided with direction outer cover 7 down, and the channel exit of bottommost one-level liquid phase disperser of the present invention preferably dispenses described outer cover 7.
As shown in Figure 4, described low speed self-priming extraction equipment of the present invention is in extraction process, oil phase feed liquid enters into the hollow rotating shaft 4 of single-stage liquid phase disperser from charging aperture 3, under the suction function producing at hollow rotary drum 5 centers of rotation, oil phase feed liquid constantly declines, and along with the increase of rotating speed, the negative pressure producing increases, and the degree of depth that oil phase feed liquid declines also increases thereupon.When rotating speed increase makes pressure reach certain value, the oil phase feed liquid in hollow rotating shaft 4 enters into the hollow rotary drum 5 of the first order, and meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 of the first order enters into water from first order discharging opening 6; The oil droplet of water coalescence under the stopping of first order outer cover 7 is oil phase, from the charging aperture of second level liquid phase disperser, enter hollow rotating shaft 4, under the suction function producing at hollow rotary drum 5 centers, the second level of rotation, feed liquid in hollow rotating shaft enters into the hollow rotary drum 5 in the second level, meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 in the second level enters into water from second level discharging opening 6; The oil droplet of water under the stopping of second level outer cover 7 again coalescence be oil phase, from the charging aperture of third level liquid phase disperser, enter hollow rotating shaft, under the suction function producing at the hollow rotary drum of the third level 5 centers of rotation, oil phase feed liquid in hollow rotating shaft 4 enters into the hollow rotary drum 5 of the third level, meanwhile, the oil phase feed liquid that enters into the hollow rotary drum 5 of the third level enters into water from third level discharging opening 6.Take this principle as basis, can carry out the self-priming extracting operation of N (N > 3) level.
The cooperation of the direction arranging by the series connection of single-stage liquid phase disperser and the channel exit of liquid phase disperser outer cover 7 down, make hollow rotary drum 5 discharging openings 6 of upper level oil phase drop (oil droplet) out, not directly along water, to rise to oil phase layer, but under the cooperation of outer cover, enter the charging aperture of the hollow rotating shaft 4 of next stage liquid phase disperser, thus further operation.This just makes it when reaching similarly dispersion effect, and rotating speed is reduced greatly.
Embodiment mono-
Organic phase is kerosene, and in kerosene, to add developer, water be deionized water, and the ratio of organic phase and water is 1: 10.The light phase intake port of this low rotating speed self-priming extraction equipment is 5mm, and is located at the relative position of cavity rotating shaft, take oil phase as decentralized photo, and rotating shaft cavity diameter is 6mm, rotary drum cavity diameter 30mm, and it is relative to be provided with 12 positions, the aperture that diameter is 4mm.Reach similarly dispersion effect, the required rotating speed of single-stage and self-priming extraction equipment is 500rpm, and the required rotating speed of low rotating speed self-priming extraction equipment is 170rpm.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.

Claims (4)

1. a low rotating speed self-priming extraction equipment, described extraction equipment comprises at least 2 grades of single-stage liquid phase disperser; Described every grade of single-stage liquid phase disperser includes hollow rotating shaft (4) and hollow rotary drum (5), on the top axial wall (2) of described hollow rotating shaft (4), there is charging aperture (3), hollow rotating shaft (4) end is communicated with hollow rotary drum (5), and the sidewall of hollow rotary drum (5) has discharging opening (6); The hollow rotating shaft (4) of the single-stage liquid phase disperser of the upper level of extractor is connected with rotating shaft (1), and rotating shaft (1) is connected with motor, and all the other hollow rotating shafts at different levels (4) are all connected with the hollow rotary drum of upper level (5); Between each single-stage disperser, by physics, do not communicate; The channel exit of every grade of liquid phase disperser is provided with direction outer cover (7) down, and the channel exit of bottommost one-level liquid phase disperser dispenses described outer cover (7).
2. low rotating speed self-priming extraction equipment as claimed in claim 1, described extraction equipment comprises 2~6 grades of single-stage liquid phase disperser.
3. low rotating speed self-priming extraction equipment as claimed in claim 1 or 2, is characterized in that, the lower edge of described outer cover is lower than the lower edge of the charging aperture of next stage.
4. low rotating speed self-priming extraction equipment as claimed in claim 2, is characterized in that, described extraction equipment comprises 2 grades, 3 grades or 4 grades of single-stage liquid phase disperser.
CN201110280248.4A 2011-09-20 2011-09-20 Low rotating speed self-priming extraction equipment Expired - Fee Related CN102430264B (en)

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CN108452551B (en) * 2018-01-30 2020-11-03 中国科学院过程工程研究所 Device for uniformly distributing fluid and processing method and application thereof

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