CN1132651C - Self-absorption multichannel phase dispersing extractor - Google Patents
Self-absorption multichannel phase dispersing extractor Download PDFInfo
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- CN1132651C CN1132651C CN00105691A CN00105691A CN1132651C CN 1132651 C CN1132651 C CN 1132651C CN 00105691 A CN00105691 A CN 00105691A CN 00105691 A CN00105691 A CN 00105691A CN 1132651 C CN1132651 C CN 1132651C
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Abstract
The present invention relates to a self-absorption type multichannel phase dispersing extraction device. A hollow rotating shaft and a liquid phase disperser are arranged in an extraction tank, wherein the shaft wall of the hollow rotating shaft is provided with a material inlet; the liquid phase disperser is fixed in the middle of the rotating shaft or is fixed at the bottom end of the rotating shaft. The rotating shaft is connected with a motor. The liquid phase disperser is a hollow cylinder body of which one side wall is provided with a material outlet. The cavity is communicated with a cavity of the rotating shaft. One, two or a plurality of sleeve barrels are fixed arranged on the upper part or the lower part of a liquid phase disperser the negative pressure can be generated at low rotation speed, the light phase / or the heavy phase is uniformly dispersed in the other phase, and the emulsion phenomenon is avoided. The multichannel phase dispersing extraction device can continuously operate under the condition of vivid two-phase interfaces, and solve the problem of difficult phase separation of mixed solvents.
Description
The present invention relates to the extraction equipment of solvent in medicine, the biological chemical field, particularly a kind of self-absorption multichannel phase dispersing extractor.
In metallurgy, oil, pharmacy, food industry, emulsion is to compare distinct issues in the extraction process.Because living things system is all very sensitive to soda acid, organic solvent and mechanical shear stress etc., adopt the violent extraction mode of mixing of common stirring arm to be easy to cause inactivation and decomposition.In the separation and purification of biological product, emulsion is more outstanding.Such as: contain a large amount of protein and sugar etc. in the antibiotic zymotic fluid, protein molecule is easy to sex change in the organic solvent extraction process.If adopt common alr mode to mix, speed is too low can not finish extraction process, and high speed shear is broken and is produced a large amount of emulsion granular boundaries and can adsorb the protein of a large amount of sex change, forms firm interfacial film even protein cross structure, makes emulsion become highly stable.The formation of emulsion is very unfavorable for extraction process.Emulsification causes the useless zymotic fluid of raffinate to carry solvent secretly, reduces product yield.Simultaneously, carry zymotic fluid in the organic facies secretly and also cause difficulty to recycling.
For example: solvent extraction extracting penicillin from zymotic fluid has the history in year surplus in the of 50, but its extraction process does not have to change substantially: used extraction equipment adopts drum-type centrifugal extractor and decanter at present mostly, used extractant mainly is acetate fourth (a penta) ester, methylisobutylketone etc.The extracting operation condition is: pH1.8-2.2, and organic facies and water volume ratio O/A=1/2, O/A=2/1 is compared in back extraction pH6.7～7.2.Following two characteristics are arranged in its extraction process: 1, penicillin is easily destroyed, and is more stable relatively in pH4～8 scopes, in pH＜4 or pH＞8 all easily decompose.At pH2.0, under 10 ℃, the half-life of penicillin is 1.3 hours, and extraction will be finished in very short time.2, contain a large amount of protein, organic pigment and other biological byproduct owing in the zymotic fluid, so emulsification is serious in the extraction process.
The composition of one extracting penicillin is disclosed among the Chinese invention patent ZL 89103178, promptly in butyl acetate, add neutral phosphor (seeing) class or sulfoxide compound, make itself and butyl acetate form mixed extractant solvent penicillin, can make operating condition bring up to 3.0～3.5 from pH1.8～2.2, yield improves 3%.But this technology does not change on extraction equipment, and the effect that this method is obtained in actual applications is not fairly obvious.
The emulsification problem that Centrifugical extraction solves the bout solvent is carried out in industrial common employing at present centrifugal extractor efficiently, but these equipment investments are bigger, and adopts centrifugal way also to be difficult to emulsification is eliminated, and must use demulsifier in its technical process.With the North China Pharmaceutical Factory is example, and in the annual penicillin production technology, the annual demulsifier consumption that needs just reaches more than 1,000,000 yuan." liquid-liquid extraction process and equipment " (Atomic Energy Press,, Fei Weiyang etc. in 1993) 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 a complex structure, manufacturing, operation and maintenance costs are than higher, for quick stirring, shearing force causes more serious emulsion than Da Yi in addition.The formula of drenching with rain extractor is a kind of horizontal continuous extraction device, be suitable for handling usually emulsification easily and contain the material of solid particle, but that shortcoming is a rotating speed is slow that mass transfer rate is low, and is lower than loading.
The applicant has applied for a kind of " mutually light or heavy phase disperses low subtracting to cut self-priming stirring extraction device and method of operating " (application number is 00102749.2) on February 22nd, 2000, this application has disclosed a kind of self-priming stirring extraction device, its structure is: the hollow shaft of band charging aperture on the axial wall is installed in the extractor jar and is fixedly installed in the middle part of the hollow shaft or the hollow rotary drum of bottom, hollow shaft links to each other with motor, motor drives hollow shaft rotation, hollow rotary drum is the hollow cylinder that a sidewall is provided with discharging opening, and its cavity is connected with the cavity of hollow shaft.This device is owing to belong to the single channel extraction equipment, and when disperseing mutually, it is long to reach balance time, causes phenomenons such as biological substance inactivation, emulsification sex change easily.
The object of the invention is: a kind of self-absorption multichannel phase dispersing extractor is provided, can solve the problem of the difficulty that is separated in mixed extractant solvent (such as the extraction of the penicillin) technology effectively, can effectively avoid emulsion, and this equipment investment is little, easy to operate, is applicable to the extraction process of mixed solvent of the easy emulsification of biochemical industry, hydrometallurgy, pharmaceuticals industry, petrochemical industry, oil prodution industry, food industry etc.
Embodiment of the present invention are as follows:
Self-absorption multichannel phase dispersing extractor provided by the invention, the hollow rotating shaft of band charging aperture on the axial wall is installed in the extractor jar and is fixedly installed in the middle part of the hollow rotating shaft or the liquid phase disperser of bottom, hollow rotating shaft links to each other with CD-ROM drive motor, the rotation of drive motor hollow rotating shaft, liquid phase disperser is the hollow cylinder that a sidewall is provided with discharging opening, the cavity of its hollow cylinder is connected with the cavity of hollow rotating shaft, it is characterized in that: fixed installation is one above or below the described liquid phase disperser, two or more are concentric with hollow rotating shaft, uncovered sleeve up or down, form internal channel between hollow rotating shaft and inner sleeve, internal channel is by being located at discharging opening and the extractor intracavity inter-connection on the outer sleeve sidewall; Form outer tunnel between inner sleeve and the outer sleeve, outer tunnel is by being located at discharging opening and the extractor intracavity inter-connection on the outer sleeve sidewall; Liquid phase disperser is combined by a uncovered rotating cylinder down and the chassis that is threadedly connected to the rotating cylinder bottom.
Self-absorption multichannel phase dispersing extractor provided by the invention has following advantage:
Self-absorption multichannel phase dispersing extractor provided by the invention solved effectively be separated in mixed extractant solvent (such as the extraction of the penicillin) technology difficulty problem, can effectively avoid emulsion, two and this equipment investment little, easy to operate; It is low that the work drive motor rotating speed requires, and not only power consumption is low, the more important thing is also lowly to the shearing force of solution than the separation under the slow-speed of revolution, helps the maintenance of biological substance activity such as protein.This device can be used for interrupted extraction operation and continuous extraction operation, and the scope of application is big.Especially for the continuous extraction process, can save defecator, significantly reduce the hold-up of material and solvent, reduce occupation area of equipment, thereby reduce the production cost of extraction process greatly.The present invention is applicable to the extraction process of mixed solvent of the easy emulsification of biochemical industry, hydrometallurgy, pharmaceuticals industry, petrochemical industry, oil prodution industry, food industry etc.
Further describe the present invention below in conjunction with drawings and Examples:
Accompanying drawing 1 is the schematic diagram that is used for the light self-priming single channel extraction equipment that disperses mutually of prior art;
Accompanying drawing 2 is the schematic diagram of the self-priming single channel extraction equipment that is used for the heavy phase dispersion of prior art;
Accompanying drawing 3 is used for the schematic diagram of the light self-absorption multichannel phase dispersing extractor that disperses mutually for the present invention;
Accompanying drawing 5 is the structural representation of liquid phase disperser:
Wherein: hollow rotating shaft 1 rotating cylinder 2 charging apertures 3
Discharging opening 4,5,6 inner sleeves 7 extractors 8
Chassis 21
The extraction yield of--expression when gently disperseing the single channel extraction equipment to extract mutually
The extraction yield of-▲-expression when gently disperseing the multichannel extraction equipment to extract mutually
Extraction yield when--expression disperses the single channel extraction equipment to extract with heavy phase
Extraction yield when-△-expression disperses the multichannel extraction equipment to extract with heavy phase
Fig. 1 is the structural representation that is used for the light self-priming single channel phase dispersing extractor that disperses mutually of prior art.As seen from the figure, the hollow rotating shaft 1 that axial wall is provided with charging aperture 3 is connected with the CD-ROM drive motor (not shown), 1 rotation of drive motor hollow rotating shaft, the bottom fixed installation liquid phase disperser of hollow rotating shaft 1, liquid phase disperser is the hollow cylinder that a sidewall is provided with discharging opening 4, and the cavity of its hollow cylinder is connected with the cavity of hollow rotating shaft 1.During work, self-priming single channel phase dispersing extractor is placed in the extractor 8, and liquid phase disperser is positioned at the bottom of extractor 8.The liquid phase disperser rotation that hollow rotating shaft 1 drives with certain rotating speed under the drive of CD-ROM drive motor, produce negative pressure at discharge opening 4 places, the light hollow passageway on upper strata along hollow rotating shaft 1 flow downward arrive the back, bottom by discharging opening 4 will organic light phase uniformly dispersing following mutually in.Light phase drop contacts and realizes mass transfer at uphill process with the heavy phase feed liquid.Light phase drop arrives the interface coalescence, enters light phase feed liquid then.Reach the mixing of two-phase up and down by above-mentioned process and finish the extracting operation process.But because this device belongs to the single channel extraction equipment, when disperseing mutually, it is long to reach balance time, causes phenomenons such as biological substance inactivation, emulsification sex change easily.
Fig. 3 is used for the schematic diagram of the light self-absorption multichannel extraction equipment that disperses mutually for the present invention, as seen from the figure, be actually on the basis of Fig. 1, installed with hollow rotating shaft 1 concentric in the upper fixed of liquid phase disperser, and uncovered inner sleeve that makes progress 7 and outer sleeve 9 are (certainly, sleeve also can be one, three, five or more, can require to decide according to the size and the extraction of liquid phase disperser in the extraction equipment), thereby the multichannel self-absorption multichannel phase dispersing extractor that constitutes, the internal channel 71 that between hollow rotating shaft 1 and inner sleeve 7, forms, internal channel 71 is connected by discharging opening 5 and the extractor 8 that is located on outer sleeve 9 sidewalls; Form outer tunnel 91 between inner sleeve 7 and the outer sleeve 9, outer tunnel 91 is connected by discharging opening 6 and the extractor 8 that is located on outer sleeve 9 sidewalls.During work, the liquid phase disperser rotation that hollow rotating shaft 1 drives with certain rotating speed under the drive of CD-ROM drive motor produces negative pressure simultaneously at charging aperture 3 and internal channel 71 and outer tunnel 91, makes the feeding-passage that gently hands down arrive discharging opening 4,5,6 respectively.Gently evenly spread in the heavy phase mutually.Light phase drop contacts and realizes mass transfer at uphill process with the heavy phase feed liquid.Light phase drop arrives the interface coalescence, enters light phase feed liquid then.Reach the mixing of two-phase up and down by above-mentioned process and finish the extracting operation process.
The self-priming single channel phase dispersing extractor that is used for light dispersion mutually of comparison diagram 1 and extraction and the emulsification situation that is used for the light self-absorption multichannel phase dispersing extractor that disperses mutually of the present invention.
With organic facies is the butyl acetate solution of 40ml 5.7% (wt%) tributylphosphine oxide (TBPO), and water is that 80ml contains the 1mg/ml lactalbumin, and the benzylpenicillin potassium saline solution of 0.05M places the graduated cylinder of 250ml.With self-priming single channel phase dispersing extractor shown in Figure 1 and self-priming single channel phase dispersing extractor shown in Figure 3 this system is extracted respectively.H with 10%
2SO
4Regulating pH is 4.And fixed rotating speed is 600 commentaries on classics.Immediately measure the variation of the concentration of penicillin in the organic facies with automatic polarimeter.If emulsification then with measuring after the centrifuge phase-splitting.Extraction yield relatively see Fig. 6.The emulsification situation sees Table 1.
Fig. 2 is the structural representation of the self-priming single channel phase dispersing extractor that is used for the heavy phase dispersion of prior art.As seen from the figure, hollow rotating shaft 1 is connected with the CD-ROM drive motor (not shown), 1 rotation of drive motor hollow rotating shaft, the middle part fixed installation liquid phase disperser of hollow rotating shaft 1, liquid phase disperser is the hollow cylinder that a sidewall is provided with discharging opening 4, and the cavity of its hollow cylinder is connected with the cavity of hollow rotating shaft 1.During work, self-priming single channel phase dispersion extractor is placed in the extractor 8, and liquid phase disperser is positioned at the middle part of extractor 8.The liquid phase disperser rotation that hollow rotating shaft 1 drives with certain rotating speed under the drive of CD-ROM drive motor, produce certain negative pressure at discharging opening 4 places, during the heavy phase of lower floor is dispersed in the heavy phase uniform particles mutually by discharging opening 4 behind the upwards mobile arrival of the hollow passageway top of hollow rotating shaft 1.Heavy-phase liquid drops in decline process and light contact of feed liquid mutually and realization mass transfer.Heavy-phase liquid drips to and reaches the interface coalescence, enters the heavy phase feed liquid then.Reach the mixing of two-phase up and down by above-mentioned process and finish the extracting operation process.But because this device belongs to the single channel extraction equipment, when disperseing mutually, it is long to reach balance time, causes phenomenons such as biological substance inactivation, emulsification sex change easily.
Fig. 4 is used for the structural representation of the self-absorption multichannel phase dispersing extractor of heavy phase dispersion for the present invention, as seen from the figure, be actually on the basis of Fig. 2, below liquid phase disperser, fixedly mounted with hollow rotating shaft 1 concentric, and uncovered downward inner sleeve 7 and outer sleeve 9 are (certainly, sleeve also can be one, three, five or more, can require to decide according to the size and the extraction of liquid phase disperser in the extraction equipment), thereby the multichannel self-absorption multichannel phase dispersing extractor that constitutes, the internal channel 71 that between hollow rotating shaft 1 and inner sleeve 7, forms, internal channel 71 is connected by discharging opening 5 and the extractor 8 that is located on outer sleeve 9 sidewalls, form outer tunnel 91 between inner sleeve 7 and the outer sleeve 9, outer tunnel 91 is connected by discharging opening 6 and the extractor 8 that is located on outer sleeve 9 sidewalls.The liquid phase disperser of present embodiment is actually by the rotating cylinder 2 of mouth down to be formed with the chassis 7 that is threaded in rotating cylinder 2 bottoms.During work, the liquid phase disperser rotation that hollow rotating shaft 1 drives with certain rotating speed under the drive of CD-ROM drive motor, charging aperture 3 (the lower end mouth of pipe of hollow rotating shaft 1 is as charging aperture 3) is located to produce negative pressure simultaneously with internal channel 71 and outer tunnel 91, makes heavy phase arrive discharging opening 4,5,6 respectively along the feeding-passage passage.During heavy phase evenly spreads to gently mutually.Reach the mixing of two-phase up and down by said process and finish the extracting operation process.Heavy-phase liquid drops in decline process and light contact of feed liquid mutually and realization mass transfer.Heavy-phase liquid drips to and reaches the interface coalescence, enters the heavy phase feed liquid then.
The extraction and the emulsification situation of the self-priming single channel phase dispersing extractor that is used for the heavy phase dispersion of comparison diagram 2 and the self-absorption multichannel phase dispersing extractor that is used for the heavy phase dispersion of Fig. 4.
With organic facies is the butyl acetate solution of 40ml5.7% (wt%) tributylphosphine oxide (TBPO), and water is that 80ml contains the 1mg/ml lactalbumin, and the benzylpenicillin potassium saline solution of 0.05M places the graduated cylinder of 250ml.With self-priming single channel phase dispersing extractor shown in Figure 2 and self-absorption multichannel phase dispersing extractor shown in Figure 4 this system is extracted respectively.H with 10%
2SO
4Regulating pH is 4.And fixed rotating speed is 600 commentaries on classics.Immediately measure the variation of the concentration of penicillin in the organic facies with automatic polarimeter.If emulsification then with measuring after the centrifuge phase-splitting.Extraction yield relatively see Fig. 7.The emulsification situation sees Table 1.Table 1: the extraction equilibrium and the emulsification situation table of comparisons
| The extraction equipment type | Rotating speed (rev/min) | Reach the extraction the needed time in a basic balance (minute) | Emulsification and phase-splitting situation |
| The light phase dispersion extraction of self-priming single channel | 600 | 9 | But leave standstill phase-splitting, but boundary layer some is fuzzy |
| The light phase dispersion extraction of self-priming triple channel | 300 | 88 (pharmacy group in North China doubly reaches company, penicillin fermentation filtrate) | Leave standstill in 10 seconds, phase-splitting was left standstill in 10 seconds fully, phase-splitting fully |
| 600 | 2 | Left standstill phase-splitting fully 25 seconds | |
| 2 (pharmacy group in North China doubly reaches company, penicillin fermentation filtrate) 1 (no albumen) | Slightly emulsification, centrifugal can not emulsification of phase-splitting | ||
| Self-priming single channel heavy phase dispersion extraction | 600 | 12 | Emulsification takes place, and needs centrifugal phase-splitting |
| Self-priming triple channel heavy phase dispersion extraction | 600 | 3.5 1.5 (no albumen) | Left standstill 21 seconds, fully not emulsification of phase-splitting |
As seen from the above table: to same 1mg/ml lactalbumin, when the benzylpenicillin potassium saline solution of 0.05M extracts.When rotating speed was 600 commentaries on classics, the light phase dispersion extraction of self-priming single channel need just reach balance in 9 minutes.And boundary layer some is fuzzy, this is the product of protein denaturation.The light phase dispersion extraction of self-priming triple channel only needed 2 minutes can reach balance, 25 interior phase-splittings fully.Even when 300 change, also can reach balance in 8 minutes, leave standstill and got final product complete phase-splitting in 10 seconds.When rotating speed was 600 commentaries on classics, self-priming single channel heavy phase phase dispersion extraction needed 12 minutes reach balance, needed the phase-splitting of centrifugal ability.Self-priming triple channel heavy phase phase dispersion extraction only needs 3.5 minutes.Emulsification does not take place, and leaves standstill phase-splitting fully in 21 seconds.As seen adopt the multichannel extraction to strengthen the mass transfer flux effectively, shortened the needed time of balance that reaches widely, the sex change emulsification that can alleviate biological substances such as protein significantly.
Claims (3)
1. self-absorption multichannel phase dispersing extractor, the hollow rotating shaft of band charging aperture on the axial wall is installed in the extractor jar with one heart and is fixedly connected in the middle part of the hollow rotating shaft or the liquid phase disperser of bottom, hollow rotating shaft links to each other with CD-ROM drive motor, the rotation of drive motor hollow rotating shaft, liquid phase disperser is the hollow cylinder that a sidewall is provided with discharging opening, the cavity of its hollow cylinder is connected with the cavity of hollow rotating shaft, it is characterized in that: can fixedly mount one on the described liquid phase disperser, two or more are concentric with hollow rotating shaft, and the uncovered sleeve that makes progress, the internal channel that forms between hollow rotating shaft and the inner sleeve, internal channel is connected by discharging opening and the extractor that is located on the outer sleeve sidewall, form outer tunnel between inner sleeve and the outer sleeve, outer tunnel is connected by discharging opening and the extractor that is located on the outer sleeve sidewall.
2. by the described self-absorption multichannel phase dispersing extractor of claim 1, it is characterized in that: one of the below of described liquid phase disperser fixed installation, two or more are concentric with hollow rotating shaft, and uncovered downward sleeve, the internal channel that between hollow rotating shaft and inner sleeve, forms, internal channel is connected by discharging opening and the extractor that is located on the outer sleeve sidewall, form outer tunnel between inner sleeve and the outer sleeve, outer tunnel is connected by discharging opening and the extractor that is located on the outer sleeve sidewall.
3. by claim 1 or 2 described self-absorption multichannel phase dispersing extractors, it is characterized in that: liquid phase disperser is combined by a uncovered rotating cylinder down and the chassis that is threadedly connected to the rotating cylinder bottom.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00105691A CN1132651C (en) | 2000-04-14 | 2000-04-14 | Self-absorption multichannel phase dispersing extractor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN00105691A CN1132651C (en) | 2000-04-14 | 2000-04-14 | Self-absorption multichannel phase dispersing extractor |
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| CN1318422A CN1318422A (en) | 2001-10-24 |
| CN1132651C true CN1132651C (en) | 2003-12-31 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862549B (en) * | 2010-06-08 | 2014-12-24 | 中国科学院过程工程研究所 | Clarifying chamber-free continuous extracting device of large-phase ratio easy emulsifying system and operating method |
| CN102284192B (en) * | 2011-06-16 | 2013-06-12 | 北京科技大学 | Equipment and process for performing continuous back extraction on penicillin through parallel flow and reverse flow coupling |
| CN102772913B (en) * | 2012-07-16 | 2014-12-24 | 中国科学院过程工程研究所 | Column type extraction device for pipe bundle multi-channel phase-dispersing and extraction method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2174245Y (en) * | 1993-12-11 | 1994-08-17 | 浙江大学 | Fast-acting continuous extracting device for tea polyphenols |
| CN1200051A (en) * | 1995-10-19 | 1998-11-25 | 拜尔公司 | Multiple phase extractor |
| CN1235855A (en) * | 1999-04-29 | 1999-11-24 | 清华大学 | Rotary-disc extracting tower provided with interstage rotary baffle plate |
-
2000
- 2000-04-14 CN CN00105691A patent/CN1132651C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2174245Y (en) * | 1993-12-11 | 1994-08-17 | 浙江大学 | Fast-acting continuous extracting device for tea polyphenols |
| CN1200051A (en) * | 1995-10-19 | 1998-11-25 | 拜尔公司 | Multiple phase extractor |
| CN1235855A (en) * | 1999-04-29 | 1999-11-24 | 清华大学 | Rotary-disc extracting tower provided with interstage rotary baffle plate |
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