CN102234617B - Method for separating and collecting microalgae by using magnetic medium - Google Patents
Method for separating and collecting microalgae by using magnetic medium Download PDFInfo
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- CN102234617B CN102234617B CN2010101719038A CN201010171903A CN102234617B CN 102234617 B CN102234617 B CN 102234617B CN 2010101719038 A CN2010101719038 A CN 2010101719038A CN 201010171903 A CN201010171903 A CN 201010171903A CN 102234617 B CN102234617 B CN 102234617B
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Abstract
The invention belongs to the field of microalgae separation, and in particular relates to a method for separating and collecting microalgae by using a magnetic medium. The method comprises the following steps: (1) preparing Fe3O4 nano particles and dispersing the Fe3O4 nano particles so as to form a stable suspension; (2) regulating the pH value of a microalgae culture liquid to 8-10; (3) adding a magnetic separation medium obtained in the step (1) and stirring, wherein the use amount of the magnetic separation medium is 0.01-0.04% (w/v); and (4) carrying out magnetic separation on the microalgae obtained in the step (3), and collecting the microalgae obtained by separation. According to the invention, the method using the magnetic separation medium has simple synthesis steps and is easy to amplify; the use amount of the magnetic separation medium is less; and stirring time is short, efficiency is high, separation operation process is simple, and the magnetic separation medium can be repeatedly used, thereby being beneficial to reduction of production cost.
Description
Technical field
The invention belongs to little algae separation field, particularly, the present invention relates to a kind of method that adopts magnetic medium to separate, collect little algae.
Background technology
Little algae is cultivated and has been widely used in fields such as mariculture, food, pharmacy and the energy, cultivates extensive one of the principal element of amplifying yet separation of little algae and collection become the little algae of restriction.The separation of present little algae and the method for collection mainly comprise: centrifugal, filtration, flocculation, air supporting.Adopt centrifugal method to need expensive fixed capital (whizzer) investment and energy consumption big; Adopt the efficient of filter method low, the film easy blocking, operation easier is big; The employing flucculation process separates and collects little algae and need use various magnetic resolution media, and magnetic resolution medium and little algae separation difficulty cause the pollution of title product easily; Dissolved air flotation needs the auxiliary of magnetic resolution medium or tensio-active agent usually when in little algae, using, exist the problem same with flucculation process.
Because magneticsubstance has the separation of being easy to, lock out operation characteristic of simple, in recent years, adopted magneticsubstance to carry out the existing report of the isolating method of little algae.Gao and Peng etc. adopt the mixture of smectite and copper ferriferous oxide, and from water, separating of success is harmful to little algae microcystic aeruginosa (Microcystis aeruginosa), and its magnetic resolution medium can be reused; But synthetic comparatively loaded down with trivial details and large usage quantity (Gao Z.W., Peng X.J., the Zhang H.M. of this magnetic composite; Luan Z.K., Fan B.Desalination, 2009; 247,337); Liu and Li etc. adopt chitosan-modified magnetic polymer as the magnetic resolution medium, successfully remove the algal tufa in the fresh water, but its magnetic resolution medium is synthetic comparatively complicated; The magnetic resolution medium can't be reused; Receive ionic strength affect big (Liu D., Li F.T., Zhang B.R.Water Sci.Technol.2009; 59,1085).This shows; Adopt existing magneticsubstance to carry out the separated and collected of little algae, its material is synthetic complicated, and toward contact need modification or encapsulate polymkeric substance with the frustule coupling; This has greatly increased cost; Therefore, the large-scale application difficulty is bigger, and it separates the little algae of nutrient solution system and does not obtain the checking of testing as yet.
Summary of the invention
The object of the present invention is to provide a kind of is efficiently little fast algae separation, the collection method of magnetic resolution medium with the magnetic nanoparticle.
The present invention is with Fe
3O
4Nano particle is the magnetic resolution medium, after little algae cultivation end back adds this magnetic resolution medium, reaches thorough mixing through stirring, adopts permanent magnet to realize magnetic resolution and the collection of little algae.
Method according to employing magnetic medium separation of the present invention, the little algae of collection said method comprising the steps of:
(1) preparation Fe
3O
4Nano particle makes it disperse to form steady suspension, and it is subsequent use to obtain the magnetic resolution medium;
(2) the pH value of adjusting micro algae culturing liquid is 8-10, and in this pH scope, frustule is positively charged, thereby can combine through charge effect power with magnetic medium;
(3) add the magnetic resolution medium that step (1) obtains, the consumption of magnetic resolution medium is 0.01-0.04%w/v, and stirs;
(4) the little algae that obtains in the step (3) is carried out magnetic and separate, remove supernatant liquid, collect and separate the little algae that obtains, wherein Fe
3O
4Nanometer can with the microalgae cell surface bonding, also can get in little algae, combine with it.
Preferably, according to the method for the invention, in step (2), said micro algae culturing liquid is inserted in the stirred reactor, the temperature of regulating in the stirred reactor is 20-35 ℃, and churning time is 1-3 minute, the too short then Fe of churning time
3O
4Nanometer can't fully combine with microalgae cell, and the oversize meeting of churning time causes the Fe of churned mechanically shearing force with surface bonding
3O
4Nanometer and microalgae cell are broken up again, and these all can reduce the separating effect of little algae.
Preferably, according to the method for employing magnetic medium separation of the present invention, the little algae of collection, wherein, in step (4), it is the 1000-3000 oersted that little algae carries out selecting magneticstrength for use when magnetic separates.
The method of separating, collecting little algae according to employing magnetic medium of the present invention; Wherein, Little algae that step (4) is collected carries out the extraction of purpose meta-bolites; The little algae residue that contains the magnetic resolution medium that obtains after the separation is calcined under high temperature 200-400 ℃ nitrogen atmosphere and was removed cell residue in 1-2 hour, reclaims to obtain Fe
3O
4Nano particle is reused for the separated and collected of little algae.
According to the employing magnetic medium separate, collect the method for little algae, Fe
3O
4The concentration of nano granule suspension is 1-5%w/v, preferred 2%w/v.The too rare addition that can increase nano granule suspension in little algae culture system of suspension concentration can cause microalgae cell concentration diluted, reduces the separating effect of little algae; Suspension concentration is too high to have increased the probability of collision of nano particle in the suspension-s, causes nano particle to take place to reunite and finally precipitate, and suspension-s is difficult for preservation, the separating effect decline of little algae.
Therefore, preferably, the method for separating, collecting little algae according to employing magnetic medium of the present invention may further comprise the steps:
(1) adopts existing literature reported method (Peng Z.G., Hidajat K., Uddin M.S., J.ColloidInterface Sci., 2004,271,277) preparation Fe
3O
4Nano particle is scattered in the deionized water it through ultrasonic, forms steady suspension, promptly obtains the magnetic resolution medium, puts into refrigerator and cooled then and hides subsequent use;
(2) will cultivate the micro algae culturing liquid that obtains and insert in the stirred reactor, the temperature of regulating in the stirred reactor is 20-30 ℃, pH value 8-10;
(3) under the rotating speed of 100-300rpm, add the magnetic resolution medium that step (1) obtains, the little algae in the nutrient solution is separated, the consumption of magnetic resolution medium is 0.01-0.04% (w/v), churning time is 1-3 minute;
Said magnetic resolution medium is for being solution shape, Fe
3O
4Nano particle is the effective constituent of this magnetic resolution medium, in solution, is uniformly dispersed, and concentration is controlled at 1-5% (w/v), makes it in the process of refrigerator preservation, still keep high reactivity, and its preferred value is 2% (w/v);
(4) selecting magneticstrength for use is that the permanent magnet of 1000-3000 oersted is positioned over reactor bottom, the little algae in the step (3) is carried out magnetic separate, and leaving standstill the magnetic separation time is 1-3 minute, removes supernatant liquid at last, collects and separates the microalgae cell that obtains;
(5) microalgae cell of step (4) being collected (containing the magnetic resolution medium) carries out the extraction of purpose meta-bolites; The microalgae cell residue that obtains after the separation (containing the magnetic resolution medium) is calcined under high temperature 200-400 ℃ nitrogen atmosphere and was removed little algae residue in 1-2 hour; Temperature rise rate 2-5 ℃/minute, the Fe of recovery
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, use power 200-400w again supersound process 10-30 minute, is mixed with the separated and collected that the magnetic resolution medium is reused for little algae with deionized water.
Processing such as the microalgae cell of collecting in the said step (5) (magnetic resolution medium) can not extract are according to the actual requirements yet directly calcined and subsequent disposal according to the condition in the step (5), realize the repeated use of magnetic resolution medium.
Of the present invention is that the microalgae cell separation of magnetic resolution medium, the advantage of collection method are with the magnetic nanoparticle:
(1) synthesis step of magnetic resolution medium is simple, is easy to amplify;
(2) because the specific surface area of magnetic nanoparticle is big, magnetic resolution medium consumption is little;
(3) churning time is short, and efficient is high, and sepn process is simple to operate;
(4) the magnetic resolution medium is reusable, helps reducing production costs.
Description of drawings
The transmission electron microscope TEM photo of the grape algae that Fig. 1 obtains after this separates for the embodiment of the invention 1.
Fig. 2 be in the embodiment of the invention 1 churning time to the influence of grape algae separating effect.
Embodiment
Embodiment 1
With the grape algae in the method separated and collected grape algae culturing liquid of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 2% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the grape algae culturing liquid that obtains, the temperature of regulating in the stirred reactor is 20 ℃, and pH value 8 adds the magnetic resolution medium under the rotating speed of 100rpm, and the consumption of magnetic resolution medium is 0.04% (w/v), and churning time is 1 minute; Selecting magneticstrength for use is that the permanent magnet of 1000 oersteds is positioned over reactor bottom, the grape algae is carried out magnetic separate, and leaves standstill 1 minute, removes supernatant liquid, collects and separates the grape algae that obtains, and the recovery of grape algae reaches 99.8%.After the grape algae (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction, separate the grape algae residue (containing the magnetic resolution medium) that obtains and under the nitrogen atmosphere of 200 ℃ of high temperature, calcine and removed microalgae cell residue, 2 ℃/minute of temperature rise rates, the Fe of recovery in 2 hours
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 30 minutes of power 200w again, is mixed with the separated and collected that the magnetic resolution medium is reused for the grape algae with deionized water.The transmission electron microscope TEM photo of the grape algae that obtains after the separation is as shown in Figure 1, and churning time is as shown in Figure 2 to the influence of grape algae separating effect.
Embodiment 2
With the grape algae in the method separated and collected grape algae culturing liquid of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 1% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the grape algae culturing liquid that obtains, the temperature of regulating in the stirred reactor is 30 ℃, and pH value 10 adds the magnetic resolution medium under the rotating speed of 300rpm, and the consumption of magnetic resolution medium is 0.02% (w/v), and churning time is 2 minutes; Selecting magneticstrength for use is that the permanent magnet of 2000 oersteds is positioned over reactor bottom, the grape algae is carried out magnetic separate, and leaves standstill 2 minutes, removes supernatant liquid, collects and separates the grape algae that obtains, and the recovery of grape algae reaches 97.5%.After the grape algae (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction, separate the grape algae residue (containing the magnetic resolution medium) that obtains and under the nitrogen atmosphere of 400 ℃ of high temperature, calcine and removed microalgae cell residue, 5 ℃/minute of temperature rise rates, the Fe of recovery in 1 hour
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 10 minutes of power 400w again, is mixed with the separated and collected that the magnetic resolution medium is reused for the grape algae with deionized water.
With the grape algae in the method separated and collected grape algae culturing liquid of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 5% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the grape algae culturing liquid that obtains, the temperature of regulating in the stirred reactor is 25 ℃, and pH value 9 adds the magnetic resolution medium under the rotating speed of 200rpm, and the consumption of magnetic resolution medium is 0.01% (w/v), and churning time is 3 minutes; Selecting magneticstrength for use is that the permanent magnet of 3000 oersteds is positioned over reactor bottom, the grape algae is carried out magnetic separate, and leaves standstill 3 minutes, removes supernatant liquid at last, collects and separates the grape algae that obtains, and the recovery of grape algae reaches 98.6%.After the grape algae (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction; The grape algae residue (containing the magnetic resolution medium) that separation obtains is calcined under the nitrogen atmosphere of 300 ℃ of high temperature and was removed the microalgae cell residue in 1.5 hours; 3 ℃/minute of temperature rise rates, the Fe of recovery
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 20 minutes of power 300w again, is mixed with the separated and collected that the magnetic resolution medium is reused for the grape algae with deionized water.
Embodiment 4
With the chlorella in the method separated and collected chlorella nutrient solution of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 2% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the chlorella nutrient solution that obtains, the temperature of regulating in the stirred reactor is 25 ℃, and pH value 10 adds the magnetic resolution medium under the rotating speed of 300rpm, and the consumption of magnetic resolution medium is 0.04% (w/v), and churning time is 2 minutes; Selecting magneticstrength for use is that the permanent magnet of 1000 oersteds is positioned over reactor bottom, chlorella is carried out magnetic separate, and leaves standstill 2 minutes, removes supernatant liquid at last, collects and separates the chlorella that obtains, and the recovery of chlorella reaches 98.9%.After the chlorella (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction; The chlorella residue (containing the magnetic resolution medium) that separation obtains is calcined under the nitrogen atmosphere of 400 ℃ of high temperature and was removed the chlorella cells residue in 1 hour; 5 ℃/minute of temperature rise rates, the Fe of recovery
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 10 minutes of power 400w again, is mixed with the separated and collected that the magnetic resolution medium is reused for chlorella with deionized water.
Embodiment 5
With the chlorella in the method separated and collected chlorella nutrient solution of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 1% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the chlorella nutrient solution that obtains, the temperature of regulating in the stirred reactor is 20 ℃, and pH value 8 adds the magnetic resolution medium under the rotating speed of 200rpm, and the consumption of magnetic resolution medium is 0.01% (w/v), and churning time is 3 minutes; Selecting magneticstrength for use is that the permanent magnet of 3000 oersteds is positioned over reactor bottom, chlorella is carried out magnetic separate, and leaves standstill 3 minutes, removes supernatant liquid at last, collects and separates the chlorella that obtains, and the recovery of chlorella reaches 99.5%.After the chlorella (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction; The chlorella residue (containing the magnetic resolution medium) that separation obtains is calcined under the nitrogen atmosphere of 200 ℃ of high temperature and was removed the chlorella cells residue in 2 hours; 2 ℃/minute of temperature rise rates, the Fe of recovery
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 30 minutes of power 200w again, is mixed with the separated and collected that the magnetic resolution medium is reused for chlorella with deionized water.
With the chlorella in the method separated and collected chlorella nutrient solution of the present invention, its step is following:
With the Fe for preparing
3O
4Nanoparticulate dispersed forms stable suspension in deionized water, being mixed with concentration is the magnetic resolution medium of 5% (w/v), puts into refrigerator and cooled then and hides subsequent use.Insert in the stirred reactor cultivating the chlorella nutrient solution that obtains, the temperature of regulating in the stirred reactor is 30 ℃, and pH value 9 adds the magnetic resolution medium under the rotating speed of 100rpm, and the consumption of magnetic resolution medium is 0.03% (w/v), and churning time is 1 minute; Selecting magneticstrength for use is that the permanent magnet of 2000 oersteds is positioned over reactor bottom, the flocculation chlorella is carried out magnetic separate, and leaves standstill 1 minute, removes supernatant liquid at last, collects and separates the chlorella that obtains, and the recovery of chlorella reaches 97.8%.After the chlorella (containing the magnetic resolution medium) that separate to obtain carried out greasy extraction; The chlorella residue (containing the magnetic resolution medium) that separation obtains is calcined under the nitrogen atmosphere of 300 ℃ of high temperature and was removed the chlorella cells residue in 1.5 hours; 4 ℃/minute of temperature rise rates, the Fe of recovery
3O
4Nano particle is removed a small amount of ash content 3 times with deionized water wash, uses the supersound process 20 minutes of power 300w again, is mixed with the separated and collected that the magnetic resolution medium is reused for chlorella with deionized water.
Claims (3)
1. method that adopts magnetic medium to separate, collect little algae said method comprising the steps of:
(1) preparation Fe
3O
4Nano particle, making it disperse to form stable concentration is 1-5%w/v suspension-s, it is subsequent use to obtain the magnetic resolution medium;
(2) the pH value of adjusting micro algae culturing liquid is 8-10;
(3) add the magnetic resolution medium that step (1) obtains, the consumption of magnetic resolution medium is 0.01-0.04%w/v, and stirs 1-3 minute in 20-30 ℃;
(4) the little algae that obtains in the step (3) is carried out magnetic and separate, remove supernatant liquid, collect and separate the little algae that obtains; When little algae carried out the magnetic separation, selecting magneticstrength for use was the 1000-3000 oersted.
2. employing magnetic medium according to claim 1 separates, collects the method for little algae, it is characterized in that Fe
3O
4The concentration of nano granule suspension is 2%w/v.
3. employing magnetic medium according to claim 1 separates, collects the method for little algae; It is characterized in that; Little algae that step (4) is collected carries out the extraction of purpose meta-bolites, and the little algae residue that contains the magnetic resolution medium that obtains after the separation was calcined 1-2 hour under high temperature 200-400 ℃ nitrogen atmosphere, removed a small amount of ash content 3 times with deionized water wash; Use power 200-400w again supersound process 10-30 minute, obtain Fe
3O
4Nano particle is reused for the separated and collected of little algae.
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| CN102234617B true CN102234617B (en) | 2012-11-28 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586101B (en) * | 2012-01-16 | 2013-07-31 | 中国科学院过程工程研究所 | Industrial microalgae magnetic separation and collection device |
| CN103194394A (en) * | 2013-04-10 | 2013-07-10 | 中国科学院过程工程研究所 | Method for separating microalgae by taking polyethyleneimine modified Fe3O4 nanoparticles as flocculating agent |
| CN103289895B (en) * | 2013-05-16 | 2014-12-24 | 中国科学院过程工程研究所 | Magnetic separating device and method for microalgae recovery |
| CN108569816B (en) * | 2018-05-08 | 2020-10-20 | 吉林建筑大学 | Little algae collection device of water treatment |
| CN108970588A (en) * | 2018-07-11 | 2018-12-11 | 浙江海洋大学 | It is a kind of for adsorbing the preparation method of the magnetic microalgae biological adsorption agent of Pb In Exhausted Water |
| CN109225163A (en) * | 2018-11-14 | 2019-01-18 | 浙江海洋大学 | A kind of method of cadmium in compound magnetic microalgae biological adsorption agent and its absorption waste water |
| CN109536484B (en) * | 2018-11-23 | 2022-06-21 | 江苏大学 | Method for improving biomass and metabolite of chrysophyceae by magnetic field intervention |
| CN110684655B (en) * | 2019-10-18 | 2023-03-17 | 江苏大学 | Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof |
| CN112175937B (en) * | 2020-09-09 | 2021-08-27 | 深圳大学 | Method for separating microalgae |
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2010
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Non-Patent Citations (4)
| Title |
|---|
| Dan Liu，Fengting Li and Bingru Zhang."Removal or algal blooms in freshwater using magnetic polymer".《Water science and technology》.2009,第59卷(第6期),pages 1085-1091. |
| Dan Liu,Fengting Li and Bingru Zhang."Removal or algal blooms in freshwater using magnetic polymer".《Water science and technology》.2009,第59卷(第6期),pages 1085-1091. * |
| Zhengwen Gao，Xianjia Peng et al.,."Montmorillonite-Cu(II)/Fe(III) oxides magnetic material for removal of cyanobacterial Microcystis aeruginosa and its regeneration".《Desalination》.2009,第247卷(第1-3期),pages 337-345. |
| Zhengwen Gao,Xianjia Peng et al.,."Montmorillonite-Cu(II)/Fe(III) oxides magnetic material for removal of cyanobacterial Microcystis aeruginosa and its regeneration".《Desalination》.2009,第247卷(第1-3期),pages 337-345. * |
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