CN110684655A - Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof - Google Patents
Microalgae separation gradient magnetic stabilization fluidized bed device and microalgae harvesting method thereof Download PDFInfo
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- C12M25/00—Means for supporting, enclosing or fixing the microorganisms, e.g. immunocoatings
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- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/12—Unicellular algae; Culture media therefor
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Abstract
The invention discloses a method for harvesting microalgae by a gradient magnetic stabilization fluidized bed device, which can select a magnetic nano medium and microalgae species according to pre-experimental data and actual requirements, and set the dosage and concentration of the magnetic nano medium according to the adsorption capacity of the magnetic nano medium, thereby achieving the purpose of controlling the content of solid matters in a bed body; the harvesting efficiency can reach more than 95%; the processing capacity per unit volume of the composite material reaches more than 1L/min/L, which is far higher than the level reported in the literature. The invention solves the problems of the existing microalgae magnetic separation technology in industrial application, and can carry out large-scale semi-continuous harvesting on microalgae. The device has the advantages of simple structure, convenient operation, high microalgae harvesting efficiency, low cost and easy industrial amplification.
Description
Technical Field
The invention relates to a microalgae separation gradient magnetic stabilization fluidized bed device and a microalgae harvesting method thereof.
Background
Microalgae are microorganisms which are widely distributed on land and sea, rich in nutrition and high in photosynthetic efficiency, can synthesize a plurality of high-value natural active substances with unique structures and specific functions through various metabolic pathways in cells, and are widely applied to the aspects of medicine industry, food industry, animal feed and the like. On the other hand, the microalgae is a great raw material of biodiesel with great prospect due to high oil content and is considered to be possible to be a substitute of fossil energy; compared with other oil-producing crops, the microalgae serving as the biodiesel raw material has the advantages of high oil content, high growth speed, high photosynthetic efficiency and the like. However, the harvesting cost of the microalgae accounts for 20-30% of the whole production cost, and the capital investment of equipment for harvesting and dehydrating the outdoor cultured microalgae accounts for 90% of the investment of the whole microalgae production equipment, so that the method is an important factor influencing the industrialization of microalgae production.
Since the microalgae cells are small (about 2-40 μm), the concentration of the microalgae culture solution is low (about 0.3-5 kg/m dry weight of microalgae cells)3) Meanwhile, the electric charge of the microalgae cells enables the microalgae to maintain a stable state in the culture solution, so that the microalgae is large in recovery and treatment capacity and high in difficulty. The existing microalgae harvesting method mainly comprises the following steps: centrifugation, flocculation, filtration, gravity sedimentation, flotation, electrochemical methods, and the like. The centrifugation method is a simple method for rapidly settling microalgae cells by using centrifugal force. Although centrifugation is an effective harvesting method, the centrifugation method is mainly used for further reducing the water content after harvesting microalgae by methods such as flocculation and the like or separating some microalgae with high added value in consideration of the reasons that the operation energy consumption is large, the equipment cost and the operation cost are high, the operation is complex and the like when the centrifugation method is used for harvesting microalgae. The filtration method is a method for intercepting and separating water and microalgae cells by using a filter screen under the action of pressure or vacuum suction, but the filtration method is not suitable for microalgae with smaller diameter. The biggest problem of filtration is that microalgae cells can block filter holes, cause membrane pollution, need to periodically clean the filter screen, influence the harvesting speed and increase the harvesting cost. Flocculation is the process by which dispersed material in a solution forms large flocks by colliding and adhering together. Flocculation is a microalgae harvesting technology which is widely applied, and can simultaneously treat a large amount of microalgae solution; but settling of microalgae flocsThe speed is low, and the method needs to be applied in combination with other methods; meanwhile, the residue of the flocculating agent limits the application of the flocculating agent in the fields of food, medicines and the like. The gravity sedimentation method is a process of separating microalgae cells from a clear liquid layer by allowing the microalgae cells to settle to the bottom layer of a culture solution under the action of gravity. The gravity settling method takes long time to collect the microalgae, needs a larger settling pond, and has high water content of the collected microalgae. The flotation method is a process of introducing a large amount of micro-fine bubbles into a microalgae solution and bringing solid particles to the surface of the liquid by means of buoyancy. The method for collecting microalgae by flotation has the characteristics of simple equipment, simple and convenient operation and low energy consumption, but has the problem of low water removal rate. The electrochemical method is a method of separating microalgae cells by using an electric field according to their charged properties. The metal ions generated by dissolving the reaction electrode can be used as a flocculating agent to induce the microalgae cells to aggregate and then the microalgae is obtained. But the electrochemical method has high energy consumption, and the electrolytic solution is easy to generate secondary pollution.
In the aspect of microalgae magnetic separation devices, researches on microalgae harvesting by using magnetic separation devices are also reported, but the magnetic separation devices need to mix and react magnetic nano media with algae liquid in advance and then introduce the magnetic nano media into the magnetic separation devices for separation, and a high-gradient magnetic field is realized by arranging stainless steel meshes or stainless steel filaments in the magnetic separation devices. Therefore, the search for an efficient magnetic separation device becomes the key of the large-scale application of the magnetic separation technology in the microalgae separation.
Disclosure of Invention
The invention aims to overcome the defects of low magnetic separation efficiency, low processing capacity and the like of microalgae in the prior art and provides a microalgae separation gradient magnetic stabilization fluidized bed device and a method for harvesting microalgae by using the same.
In order to solve the technical problems, the invention provides the following technical scheme:
a microalgae separation gradient magnetic stabilization fluidized bed device comprises a magnetic nano medium storage tank, a water storage tank, an algae liquid storage tank, a feed liquid pump, a four-way valve, a gradient magnetic stabilization fluidized bed and a liquid outlet storage tank, wherein the gradient magnetic stabilization fluidized bed comprises a bed body, a discharge hole is formed in the bottom of the bed body, an electromagnetic coil capable of forming an axial uniform gradient magnetic field is arranged outside the bed body, and the electromagnetic coil is connected with a power supply; the liquid in the magnetic nano medium storage tank, the water storage tank and the algae liquid storage tank enters the bed body through the four-way valve by the feed liquid pump, the aggregate of the microalgae cells and the magnetic nano medium is discharged through the discharge port, and the separated liquid flows into the liquid outlet storage tank through the liquid outlet at the top of the bed body.
The magnetic nano medium storage tank adopts non-ferromagnetic materials, such as plastic, glass, aluminum and the like.
Furthermore, the electromagnetic coil is composed of two groups of electromagnetic coils, the first group of electromagnetic coils is 2 electromagnetic coils with the radius of R1, and the distance between the two electromagnetic coils is
The current in the two coils is equal in magnitude and opposite in direction; the second group of electromagnetic coils are 2 electromagnetic coils with the radius of R2, the distance between the two coils is R2, the currents in the two coils are equal in magnitude and same in direction; and R2 is more than R1, the first group of electromagnetic coils are positioned between two electromagnetic coils of the second group of electromagnetic coils; by adjusting the current of the two groups of electromagnetic coils, the axial uniform gradient magnetic field with different field gradients and different strengths can be obtained.
Furthermore, the main body of the bed body is in a circular truncated cone shape, the diameter of the upper bottom surface of the bed body is larger than that of the lower bottom surface of the bed body, the included angle between a generatrix of the circular truncated cone and the central shaft is 3-15 degrees, and the more preferable included angle can be 5-12 degrees or 7-9 degrees; the ratio of the height of the circular truncated cone to the diameter of the middle section is 3-10: 1, more preferably 5-8: 1, and still more preferably 6-7: 1. Preferably, the main body of the bed body is made of non-ferromagnetic material, such as plastic, glass, aluminum, etc. The two ends of the bed body are connected with the plug and the main body round platform in a flange connection mode, so that the bed is convenient to disassemble, and the plug and the flange are made of magnetic conductive materials which are not easy to magnetize.
Furthermore, the power supply adopts a direct current power supply and can provide two paths of direct current power supply outputs which are independently controlled.
Further, the magnetic nano-medium is a naked magnetic material or a surface functionalized magnetic material which can be used for microalgae separation, such as magnetic nano-Fe3O4Magnetic nano-Fe coated with silicon dioxide3O4Magnetic nano Fe modified by polyethyleneimine3O4。
Furthermore, the concentration of the magnetic nano medium is 100-600 g/L. Preferably 200-500g/L, and further preferably 300-400 g/L. The concentration of the magnetic nanomedia facilitates the transport of the particles.
A method for harvesting microalgae by adopting a gradient magnetic stabilized fluidized bed device comprises the following steps:
1) pumping the high-concentration magnetic nano medium in the magnetic nano medium storage tank into the bottom of the gradient magnetic stable fluidized bed, and pumping water through a four-way valve under the conditions of preset fluidized bed flow rate and gradient magnetic field parameters to obtain stable fluidization under different parameter conditions;
2) and switching the water at the inlet into microalgae culture solution through the four-way valve, adsorbing microalgae cells by magnetic nano medium particles in the fluidized bed, keeping the microalgae concentration at the liquid outlet to be very low and stable, stopping inputting the microalgae culture solution after the microalgae concentration in the effluent liquid of the liquid outlet is obviously increased, discharging the mixture in the bed body from the discharge port, and collecting the obtained aggregates of the microalgae cells and the magnetic nano medium.
3) And repeating the steps 1) and 2), thus realizing the semi-continuous magnetic separation of the microalgae in the microalgae culture solution.
Further, the axial velocity of the fluid in the bed is 3-50 cm/min. Preferably 10-40cm/min, more preferably 15-30 cm/min.
Further, the magnetic field intensity of the bed body changes linearly along the central axis, the magnetic field intensity at the bottom of the bed body is lowest, and the magnetic field intensity at the top is highest; the bottom magnetic field intensity is 20-100Gs, preferably 30-90Gs, further preferably 40-70 Gs; the magnetic field intensity at the top is 300-; the gradient of the variation of the magnetic field strength is 1-10Gs/cm, preferably 2-8Gs/cm, more preferably 3-6 Gs/cm.
Further, the direction of the magnetic field of the bed is opposite to the direction of the liquid flow.
Further, the content of dry substances in the bed body is controlled to be 50-300 g/L; preferably 90-250g/L, and further preferably 150-200 g/L.
The invention has the following beneficial effects: the method collects the microalgae through the gradient magnetic stabilization fluidized bed device, can select the magnetic nano medium and the microalgae species according to pre-experimental data and actual requirements, and sets the dosage and the concentration of the magnetic nano medium according to the adsorption capacity of the magnetic nano medium, thereby achieving the purpose of controlling the solid content in the bed body; the harvesting efficiency can reach more than 95%; the processing capacity per unit volume of the composite material reaches 1L/min/L, which is far higher than the level reported in the literature. The invention solves the problems of the existing microalgae magnetic separation technology in industrial application, and can carry out large-scale semi-continuous harvesting on microalgae. The device has the advantages of simple structure, convenient operation, high microalgae harvesting efficiency, low cost and easy industrial amplification.
Compared with the prior art, the invention has the following beneficial effects:
according to the device for separating microalgae based on the gradient magnetic stabilized fluidized bed, the main body of the bed body is in the shape of a circular truncated cone with the diameter of the upper bottom surface larger than that of the lower bottom surface, so that the axial speed of fluid in the bed body can be gradually reduced along the flowing direction to a certain extent, the magnetically stabilized fluidized state of the bed layer is not influenced, and the outflow probability of a magnetic nano medium is reduced;
the microalgae separation gradient magnetic stabilization fluidized bed device adopts the design of a gradient magnetic field, the magnetic field intensity at the outlet is high, the magnetic nano medium can be ensured not to be washed out, the magnetic field intensity at the inlet is low, and the bed layer blockage caused by the large adsorption amount of algae at the lower part of the bed layer in the operation process can be avoided;
the microalgae separation gradient magnetic stabilization fluidized bed device provided by the invention has the advantages that the treatment capacity in unit time is 5-10 times of that of a uniform magnetic field magnetic stabilization fluidized bed, the treatment capacity of the magnetic stabilization fluidized bed is greatly improved, and the requirement of large-scale application is met;
(4) the device and the method for separating microalgae by the gradient magnetically stabilized fluidized bed provided by the invention have simple process and are easy to amplify.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic structural view of the present invention;
1-magnetic nano medium storage tank; 2-a water storage tank; 3-algae liquid storage tank; 4-a feed liquid pump; 5-a four-way valve; 6-an electromagnetic coil; 7-bed body; 8-discharging port; 9-a power supply; 10-liquid storage tank.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Examples
As shown in fig. 1, a microalgae separation gradient magnetic stabilization fluidized bed device comprises a magnetic nano medium storage tank 1, a water storage tank 2, an algae liquid storage tank 3, a feed liquid pump 4, a four-way valve 5, a gradient magnetic stabilization fluidized bed and a liquid outlet storage tank 10, wherein the gradient magnetic stabilization fluidized bed comprises a bed body 7, a discharge hole 8 is arranged at the bottom of the bed body 7, an electromagnetic coil 6 capable of forming an axial uniform gradient magnetic field is arranged outside the bed body 7, and the electromagnetic coil 6 is connected with a power supply 9; the liquid in the magnetic nano medium storage tank 1, the water storage tank 2 and the algae liquid storage tank 3 enters the bed body 7 through the four-way valve 5 by the liquid feed pump 4, the aggregate of the microalgae cells and the magnetic nano medium is discharged through the discharge port 8, and the separated liquid flows into the liquid outlet storage tank 10 through the liquid outlet at the top of the bed body 7.
The electromagnetic coil 6 consists of two groups of electromagnetic coils, the first group of electromagnetic coils is 2 electromagnetic coils with the radius of R1, the distance between the two electromagnetic coils is R1, the current in the two coils is equal in magnitude, and the current directions are opposite; the second group of electromagnetic coils are 2 electromagnetic coils with the radius of R2, the distance between the two coils is R2, the currents in the two coils are equal in magnitude and same in direction; and R2 is more than R1, the first group of electromagnetic coils are positioned between two electromagnetic coils of the second group of electromagnetic coils; by adjusting the current of the two groups of electromagnetic coils, the axial uniform gradient magnetic field with different field gradients and different strengths can be obtained.
The main body of the bed body 7 is in a circular truncated cone shape, the diameter of the upper bottom surface of the bed body is larger than that of the lower bottom surface of the bed body, the included angle between a generatrix of the circular truncated cone and a central shaft is 3-15 degrees, and the ratio of the height of the circular truncated cone to the diameter of the middle section is 3-10: 1.
Adopting naked magnetic nano Fe3O4Separating and harvesting microalgae in the chlorella culture solution:
1) storing the high-concentration exposed magnetic nano Fe in the magnetic nano medium storage tank3O4Pumping into the bottom of the gradient magnetic stabilization fluidized bed, and then presetting the flow rate of the fluidized bed to be 10cm/min, the magnetic field intensity at the bottom to be 30Gs, the magnetic field intensity at the top to be 400Gs, and the variation gradient of the magnetic field intensity to be 2-8 Gs/cm; pumping water through a four-way valve to obtain unstable fluidization;
2) switching the water from the inlet into chlorella culture solution through the four-way valve, adsorbing chlorella cells by magnetic nano medium particles in the fluidized bed, keeping the chlorella concentration at the liquid outlet to be very low and stable, stopping inputting the chlorella culture solution after the chlorella concentration in the effluent liquid of the liquid outlet is obviously increased, discharging the mixture in the bed body from the discharge port, and collecting the obtained aggregates of the chlorella cells and the magnetic nano medium. The content of Chlorella and granule in the liquid storage tank are measured, the recovery rate of Chlorella is 97%, and the granule loss rate is 0.5%.
Separating and harvesting the microalgae in the botryococcus braunii culture solution with the magnetic particles coated by the silicon dioxide:
1) pumping the high-concentration silicon dioxide coated magnetic particles in the magnetic nano medium storage tank into the bottom of a gradient magnetic stabilization fluidized bed, and then presetting the flow rate of the fluidized bed to be 40cm/min, the magnetic field intensity at the bottom to be 90Gs, the magnetic field intensity at the top to be 800Gs, and the variation gradient of the magnetic field intensity to be 8-10 Gs/cm; pumping water through a four-way valve to obtain stable fluidization under different parameter conditions; pumping water through a four-way valve to obtain stable fluidization;
2) and switching the water from the inlet into the botryococcus braunii culture solution through the four-way valve, adsorbing the microalgae cells by magnetic nano medium particles in the fluidized bed, keeping the botryococcus braunii concentration at the liquid outlet to be very low and stable, stopping inputting the microalgae culture solution after the botryococcus braunii concentration in the effluent liquid of the liquid outlet is obviously increased, discharging the mixture in the bed body from the discharge hole, and collecting the obtained aggregates of the botryococcus braunii cells and the magnetic nano medium. And (3) measuring the content and the particle content of the botryococcus braunii in the liquid outlet storage tank, wherein the recovery rate of the botryococcus braunii algae is 98%, and the particle loss rate is 0.3%.
Separating and collecting microalgae in nannochloropsis oculata culture solution with polyethyleneimine modified magnetic particles
1) Pumping the polyethyleneimine modified magnetic particles in the magnetic nano medium storage tank into the bottom of a gradient magnetic stabilization fluidized bed, and then setting the flow rate of the fluidized bed to be 20cm/min, the magnetic field intensity at the bottom to be 40Gs, the magnetic field intensity at the top to be 800Gs, and the variation gradient of the magnetic field intensity to be 3-6 Gs/cm; pumping water through a four-way valve to obtain stable fluidization;
2) and switching the water from the inlet into a nannochloropsis oculata culture solution through the four-way valve, adsorbing cells of the nannochloropsis oculata culture solution by magnetic nano-medium particles in the fluidized bed, keeping the concentration of the nannochloropsis oculata culture solution at the liquid outlet stable, stopping inputting the nannochloropsis oculata culture solution after the concentration of the nannochloropsis oculata culture solution in the effluent liquid of the liquid outlet is obviously increased, discharging the mixture in the bed body from the discharge port, and collecting the obtained aggregates of the nannochloropsis oculata cells and the magnetic nano-medium. The content of nannochloropsis oculata and the content of particles in the liquid storage tank are measured, the recovery rate of nannochloropsis oculata is 95%, and the particle loss rate is 0.4%.
The invention solves the problems of the existing microalgae magnetic separation technology in industrial application, and can carry out large-scale continuous recovery on microalgae. The device has the advantages of simple structure, convenient operation, high microalgae harvesting efficiency, low cost and easy amplification.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A microalgae separation gradient magnetic stabilization fluidized bed device is characterized by comprising a magnetic nano medium storage tank (1), a water storage tank (2), an algae liquid storage tank (3), a feed liquid pump (4), a four-way valve (5), a gradient magnetic stabilization fluidized bed and a liquid outlet storage tank (10), wherein the gradient magnetic stabilization fluidized bed comprises a bed body (7), a discharge hole (8) is formed in the bottom of the bed body (7), an electromagnetic coil (6) capable of forming an axial uniform gradient magnetic field is arranged outside the bed body (7), and the electromagnetic coil (6) is connected with a power supply (9); the liquid in the magnetic nano medium storage tank (1), the water storage tank (2) and the algae liquid storage tank (3) enters the bed body (7) through the four-way valve (5) by the feed liquid pump (4), the aggregates of the microalgae cells and the magnetic nano medium are discharged through the discharge hole (8), and the separated liquid flows into the liquid outlet storage tank (10) through the liquid outlet at the top of the bed body (7).
2. The microalgae separation gradient magnetic stabilization fluidized bed apparatus according to claim 1, wherein the electromagnetic coil (6) is composed of two groups of electromagnetic coils, the first group of electromagnetic coils is 2 electromagnetic coils with radius R1, and the distance between the two electromagnetic coils is
The current in the two coils is equal in magnitude and opposite in direction; the second group of electromagnetic coils are 2 electromagnetic coils with the radius of R2, the distance between the two coils is R2, the currents in the two coils are equal in magnitude and same in direction; and R2 is more than R1, the first group of electromagnetic coils are positioned between two electromagnetic coils of the second group of electromagnetic coils; by adjusting the current of the two groups of electromagnetic coils, the axial uniform gradient magnetic field with different field gradients and different strengths can be obtained.
3. The microalgae separation gradient magnetic stabilization fluidized bed device according to claim 1 or 2, characterized in that the main body of the bed body (7) is in a circular truncated cone shape, the diameter of the upper bottom surface is larger than that of the lower bottom surface, the included angle between the generatrix of the circular truncated cone and the central axis is 3-15 degrees, and the ratio of the height of the circular truncated cone to the diameter of the middle section is 3-10: 1.
4. The microalgae separation gradient magnetic stabilization fluidized bed apparatus of claim 3, wherein the magnetic nano-media is magnetic nano-Fe3O4Magnetic nano Fe coated by silicon dioxide3O4Or polyethyleneimine modified magnetic nano Fe3O4Any one or more of.
5. The magnetic stabilized fluidized bed apparatus for microalgae separation gradient of claim 3, wherein the concentration of the magnetic nano-media is 100-600 g/L.
6. A method for harvesting microalgae using the gradient magnetically stabilized fluidized bed apparatus of claim 1, comprising the steps of:
1) pumping the high-concentration magnetic nano medium in the magnetic nano medium storage tank (1) into the bottom of the gradient magnetic stable fluidized bed, and pumping water through a four-way valve (5) under the conditions of preset fluidized bed flow rate and gradient magnetic field parameters to obtain stable fluidization under different parameter conditions;
2) and the water at the inlet is switched into microalgae culture solution through the four-way valve, microalgae cells are adsorbed by magnetic nano medium particles in the fluidized bed, the concentration of microalgae at the liquid outlet is very low and is kept stable, the microalgae culture solution is stopped to be input after the concentration of the microalgae in the effluent liquid of the liquid outlet is obviously increased, the mixture in the bed body (7) is discharged from the discharge port (8), and the obtained aggregates of the microalgae cells and the magnetic nano medium are collected.
3) And repeating the steps 1) and 2), thus realizing the semi-continuous magnetic separation of the microalgae in the microalgae culture solution.
7. The microalgae recovery method according to claim 6, characterized in that the axial velocity of the fluid in the bed (7) is 3-50 cm/min.
8. The microalgae harvesting method according to claim 6, characterized in that the magnetic field strength of the bed (7) varies linearly along the central axis, the magnetic field strength at the bottom of the bed being the lowest and the top being the highest; the magnetic field intensity at the bottom is 20-100Gs, and the magnetic field intensity at the top is 300-1000 Gs; the gradient of the magnetic field intensity is 1-10 Gs/cm.
9. The microalgae harvesting method according to claim 8, characterized in that the direction of the magnetic field of the bed (7) is opposite to the direction of the liquid flow.
10. The microalgae harvesting method according to claim 6, characterized in that the content of dry matter in the bed (7) is controlled to 50-300 g/L.
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| CN113684110A (en) * | 2021-08-26 | 2021-11-23 | 德州六顺电气自动化设备有限公司 | Microalgae magnetic flocculation separation equipment and separation method thereof |
| CN114212890A (en) * | 2021-11-30 | 2022-03-22 | 华中科技大学 | High-value utilization method of microalgae energy |
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| CN114212890A (en) * | 2021-11-30 | 2022-03-22 | 华中科技大学 | High-value utilization method of microalgae energy |
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