CN113058743A - Method and device for screening polydisperse magnetic polymer microspheres - Google Patents
Method and device for screening polydisperse magnetic polymer microspheres Download PDFInfo
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- CN113058743A CN113058743A CN202110338237.0A CN202110338237A CN113058743A CN 113058743 A CN113058743 A CN 113058743A CN 202110338237 A CN202110338237 A CN 202110338237A CN 113058743 A CN113058743 A CN 113058743A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/32—Magnetic separation acting on the medium containing the substance being separated, e.g. magneto-gravimetric-, magnetohydrostatic-, or magnetohydrodynamic separation
Abstract
The invention relates to the technical field of microsphere processing, and discloses a screening method and a screening device for polydisperse magnetic polymer microspheres, wherein the method comprises the following steps: insulating and plastic-packaging the electromagnet, placing the electromagnet into a container, effectively contacting with a polydisperse magnetic polymer microsphere turbid liquid in which obvious columnar layering appears after standing and settling, applying current with preset intensity to the electromagnet to form a preset magnetic field, and adsorbing the uppermost magnetic microsphere in a smaller particle size range in the columnar layering on the electromagnet; after the magnetic microspheres on the uppermost layer are stably adsorbed on the surface of the electromagnet, taking the electromagnet out of the container, powering off, and collecting the magnetic microspheres on the uppermost layer; and sequentially increasing the intensity of the current applied to the electromagnet, and repeating the steps until the magnetic microspheres in each layer with different particle size ranges in the columnar layering are sequentially collected according to the sequence of the particle size from small to large.
Description
Technical Field
The invention relates to the technical field of microsphere processing, in particular to a screening method and a screening device for polydisperse magnetic polymer microspheres.
Background
Magnetic polymer microspheres refer to high molecular particles with diameters in the range of tens of nanometers to hundreds of micrometers. The small particle size and volume make the entire particle responsive to external stimuli and fast reaction rates when used as a microreactor. The high-quality monodisperse polymer microsphere has the characteristics of large specific surface area, controllable particle size and the like, can be used for the separation and purification of biological molecules such as filler, protein, amino acid and the like, the sustained release of drugs, the diagnosis of diseases, high-added-value products such as novel ceramic materials and raw materials of liquid crystal displays, can also be used as an ultrapure water treatment material in the industries such as medicines and semiconductors, and can also be used as an additive of bulk products such as coatings, paper surface coatings, cosmetics and the like.
The particle size of the magnetic polymer microspheres may not be uniform due to the influence of objective factors during the preparation process. The existing microsphere screening technology in the industry is not mature enough, and the ultrafiltration membrane with good screening effect is too expensive, so that a set of screening technology is urgently needed to be developed to obtain monodisperse microspheres with different particle sizes, and the use value of the polydisperse microspheres is improved.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a method and a device for screening polydisperse magnetic polymer microspheres, which can effectively screen the polydisperse magnetic polymer microspheres by controlling the magnetic size of an electromagnet to control the particle size range of the magnetic polymer microspheres adsorbed on the electromagnet, so as to obtain the magnetic microspheres with different particle size ranges and relatively uniform particle size ranges.
The technical scheme is as follows: the invention provides a screening method of polydisperse magnetic polymer microspheres, which comprises the following steps: s1: injecting the polydisperse magnetic polymer microsphere turbid liquid subjected to ultrasonic oscillation into a container, adding a solvent to a preset scale, sealing the container, standing and settling at a dark place until obvious columnar layering occurs; s2: after insulating and plastic-packaging the electromagnet, putting the electromagnet into the container, effectively contacting the electromagnet with the polydisperse magnetic polymer microsphere suspension, applying voltage and current with preset intensity to the electromagnet to form a preset magnetic field, and adsorbing the uppermost magnetic microsphere in a smaller particle size range in the columnar lamination on the electromagnet; s3: after the magnetic microspheres on the uppermost layer are stably adsorbed on the surface of the electromagnet, taking the electromagnet out of the container, powering off, and collecting the magnetic microspheres on the uppermost layer; s4: and sequentially increasing the intensity of the current applied to the electromagnet, and repeatedly executing S2 and S3 until the magnetic microspheres in each layer in different particle size ranges in the columnar layering are sequentially collected according to the sequence of the particle size from small to large.
Further, before the step S1, the method further includes the following steps: and centrifuging the to-be-screened polydisperse magnetic polymer microsphere turbid liquid, and then taking the lower polydisperse magnetic polymer microsphere turbid liquid for subsequent screening operation.
Preferably, the rotating speed during centrifugation is 500-5500 r/min, and the centrifugation time is 25-35 min.
Preferably, in S1, the particle size of the suspension of polydisperse magnetic polymer microspheres to be sieved is in the range of 100 to 5000 nm.
Preferably, in S1, the power of the ultrasonic oscillation is 85-95%, and the duration of the ultrasonic oscillation is 20-30 min.
Preferably, in S2, the preset voltage strength applied to the electromagnet is: 110-220V, the predetermined current intensity is 0-3.8A. Preferably, when the preset voltage intensity is 110V and the preset intensity of the current applied to the electromagnet is 0-1.2A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 10-600 nm; when the preset intensity of the current applied to the electromagnet is 1.2-2.4A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 600-1200 nm; when the preset intensity of the current applied to the electromagnet is 2.4-3.8A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 1200-2000 nm.
Preferably, the selected solvent is any one or combination of the following: deionized water, ethanol, ethylene glycol and glycerol.
Preferably, the magnetic polymer microspheres in the polydisperse magnetic polymer microsphere suspension to be screened are any one or a combination of the following: ferroferric oxide nano-microspheres, ferroferric oxide-polymer compound nano-microspheres, ferroferric oxide-silica shell core type nano-microspheres, immune magnetic nano-microspheres or chitosan magnetic nano-microspheres.
The invention also provides a screening device for the polydisperse magnetic polymer microspheres, which comprises a bracket, a container and an electromagnet, wherein the outer wall of the electromagnet is wrapped with an insulating plastic packaging film; when the electromagnet is electrified, the electromagnet is positioned in the container and is effectively contacted with the polydisperse magnetic polymer microsphere turbid liquid to be screened in the container.
Further, the screening device for the polydisperse magnetic polymer microspheres further comprises a lifting table, wherein the lifting table is arranged on the support, and the container is arranged on the lifting table. The setting of elevating platform makes the container can descend or rise, is convenient for can contact the separation of electro-magnet and polydisperse magnetic polymer microballon turbid liquid, and subsequent separation process of being convenient for goes on smoothly.
Further, the electromagnet is installed on the bracket through a rotating clamping rod. After once adsorbing, the elevating platform descends, and rotatory this rotatory clamping bar can make the electro-magnet be moved to the next door, is convenient for collect the magnetism microballon that adsorbs above that.
Preferably, the container is made of an insulating material. When the container made of insulating materials is used, the electromagnet is electrified, so that the magnetic field is not affected, and the smooth proceeding of adsorption and screening is ensured.
Preferably, the container is a transparent glass container. The transparent glass container can obviously show the columnar layering in the container, thereby facilitating the real-time observation of the screening condition.
Has the advantages that: the invention utilizes the magnetic property of magnetic polymer microspheres, firstly, the suspension of polydisperse magnetic polymer microspheres is settled and then layered in a column shape, so that the magnetic microspheres in different particle size ranges are layered, usually, the magnetic microspheres with smaller particle size are positioned at the upper layer of the column-shaped layered, and the magnetic microspheres with larger particle size are positioned at the lower layer of the column-shaped layered, therefore, the invention arranges the electromagnet which is sealed in an insulating plastic on the surface of the suspension of polydisperse magnetic polymer microspheres and effectively contacts with the suspension, then, a current with smaller intensity is firstly applied to the electromagnet, a magnetic field with smaller intensity can be generated, the formation of the magnetic field can lead the magnetic microspheres in the smaller particle size range in the polydisperse magnetic polymer microspheres suspension to be adsorbed on the electromagnet, and the magnetic microspheres in the larger particle size range can be adsorbed on the electromagnet due to the larger magnetic field, when a circuit with smaller strength is applied to the electromagnet, the magnetic microspheres with larger grain sizes cannot be adsorbed. According to the principle, the current with lower intensity is firstly applied to the electromagnet, the magnetic microspheres in the smaller particle size range of the uppermost layer are adsorbed and screened, then the current intensity applied to the electromagnet is increased, the magnetic microspheres in the second layer with larger particle size range are adsorbed and screened, and by analogy, the magnetic microspheres in each layer in different particle size ranges in the polydisperse magnetic polymer microsphere turbid liquid can be sequentially collected according to the sequence of the particle sizes from small to large.
The screening method of the polydisperse magnetic polymer microspheres belongs to physical screening, and is green, environment-friendly, simple and convenient to operate and low in cost.
Drawings
FIG. 1 is a schematic diagram of a sieving apparatus for polydispersed magnetic polymeric microspheres;
FIG. 2 is a schematic diagram of a sieving process of polydispersed magnetic polymeric microspheres.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The embodiment provides a screening method of polydisperse magnetic polymer microspheres, and the specific tools/instruments used in the method are as follows: an ultrasonic disperser, a rubber dropper, a circular electromagnet, a cylindrical transparent glass container made of special insulating materials, a centrifuge and a collecting container.
The screening device of the polydisperse magnetic polymer microspheres in the embodiment is as shown in fig. 1, and mainly comprises a bracket 1, a cylindrical transparent glass container 2 and an electromagnet 4, wherein the outer wall of the electromagnet 4 is wrapped by an insulating plastic packaging film 3, the electromagnet 4 is installed on the bracket 1 through a rotary clamping rod 7, the container 2 is placed on a lifting table 6, the lifting table 6 is installed on the bracket 1, and the electromagnet 4 is connected with a power supply through a lead 5; when the electromagnet 4 is electrified, the electromagnet 4 is positioned in the container 2 and is in effective contact with the polydisperse magnetic polymer microsphere suspension to be screened in the container 2.
The implementation flow of the sieving method of the polydisperse magnetic polymer microspheres in the embodiment is shown in fig. 2, and mainly comprises material selection → centrifugation → ultrasonic oscillation → electromagnetic adsorption → standing sedimentation → microsphere collection → repeated experiments.
The method comprises the following specific steps:
selecting materials: selecting a poly-dispersed magnetic polymer microsphere suspension to be screened, wherein the particle size of the poly-dispersed magnetic polymer microsphere suspension is 10-2000 nm.
Centrifuging: centrifuging the poly-dispersed magnetic polymer microsphere suspension to be screened by using a centrifugal machine, and setting parameters as follows: the rotating speed is 500-5500 r/min, the temperature is 25 ℃, and the centrifugation time is 30 min. And after centrifugation, taking the lower-layer polydisperse magnetic polymer microsphere suspension for subsequent screening.
Ultrasonic oscillation: and (3) carrying out ultrasonic oscillation on the lower-layer poly-dispersed magnetic polymer microsphere turbid liquid, setting the power of an ultrasonic oscillation device to be 90%, the temperature to be 25 ℃, and the duration to be 25 min.
Standing and settling: firstly, injecting the polydisperse magnetic polymer microsphere turbid liquid subjected to ultrasonic oscillation into a container 2, injecting deionized water to enable the polydisperse magnetic polymer microsphere turbid liquid to reach the marked scale mark, sealing the container 2, placing the container in a dark place, standing and settling until obvious columnar layering occurs;
first electromagnetic adsorption: the circular electromagnet 4 is subjected to insulation plastic packaging by using an insulation plastic packaging film, is installed on the bracket 1 through a rotary clamping rod 7, and is then connected with a power supply through a lead 5; the container 2 is placed on a lifting platform 6, the electromagnet 4 is placed in the container 2 and is in effective contact with the polydisperse magnetic polymer microsphere turbid liquid in the container, then the power supply voltage is controlled to be 110V, 0-1.2A of current is applied to the electromagnet to form a first magnetic field, and the uppermost layer of magnetic microspheres with the particle size within the range of 10-600 nm in the columnar lamination in the container 2 are adsorbed on the surface of the electromagnet 4.
Collecting microspheres for the first time: after the uppermost layer of magnetic microspheres are stably adsorbed on the surface of the electromagnet 4, the container 2 is descended through the lifting platform 6, the electromagnet 4 is positioned above an opening above the container 2, then the electromagnet 4 is rotated aside through the rotary clamping rod 7, the microsphere collecting container is placed below the electromagnet 4, and the magnetic microspheres with the grain diameter within the range of 10-600 nm adsorbed on the electromagnet 4 are separated and fall into the collecting container after the power supply is cut off.
Second electromagnetic adsorption: the electromagnet 4 is moved to the original position again through the rotating clamping rod 7, the container 2 is lifted to the position that the electromagnet 4 is in effective contact with the poly-dispersed magnetic polymer microsphere turbid liquid again through the lifting platform 6, then the power supply voltage is kept at 110V, 1.2-2.4A of current is applied to the electromagnet 4, a second magnetic field is formed, and second layers of magnetic microspheres with the particle size within the range of 600-1200 nm in the columnar layering in the container 2 are adsorbed on the surface of the electromagnet 4.
And (3) collecting microspheres for the second time: after the second layer of magnetic microspheres are stably adsorbed on the surface of the electromagnet 4, the power supply is cut off in the same way, and the magnetic microspheres adsorbed on the electromagnet 4 and having the particle size within the range of 600-1200 nm are separated and fall into a collection container.
And (3) electromagnetic adsorption for the third time: and moving the electromagnet 4 to be in effective contact with the polydisperse magnetic polymer microsphere turbid liquid again in the same manner, keeping the power supply voltage at 110V, applying a current of 2.4-3.8A to the electromagnet 4 to form a third magnetic field, and adsorbing a third layer of magnetic microspheres with the particle size of 1200-2000 nm in the columnar lamination in the container 2 on the surface of the electromagnet 4.
And (3) collecting microspheres for the third time: after the third layer of magnetic microspheres are stably adsorbed on the surface of the electromagnet 4, the power supply is cut off in the same way, and the magnetic microspheres adsorbed on the electromagnet 4 with the particle size of 1200-2000 nm are separated and fall into a collection container.
Through the steps, all layers of magnetic microspheres in different particle size ranges in the polydisperse magnetic polymer microsphere turbid liquid can be sequentially collected according to the sequence of particle sizes from small to large, and the magnetic microspheres with relatively uniform particle sizes are obtained.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A screening method of polydisperse magnetic polymer microspheres is characterized by comprising the following steps:
s1: injecting the polydisperse magnetic polymer microsphere suspension to be screened after ultrasonic oscillation into a container, adding a solvent to a preset scale, sealing the container, standing and settling at a dark place until obvious columnar layering occurs;
s2: after insulating and plastic-packaging the electromagnet, putting the electromagnet into the container, effectively contacting the electromagnet with the polydisperse magnetic polymer microsphere suspension, applying voltage and current with preset intensity to the electromagnet to form a preset magnetic field, and adsorbing the uppermost magnetic microsphere in a smaller particle size range in the columnar lamination on the electromagnet;
s3: after the magnetic microspheres on the uppermost layer are stably adsorbed on the surface of the electromagnet, taking the electromagnet out of the container, powering off, and collecting the magnetic microspheres on the uppermost layer;
s4: and sequentially increasing the intensity of the current applied to the electromagnet, and repeatedly executing S2 and S3 until the magnetic microspheres in each layer in different particle size ranges in the columnar layering are sequentially collected according to the sequence of the particle size from small to large.
2. The method for sieving polydisperse magnetic polymer microspheres according to claim 1, further comprising, before the step of S1, the steps of:
centrifuging the to-be-screened polydisperse magnetic polymer microsphere suspension, and then taking the lower polydisperse magnetic polymer microsphere suspension for subsequent screening operation;
the rotating speed during centrifugation is 500-5500 r/min, and the centrifugation time is 25-35 min.
3. The method for sieving polydisperse magnetic polymer microspheres according to claim 1, wherein in the step S2, the preset voltage strength applied to the electromagnet is: 110-220V, the predetermined current intensity is 0-3.8A.
4. The method for screening polydisperse magnetic polymer microspheres according to claim 3, wherein when the preset voltage intensity is 110V, and the preset intensity of the current applied to the electromagnet is 0-1.2A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 10-600 nm; when the preset intensity of the current applied to the electromagnet is 1.2-2.4A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 600-1200 nm; when the preset intensity of the current applied to the electromagnet is 2.4-3.8A, the particle size of the magnetic microspheres adsorbed on the surface of the electromagnet is 1200-2000 nm.
5. A method for sieving polydispersed magnetic polymeric microspheres according to any one of claims 1 to 4, wherein the selected solvent is any one or combination of the following:
deionized water, ethanol, ethylene glycol and glycerol.
6. The method for sieving polydisperse magnetic polymer microspheres according to any one of claims 1 to 4, wherein the magnetic polymer microspheres in the polydisperse magnetic polymer microsphere suspension to be sieved are any one or a combination of the following:
ferroferric oxide nano-microspheres, ferroferric oxide-polymer compound nano-microspheres, ferroferric oxide-silica shell core type nano-microspheres, immune magnetic nano-microspheres or chitosan magnetic nano-microspheres.
7. The screening device for the polydisperse magnetic polymer microspheres is characterized by comprising a support (1), a container (2) and an electromagnet (4) of which the outer wall is wrapped with an insulating plastic packaging film (3), wherein the electromagnet (4) is installed on the support (1), the container (2) is arranged on the support (1), and the electromagnet (4) is connected with a power supply through a wire (5); when the electromagnet (4) is electrified, the electromagnet (4) is positioned in the container (2) and is in effective contact with the polydisperse magnetic polymer microsphere suspension to be screened in the container (2).
8. A sieving apparatus for polydisperse magnetic polymer microspheres according to claim 7, further comprising an elevating platform (6), wherein the elevating platform (6) is arranged on the bracket (1), and the container (2) is placed on the elevating platform (6).
9. A sieving device of polydisperse magnetic polymer microspheres according to claim 8, characterized in that the electromagnets (4) are mounted on the bracket (1) by rotating clamping bars (7).
10. A sieving device for polydisperse magnetic polymer microspheres according to any one of claims 7 to 9, wherein the container is a transparent glass container of insulating material.
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Application publication date: 20210702 |