CN111701544B - Preparation method of magnetic polystyrene microspheres - Google Patents
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Abstract
The invention discloses a preparation method of magnetic polystyrene microspheres, which comprises the following steps: obtaining porous polystyrene microspheres, and dispersing the porous polystyrene microspheres in an organic solution to obtain a mixed solution A, wherein the organic solution is dichloromethane/cyclohexanol or dichloromethane/xylene, and the volume ratio of dichloromethane/cyclohexanol is (90-99): 1-10, wherein the volume ratio of dichloromethane/dimethylbenzene is 1-10: 1; dispersing the oleic acid modified magnetic ferroferric oxide in a xylene solution to obtain a mixed solution B; and uniformly mixing the mixed solution A and the mixed solution B, swelling at room temperature, drying and washing to obtain the magnetic polystyrene microsphere. The prepared magnetic polystyrene microspheres are uniform in size and have an average particle size of 3-10 um; good monodispersity, and the dispersion coefficient is less than 5%.
Description
Technical Field
The invention relates to the technical field of preparation of polymer materials, in particular to a preparation method of magnetic polystyrene microspheres.
Background
The magnetic polymer microsphere is a composite microsphere formed by combining inorganic magnetic particles and a polymer material, and is a novel functional material. The magnetic microsphere has the characteristics of polymer microsphere and magnetic particle, so that the magnetic microsphere can be dispersed in the solution uniformly and stably without an external magnetic field, and can be separated simply and quickly by adding the external magnetic field. And multiple reactive functional groups can be endowed on the surface of the material through copolymerization and surface modification, and the material has good biocompatibility, so that the material has wide application prospects in the biomedical and bioengineering fields of cell separation and affinity purification, immobilized enzymes, targeted drugs, analytical detection, immunoassay and the like.
Magnetic polyphenylEthylene microspheres (PS/Fe)3O4) The magnetic polymer microsphere is most commonly applied, and the synthesis method mainly comprises an embedding method and a monomer polymerization method, wherein the monomer polymerization method comprises suspension polymerization, emulsion polymerization, dispersion polymerization and the like. The existing method has poor swelling effect, thereby causing the size of the magnetic polystyrene microsphere to be nonuniform.
How to prepare a magnetic polystyrene microsphere with uniform size becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of magnetic polystyrene microspheres, and compared with the prior art for preparing magnetic polymer composite microspheres, the microspheres prepared by the method have uniform size; the synthetic route has simple process and is easy to realize industrialization.
The invention is realized by the following steps:
the invention aims to provide a preparation method of the magnetic polystyrene microsphere, which comprises the following steps:
obtaining porous polystyrene microspheres, and dispersing the porous polystyrene microspheres in an organic solution to obtain a mixed solution A, wherein the organic solution is dichloromethane/cyclohexanol or dichloromethane/xylene, and the volume ratio of dichloromethane/cyclohexanol is (90-99): 1-10, wherein the volume ratio of dichloromethane/dimethylbenzene is 1-10: 1;
obtaining oleic acid modified magnetic ferroferric oxide, and dispersing the oleic acid modified magnetic ferroferric oxide in a xylene solution to obtain a mixed solution B;
and uniformly mixing the mixed solution A and the mixed solution B, swelling and adsorbing at room temperature, drying and washing to obtain the magnetic polystyrene microsphere.
Further, the volume ratio of the mass of the porous polystyrene microspheres to the organic mixed solution is 5 mg/mL-50 mg/mL.
Further, the volume ratio of the mass of the porous polystyrene microspheres to the organic mixed solution is 10 mg/mL-20 mg/mL; the organic solution is dichloromethane/cyclohexanol or dichloromethane/xylene, and the volume ratio of dichloromethane/cyclohexanol is 93-97: 3-7, wherein the volume ratio of dichloromethane/dimethylbenzene is 6-9: 1.
further, the ratio of the mass of the porous polystyrene microspheres to the volume of the organic mixed solution is 15 mg/mL; the organic solution is dichloromethane/cyclohexanol or dichloromethane/xylene, and the volume ratio of dichloromethane/cyclohexanol is 95: 5, the volume ratio of the dichloromethane to the xylene is 8: 1.
further, the above porous polystyrene microspheres may be commercially available or prepared by polymerization; polymerization reactions include emulsion polymerization, soap-free emulsion polymerization, microemulsion polymerization, miniemulsion polymerization, dispersion polymerization, suspension polymerization, and seed polymerization.
Further, the mass ratio of the oleic acid modified magnetic ferroferric oxide to the volume ratio of the xylene solution is 30 mg/mL-60 mg/mL.
Further, when the mixed solution A and the mixed solution B are uniformly mixed, the mixing ratio is as follows 100: and (3) uniformly mixing the components in a volume ratio of 10-30.
Further, the method for obtaining the oleic acid modified magnetic ferroferric oxide comprises the following steps:
weighing ferric acetylacetonate, dissolving the ferric acetylacetonate in the oleic acid/oleylamine/benzyl alcohol mixed solution, uniformly mixing, reacting for 6-12 h at 100-220 ℃, cooling to room temperature, washing, sequentially adding oleic acid, oleylamine and cyclohexane, performing ultrasonic dispersion, and washing to obtain the oleic acid modified magnetic ferroferric oxide.
Furthermore, the volume ratio of oleic acid, oleylamine and benzyl alcohol in the oleic acid/oleylamine/benzyl alcohol mixed solution is 1-3: 1-3: 6-10; the ratio of the mass of the iron acetylacetonate to the volume of the oleic acid/oleylamine/benzyl alcohol mixed solution is 1: 0.001-1 g/ml; the volume ratio of the oleic acid, the oleylamine and the cyclohexane is 0.1-0.3: 0.1-0.3: 1-5; the volume ratio of the mass of the iron acetylacetonate to the cyclohexane (1 g/ml-3 g/ml) is as follows: (1 g/ml-5 g/ml).
Further, the drying includes: and (3) drying at 40-50 ℃ in vacuum for 6-12 h to swell and adsorb at room temperature.
Further, the washing includes: and repeatedly washing the solid after the solvent is removed by drying with 10% ethanol for many times, treating with 1-3M hydrochloric acid for 2-10 h, and washing with 10% ethanol for many times to obtain the magnetic polystyrene microspheres.
Compared with the prior art, the invention has the following advantages and effects:
the preparation method of the magnetic polystyrene microsphere provided by the invention comprises the steps of dispersing the porous polystyrene microsphere and the oleic acid modified magnetic ferroferric oxide in different solvents respectively, then uniformly mixing the porous polystyrene microsphere and the oleic acid modified magnetic ferroferric oxide according to a certain volume ratio for swelling adsorption, swelling the porous polystyrene microsphere, and penetrating the hydrophobic oleic acid modified magnetic ferroferric oxide into the porous polystyrene microsphere; after the solvent is removed by drying, the organic solvent is volatilized, the porous polystyrene microsphere is deswelled, and the pores of the porous polystyrene microsphere can shrink, so that the magnetic ferroferric oxide particles are firmly arranged in the porous polystyrene microsphere.
The inventor discovers through experimental exploration that the swelling effect of the porous polystyrene microspheres in a dichloromethane/cyclohexanol mixed solution is good; and controlling the organic solution to be dichloromethane/cyclohexanol or dichloromethane/xylene, wherein the volume ratio of dichloromethane/cyclohexanol is 90-99: 1-10, wherein the volume ratio of dichloromethane/dimethylbenzene is 1-10: 1; thereby successfully swelling the magnetic nanoparticles into the interior of the porous polystyrene microspheres. The finally prepared magnetic polystyrene microspheres are uniform in size and have an average particle size of 3-10 um; the monodispersity is good, and the dispersion coefficient is less than 5 percent; the specific saturation magnetization is high, the magnetic content is uniformly distributed, and the saturation magnetization is 41-53 wt%.
Drawings
FIG. 1 is an electron micrograph of magnetic polystyrene microspheres prepared in example 1 of the present invention;
FIG. 2 is an electron micrograph of magnetic polystyrene microspheres prepared in example 2 of the present invention;
FIG. 3 is an electron micrograph of magnetic polystyrene microspheres prepared in example 3 of the present invention;
FIG. 4 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 1 of the present invention;
FIG. 5 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 2 of the present invention;
FIG. 6 is an electron micrograph of magnetic polystyrene microspheres prepared in comparative example 3 according to the present invention;
FIG. 7 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 4 of the present invention;
FIG. 8 is an electron micrograph of magnetic polystyrene microspheres prepared in example 12 of the present invention;
FIG. 9 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 7 of the present invention;
FIG. 10 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 8 of the present invention;
FIG. 11 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 9 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be obtained by an existing method.
The technical scheme provided by the embodiment of the invention is to provide a preparation method of magnetic polystyrene microspheres, and the general idea is as follows:
step 1, obtaining porous polystyrene microspheres, dispersing the porous polystyrene microspheres in an organic solution to obtain a mixed solution A, wherein the volume ratio of the mass of the porous polystyrene microspheres to the volume of the organic mixed solution is 5 mg/mL-50 mg/mL; if the mass-to-volume ratio is less than 5mg/mL, the concentration is too low, the reaction system is too large, the required reaction time, the required container, the required raw material dosage and the like need to be increased, and the operation difficulty and the cost are increased; if the mass-to-volume ratio is more than 50mg/mL, the concentration is too high, agglomeration is easy, and the system is not uniform.
The first scheme is as follows: the organic solution is dichloromethane/cyclohexanol, and the volume ratio of the dichloromethane to the cyclohexanol is (90-99): 1 to 10. The applicant has found that better swelling is obtained with said dichloromethane/cyclohexanol, if the dichloromethane/cyclohexanol volume ratio is less than 90: 10 or a dichloromethane/cyclohexanol volume ratio greater than 99: 1 is not beneficial to the swelling effect of the microspheres, and the magnetic particles are not easy to load in the microspheres.
Scheme II: the organic solution is dichloromethane/xylene, and the volume ratio of the dichloromethane to the xylene is 1-10: 1. the applicant has found that better swelling is obtained by selecting said dichloromethane/xylene if the dichloromethane/xylene volume ratio is less than 1: 1 or a dichloromethane/xylene volume ratio greater than 9: 1 is not beneficial to the swelling effect of the microspheres, and the magnetic particles are not easy to load in the microspheres.
And 3, uniformly mixing the mixed solution A and the mixed solution B, performing swelling adsorption at room temperature, drying and washing to obtain the magnetic polystyrene microsphere. When the mixed solution A and the mixed solution B are uniformly mixed, the mixing ratio is 100: and (3) uniformly mixing according to the volume ratio of 10-30. Therefore, the selection of 100: the volume ratio of 10-30 is uniformly mixed mainly for ensuring the sufficient magnetic content of the microspheres, and if the volume ratio is less than 100: 30, if the volume ratio is more than 100: 10 the microspheres prepared are easily agglomerated.
According to the preparation method of the magnetic polystyrene microsphere, the porous polystyrene microsphere and the oleic acid modified magnetic ferroferric oxide are dispersed in different solvents respectively, then are uniformly mixed according to a certain volume ratio for swelling adsorption, the porous polystyrene microsphere is swelled, and the hydrophobic oleic acid modified magnetic ferroferric oxide is permeated into the porous polystyrene microsphere; after the solvent is removed by drying, the organic solvent is volatilized, the porous polystyrene microsphere is deswelled, and the pores of the porous polystyrene microsphere can shrink, so that the magnetic ferroferric oxide particles are firmly arranged in the porous polystyrene microsphere. The inventor discovers through experimental exploration that the swelling effect of the porous polystyrene microspheres in a dichloromethane/cyclohexanol mixed solution is good; the finally prepared magnetic polystyrene microspheres are uniform in size and have an average particle size of 3-10 um; the monodispersity is good, and the dispersion coefficient is less than 5 percent; has higher saturation magnetization and uniform magnetic content distribution, and the saturation magnetization rate is 41 to 53wt percent.
The precipitation strengthening type high strength and toughness medium manganese steel plate and the preparation method thereof will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
1. Preparing porous polystyrene microspheres:
2. weighing 2g of iron acetylacetonate, dissolving the iron acetylacetonate in an oleic acid/oleylamine/benzyl alcohol mixed solution (the volume ratio of oleic acid/oleylamine/benzyl alcohol is 2: 2: 7), transferring the mixture to a polytetrafluoroethylene-lined high-temperature reaction kettle, reacting for 6 to 12 hours at 150 ℃, cooling to room temperature, repeatedly washing for three times by using 95% alcohol, sequentially supplementing 0.2mL of oleic acid, 0.2mL of oleylamine and 3mL of cyclohexane, and repeatedly washing for three times by using 95% after ultrasonic dispersion to obtain the oleic acid-modified magnetic ferroferric oxide.
3. Swelling the magnetic nano-particles into the porous polystyrene microspheres to obtain the magnetic polystyrene microspheres, which comprises the following steps:
step 1, dispersing prepared porous polystyrene microspheres in a dichloromethane/cyclohexanol mixed solution, wherein the volume ratio of the mass of the porous polystyrene microspheres to the dichloromethane/cyclohexanol mixed solution is 5mg/mL, so as to obtain a mixed solution A;
step 3, mixing the mixed solution A and the mixed solution B according to the ratio of 5: and (2) uniformly mixing in a volume ratio of 995, swelling and adsorbing at room temperature for 6-12 h, drying at 40-50 ℃ under vacuum to remove the solvent, washing (repeatedly washing with 10% ethanol for multiple times, then treating the solid matter with 1-3M hydrochloric acid for 2-10 h, and repeatedly washing with 10% ethanol for multiple times) to obtain the magnetic polystyrene microsphere.
4. The properties of the magnetic polystyrene microspheres prepared are shown in table 5. The electron micrograph of the magnetic polystyrene microsphere is shown in figure 1.
Example 2
1. Preparing the porous polystyrene microspheres.
2. Weighing 1g of iron acetylacetonate, dissolving in an oleic acid/oleylamine/benzyl alcohol mixed solution (the volume ratio of oleic acid/oleylamine/benzyl alcohol is 1: 1: 10), transferring the mixture to a polytetrafluoroethylene-lined high-temperature reaction kettle, reacting for 6-12 h at 100 ℃, cooling to room temperature, repeatedly washing with 95% alcohol for three times, sequentially supplementing 0.3mL of oleic acid, 0.1mL of oleylamine and 1mL of cyclohexane, and repeatedly washing with 95% for three times after ultrasonic dispersion to obtain the oleic acid-modified magnetic ferroferric oxide.
3. Swelling the magnetic nano-particles into the porous polystyrene microspheres to obtain the magnetic polystyrene microspheres, which comprises the following steps:
step 1, dispersing prepared porous polystyrene microspheres in a dichloromethane/cyclohexanol mixed solution, wherein the volume ratio of the mass of the porous polystyrene microspheres to the dichloromethane/cyclohexanol mixed solution is 1mg/mL, so as to obtain a mixed solution A;
and 3, mixing the mixed solution A and the mixed solution B according to the ratio of 1: 999 volume ratio mixing, swelling and adsorbing for 6-12 h at room temperature, drying to remove the solvent, washing (repeatedly washing with 10% ethanol for many times, then treating the solid matter with 1-3M hydrochloric acid for 2-10 h, and repeatedly washing with 10% ethanol for many times) to obtain the magnetic polystyrene microsphere.
4. The properties of the prepared magnetic polystyrene microspheres are shown in table 5; the electron micrograph of the magnetic polystyrene microsphere is shown in FIG. 2.
Example 3
1. Preparing porous polystyrene microspheres:
2. weighing 3g of iron acetylacetonate, dissolving the iron acetylacetonate in an oleic acid/oleylamine/benzyl alcohol mixed solution (the volume ratio of oleic acid/oleylamine/benzyl alcohol is 3: 3: 6), transferring the mixture to a polytetrafluoroethylene-lined high-temperature reaction kettle, reacting for 6 to 12 hours at 220 ℃, cooling to room temperature, repeatedly washing for three times by using 95% alcohol, sequentially supplementing 0.1mL of oleic acid, 0.3mL of oleylamine and 5mL of cyclohexane, and repeatedly washing for three times by using 95% after ultrasonic dispersion to obtain the oleic acid-modified magnetic ferroferric oxide.
3. Swelling the magnetic nano-particles into the porous polystyrene microspheres to obtain the magnetic polystyrene microspheres, which comprises the following steps:
step 1, dispersing prepared porous polystyrene microspheres in a dichloromethane/cyclohexanol mixed solution, wherein the volume ratio of the mass of the porous polystyrene microspheres to the dichloromethane/cyclohexanol mixed solution is 10mg/mL, and obtaining a mixed solution A;
step 3, mixing the mixed solution A and the mixed solution B according to the ratio of 10: 990 volume ratio, swelling and adsorbing for 6-12 h at room temperature, drying to remove the solvent, washing (repeatedly washing with 10% ethanol for many times, then treating the solid matter with 1-3M hydrochloric acid for 2-10 h, and repeatedly washing with 10% ethanol for many times) to obtain the magnetic polystyrene microsphere.
4. The properties of the prepared magnetic polystyrene microspheres are shown in table 5; the electron micrograph of the magnetic polystyrene microsphere is shown in FIG. 3.
For convenience of illustration, each of examples and comparative examples is summarized in tables 1 to 4, and other parameters not listed in the tables are the same as those of example 1.
TABLE 1 organic solutions of dichloromethane/cyclohexanol in different volume ratios
TABLE 2 Mass-to-volume ratios of porous polystyrene microspheres to the organic mixed solution in each group
TABLE 3 organic solutions of dichloromethane/xylene in different volume ratios
TABLE 4 volume ratio of mixed solution A to mixed solution B in different groups
The magnetic polystyrene microspheres prepared for each group are shown in tables 5-8.
TABLE 5 influence of organic solutions of dichloromethane/cyclohexanol in different volume ratios on microsphere Performance
TABLE 6 influence of Mass-to-volume ratio of porous polystyrene microspheres to the organic mixed solution on microsphere Performance
| Group of | Average particle diameter um | Coefficient of dispersion% | Saturation magnetic susceptibility wt% | Skeleton density (kg.m)-3) |
| Comparative example 5 | 5.4 | 5.4 | 36 | 1.2 |
| Example 6 | 5.3 | 3.1 | 45 | 1.3 |
| Example 7 | 5.4 | 2.1 | 42 | 1.5 |
| Example 8 | 5.3 | 2.3 | 44 | 1.6 |
| Example 9 | 5.4 | 2.8 | 45 | 1.4 |
| Comparative example 6 | 5.3 | 5.1 | 39 | 1.2 |
TABLE 7 influence of organic solutions of different volume ratios of dichloromethane/xylene on microsphere Properties
| Group of | Average particle diameter um | Coefficient of dispersion% | Saturation magnetic susceptibility wt% | Skeleton density (kg.m)-3) |
| Comparative example 7 | 5.4 | 3.3 | 37 | 1.0 |
| Example 10 | 5.4 | 3.4 | 42 | 1.3 |
| Example 11 | 5.3 | 3.2 | 44 | 1.4 |
| Example 12 | 5.4 | 2.4 | 52 | 1.8 |
| Example 13 | 5.3 | 2.2 | 51 | 1.6 |
| Example 14 | 5.2 | 1.9 | 46 | 1.7 |
| Comparative example 8 | 5.3 | 3.1 | 24 | 1.2 |
| Comparative example 3 | 5.4 | 3.3 | 16 | 1.1 |
| Comparative example 9 | 5.3 | 3.1 | 17 | 1.2 |
TABLE 8 influence of the volume ratio of the mixed solution A and the mixed solution B on the performance of the microspheres
| Group of | Average particle diameter um | Coefficient of dispersion% | Saturation magnetic susceptibility wt% | Skeleton density (kg.m)-3) |
| Comparative example 10 | 5.4 | 5.4 | 31 | 1.3 |
| Example 15 | 5.3 | 2.1 | 45 | 1.5 |
| Example 1 | 5.2 | 1.8 | 53 | 2.0 |
| Example 16 | 5.3 | 2.3 | 46 | 1.7 |
| Comparative example 11 | 5.4 | 6.1 | 24 | 1.2 |
1. As can be seen from Table 5, the magnetic polystyrene microspheres in examples 1 to 5 of the present invention have higher saturation magnetic susceptibility than those in comparative examples 1 to 4;
FIG. 1 is an electron micrograph of magnetic polystyrene microspheres prepared in example 1 of the present invention; as can be seen from FIG. 1, the surface of the microsphere is smooth, the amount of the residual magnetic nanoparticles and the residual amount on the surface are small, and the magnetic nanoparticles are well in the microsphere.
FIG. 4 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 1 of the present invention; FIG. 5 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 2 of the present invention; FIG. 6 is an electron micrograph of magnetic polystyrene microspheres prepared in comparative example 3 according to the present invention; FIG. 7 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 4 of the present invention; the number of magnetic nanoparticles remaining in fig. 4-7, as well as the residual amount on the surface, was large, and the surface of the microspheres was not smooth.
In conclusion, the volume ratio of dichloromethane to cyclohexanol is 90-99: 1-10, the swelling effect of the microspheres is facilitated, and the magnetic particles are easily loaded into the microspheres.
2. As can be seen from Table 6, the more the dispersion coefficients of examples 6 to 9 of the present invention are close to 1, the better the uniformity is, compared with comparative examples 5 to 6, indicating that the ratio of the mass of the porous polystyrene microspheres to the volume of the organic mixed solution is 5mg/mL to 50mg/mL, which is advantageous for the uniformity of the system.
3. As can be seen from Table 7, the magnetic polystyrene microspheres in examples 10 to 14 of the present invention have higher saturation magnetic susceptibility than those in comparative examples 7 to 9;
FIG. 8 is an electron micrograph of magnetic polystyrene microspheres prepared in example 12 of the present invention; from fig. 8, it can be seen that the surface of the microsphere is smooth, the amount of the residual magnetic nanoparticles and the residual amount on the surface are small, and the magnetic nanoparticles are well in the interior of the microsphere.
FIG. 9 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 7 of the present invention; FIG. 10 is an electron micrograph of magnetic polystyrene microspheres prepared according to comparative example 8 of the present invention; FIG. 11 is an electron micrograph of magnetic polystyrene microspheres according to comparative example 9 of the present invention; the number of magnetic nanoparticles remaining in fig. 9-11, as well as the residual amount on the surface, was large, and the surface of the microspheres was not smooth.
In conclusion, the volume ratio of dichloromethane to xylene is 1-10: 1, the swelling effect of the microspheres is facilitated, and the magnetic particles are easily loaded in the microspheres.
3. As can be seen from Table 8, the magnetic polystyrene microspheres of examples 1 and 15 to 16 of the present invention had dispersion coefficients closer to 1 and higher saturation magnetizations than those of comparative examples 10 to 11; the volume ratio of the mixed solution a to the mixed solution B was shown to be 100: 10-30 is beneficial to the uniformity of the system and simultaneously ensures the sufficient magnetic content of the microspheres.
To sum up, this application is through controlling organic solution is dichloromethane/cyclohexanol or dichloromethane/xylene, dichloromethane/cyclohexanol volume ratio is 90 ~ 99: 1-10, wherein the volume ratio of dichloromethane/dimethylbenzene is 1-10: 1; thereby successfully swelling the magnetic nanoparticles into the interior of the porous polystyrene microspheres. The finally prepared magnetic polystyrene microspheres are uniform in size and have an average particle size of 3-10 um; the monodispersity is good, and the dispersion coefficient is less than 5 percent; the specific saturation magnetization is high, the magnetic content is uniformly distributed, and the saturation magnetization is 41-53 wt%.
The invention is not to be considered as limited to the particular embodiments shown, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The preparation method of the magnetic polystyrene microsphere is characterized by comprising the following steps of:
obtaining porous polystyrene microspheres, and dispersing the porous polystyrene microspheres in an organic solution to obtain a mixed solution A, wherein the organic solution is dichloromethane/cyclohexanol, and the volume ratio of the dichloromethane to the cyclohexanol is (90-99): 1-10;
obtaining oleic acid modified magnetic ferroferric oxide, and dispersing the oleic acid modified magnetic ferroferric oxide in a dimethylbenzene solution to obtain a mixed solution B;
uniformly mixing the mixed solution A and the mixed solution B, performing swelling adsorption at room temperature, drying and washing to obtain magnetic polystyrene microspheres; the volume ratio of the mass of the porous polystyrene microspheres to the organic mixed solution is 5 mg/mL-50 mg/mL.
2. The method for preparing magnetic polystyrene microspheres as claimed in claim 1, wherein the ratio of the mass of the porous polystyrene microspheres to the volume of the organic mixed solution is 10mg/mL to 20 mg/mL; the organic solution is dichloromethane/cyclohexanol, and the volume ratio of dichloromethane to cyclohexanol is 93-97: 3 to 7.
3. The method for preparing magnetic polystyrene microspheres as claimed in claim 1, wherein the ratio of the mass of the porous polystyrene microspheres to the volume of the organic mixed solution is 15 mg/mL; the organic solution is dichloromethane/cyclohexanol, and the volume ratio of dichloromethane/cyclohexanol is 95: 5.
4. the method for preparing magnetic polystyrene microspheres as claimed in claim 1, wherein the volume ratio of the mass of the oleic acid-modified magnetic ferroferric oxide to the xylene solution is 30 mg/mL-60 mg/mL.
5. The method for preparing magnetic polystyrene microspheres according to claim 1, wherein the ratio of the mixed solution A to the mixed solution B is 100: and (3) uniformly mixing the components in a volume ratio of 10-30.
6. The preparation method of the magnetic polystyrene microsphere as claimed in claim 1, wherein the step of obtaining the oleic acid modified magnetic ferroferric oxide comprises the following steps:
weighing ferric acetylacetonate, dissolving the ferric acetylacetonate in the oleic acid/oleylamine/benzyl alcohol mixed solution, uniformly mixing, reacting for 6-12 h at 100-220 ℃, cooling to room temperature, washing, sequentially adding oleic acid, oleylamine and cyclohexane, performing ultrasonic dispersion, and washing to obtain the oleic acid modified magnetic ferroferric oxide.
7. The method of claim 1, wherein the drying comprises: drying at 40-50 ℃ in vacuum, and swelling and adsorbing at room temperature for 6-12 h.
8. The method of claim 1, wherein the washing comprises: and repeatedly washing the solid after the solvent is removed by drying with 10% ethanol for many times, treating the solid with 1M-3M hydrochloric acid for 2 h-10 h, and washing with 10% ethanol for many times to obtain the magnetic polystyrene microsphere.
9. Magnetic polystyrene microspheres prepared by the process according to any one of claims 1 to 8.
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