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Method of producing magnetic microsphere with surface functional group

A technology of surface functional groups and magnetic microspheres, applied in the field of composite materials, can solve problems such as limiting applications

Inactive Publication Date: 2008-05-21
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of magnetic nanospheres prepared in this patent is mainly concentrated in 20nm-125nm, and its preparation method is limited to hydrophilic monomers, and does not involve the control of surface functional groups. These characteristics greatly limit its practical application.

Method used

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  • Method of producing magnetic microsphere with surface functional group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 10ml styrene, 0.79g polyvinylpyrrolidone (PVP K30), 0.099g azobisisobutyronitrile, 0.095g magnetic Fe 3 o 4 Add 50ml of ethanol solution and 6ml of deionized water into the three-necked flask, and ultrasonically disperse them evenly. Then nitrogen gas (N 2 ) to deoxygenate for 5 minutes, and under the action of stirring (120 rpm), the reaction temperature was raised to 70° C. for 24 hours. After the reaction is completed, the mixed solution is first subjected to magnetic separation using ethanol as a solvent for 3-5 times, and the supernatant is removed; then, it is dispersed and magnetically separated for 3-5 times with deionized water, and finally the obtained magnetic precipitate is lyophilized and stored.

[0019] Take 2 g of the above magnetic microspheres, add 66.7ml of 98% concentrated sulfuric acid, and disperse the microspheres evenly with ultrasound. Then the mixed solution was heated to 50° C. and reacted for 6 h under the condition of magnetic stirri...

Embodiment 2

[0022] Take 4ml styrene, 2.5ml acrylic acid, 0.4g polyvinylpyrrolidone (PVP K30), 0.032g azobisisoheptanonitrile, 0.0325g magnetic Fe 3 o 4 Add 56ml of ethanol solution into the three-necked flask, and ultrasonically disperse it evenly. Then nitrogen gas (N 2 ) to deoxygenate for 15 minutes, and under the action of stirring (80 rpm), the reaction temperature was raised to 75° C. for 12 hours. After the reaction is completed, the mixed solution is first subjected to magnetic separation using ethanol as a solvent for 3-4 times, and the supernatant is removed; then, magnetic separation is performed 3-4 times with deionized water.

[0023] The particle size of the magnetic microspheres prepared by the above reaction is about 650nm observed by scanning electron microscope, and it can be observed by transmission electron microscope that the inside of the microspheres contains a plurality of magnetic nanoparticles. Using a vibrating sample magnetometer to test the obtained magneti...

Embodiment 3

[0025] Take 1 g of the magnetic microspheres prepared in Example 2, add 20 ml of 98% concentrated sulfuric acid, and disperse the microspheres evenly with ultrasound. Then react at room temperature (25° C.) for 6 h under the condition of magnetic stirring. After the reaction is complete, freeze the mixed solution and add deionized water for magnetic separation, remove the supernatant after separation, and add deionized water again, repeat the above process 8-10 times. The precipitate was freeze-dried for later use.

[0026] The particle size of the magnetic microspheres prepared by the above reaction is about 650nm observed by scanning electron microscope, and it can be observed by transmission electron microscope that the inside of the microspheres contains a plurality of magnetic nanoparticles. Using a vibrating sample magnetometer to test the obtained magnetic microspheres, the saturation magnetization can reach 18emu / g. Microspheres with sulfonate groups, carboxyl groups...

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Abstract

The invention relates to a preparation method of a magnetic microsphere with surface functional groups in the composite material technical field. Under the condition that magnetic nanometer particles exist, dispersion-polymerization is performed; during dispersion-polymerization functional monomers are added to make the surfaces of the magnetic nanometer particles carry functional groups, or / and after finishing the dispersion-polymerization the magnetic microsphere is sulfonated to make the surfaces carry tetrafunctional groups; finally magnetic polymer microsphere solution is gotten, and then the magnetic polymer microsphere solution is magnetically separated, cleaned and dried to get a magnetic microsphere with surface functional groups. The magnetic microsphere has an advantage that the particle size and the surface functional groups are controllable. The invention has the advantages of simple and accurate method, high efficiency, low cost, and capability of application in the biology field.

Description

technical field [0001] The invention relates to a preparation method in the technical field of composite materials, in particular to a preparation method of magnetic microspheres with surface functional groups. Background technique [0002] The research on magnetic microspheres can be traced back to the 1970s. It is a widely used material in the field of biomedicine. It can be mainly used in controlled release of drugs, targeted drug delivery, immobilized enzymes, cell separation, and separation of nucleic acids. and purification, immunoassay, etc. The so-called magnetic microspheres refer to magnetic materials (such as oxides of Fe, Ni, Co or other magnetic materials) contained inside or on the surface (ie, the shell) of the microspheres (diameter 0.5 μm-100 μm), and finally make the microspheres The ball is a material that has a magnetic response under the action of an external magnetic field. In addition to its magnetic responsiveness, the surface-functionalized magneti...

Claims

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Application Information

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IPC IPC(8): H01F1/42C08F2/44C08F12/08C08F20/10C08F4/04C08F2/38C08K3/22
Inventor 孙康窦红静马武伟
Owner SHANGHAI JIAO TONG UNIV
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