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Nano/micron microsphere with superparamagnetism and preparation method

A superparamagnetic and nano-microsphere technology, applied in the direction of the magnetism of inorganic materials, can solve the problems of large changes in the magnetic content of particles, irregular particle shapes, and affecting the use effect, etc., and achieve stable physical and chemical properties, uniform size, and spherical formation. Good results

Inactive Publication Date: 2004-08-11
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the particle size of the magnetic particles is too small, the agglomeration phenomenon is inevitable during the reaction process, the shape of the obtained particles is irregular, and the synthesized microspheres have some defects in performance, such as some Fe 3 o 4 The particles are exposed outside, the magnetic content of different particles varies greatly, and the uniformity is poor. In practical applications, it is easy to agglomerate and affect the use effect.

Method used

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  • Nano/micron microsphere with superparamagnetism and preparation method
  • Nano/micron microsphere with superparamagnetism and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Magnetic Fe by Co-precipitation 3 o 4 nanoparticles

[0032] Add 0.043 molar FeCl to a 1-liter stirred reactor containing 500 ml deionized water 2 4H 2 O and 0.086 mol FeCl 3 ·6H 2 O, under the protection of nitrogen, the temperature was raised to 85-90 ° C, and the mixture containing 0.478 moles of NH was poured into 3 ·H 2 O aqueous solution, the color of the solution turns black immediately, and then the deposited product is separated by using a magnetic field and washed once with deionized water and 0.02M NaCl respectively.

[0033] The total weight of the above-mentioned magnetic aggregates is about 30g, of which Fe 3 o 4 About 10g, observed by transmission electron microscope Fe 3 o 4 The particles are nearly spherical, with superparamagnetic properties, and the average particle size is 8nm.

Embodiment 2

[0035] Add 0.21 molar FeCl to a 1 liter stirred reactor containing 700 ml deionized water 2 4H 2 O and 0.31 mol FeCl 3 ·6H 2 O, heat up to 70°C, pour 100ml of NaHCO containing 1 mole 3 aqueous solution, magnetic separation and decanting supernatant to obtain freshly prepared Fe 3 o 4 nanoparticles.

[0036] The total weight of the above-mentioned magnetic aggregates is about 60g, of which Fe 3 o 4 About 35g, observed by transmission electron microscope Fe 3 o 4 The particles are nearly spherical, with superparamagnetic properties, and the average particle size is 15nm.

Embodiment 3

[0038] Preparation of SiO by Acidification 2 coated magnetic microspheres

[0039] Calculate 10g Fe 3 o 4 Coated with 20g SiO 2 Need corresponding Na 2 SiO 3 9H 2 O about 95g, pre-adjusted Na 2 SiO 3 Solution pH to 12-13

[0040] (1). The fresh Fe prepared in Example 1 3 o 4 Nanoparticles, ultrasonically dispersed in pretreated Na 2 SiO 3 in solution.

[0041] (2).Heat the solution to 85°C, add hydrochloric acid with a concentration of about 2mol / l to the solution under high-speed stirring; adjust the pH value of the solution from alkaline to about 5-7, separate the product with a magnet and use Wash with deionized water 3-4 times and dry. get surface-coated SiO 2 Magnetic microspheres, SiO 2 and Fe 3 o 4 The weight ratio is 2:1.

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Abstract

The invention is specially related to method for preparing nano / micron microsphere with superparamagnetism through silanization. SiO2 with different content and number of layer are utilized to cover surface of Fe3O4 nano granule of new prepared in order to control grain size and avoid agglomeration. Then, under a moderate condition, silanization is carried out for surface of magnetic microsphere with silicon covered so as to obtain superparamagnetism microsphere with functional groups on surface. Grain size is in 30 nm-1000 nm / 1-20 um. Magnetic Fe3O4 is in 0.5-60% (weight percent) of whole microsphere. The invention features of controllable grain size, good sphericity, even magnetism content, and stable physical and chemical performances.

Description

technical field [0001] The invention belongs to the field of superparamagnetic functional microspheres, in particular to superparamagnetic nano / micro microspheres and a method for preparing superparamagnetic nano / micro microspheres by silanization. Background technique [0002] Magnetic microspheres, especially nano-scale magnetic functional microspheres, can be chemically coupled to the surface of enzymes, antibodies, antigens and other biologically active substances. , No remanence, to achieve fast and easy separation of reactants. It has attractive application prospects in biomedical fields such as immobilized enzymes, immunoassays, protein purification, targeted delivery, and stem cell separation, and belongs to the frontier field of current disciplines. [0003] The methods for synthesizing superparamagnetic microspheres in the prior art mainly include embedding method, monomer copolymerization method, chemical conversion method, polymer chemical r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/26C04B35/628H01F1/36
Inventor 刘先桥刘会洲邢建民张冠东
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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