Preparation method of nanosilver and sulfydryl jointly modified magnetic microspheres

Abstract

The invention belongs to the technical field of magnetic materials and in particular relates to a preparation method of nanosilver and sulfydryl jointly modified magnetic microspheres. The preparation method comprises the following steps of: 1) preparing Fe3O4 magnetic microspheres; 2) preparing SiO2 wrapped Fe3O4 magnetic microspheres; (3) preparing sulfydryl modified SiO2 wrapped Fe3O4 magnetic microspheres; and 4) preparing nanosilver and sulfydryl jointly modified SiO2 wrapped Fe3O4 magnetic microspheres. According to the method, nano Fe3O4 is wrapped by a silane coupling agent and the stability and the acid-base resistance are improved due to the safety and the stability of silica; and a functional sulfydryl group is introduced into the surface through chemical reaction, so that novel modified magnetic nanoparticles are obtained. Due to investment and development of biological technology industry, life science and diagnostic reagent industry, the development of biological magnetic bead products with the technological advantage and the cost performance advantage is greatly promoted.

Description

technical field

[0001] The invention belongs to the technical field of magnetic materials, in particular to a method for preparing magnetic microspheres co-modified with nano-silver and mercapto groups. Background technique

[0002] The synthesis of nanostructured magnetic materials has become a very important research field due to their potential applications such as ferrofluids, catalysts, color pigments, high-density magnetic recording media, and magnetic pharmaceuticals, etc. Among many magnetic materials, Fe3O4 has excellent ferromagnetic properties and has been widely used in various fields, most notably as a magnetic recording medium material. Due to the advantages of high chemical stability, good biocompatibility and good thermal stability of Fe3O4 nanoparticles in the alternating field, the ferrofluid of Fe3O4 nanoparticles is used as a high-temperature magnetic fluid (MFH) for the treatment of tumors. cure. The preparation of Fe3O4 nanoparticles by wet chemical m...

Examples

Embodiment 1

[0030] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 5g of anhydrous ferric chloride and add it to 80mL of glycerol solvent, then add sodium hexametaphosphate with an equimolar number to ferric chloride, treat with ultrasonic waves with a frequency of 20kHz for 30min, and stir The speed is 1000 rev / min, magnetically stirred for 1 hour until a uniform mixed system is obtained, poured into a PTFE-lined reaction kettle with a volume of 100mL, then placed in a drying oven, and reacted at a constant temperature of 220°C for 6 hours , after cooling to room temperature, the precipitate was repeatedly washed with absolute ethanol and distilled water until the pH of the washing solution was 7, and dried in vacuum under the condition of a vacuum of -0.1Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0031] 2) SiO2 2 Preparation of coated magnetic microspheres: the Fe obtained in step 1) 3 o 4 Place 0.5g of magnetic microspheres evenly in a sodium hexametaphospha...

Embodiment 2

[0036] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 60g of ferric chloride hydrate and add it to 400mL of ethylene glycol solvent, then add ethylenediamine which is 3 times the molar number of ferric chloride, ultrasonic for 30min, stirring speed is 1000 rpm, Stir magnetically for 1 hour until a uniform mixed system is obtained, pour it into a PTFE-lined reaction kettle with a volume of 500mL, and then place it in a drying oven, react at a constant temperature of 180°C for 36 hours, and cool to room temperature. Repeated washing with absolute ethanol and distilled water until the pH of the washing solution = 7, and vacuum drying under the condition of a vacuum degree of -0.08Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0037] 2) SiO2 2 Preparation of wrapped magnetic microspheres: Place 0.5 g of magnetic microspheres obtained in step 1 evenly in a disodium edetate solution with a mass concentration of 10 g / L, soak for 6 hours, filter, and then disper...

Embodiment 3

[0042] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 2g of ferric nitrate hydrate and add it to 40mL of propylene glycol solvent, then add trisodium citrate with the same molar number as ferric nitrate, ultrasonic 30min, stirring speed is 1000rpm, magnetic stirring for 1 hour until Obtain a uniform mixed system, pour it into a polytetrafluoroethylene-lined reaction kettle with a volume of 50mL, then place it in a drying box, and react at a constant temperature of 190°C for 20 hours. After cooling to room temperature, the precipitate is washed with absolute ethanol and Repeated washing with distilled water until the pH of the washing solution = 7, and vacuum drying under the condition of a vacuum degree of -0.08Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0043] 2) SiO2 2 Preparation of wrapped magnetic microspheres: Place 0.5 g of magnetic microspheres obtained in step 1 evenly in a disodium edetate solution with a mass concentration of 30 g / L, soak f...

technical field

[0001] The invention belongs to the technical field of magnetic materials, in particular to a method for preparing magnetic microspheres co-modified with nano-silver and mercapto groups. Background technique

[0002] The synthesis of nanostructured magnetic materials has become a very important research field due to their potential applications such as ferrofluids, catalysts, color pigments, high-density magnetic recording media, and magnetic pharmaceuticals, etc. Among many magnetic materials, Fe3O4 has excellent ferromagnetic properties and has been widely used in various fields, most notably as a magnetic recording medium material. Due to the advantages of high chemical stability, good biocompatibility and good thermal stability of Fe3O4 nanoparticles in the alternating field, the ferrofluid of Fe3O4 nanoparticles is used as a high-temperature magnetic fluid (MFH) for the treatment of tumors. cure. The preparation of Fe3O4 nanoparticles by wet chemical m...

Examples

Embodiment 1

[0030] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 5g of anhydrous ferric chloride and add it to 80mL of glycerol solvent, then add sodium hexametaphosphate with an equimolar number to ferric chloride, treat with ultrasonic waves with a frequency of 20kHz for 30min, and stir The speed is 1000 rev / min, magnetically stirred for 1 hour until a uniform mixed system is obtained, poured into a PTFE-lined reaction kettle with a volume of 100mL, then placed in a drying oven, and reacted at a constant temperature of 220°C for 6 hours , after cooling to room temperature, the precipitate was repeatedly washed with absolute ethanol and distilled water until the pH of the washing solution was 7, and dried in vacuum under the condition of a vacuum of -0.1Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0031] 2) SiO2 2 Preparation of coated magnetic microspheres: the Fe obtained in step 1) 3 o 4 Place 0.5g of magnetic microspheres evenly in a sodium hexametaphospha...

Embodiment 2

[0036] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 60g of ferric chloride hydrate and add it to 400mL of ethylene glycol solvent, then add ethylenediamine which is 3 times the molar number of ferric chloride, ultrasonic for 30min, stirring speed is 1000 rpm, Stir magnetically for 1 hour until a uniform mixed system is obtained, pour it into a PTFE-lined reaction kettle with a volume of 500mL, and then place it in a drying oven, react at a constant temperature of 180°C for 36 hours, and cool to room temperature. Repeated washing with absolute ethanol and distilled water until the pH of the washing solution = 7, and vacuum drying under the condition of a vacuum degree of -0.08Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0037] 2) SiO2 2 Preparation of wrapped magnetic microspheres: Place 0.5 g of magnetic microspheres obtained in step 1 evenly in a disodium edetate solution with a mass concentration of 10 g / L, soak for 6 hours, filter, and then disper...

Embodiment 3

[0042] 1) Magnetic Fe 3 o 4 Preparation of microsphere particles: Weigh 2g of ferric nitrate hydrate and add it to 40mL of propylene glycol solvent, then add trisodium citrate with the same molar number as ferric nitrate, ultrasonic 30min, stirring speed is 1000rpm, magnetic stirring for 1 hour until Obtain a uniform mixed system, pour it into a polytetrafluoroethylene-lined reaction kettle with a volume of 50mL, then place it in a drying box, and react at a constant temperature of 190°C for 20 hours. After cooling to room temperature, the precipitate is washed with absolute ethanol and Repeated washing with distilled water until the pH of the washing solution = 7, and vacuum drying under the condition of a vacuum degree of -0.08Mpa to obtain Fe 3 o 4 Magnetic microspheres;

[0043] 2) SiO2 2 Preparation of wrapped magnetic microspheres: Place 0.5 g of magnetic microspheres obtained in step 1 evenly in a disodium edetate solution with a mass concentration of 30 g / L, soak f...

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