Method for preparing monodisperse magnetic silica dioxide nano particles

Abstract

The invention relates to a preparation method to prepare silicon dioxide nanoparticles with the magnetic monodisperse. The processes are as follows: (1) excess ammonia is added into the aqueous solution containing Fe3+ and Fe2+ salts to obtain the black precipitate of Fe3O4; (2) the precipitate is transferred to the alcohol-water solution of sodium oleate and the pH value is regulated to the acidity; (3) sodium silicate is added into the solution, heated and ultrasonically treated and then the silicon dioxide nanoparticles with magnetic disperse is obtained; (4) the coupling agent is added to react to obtain the silicon dioxide nanoparticles with surface modified magnetic monodisperse. The method is provided with low-cost raw material, simple process, low energy consumption and small amount for the necessary equipment. The silicon dioxide nanoparticles produced by the method is provided with excellent performance, which can fully meet the application requirement in the a plurality of fields such as: the drug carrier, the immobilization of the enzyme, the cell sorting, the immunity detection, the separation and hybridization of the nucleic acid.

Description

technical field

[0001] The invention belongs to a preparation method of silica nanoparticles, in particular to a preparation method of monodisperse magnetic silica nanoparticles. Background technique

[0002] In recent years, many organic and inorganic materials have been widely used to coat superparamagnetic nano-Fe 3 o 4 Particles, including natural polymers (such as albumin, chitosan, starch and gelatin, etc.), synthetic polymers (such as polystyrene, polymethyl methacrylate, polylactic acid and polycaprolactone, etc.) and inorganic Materials (such as silicon dioxide and nano-carbon, etc.). Such core-shell composite particles are favored due to their unique advantages in electrical, optical, magnetic, catalytic, and mechanical properties.

[0003] In the field of drug delivery, organic composite particles are limited by their poor thermal and chemical stability and their rapid clearance by the immune system. On the contrary, inorganic composite particles have the foll...

Examples

Embodiment 1

[0034] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 6 with 0.1 mol / l perchloric acid. Add 0.015g of sodium silicate to the above reaction system, then raise the temperature to 80°C, and maintain the temperature for ultrasonic dispersion for 30min. After the sonication is finished, turn to room temperature and add 30 μl (3-mercaptopropyl)trimethoxysi...

Embodiment 2

[0036] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 6 with 0.1 mol / l perchloric acid. Add 30 μl of (3-mercaptopropyl)trimethoxysilane (MPS) and 0.015 g of sodium silicate to the above reaction system, then raise the temperature to 80° C., and maintain the temperature for ultrasonic dispersion for 30 minutes. After the sonication is finished, turn to...

Embodiment 3

[0038] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 5.6 with 0.1 mol / l perchloric acid. Add 0.015g of sodium silicate to the above reaction system, then raise the temperature to 70°C, and maintain the temperature for ultrasonic dispersion for 30min. After the sonication is finished, turn to room temperature and add 40 μl of (3-mercaptopropyl)trimeth...

technical field

[0001] The invention belongs to a preparation method of silica nanoparticles, in particular to a preparation method of monodisperse magnetic silica nanoparticles. Background technique

[0002] In recent years, many organic and inorganic materials have been widely used to coat superparamagnetic nano-Fe 3 o 4 Particles, including natural polymers (such as albumin, chitosan, starch and gelatin, etc.), synthetic polymers (such as polystyrene, polymethyl methacrylate, polylactic acid and polycaprolactone, etc.) and inorganic Materials (such as silicon dioxide and nano-carbon, etc.). Such core-shell composite particles are favored due to their unique advantages in electrical, optical, magnetic, catalytic, and mechanical properties.

[0003] In the field of drug delivery, organic composite particles are limited by their poor thermal and chemical stability and their rapid clearance by the immune system. On the contrary, inorganic composite particles have the foll...

Examples

Embodiment 1

[0034] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 6 with 0.1 mol / l perchloric acid. Add 0.015g of sodium silicate to the above reaction system, then raise the temperature to 80°C, and maintain the temperature for ultrasonic dispersion for 30min. After the sonication is finished, turn to room temperature and add 30 μl (3-mercaptopropyl)trimethoxysi...

Embodiment 2

[0036] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 6 with 0.1 mol / l perchloric acid. Add 30 μl of (3-mercaptopropyl)trimethoxysilane (MPS) and 0.015 g of sodium silicate to the above reaction system, then raise the temperature to 80° C., and maintain the temperature for ultrasonic dispersion for 30 minutes. After the sonication is finished, turn to...

Embodiment 3

[0038] Weigh 2.16g (0.008mol) FeCl 3 ·6H 2 O and 1.11g (0.004mol) FeSO 4 ·7H 2 O was dissolved in 40ml of deionized water, and under the protection of nitrogen at room temperature, 20ml of ammonia water with a concentration of 1.5mol / l was added point by point to the above solution to obtain a black precipitate. The precipitate was fully washed 5 times with deionized water by means of magnetic separation to obtain a black precipitate for future use. Under stirring conditions, 0.0009g Fe 3 o 4 The precipitate was pipetted into a solution of 0.8ml ethanol and 20ml water, and the solution contained 0.00009g sodium oleate. The pH value of the above reaction system was adjusted to 5.6 with 0.1 mol / l perchloric acid. Add 0.015g of sodium silicate to the above reaction system, then raise the temperature to 70°C, and maintain the temperature for ultrasonic dispersion for 30min. After the sonication is finished, turn to room temperature and add 40 μl of (3-mercaptopropyl)trimeth...

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