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Preparation method of mesoporous silica microspheres with pores formed by multi-walled carbon nanotubes

A technology of multi-walled carbon nanotubes and mesoporous silica, applied in the field of preparation of mesoporous silica microspheres, can solve the problems of uneven pore size of mesoporous silica microspheres, unstable micelles, etc. Uniform pore size, high synthesis yield and mild reaction conditions

Pending Publication Date: 2022-02-08
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the general instability of micelles, the pore size of different batches of mesoporous silica microspheres prepared by the same method is not uniform

Method used

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  • Preparation method of mesoporous silica microspheres with pores formed by multi-walled carbon nanotubes
  • Preparation method of mesoporous silica microspheres with pores formed by multi-walled carbon nanotubes
  • Preparation method of mesoporous silica microspheres with pores formed by multi-walled carbon nanotubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Weigh 100mg carboxylated multi-walled carbon nanotubes, 600mg (3-aminopropyl) trimethoxysilane and 150mL ultrapure water respectively in a 250mL beaker, stir magnetically for 10min, filter under reduced pressure to obtain a black solid, and use 250 mL of ethanol was fully washed to remove unreacted (3-aminopropyl)trimethoxysilane, dried in vacuo, and weighed to obtain 558 mg.

[0029] (2) Weigh 240 mg of the silicon source precursor prepared in step 1, 300 mg of tetraethyl orthosilicate, 27 mg of triethylamine and 120 mL of ethanol in a 250 mL single-necked round bottom flask, stir magnetically for 20 min, and heat the round bottom flask to 80 °C , continued to react for 12 hours, cooled to room temperature, and filtered under reduced pressure to obtain a gray solid, which was washed with 150 mL of ethanol to remove unreacted ethyl orthosilicate, dried in vacuo, and weighed to obtain 445 mg.

[0030] (3) Weigh 120 mg of the carboxylated multi-walled carbon nanotube-...

Embodiment 2

[0032] The influence of different porogenic materials on the product:

[0033] (1) Weigh 100mg of different porogenic materials, 600mg (3-aminopropyl)trimethoxysilane and 150mL ultrapure water in a 250mL beaker, stir magnetically for 10min, filter under reduced pressure to obtain a black solid, and wash it thoroughly with 250mL ethanol washing to remove unreacted (3-aminopropyl)trimethoxysilane, and vacuum drying to obtain a silicon source precursor.

[0034] (2) Weigh 240 mg of the silicon source precursor prepared in step 1, 300 mg of tetraethyl orthosilicate, 27 mg of triethylamine and 120 mL of ethanol in a 250 mL single-necked round bottom flask, stir magnetically for 20 min, and heat the round bottom flask to 80 °C , continued to react for 12 hours, cooled to room temperature, filtered under reduced pressure to obtain a gray solid, and washed with 150 mL of ethanol to remove unreacted ethyl orthosilicate, and dried in vacuum to obtain carboxylated multi-walled carbon nan...

Embodiment 3

[0040] The influence of different temperature on the product:

[0041](1) Weigh 100mg carboxylated multi-walled carbon nanotubes, 600mg (3-aminopropyl) trimethoxysilane and 150mL ultrapure water respectively in a 250mL beaker, stir magnetically for 10min, filter under reduced pressure to obtain a black solid, and use 250 mL of ethanol was fully washed to remove unreacted (3-aminopropyl)trimethoxysilane, and vacuum-dried to obtain a silicon source precursor.

[0042] (2) Weigh 240 mg of the silicon source precursor prepared in step 1, 300 mg of tetraethyl orthosilicate, 27 mg of triethylamine and 120 mL of ethanol in a 250 mL single-necked round bottom flask, stir magnetically for 20 min, and heat the round bottom flask to 80 °C , continue to react for 12 hours, cool to room temperature, filter under reduced pressure to obtain a gray solid, and fully wash with 150mL ethanol to remove unreacted ethyl orthosilicate, and dry in vacuo to obtain carboxylated multi-walled carbon nano...

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Abstract

The invention provides a simple preparation method of mesoporous silica microspheres, the mesoporous silica microspheres can be successfully prepared at the temperature of 800-1100 DEG C, the highest yield can reach 65%, the uniform size of the pore diameter is about 7.0 + / -0.4 nm, and the influence of solvent types and ph on the pore diameter can also be reduced when the mesoporous silica microspheres are prepared by using carboxylated multi-walled carbon nanotubes. The method has the advantages of mild reaction conditions, high synthesis yield, uniform pore diameter and the like.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a preparation method of multi-walled carbon nanotube-caused mesoporous silica microspheres. Background technique [0002] Mesoporous silica microspheres are an important functional adsorption carrier, which can shield the dipole interaction between magnetic particles, prevent particle agglomeration, and have good biocompatibility and hydrophilicity. Monodisperse porous silica microspheres have been widely used in drug controlled release, Separation and purification, immunoassay assay and other fields. The existing preparation methods of mesoporous silica microspheres include sol-gel method, improved Stober method, inverse microemulsion method and so on. Among them, surfactants that can form micelles are generally selected to achieve the purpose of pore formation, such as cetyltrimethylammonium bromide, polyethylene glycol, Span 80, and the like. Howeve...

Claims

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Application Information

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IPC IPC(8): C01B33/18
CPCC01B33/18C01P2006/16
Inventor 吴大同马聪潘菲
Owner CHANGZHOU UNIV