CN111017936A - Preparation method of ordered short-channel mesoporous material capable of loading ferroferric oxide - Google Patents

Abstract

The invention relates to a preparation method of a ferroferric oxide-loadable ordered short-pore-channel mesoporous material, Fe₃O₄Dissolving in ammonia water at 20 + -0.8 deg.C, and stirring to obtain Fe₃O₄Nanoparticle solution (solution a); slowly dripping TEOS (tetraethyl orthosilicate) into the solution a by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄The silica nanoparticle solution of (a); feeding the coated nano particles into a sealed heating plate, and reacting for 20min at 90-110 ℃; then carrying out suction filtration, washing with water and placing in a drying ovenDrying to obtain granular powder; and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size. Can be used for chemical catalysis, cell separation, environmental management and the like.

Description

Preparation method of ordered short-channel mesoporous material capable of loading ferroferric oxide

Technical Field

The invention relates to a preparation method of a ferroferric oxide loadable ordered short-pore mesoporous material, belonging to the field of material preparation.

Background

The ordered mesoporous material has very high specific surface and pore size of 5-40nm, continuously adjustable pore size, stable surface group, functionalization, excellent heat stability, biocompatibility and other features, and may be used in various fields, such as chemical catalysis, cell separation, environment control, medicine loading, etc.

In recent years, many methods for synthesizing ordered mesoporous materials have been reported. The loading of other materials in mesoporous materials has become the mainstream research direction, researchers at mobil corporation in 1992 obtain mesoporous M41S silicon oxide materials by a sol-gel method, and the synthesis of mesoporous materials has gradually attracted public attention. The Zhao Dongyuan project group prepared ordered large-pore mesoporous molecular sieve SBA-15 in 1998, bringing about breakthrough progress of mesoporous material synthesis.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a preparation method of a ferroferric oxide loadable ordered short-pore-channel mesoporous material, namely a material capable of loading Fe₃O₄The preparation method of the mesoporous material has short and ordered pore channels and uniform material grain diameter.

The purpose of the invention is realized by the following scheme: a preparation method of a ferroferric oxide-loadable ordered short-pore mesoporous material is characterized by comprising the following steps:

（1）Fe₃O₄dissolving in ammonia water at 20 + -0.8 deg.C, and stirring to obtain Fe₃O₄Nanoparticle solution (solution a);

(2) slowly dripping TEOS (tetraethyl orthosilicate) into the solution a by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄The silica nanoparticle solution of (a);

(3) feeding the coated nano particles into a sealed heating plate, and reacting for 20min at 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

The invention provides a supported ferroferric oxide ordered short-pore mesoporous material, which is characterized by comprising the following steps:

(1) 50g of Fe are weighed out₃O₄Dissolving in 500ml 1 mol/L ammonia water, at 20 + -0.8 deg.C, and stirring at uniform speed to obtain Fe₃O₄Nanoparticle solution (solution a);

(2) slowly dripping 6-10g TEOS (tetraethyl orthosilicate) into the solution a by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄The silica nanoparticle solution of (a);

(3) feeding the coated nano particles into a sealed heating plate, and reacting for 20min at 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

The Fe load can be prepared by the method₃O₄And the particle size is uniform.

In the method, an auxiliary active agent can be added in the step a: the addition of the cationic active agent, the anionic active agent and the nonionic active agent is 1 time of that of the template agent.

The pore canal is short and orderly, and the particle size of the material is uniform. Namely, the ordered short-channel mesoporous material is coated on the nano silicon particles, and can be used for chemical catalysis, cell separation, environmental management and the like.

Drawings

FIG. 1 example 1-SEM picture;

FIG. 2 example 1-TEM image;

FIG. 3 example 2-SEM picture;

FIG. 4 example 2-TEM image;

FIG. 5 example 3-SEM picture;

FIG. 6 example 3-TEM image.

Detailed description of the invention

The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.

Example 1

A ferroferric oxide-supported ordered short-pore mesoporous material is prepared by the following steps:

(1) 50g of Fe are weighed out₃O₄Dissolving in 500ml 1 mol/L ammonia water, at 20 + -0.8 deg.C, and stirring at uniform speed to obtain Fe₃O₄A nanoparticle solution A;

(2) then slowly dripping 10g TEOS into the solution A by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄Silica nanoparticle solution B of (a);

(3) will carry Fe₃O₄Feeding the silicon dioxide nano-particle solution B into a sealed heating plate, and reacting for 20min at the temperature of 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain a reaction product of granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

Referring to fig. 1 and fig. 2, a scanning electron microscope and a transmission electron microscope show that the silica nanoparticles loaded with Fe3O4 have an average length of 852nm, which is between 1 to 2 um. The pore diameter is 2 to 3 nm.

Example 2

A ferroferric oxide-supported ordered short-pore mesoporous material is prepared by the following steps:

(1) 40g of Fe are weighed out₃O₄Dissolving in 500ml 1 mol/L ammonia water, at 20 + -0.8 deg.C, and stirring at uniform speed to obtain Fe₃O₄A nanoparticle solution A;

(2) then slowly dripping 8g TEOS into the solution A by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄Silica nanoparticle solution B of (a);

(3) will carry Fe₃O₄Feeding the silicon dioxide nano-particle solution B into a sealed heating plate, and reacting for 20min at the temperature of 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain a reaction product of granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

As shown in FIGS. 3 and 4, a scanning electron microscope and a transmission electron microscope show that the silica nanoparticles loaded with Fe3O4 have an average length of 1.2um and an average length of 1.2-2.0 um. The pore diameter is 4-6 nm.

Example 3

A ferroferric oxide-supported ordered short-pore mesoporous material is prepared by the following steps:

(1) 300g of Fe are weighed₃O₄Dissolving in 500ml 1 mol/L ammonia water, at 20 + -0.8 deg.C, and stirring at uniform speed to obtain Fe₃O₄A nanoparticle solution A;

(2) then slowly dripping 6g TEOS into the solution A by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain Fe-loaded Fe₃O₄Silica nanoparticle solution B of (a);

(3) will carry Fe₃O₄Silica nanoparticle solution of (2)B, feeding the mixture into a sealed heating plate, and reacting for 20min at the temperature of 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain a reaction product of granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

As shown in FIGS. 5 and 6, a scanning electron microscope and a transmission electron microscope show that the silica nanoparticles loaded with Fe3O4 have an average length of 755nm, which is between 0.6 and 0.8 um. The pore diameter is 2-4 nm.

Claims (2)

1. A preparation method of a ferroferric oxide-loadable ordered short-pore mesoporous material is characterized by comprising the following steps:

（1）Fe₃O₄dissolving in ammonia water at 20 + -0.8 deg.C, and stirring to obtain Fe₃O₄A nanoparticle solution A;

(2) slowly adding tetraethyl orthosilicate (TEOS) into the solution A by using a burette, stirring at a high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain the Fe-loaded Fe₃O₄Silica nanoparticle solution B of (a);

(3) will carry Fe₃O₄Feeding the silicon dioxide nano-particle solution B into a sealed heating plate, and reacting for 20min at the temperature of 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain a reaction product of granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

2. The preparation method of the loadable ferroferric oxide ordered short-pore mesoporous material according to claim 1, which is characterized by comprising the following steps:

(1) weighing 40-300g of Fe₃O₄Dissolving in 500ml of 1 mol/L ammonia water at 20 +/-0.8 DEG CFe is prepared by a uniform speed stirrer₃O₄A nanoparticle solution A;

(2) then slowly dripping 6-10g TEOS into the solution A by using a burette, stirring at high speed for 20min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, standing in a water bath at 15 ℃, aging for 24 h, and filtering by using a filter membrane to obtain the Fe load₃O₄Silica nanoparticle solution B of (a);

(3) will carry Fe₃O₄Feeding the silicon dioxide nano-particle solution B into a sealed heating plate, and reacting for 20min at the temperature of 90-110 ℃;

(4) then carrying out suction filtration, washing with water, and drying in an oven to obtain a reaction product of granular powder;

(5) and finally, heating the reaction product to 600 ℃ at a speed of 4 ℃/min in the air, and roasting for 8 hours to prepare the ordered mesoporous material with uniform particle size.

Images