CN111017936A - Preparation method of ordered short-channel mesoporous material capable of loading ferroferric oxide - Google Patents
Preparation method of ordered short-channel mesoporous material capable of loading ferroferric oxide Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000013335 mesoporous material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000011068 loading method Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002105 nanoparticle Substances 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims description 16
- 244000282866 Euchlaena mexicana Species 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000643 oven drying Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 239000013543 active substance Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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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
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.
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2019
- 2019-12-30 CN CN201911392864.1A patent/CN111017936A/en active Pending
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| CN1486929A (en) * | 2003-08-12 | 2004-04-07 | 上海交通大学 | Prepn of mesoporous spherical nano Sio2 particle |
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Application publication date: 20200417 |