CN107175064B - Magnetic microsphere silica gel and preparation method thereof - Google Patents
Magnetic microsphere silica gel and preparation method thereof Download PDFInfo
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- CN107175064B CN107175064B CN201710382919.5A CN201710382919A CN107175064B CN 107175064 B CN107175064 B CN 107175064B CN 201710382919 A CN201710382919 A CN 201710382919A CN 107175064 B CN107175064 B CN 107175064B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
Abstract
The invention discloses magnetic microsphere silica gel and a preparation method thereof, belonging to the technical field of silica gel preparation. The invention is prepared by mixing magnetic material Fe3O4The magnetic microsphere silica gel with large specific surface area is prepared by compounding the magnetic microsphere silica gel with silica gel, wherein the magnetic microsphere silica gel comprises a magnetic core and a porous silica gel shell, the pore diameter of the magnetic microsphere silica gel is 25-65 nm, and the specific surface area is 80-350 m2The pore volume is 0.8 to 1.2 ml/g. The magnetic microsphere silica gel prepared by the invention has strong and stable magnetism and larger specific surface area, improves the performances of adsorption, filtration, extraction separation and the like of the magnetic microsphere silica gel, has simple and easy-to-operate preparation process, and is uniformly dispersed.
Description
Technical Field
The invention belongs to the technical field of silica gel preparation, and particularly relates to magnetic microsphere silica gel and a preparation method thereof.
Background
Silica gel is a high-activity adsorption material and belongs to an amorphous substance; except strong alkali and hydrofluoric acid, the paint does not react with any substance, is insoluble in water and any solvent, is nontoxic and tasteless, and has stable chemical properties. Different types of silica gel form different microporous structures due to different manufacturing methods. The chemical components and physical structure of silica gel determine that the silica gel has the characteristics that a plurality of other similar materials are difficult to replace: high adsorption performance, good thermal stability, stable chemical property, higher mechanical strength and the like. Silica gel is divided into the following according to the pore size: macroporous silica gel, B-type silica gel, fine-pored silica gel, etc.
The magnetic microsphere is a novel functional microsphere compounded by a magnetic material and a non-magnetic material, is widely applied to the fields of bioseparation, drug controlled release, disease diagnosis and the like, can quickly extract and separate target analytes in a solution under the action of an external magnetic field, and has the advantages of simple operation, high efficiency, low cost, good safety and the like, but the synthesis process is complicated, and the specific surface area of the obtained magnetic microsphere is small.
Disclosure of Invention
In view of the above disadvantages of the prior art, the technical problem to be solved by the present invention is to provide a magnetic microsphere silica gel and a preparation method thereof, wherein a magnetic material Fe is added3O4The magnetic microsphere silica gel with large specific surface area is prepared by compounding the magnetic microsphere silica gel with silica gel, and the synthetic process is simple and easy to operate.
In order to achieve the purpose, the invention adopts the technical scheme that: a magnetic microsphere silica gel comprises a magnetic core and a porous silica gel shell; the magnetismThe pore diameter of the microspherical silica gel is 25-65 nm, and the specific surface area is 80-350 m2The pore volume is 0.8 to 1.2 ml/g.
The technical scheme adopted by the invention also comprises a preparation method of the magnetic microsphere silica gel, wherein the preparation method of the magnetic microsphere silica gel comprises the following steps:
step one, adding Fe3O4Dissolving the magnetic nanoparticles in a mixed solution of ethanol and water, and ultrasonically stirring and dispersing to obtain a magnetic mixed solution;
step two, adding a sodium silicate solution into the magnetic mixed solution, and carrying out ultrasonic stirring to obtain a colloidal mixed solution;
adding an HCl aqueous solution into the colloidal mixed solution, adjusting the pH value of the mixed solution to 8-9, stirring, washing and drying to obtain the microporous magnetic microsphere silica gel;
and step four, putting the microporous magnetic microsphere silica gel into distilled water for ultrasonic dispersion, adding ammonia water until the pH value is 9-10, carrying out alkali heat treatment for 6-14 h, filtering, washing and drying to obtain the magnetic microsphere silica gel.
Fe in the first step3O4The particle size of the magnetic nanoparticles is 10-25 nm.
In the first step, the volume ratio of ethanol to water is 1: 1 to 9.
Fe in the first step3O4The mass volume ratio of the magnetic nanoparticles to the mixed solution of ethanol and water is 1g: 200-300 ml.
In the second step, the sodium silicate solution and Fe3O4The volume-mass ratio of the magnetic nanoparticles is 10-100 ml:1 g.
The temperature of the alkali heat treatment in the fourth step is 65-75 ℃.
In the invention, Fe is adopted3O4The magnetic nano particles are used as the inner core, so that the magnetic microsphere silica gel with micro-nano level can be obtained, and the magnetism of the product can be improved; the method comprises the steps of dropwise adding 25% sodium silicate solution serving as a silicon source into a magnetic mixed solution under the stirring condition, uniformly stirring the mixture to form a transparent colloid, dropwise adding HCl aqueous solution, adjusting the pH value of the mixed solution to be 8-9, and uniformly stirring the mixtureCentrifugally washing for 2-3 times by using distilled water, centrifugally washing for 2-3 times by using ethanol, and drying to obtain granular microporous magnetic microsphere silica gel; carrying out alkali heat treatment on the microporous magnetic microsphere silica gel to enlarge pores, thereby obtaining the porous magnetic microsphere silica gel with the specific surface area of 80-350 m2Magnetic microsphere silica gel per gram.
The magnetic microsphere silica gel prepared by the method has the beneficial effects that the magnetic microsphere silica gel is strong and stable in magnetism and has a larger specific surface area, the performances of adsorption, filtration, extraction separation and the like of the magnetic microsphere silica gel are improved, the preparation process is simple and easy to operate, and the prepared magnetic microsphere silica gel is uniformly dispersed.
Detailed Description
The embodiments of the present invention have been described in order to provide those skilled in the art with a more complete, accurate and thorough understanding of the inventive concepts and solutions of the present invention.
The technical scheme adopted by the invention is that the magnetic microsphere silica gel comprises a magnetic inner core and a porous silica gel shell; the pore diameter of the magnetic microsphere silica gel is 25-65 nm, and the specific surface area is 80-350 m2The pore volume is 0.8 to 1.2 ml/g.
The technical scheme adopted by the invention also comprises a preparation method of the magnetic microsphere silica gel, wherein the preparation method of the magnetic microsphere silica gel comprises the following steps:
step one, Fe with the grain diameter of 10-25 nm3O4Dissolving magnetic nanoparticles in a mixed solution of ethanol and water, and performing ultrasonic stirring and dispersion to obtain a magnetic mixed solution, wherein the volume ratio of ethanol to water in the mixed solution is 1: 1 to 9 of said Fe3O4The mass volume ratio of the magnetic nanoparticles to the mixed solution of ethanol and water is 1g: 200-300 ml;
step two, adding a sodium silicate solution into the magnetic mixed solution, and carrying out ultrasonic stirring to obtain a colloidal mixed solution, wherein the sodium silicate solution and Fe3O4The volume-mass ratio of the magnetic nanoparticles is 10-100 ml:1 g;
adding an HCl aqueous solution into the colloidal mixed solution, adjusting the pH value of the mixed solution to 8-9, stirring, washing and drying to obtain the microporous magnetic microsphere silica gel;
and step four, putting the small-pore magnetic microsphere silica gel into distilled water for ultrasonic dispersion, adding ammonia water until the pH value is 9-10, heating in a water bath to 65-75 ℃, carrying out alkali heat treatment for 6-14 h, filtering, washing and drying to obtain the magnetic microsphere silica gel.
The invention adopts Fe with the grain diameter of 10-25 nm3O4The magnetic nano particles are used as the inner core, so that the magnetic microsphere silica gel with micro-nano level can be obtained, and the magnetism of the product can be improved; the method comprises the steps of taking a 25% sodium silicate solution as a silicon source, dropwise adding the sodium silicate solution into a magnetic mixed solution under the condition of stirring, uniformly stirring to form a transparent colloid, dropwise adding an HCl aqueous solution, adjusting the pH value of the mixed solution to be 8-9, uniformly stirring, centrifugally washing for 2-3 times by using distilled water, centrifugally washing for 2-3 times by using ethanol, and drying to obtain granular microporous magnetic microsphere silica gel; carrying out alkali heat treatment on the microporous magnetic microsphere silica gel to enlarge pores, thereby obtaining the porous magnetic microsphere silica gel with the specific surface area of 80-350 m2Magnetic microsphere silica gel per gram.
Example one
On the basis of the specific implementation manner, the magnetic microsphere silica gel of the embodiment includes the following preparation processes:
step one, selecting Fe with the particle size of 15nm3O4Dissolving 1g of magnetic nanoparticles in a mixed solution consisting of 20ml of ethanol and 180ml of water, and performing ultrasonic stirring and dispersion to obtain a magnetic mixed solution;
step two, under the condition of stirring, dropwise adding 10ml of 25% sodium silicate solution into the magnetic mixed solution, and uniformly stirring to form transparent colloid;
dropwise adding HCl aqueous solution with the concentration of 0.01mol/l into the colloidal mixed solution, adjusting the pH value of the mixed solution to 8, uniformly stirring, centrifugally washing for 3 times by using distilled water, centrifugally washing for 3 times by using ethanol, placing in a vacuum box, and carrying out vacuum drying to obtain granular microporous magnetic microsphere silica gel;
and step four, putting the microporous magnetic microsphere silica gel into distilled water for ultrasonic dispersion, wherein the mass volume ratio of the microporous magnetic microsphere silica gel to the distilled water is 1g:20ml, adding an ammonia water solution with the concentration of 0.01mol/l until the pH value is 9, heating in a water bath to 65 ℃, carrying out alkali heat treatment for 14h, filtering, carrying out centrifugal washing for 3 times by using the distilled water, carrying out centrifugal washing for 3 times by using ethanol, and carrying out vacuum drying to obtain the magnetic microsphere silica gel.
The pore diameter of the magnetic microsphere silica gel prepared by the embodiment is 50nm, and the specific surface area is 280m2The pore volume is 0.9 ml/g.
Example two
On the basis of the specific implementation manner, the magnetic microsphere silica gel of the embodiment includes the following preparation processes:
step one, selecting Fe with the particle size of 20nm3O4Dissolving 1g of magnetic nanoparticles in a mixed solution consisting of 100ml of ethanol and 100ml of water, and performing ultrasonic stirring and dispersion to obtain a magnetic mixed solution;
step two, under the condition of stirring, dropwise adding 20ml of 25% sodium silicate solution into the magnetic mixed solution, and uniformly stirring to form transparent colloid;
dropwise adding HCl aqueous solution with the concentration of 0.01mol/l into the colloidal mixed solution, adjusting the pH value of the mixed solution to 9, uniformly stirring, centrifugally washing for 3 times by using distilled water, centrifugally washing for 3 times by using ethanol, placing in a vacuum box, and carrying out vacuum drying to obtain granular microporous magnetic microsphere silica gel;
and step four, putting the microporous magnetic microsphere silica gel into distilled water for ultrasonic dispersion, wherein the mass volume ratio of the microporous magnetic microsphere silica gel to the distilled water is 1g:20ml, adding an ammonia water solution with the concentration of 0.01mol/l until the pH value is 9.5, heating in a water bath to 75 ℃, carrying out alkali heat treatment for 8h, filtering, carrying out centrifugal washing for 3 times by using the distilled water, carrying out centrifugal washing for 3 times by using ethanol, and carrying out vacuum drying to obtain the magnetic microsphere silica gel.
The pore diameter of the magnetic microsphere silica gel prepared in the embodiment is 55nm, and the specific surface area is 305m2The pore volume is 1.0 ml/g.
EXAMPLE III
On the basis of the specific implementation manner, the magnetic microsphere silica gel of the embodiment includes the following preparation processes:
step one, selecting Fe with the particle size of 25nm3O4Dissolving 1g of magnetic nanoparticles in a mixed solution consisting of 200ml of ethanol and 50ml of water, and performing ultrasonic stirring and dispersion to obtain a magnetic mixed solution;
step two, under the condition of stirring, dropwise adding 20ml of 25% sodium silicate solution into the magnetic mixed solution, and uniformly stirring to form transparent colloid;
dropwise adding HCl aqueous solution with the concentration of 0.01mol/l into the colloidal mixed solution, adjusting the pH value of the mixed solution to 8, uniformly stirring, centrifugally washing for 3 times by using distilled water, centrifugally washing for 3 times by using ethanol, placing in a vacuum box, and carrying out vacuum drying to obtain granular microporous magnetic microsphere silica gel;
and step four, putting the microporous magnetic microsphere silica gel into distilled water for ultrasonic dispersion, wherein the mass volume ratio of the microporous magnetic microsphere silica gel to the distilled water is 1g:20ml, adding an ammonia water solution with the concentration of 0.01mol/l until the pH value is 9, heating in a water bath to 75 ℃, carrying out alkali heat treatment for 8h, filtering, carrying out centrifugal washing for 3 times by using the distilled water, carrying out centrifugal washing for 3 times by using ethanol, and carrying out vacuum drying to obtain the magnetic microsphere silica gel.
The pore diameter of the magnetic microsphere silica gel prepared in the embodiment is 60nm, and the specific surface area is 310m2The pore volume is 1.2 ml/g.
The invention has been described in an illustrative manner, and it is to be understood that the invention is not limited to the precise form disclosed, and that various insubstantial modifications of the inventive concepts and solutions, or their direct application to other applications without such modifications, are intended to be covered by the scope of the invention. The protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (6)
1. A magnetic microsphere silica gel is characterized by comprising a magnetic core and a porous silica gel shell; the pore diameter of the magnetic microsphere silica gel is 25-65 nm, and the specific surface area is 80-350 m2The pore volume is 0.8-1.2 ml/g;
the preparation method of the magnetic microsphere silica gel comprises the following preparation steps:
step one, adding Fe3O4Dissolving the magnetic nanoparticles in a mixed solution of ethanol and water, and ultrasonically stirring and dispersing to obtain a magnetic mixed solution;
step two, adding a sodium silicate solution into the magnetic mixed solution, and carrying out ultrasonic stirring to obtain a colloidal mixed solution;
adding an HCl aqueous solution into the colloidal mixed solution, adjusting the pH value of the mixed solution to 8-9, stirring, washing and drying to obtain the microporous magnetic microsphere silica gel;
and step four, putting the microporous magnetic microsphere silica gel into distilled water for ultrasonic dispersion, adding ammonia water until the pH value is 8-9, carrying out alkali heat treatment for 6-14 h, filtering, washing and drying to obtain the magnetic microsphere silica gel.
2. The method for preparing magnetic microsphere silica gel according to claim 1, wherein the method comprises the following steps: fe in the first step3O4The particle size of the magnetic nanoparticles is 10-25 nm.
3. The method for preparing magnetic microsphere silica gel according to claim 1, wherein the method comprises the following steps: the volume ratio of ethanol to water in the first step is 1: 1 to 9.
4. The method for preparing magnetic microsphere silica gel according to claim 1, wherein the method comprises the following steps: fe in the first step3O4The mass volume ratio of the magnetic nanoparticles to the mixed solution of ethanol and water is 1g: 200-300 ml.
5. The method for preparing magnetic microsphere silica gel according to claim 1, wherein the method comprises the following steps: in the second step, the sodium silicate solution and Fe3O4The volume-mass ratio of the magnetic nanoparticles is 10-100 ml:1 g.
6. The method for preparing magnetic microsphere silica gel according to claim 1, wherein the method comprises the following steps: the temperature of the alkali heat treatment in the fourth step is 65-75 ℃.
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| CN113304735A (en) * | 2021-03-25 | 2021-08-27 | 苏州环亚欣智能科技有限公司 | Preparation method of magnetic microspheres with high specific surface area |
| CN113083217A (en) * | 2021-03-25 | 2021-07-09 | 苏州环亚欣智能科技有限公司 | Preparation method of magnetic silica gel microspheres with controllable high pore diameters |
| CN113559830B (en) * | 2021-08-11 | 2023-08-18 | 天津博蕴纯化装备材料科技有限公司 | Magnetic porous spherical silica gel microsphere and preparation method thereof |
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| CN1480251A (en) * | 2003-07-21 | 2004-03-10 | 天津大学 | Ferromagnetic multiporous silica gel microsphere and its preparation method |
| CN102824891A (en) * | 2012-09-19 | 2012-12-19 | 清华大学 | Preparation method of compact single-layer SiO2 coated on surface of magnetic nuclear material Fe3O4 |
| CN103936019A (en) * | 2014-04-28 | 2014-07-23 | 东华大学 | Method for preparing uniform magnetic nano silicon dioxide grain |
| CN104475012A (en) * | 2014-12-16 | 2015-04-01 | 湖北工业大学 | Fe3O4@SiO2 magnetic nanospheres as well as preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480251A (en) * | 2003-07-21 | 2004-03-10 | 天津大学 | Ferromagnetic multiporous silica gel microsphere and its preparation method |
| CN102824891A (en) * | 2012-09-19 | 2012-12-19 | 清华大学 | Preparation method of compact single-layer SiO2 coated on surface of magnetic nuclear material Fe3O4 |
| CN103936019A (en) * | 2014-04-28 | 2014-07-23 | 东华大学 | Method for preparing uniform magnetic nano silicon dioxide grain |
| CN104475012A (en) * | 2014-12-16 | 2015-04-01 | 湖北工业大学 | Fe3O4@SiO2 magnetic nanospheres as well as preparation method and application thereof |
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