CN107175064A - A kind of magnetic microsphere silica gel and preparation method thereof - Google Patents
A kind of magnetic microsphere silica gel and preparation method thereof Download PDFInfo
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- CN107175064A CN107175064A CN201710382919.5A CN201710382919A CN107175064A CN 107175064 A CN107175064 A CN 107175064A CN 201710382919 A CN201710382919 A CN 201710382919A CN 107175064 A CN107175064 A CN 107175064A
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- silica gel
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- magnetic microsphere
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- 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
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Abstract
The invention discloses a kind of magnetic microsphere silica gel and preparation method thereof, belong to silica gel preparing technical field.The present invention is by by magnetic material Fe3O4It is composited with silica gel and prepares a kind of magnetic microsphere silica gel with large specific surface area, the magnetic microsphere silica gel includes magnetic kernel and Bio-sil shell, and the aperture of magnetic microsphere silica gel is 25~65nm, and specific surface area is 80~350m2/ g, pore volume is 0.8~1.2ml/g.The magnetic microsphere silica gel that the present invention is prepared, magnetic by force and stably, and with larger specific surface area, improves the performances such as absorption, filtering, the extract and separate of magnetic microsphere silica gel, and manufacture craft is simple to operation, and the magnetic microsphere colloidal silica dispersion that it is prepared is uniform.
Description
Technical field
The invention belongs to silica gel preparing technical field, and in particular to a kind of magnetic microsphere silica gel and preparation method thereof.
Background technology
Silica gel is a kind of high activity sorbing material, belongs to amorphous substance；Do not occur in addition to highly basic, hydrofluoric acid with any material
Reaction, water insoluble and any solvent is nonpoisonous and tasteless, and chemical property is stable.The silica gel of various models is different because of its manufacture method
And form different microcellular structures.The chemical composition and physical arrangement of silica gel, determine that it has many other same type of material difficult
To replace to obtain feature：Absorption property is high, heat endurance is good, chemical property is stable, have higher mechanical strength etc..Silica gel is according to it
The size in aperture is divided into：Macro porous silica gel, silochrom, Type B silica gel, Kiselgel A etc..
Magnetic microsphere is a kind of new function microballoon being composited by magnetic material and nonmagnetic substance, is had been widely used
In fields such as bio-separation, medicine controlled releasing, medicals diagnosis on disease, it can be in Rapid Extraction separation solution in the presence of externally-applied magnetic field
Target analytes, it has the advantages that, and simple to operate, efficiency high, cost be low, security is good, but building-up process is complicated, and
The specific surface area of the magnetic microsphere arrived is small.
The content of the invention
According to above the deficiencies in the prior art, the technical problems to be solved by the invention are to propose a kind of magnetic microsphere silica gel
And preparation method thereof, by by magnetic material Fe3O4It is composited with silica gel and prepares a kind of magnetic with large specific surface area
Microsphere silica gel, and the synthesis technique of the present invention is simple to operation.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of magnetic microsphere silica gel include magnetic kernel and
Bio-sil shell；The aperture of the magnetic microsphere silica gel is 25~65nm, and specific surface area is 80~350m2/ g, pore volume is 0.8
~1.2ml/g.
The technical solution adopted by the present invention also includes a kind of preparation method of magnetic microsphere silica gel, the magnetic microsphere silica gel
Preparation method comprise the following steps：
Step 1: by Fe3O4Magnetic nano-particle is dissolved in the mixed liquor of ethanol and water, and ultrasonic agitation is scattered to produce magnetic
Mixed liquor；
Step 2: adding sodium silicate solution into above-mentioned magnetic mixed liquor, ultrasonic agitation obtains gluey mixed liquor；
Step 3: HCl/water solution is added into above-mentioned gluey mixed liquor, and it is 8~9 to adjust the pH value of mixed liquor, stirring,
Washing, is dried to obtain aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, add ammoniacal liquor to pH value be 9~
10,6~14h of alkali heat-treatment, are filtered, and washing is dried to obtain magnetic microsphere silica gel.
Fe in above-mentioned steps one3O4The particle diameter of magnetic nano-particle is 10~25nm.
The volume ratio of ethanol and water is 1 in above-mentioned steps one：1~9.
Fe in above-mentioned steps one3O4The mass volume ratio of the mixed liquor of magnetic nano-particle and ethanol and water is 1g:200~
300ml。
Sodium silicate solution and Fe in above-mentioned steps two3O4The volume mass ratio of magnetic nano-particle is 10~100ml:1g.
The temperature of alkali heat-treatment is 65~75 DEG C in above-mentioned steps four.
The present invention uses Fe3O4Magnetic nano-particle can not only obtain the magnetic microsphere silicon of micro/nano level as kernel
Glue, moreover it is possible to improve the magnetic of product；The present invention uses concentration former as silicon for 25% sodium silicate solution, under conditions of stirring
It is added dropwise in magnetic mixed liquor, and the transparent shape colloid that stirs, then HCl/water solution is added dropwise, and adjust mixed liquor
PH value be 8~9, stir, using distilled water centrifuge washing 2~3 times, reuse ethanol centrifuge washing 2~3 times, dry
Obtain granular aperture magnetic microsphere silica gel；By aperture magnetic microsphere silica gel by alkali heat-treatment reaming, obtain one kind and compare table
Area is 80~350m2/ g magnetic microsphere silica gel.
Present invention has the advantages that:The magnetic microsphere silica gel that the present invention is prepared, magnetic by force and stably, and with larger
Specific surface area, improves the performances such as absorption, filtering, the extract and separate of magnetic microsphere silica gel, and manufacture craft is simple to operation, and it is made
Standby magnetic microsphere colloidal silica dispersion is uniform.
Embodiment
By the description to the embodiment of the present invention, to help those skilled in the art to inventive concept of the invention, technology
Scheme has more complete, accurate and deep understanding.
The technical solution adopted by the present invention is that a kind of magnetic microsphere silica gel includes magnetic kernel and Bio-sil shell；It is described
The aperture of magnetic microsphere silica gel is 25~65nm, and specific surface area is 80~350m2/ g, pore volume is 0.8~1.2ml/g.
The technical solution adopted by the present invention also includes a kind of preparation method of magnetic microsphere silica gel, the magnetic microsphere silica gel
Preparation method comprise the following steps：
Step 1: by particle diameter be 10~25nm Fe3O4Magnetic nano-particle is dissolved in the mixed liquor of ethanol and water, ultrasound
The volume ratio that dispersed with stirring produces ethanol and water in magnetic mixed liquor, the mixed liquor is 1：1~9, the Fe3O4Magnetic Nano
The mass volume ratio of the mixed liquor of particle and ethanol and water is 1g:200~300ml；
Step 2: adding sodium silicate solution into above-mentioned magnetic mixed liquor, ultrasonic agitation obtains gluey mixed liquor, the silicon
Acid sodium solution and Fe3O4The volume mass ratio of magnetic nano-particle is 10~100ml:1g；
Step 3: HCl/water solution is added into above-mentioned gluey mixed liquor, and it is 8~9 to adjust the pH value of mixed liquor, stirring,
Washing, is dried to obtain aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, add ammoniacal liquor to pH value be 9~
10, heating water bath is to 65~75 DEG C, and 6~14h of alkali heat-treatment is filtered, and washing is drying to obtain magnetic microsphere silica gel.
The present invention uses particle diameter for 10~25nm Fe3O4Magnetic nano-particle can not only be obtained micro-nano as kernel
The magnetic microsphere silica gel of level, moreover it is possible to improve the magnetic of product；The present invention uses concentration former as silicon for 25% sodium silicate solution,
It is added dropwise under conditions of stirring in magnetic mixed liquor, and the transparent shape colloid that stirs, then that HCl/water is added dropwise is molten
Liquid, and it is 8~9 to adjust the pH value of mixed liquor, is stirred, and using distilled water centrifuge washing 2~3 times, reuses ethanol centrifugation
Washing 2~3 times, is dried to obtain granular aperture magnetic microsphere silica gel；Aperture magnetic microsphere silica gel is expanded by alkali heat-treatment
Hole, obtains a kind of specific surface area for 80~350m2/ g magnetic microsphere silica gel.
Embodiment one
On the basis of embodiment, the magnetic microsphere silica gel of the present embodiment, including following preparation process：
Step 1: choosing the Fe that particle diameter is 15nm3O4Magnetic nano-particle 1g is dissolved in be made up of 20ml ethanol with 180ml water
Mixed liquor in, ultrasonic agitation is scattered to produce magnetic mixed liquor；
Step 2: under conditions of stirring, into above-mentioned magnetic mixed liquor, the sodium metasilicate that concentration is 25% is added dropwise molten
Liquid 10ml, and the transparent shape colloid that stirs；
Step 3: the HCl/water solution that concentration is 0.01mol/l is added dropwise into above-mentioned gluey mixed liquor, and adjust mixed
The pH value of liquid is closed to 8, is stirred, using distilled water centrifuge washing 3 times, ethanol centrifuge washing is reused 3 times, is placed in vacuum tank
In, vacuum drying obtains granular aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, aperture magnetic microsphere silica gel with
The mass volume ratio of distilled water is 1g:20ml, it is 9 to add ammonia spirit to the pH value that concentration is 0.01mol/l, heating water bath
To 65 DEG C, alkali heat-treatment 14h, filtering, using distilled water centrifuge washing 3 times, reuses ethanol centrifuge washing 3 times, is dried in vacuo
Obtain magnetic microsphere silica gel.
The aperture of magnetic microsphere silica gel made from the present embodiment is 50nm, and specific surface area is 280m2/ g, pore volume is 0.9ml/
g。
Embodiment two
On the basis of embodiment, the magnetic microsphere silica gel of the present embodiment, including following preparation process：
Step 1: choosing the Fe that particle diameter is 20nm3O4Magnetic nano-particle 1g is dissolved in be made up of 100ml ethanol with 100ml water
Mixed liquor in, ultrasonic agitation is scattered to produce magnetic mixed liquor；
Step 2: under conditions of stirring, into above-mentioned magnetic mixed liquor, the sodium metasilicate that concentration is 25% is added dropwise molten
Liquid 20ml, and the transparent shape colloid that stirs；
Step 3: the HCl/water solution that concentration is 0.01mol/l is added dropwise into above-mentioned gluey mixed liquor, and adjust mixed
The pH value of liquid is closed to 9, is stirred, using distilled water centrifuge washing 3 times, ethanol centrifuge washing is reused 3 times, is placed in vacuum tank
In, vacuum drying obtains granular aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, aperture magnetic microsphere silica gel with
The mass volume ratio of distilled water is 1g:20ml, it is 9.5 to add ammonia spirit to the pH value that concentration is 0.01mol/l, and water-bath adds
Heat is to 75 DEG C, alkali heat-treatment 8h, filtering, using distilled water centrifuge washing 3 times, reuses ethanol centrifuge washing 3 times, is dried in vacuo
Obtain magnetic microsphere silica gel.
The aperture of magnetic microsphere silica gel made from the present embodiment is 55nm, and specific surface area is 305m2/ g, pore volume is 1.0ml/
g。
Embodiment three
On the basis of embodiment, the magnetic microsphere silica gel of the present embodiment, including following preparation process：
Step 1: choosing the Fe that particle diameter is 25nm3O4Magnetic nano-particle 1g is dissolved in be made up of 200ml ethanol with 50ml water
Mixed liquor in, ultrasonic agitation is scattered to produce magnetic mixed liquor；
Step 2: under conditions of stirring, into above-mentioned magnetic mixed liquor, the sodium metasilicate that concentration is 25% is added dropwise molten
Liquid 20ml, and the transparent shape colloid that stirs；
Step 3: the HCl/water solution that concentration is 0.01mol/l is added dropwise into above-mentioned gluey mixed liquor, and adjust mixed
The pH value of liquid is closed to 8, is stirred, using distilled water centrifuge washing 3 times, ethanol centrifuge washing is reused 3 times, is placed in vacuum tank
In, vacuum drying obtains granular aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, aperture magnetic microsphere silica gel with
The mass volume ratio of distilled water is 1g:20ml, it is 9 to add ammonia spirit to the pH value that concentration is 0.01mol/l, heating water bath
To 75 DEG C, alkali heat-treatment 8h, filtering, using distilled water centrifuge washing 3 times, reuses ethanol centrifuge washing 3 times, is dried in vacuo
To magnetic microsphere silica gel.
The aperture of magnetic microsphere silica gel made from the present embodiment is 60nm, and specific surface area is 310m2/ g, pore volume is 1.2ml/
g。
The present invention is exemplarily described above, it is clear that the present invention, which is implemented, to be not subject to the restrictions described above,
As long as employing the improvement of the various unsubstantialities of inventive concept and technical scheme of the present invention progress, or not improved this is sent out
Bright design and technical scheme directly applies to other occasions, within protection scope of the present invention.The protection of the present invention
Scope should be determined by the scope of protection defined in the claims.
Claims (7)
1. a kind of magnetic microsphere silica gel, it is characterised in that：Including magnetic kernel and Bio-sil shell；The magnetic microsphere silica gel
Aperture be 25~65nm, specific surface area be 80~350m2/ g, pore volume is 0.8~1.2ml/g.
2. the preparation method of magnetic microsphere silica gel according to claim 1, it is characterised in that including following preparation process：
Step 1: by Fe3O4Magnetic nano-particle is dissolved in the mixed liquor of ethanol and water, and ultrasonic agitation is scattered to produce magnetic mixing
Liquid；
Step 2: adding sodium silicate solution into above-mentioned magnetic mixed liquor, ultrasonic agitation obtains gluey mixed liquor；
Step 3: HCl/water solution is added into above-mentioned gluey mixed liquor, and it is 8~9 to adjust the pH value of mixed liquor, stirring is washed
Wash, be dried to obtain aperture magnetic microsphere silica gel；
Step 4: above-mentioned aperture magnetic microsphere silica gel is put into ultrasonic disperse in distilled water, it is 8~9, alkali to add ammoniacal liquor to pH value
6~14h is heat-treated, is filtered, washing is dried to obtain magnetic microsphere silica gel.
3. the preparation method of magnetic microsphere silica gel according to claim 2, it is characterised in that：Fe in the step one3O4Magnetic
Property nano-particle particle diameter be 10~25nm.
4. the preparation method of magnetic microsphere silica gel according to claim 2, it is characterised in that：In the step one ethanol with
The volume ratio of water is 1：1~9.
5. the preparation method of magnetic microsphere silica gel according to claim 2, it is characterised in that：Fe in the step one3O4Magnetic
Property nano-particle and ethanol and water mixed liquor mass volume ratio be 1g:200~300ml.
6. the preparation method of magnetic microsphere silica gel according to claim 2, it is characterised in that：Sodium metasilicate in the step 2
Solution and Fe3O4The volume mass ratio of magnetic nano-particle is 10~100ml:1g.
7. the preparation method of magnetic microsphere silica gel according to claim 2, it is characterised in that：In the step 4 at alkali heat
The temperature of reason is 65~75 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113559830A (en) * | 2021-08-11 | 2021-10-29 | 天津博蕴纯化装备材料科技有限公司 | Magnetic porous spherical silica gel microspheres 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113559830A (en) * | 2021-08-11 | 2021-10-29 | 天津博蕴纯化装备材料科技有限公司 | Magnetic porous spherical silica gel microspheres and preparation method thereof |
| 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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