CN107619092A - A kind of preparation method of magnetic aeroge - Google Patents
A kind of preparation method of magnetic aeroge Download PDFInfo
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- CN107619092A CN107619092A CN201710585992.2A CN201710585992A CN107619092A CN 107619092 A CN107619092 A CN 107619092A CN 201710585992 A CN201710585992 A CN 201710585992A CN 107619092 A CN107619092 A CN 107619092A
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Abstract
The invention provides a kind of preparation method of magnetic aeroge, first by MODIFIED Fe3O4Nano-solution is added drop-wise in the bovine serum albumin aqueous solution, and glutaraldehyde water solution stirring is added after stirring, and standing obtains gel；Then standing is obtained into gel and adds organic solvent aging, then replaced with organic solvent；Finally it is dried to obtain magnetic aeroge.Present invention process is simple, and cost is low, and method is novel, and obtained aeroge has saturation magnetization height；Magnetic Isolation, recycle, it is green the features such as.
Description
Technical field
The invention belongs to the preparation of new material and application field, is related to a kind of preparation method of novel magnetic aeroge.
Background technology
Ferroso-ferric oxide is a kind of ferrimagnet with inverse spinel structure, due to good biocompatibility, saturation magnetic
It is high to change intensity, is had a good application prospect in bio-imaging field and Magnetic Isolation field.Aeroge is a kind of new, knot
The controllable porous material of structure, had a wide range of applications in absorption, catalysis and heat-insulated field.But the system of current magnetic aeroge
Standby, the preparation of especially ferroferric oxide aerogel still suffers from significant challenge, because traditional sol-gel process is difficult to prepare
Go out the ferroferric oxide aerogel of magnetic.In order to overcome the shortcomings of conventional method, by the nano ferriferrous oxide of preparation through surface
Chemical modification, then gel prepares magnetic aerogel material, and rapid magnetic divides from the aqueous solution applied to organic dyestuff
From.
The content of the invention
It is an object of the invention to provide a kind of preparation method of magnetic aeroge, and can apply to organic dyestuff from
Quick separating in the aqueous solution.
The purpose of the present invention is achieved by the following technical programs：A kind of preparation method of magnetic aeroge, its is specific
Step is as follows：
Step 1：By MODIFIED Fe3O4Nano-solution is added drop-wise in the bovine serum albumin aqueous solution of mass fraction 5%~15%,
Fe3O4Nano-solution is 1 with bovine serum albumen solution volume ratio:(0.2~3), 0.2~1h is stirred at room temperature, then adds glutaraldehyde
The aqueous solution stirs 0.5~1h, and standing obtains gel；
Step 2：Standing is obtained into gel and adds organic solvent aging, then puts the gel after aging with organic solvent
Change, until the water in gel is replaced completely；
Step 3：Magnetic aeroge is obtained after the gel of gained in step 2 is dried.
MODIFIED Fe described in preferred steps one3O4Nanoparticles solution is the amine-modified Fe of DOPA3O4The aqueous solution, wherein
Fe3O4Molar fraction is 50%~80%, the amine-modified Fe of DOPA3O4Averagely it is hydrated particle diameter 15-30nm.
It is preferred that the addition quality of glutaraldehyde accounts for the 10%~35% of bovine serum albumin quality.
The organic solvent of aging and displacement is ethanol or acetone in preferred steps two.
It is preferred that ageing time is 1~2 day；The number that gel after aging is replaced with organic solvent is 3-5 times, each 1-2
My god.
Drying mode described in preferred steps three is dry CO 2 supercritical, freeze-drying or constant pressure and dry.
The present invention passes through the Fe for the monodispersity for preparing solvent-thermal method3O4Particle surface DOPA is amine-modified so that nanometer
Particle surface has good dispersive property, while the Fe that DOPA is amine-modified3O4There is special absorption property to albumen, pass through
Glutaraldehyde cross-linking albumen, obtained magnetic gel have higher saturation magnetization and higher organic dyestuff absorption property.
The invention has the advantages that：
(1), technique is simple, and cost is low, and method is novel；
(2), saturation magnetization is high；
(3) Magnetic Isolation, recycle, it is green.
Brief description of the drawings
Fig. 1 is the pictorial diagram of the magnetic albumen aerogel block body prepared by embodiment 1.
Embodiment
Example 1
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 50%), particle are averagely hydrated particle diameter 15nm, are slowly added to
In the bovine serum albumin aqueous solution of mass fraction 10%, Fe3O4The aqueous solution is 5 with bovine serum albumin aqueous solution volume ratio:1.Then
0.5h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, controls glutaraldehyde quality
For 10% of albumen in reaction containing quality.0.5h is stirred at room temperature, is poured into beaker, stands gel.Add after ethanol in room temperature
Lower aging 2 days, add ethanol and change liquid 5 times, every time displacement 1 day.Gel after finally alcohol solvent is replaced passes through carbon dioxide
Supercritical drying, magnetic albumen aerogel block body is obtained, as shown in Figure 1.
The aeroge saturation magnetization of preparation is 60emu/g, specific surface area 400m2/ g, to the adsorbance of methylene blue
For 21mg/g.
Example 2
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 80%), particle are averagely hydrated particle diameter 15nm, are slowly added to
In the bovine serum albumin aqueous solution of mass fraction 15%, Fe3O4The aqueous solution is 1 with bovine serum albumin aqueous solution volume ratio:1.Then
0.5h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, controls glutaraldehyde quality
For 10% of albumen in reaction containing quality.0.5h is stirred at room temperature, is poured into beaker, stands gel.Add after ethanol in room temperature
Lower aging 2 days, add ethanol and change liquid 5 times, every time displacement 1 day.Gel after finally alcohol solvent is replaced passes through carbon dioxide
Supercritical drying, obtain magnetic albumen aerogel block body.
The aeroge saturation magnetization of preparation is 65emu/g, specific surface area 210m2/ g, to the adsorbance of methylene blue
For 6mg/g.
Example 3
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 50%), particle are averagely hydrated particle diameter 20nm, are slowly added to
In the bovine serum albumin aqueous solution of mass fraction 10%, Fe3O4The aqueous solution aqueous solution is 1 with bovine serum albumin aqueous solution volume ratio:
3.Then 0.5h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, control penta 2
Aldehyde quality is 10% of albumen in reaction containing quality.0.5h is stirred at room temperature, is poured into beaker, stands gel.After adding ethanol
Aging 1 day at room temperature, add ethanol and change liquid 3 times, every time displacement 2 days.Gel after finally alcohol solvent is replaced passes through second
Alcohol supercritical drying, obtain magnetic albumen aerogel block body.
The aeroge saturation magnetization of preparation is 55emu/g, specific surface area 150m2/ g, to the adsorbance of methylene blue
For 12mg/g.
Example 4
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 65%), particle are averagely hydrated particle diameter 18nm, are slowly added to
In the bovine serum albumin aqueous solution of mass fraction 5%, Fe3O4The aqueous solution aqueous solution is 2 with bovine serum albumin aqueous solution volume ratio:
3.Then 0.5h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, control penta 2
Aldehyde quality is 35% of albumen in reaction containing quality.0.5h is stirred at room temperature, is poured into beaker, stands gel.After adding acetone
Aging 2 days at room temperature, add acetone and change liquid 5 times, 1 day every time.Gel after finally acetone solvent is replaced passes through titanium dioxide
Carbon supercritical drying, obtain magnetic albumen aerogel block body.
The aeroge saturation magnetization of preparation is 58emu/g, specific surface area 413m2/ g, to the adsorbance of methylene blue
For 19mg/g.
Example 5
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 70%), particle are averagely hydrated particle diameter 18nm, are slowly added to
In the bovine serum albumin aqueous solution of mass fraction 12%, Fe3O4The aqueous solution aqueous solution is 1 with bovine serum albumin aqueous solution volume ratio:
3.Then 1h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, controls glutaraldehyde
Quality is 10% of albumen in reaction containing quality.1h is stirred at room temperature, is poured into beaker, stands gel.Add after acetone in room
The lower aging of temperature 2 days, adds acetone and changes liquid 5 times, 1 day every time.Gel after finally acetone solvent is replaced obtains by freeze-drying
To magnetic albumen aerogel block body.
Aeroge the saturation magnetization 70emu/g, specific surface area 410m of preparation2/ g, the adsorbance to methylene blue are
28mg/g。
Example 6
By dopamine MODIFIED Fe3O4The aqueous solution (molar fraction 50%) particle is averagely hydrated particle diameter 15nm, is slowly added to matter
In the bovine serum albumin aqueous solution for measuring fraction 15%, Fe3O4The aqueous solution aqueous solution is 1 with bovine serum albumin aqueous solution volume ratio:3.
Then 0.2h is stirred at room temperature, and solution is transformed into transparent dark solution.Glutaraldehyde water solution is slowly added to, controls glutaraldehyde
Quality is 35% of albumen in reaction containing quality.0.5h is stirred at room temperature, is poured into beaker, stands gel.Add acetone after
Aging 2 days at room temperature, add acetone and change liquid 5 times, 1 day every time.Gel after finally acetone solvent is replaced passes through carbon dioxide
Supercritical drying, obtain magnetic albumen aerogel block body.
Aeroge the saturation magnetization 62emu/g, specific surface area 400m of preparation2/ g, the adsorbance to methylene blue are
27mg/g。
Claims (6)
1. a kind of preparation method of magnetic aeroge, it is comprised the following steps that：
Step 1：By MODIFIED Fe3O4Nano-solution is added drop-wise in the bovine serum albumin aqueous solution of mass fraction 5%~15%, Fe3O4
Nano-solution is 1 with bovine serum albumen solution volume ratio:(0.2~3), 0.2~1h is stirred, then add glutaraldehyde water solution and stir
0.5~1h is mixed, standing obtains gel；
Step 2：Standing is obtained into gel and adds organic solvent aging, then replaces the gel after aging with organic solvent；
Step 3：Magnetic aeroge is obtained after the gel of gained in step 2 is dried.
2. preparation method as claimed in claim 1, it is characterised in that the MODIFIED Fe described in step 13O4Nanoparticles solution is
The amine-modified Fe of DOPA3O4The aqueous solution, wherein Fe3O4Molar fraction is 50%~80%, the amine-modified Fe of DOPA3O4Average hydration
Particle diameter 15-30nm.
3. preparation method as claimed in claim 1, it is characterised in that the addition quality of glutaraldehyde accounts for bovine serum albumin quality
10%~35%.
4. preparation method as claimed in claim 1, it is characterised in that the organic solvent of aging and displacement is second in step 2
Alcohol or acetone.
5. preparation method as claimed in claim 1, it is characterised in that ageing time is 1~2 day；Gel after aging is with organic
The number of solvent displacement is 3-5 times, each 1-2 days.
6. preparation method as claimed in claim 1, it is characterised in that the drying mode described in step 3 surpasses for carbon dioxide
Critical drying, freeze-drying or constant pressure and dry.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109528627A (en) * | 2018-12-03 | 2019-03-29 | 深圳大学 | A kind of Ru-BSA hydrogel and the preparation method and application thereof |
| CN112915935A (en) * | 2021-01-25 | 2021-06-08 | 合肥工业大学 | Bionic magnetic fibroin-based composite aerogel, and preparation method and application thereof |
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| US20110124790A1 (en) * | 2007-11-21 | 2011-05-26 | Centre National De La Recherche Scientifique-Cnrs | Aerogels of carbon nanotubes |
| CN102923788A (en) * | 2012-11-09 | 2013-02-13 | 北京理工大学 | Preparation method of ferroferric oxide aerogel |
| CN103903827A (en) * | 2014-03-20 | 2014-07-02 | 哈尔滨益材新材料有限公司 | Preparation method and application of magnetic silicon dioxide composite microsphere |
| CN105566673A (en) * | 2015-12-17 | 2016-05-11 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional cellulose elastic aerogel |
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2017
- 2017-07-18 CN CN201710585992.2A patent/CN107619092A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110124790A1 (en) * | 2007-11-21 | 2011-05-26 | Centre National De La Recherche Scientifique-Cnrs | Aerogels of carbon nanotubes |
| CN102923788A (en) * | 2012-11-09 | 2013-02-13 | 北京理工大学 | Preparation method of ferroferric oxide aerogel |
| CN103903827A (en) * | 2014-03-20 | 2014-07-02 | 哈尔滨益材新材料有限公司 | Preparation method and application of magnetic silicon dioxide composite microsphere |
| CN105566673A (en) * | 2015-12-17 | 2016-05-11 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional cellulose elastic aerogel |
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| 唐祥龙等: "磁性气凝胶的研究进展", 《中国材料进展》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109528627A (en) * | 2018-12-03 | 2019-03-29 | 深圳大学 | A kind of Ru-BSA hydrogel and the preparation method and application thereof |
| CN109528627B (en) * | 2018-12-03 | 2022-04-15 | 深圳大学 | Ru-BSA hydrogel and preparation method and application thereof |
| CN112915935A (en) * | 2021-01-25 | 2021-06-08 | 合肥工业大学 | Bionic magnetic fibroin-based composite aerogel, and preparation method and application thereof |
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