CN102923788A - Preparation method of ferroferric oxide aerogel - Google Patents
Preparation method of ferroferric oxide aerogel Download PDFInfo
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- CN102923788A CN102923788A CN2012104481533A CN201210448153A CN102923788A CN 102923788 A CN102923788 A CN 102923788A CN 2012104481533 A CN2012104481533 A CN 2012104481533A CN 201210448153 A CN201210448153 A CN 201210448153A CN 102923788 A CN102923788 A CN 102923788A
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Abstract
The invention relates to a preparation method of ferroferric oxide aerogel and belongs to the field of magnetic materials. The method comprises the following steps; step 1, material; under protection of nitrogen, divalent ferric salt and trivalent ferric salt are respectively dissolved into organic solvent or water to obtain a corresponding solution. A divalent ferric salt solution and a divalent ferric salt solution are respectively stirred and mixed evenly to obtain a mixed ferric salt solution; step 2, formation of gel; gel accelerant is dropwise added into the mixed ferric salt solution obtained from the step 1 so that gel is obtained; step 3, aging, the gel obtained from the step 2 is implemented still standing and aging; step 4, solvent displacement, the gel after aging is soaked into a solution a to conduct solvent displacement till the solvent in the gel can be completely displaced by the solution a; step 5, drying, the gel containing the solution a obtained from the step 4 is implemented drying to obtain the ferroferric oxide aerogel. Compared with the traditional ferroferric oxide, the thickness of the prepared ferroferric oxide aerogel is lowered by 50%-80%, and saturated magnetization can reach 52 emu/g-1.
Description
Technical field
The present invention relates to a kind of preparation method of ferroferric oxide aerogel, belong to field of magnetic material.
Background technology
Z 250 is a kind of ferromagnetic substance with spinel structure, Fe
3+With Fe
2+Be filled in the gap of the face-centered cubic framework that oxonium ion consists of, and can carry out the double cross mutual effect and seize B position in the crystal, present excellent electromagnetic property, especially absorbing property, aspect radar absorbent material, have good application prospect, also be widely used in recording materials, telecommunication apparatus material and the aspects such as catalyzer and support of the catalyst preparation.
Traditional ferrite mostly is the coated material that exists with forms such as powder and particles, although with low cost, technique is simple, but the shortcomings such as absorbing property is relatively poor under the poor high temperature stability that causes greatly because of its density and the hot environment and in the high band range, cause it in the application of the specific environments such as stealthy aircraft, to be very restricted, in order to overcome this defective, need to prepare low density material to satisfy the demands.
Summary of the invention
The objective of the invention is provides a kind of preparation method of ferroferric oxide aerogel in order to solve the large problem of traditional Z 250 density.
Purpose of the present invention is realized by following technical scheme:
The preparation method of a kind of ferroferric oxide aerogel of the present invention, concrete steps are as follows:
Step 1, material dissolution: under nitrogen protection, divalent iron salt and trivalent iron salt be dissolved in respectively obtain corresponding solution in organic solvent or the water, get respectively divalent iron salt and ferric salt solution, mix, obtain mixed molysite solution, wherein Fe
3+With Fe
2+Mol ratio be 1:12.5:1;
The formation of step 2, gel: the molysite mixed solution and dripping gel promotor to the step 1 gained obtains gel;
Step 3, aging: leave standstill the gel of step 2 gained aging;
Step 4, solvent exchange: the gel after will wearing out is dipped into and carries out solvent exchange among the solvent a, until solvent is replaced by solvent a fully in the gel, obtains containing the gel of solvent a;
Step 5, drying: the gel that contains solvent a of step 4 gained is carried out obtaining ferroferric oxide aerogel after the drying.
The described gel promotor of step 2 is organic Lewis base, is preferably small molecules epoxy compounds, the derivative of 1 α position electrophilic substitution, Racemic glycidol ether compound;
The described solvent a of step 4 is organic solvent, is preferably to be acetone or alcohol;
The described drying mode of step 5 can be supercritical drying, constant pressure and dry, lyophilize.
Beneficial effect
1, the preparation method of a kind of ferroferric oxide aerogel of the present invention, the ferroferric oxide aerogel of preparation is removed owing to the liquid in the general reticulated structure space, wet gel space in early stage is dried and is replaced by gas, and density is 1.03-2.81gcm
-1, the density of more traditional Z 250 is hanged down 50%-80%, and saturation magnetization can reach 52emug
-1
2, the preparation method of a kind of ferroferric oxide aerogel of the present invention, simple to operate, safety at room temperature can realize.
3, the preparation method of a kind of ferroferric oxide aerogel of the present invention keeps former being magnetic not to be destroyed.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Under nitrogen protection, in the 50ml container of magnetic stir bar is housed, add successively iron(ic) chloride 0.947g under the room temperature, iron protochloride 0.398g, dehydrated alcohol 5.5ml fully stir until solution mixes.Temperature transfers to 25 ℃, slowly drips the 3.05g propylene oxide, stops after dropwising stirring, and leaves standstill to gel formation.7d namely is dipped into gel in the acetone after 7 days, changes acetone one time every 5h, continues displacement 1d.Then the gel behind the solvent exchange is carried out the supercritical co drying, temperature 50 C, pressure 12MPa, carbonic acid gas flow velocity 5mL/min, time of drying, 24h obtained granular ferroferric oxide aerogel particle.Ferroferric oxide aerogel magneticsubstance of the present invention obtains crystal grain with the SEM observation and is about 50nm, and recording saturation magnetization with vibrating sample magnetometer is 32.52emug
-1, density is 1.81gcm
-1, specific surface area is 330.20m
2G
-1, mean pore size is 9.4nm.
Embodiment 2
Under nitrogen protection, in the 50ml container of magnetic stir bar is housed, add successively iron(ic) chloride 0.947g under the room temperature, iron protochloride 0.398g, dehydrated alcohol 3ml fully stir until solution mixes.Temperature transfers to 20 ℃, slowly drips the 1.218g propylene oxide, stops after dropwising stirring, and leaves standstill to gel formation.Behind the 3d gel is dipped in the ethanol, changes ethanol one time every 5h, continue displacement 1d.Then the gel behind the solvent exchange is carried out the supercritical co drying, temperature 50 C, pressure 12MPa, carbonic acid gas flow velocity 5mL/min, time of drying, 12h obtained granular ferroferric oxide aerogel particle.Ferroferric oxide aerogel magneticsubstance of the present invention obtains crystal grain with the SEM observation and is about 40nm, and recording saturation magnetization with vibrating sample magnetometer is 52.28emug
-1, density is 2.09gcm
-1, specific surface area is 728.842
2G
-1, mean pore size is 16.35nm.
Embodiment 3
Under nitrogen protection, in the 50ml container of magnetic stir bar is housed, add successively iron(ic) chloride 0.812g under the room temperature, iron protochloride 0.398g, dehydrated alcohol 2.5ml fully stir until solution mixes.Temperature transfers to 25 ℃, slowly drips the 2.09g propylene oxide, stops after dropwising stirring, and leaves standstill to gel formation.Behind the 5d gel is dipped in the acetone, changes acetone one time every 5h, continue displacement 1d.Then the gel behind the solvent exchange is carried out the supercritical co drying, temperature 50 C, pressure 12MPa, carbonic acid gas flow velocity 10mL/min, time of drying, 15h obtained granular ferroferric oxide aerogel particle.Ferroferric oxide aerogel magneticsubstance of the present invention obtains crystal grain with the SEM observation and is about 50nm, and recording saturation magnetization with vibrating sample magnetometer is 41.53emug
-1, density is 2.37gcm
-1, specific surface area is 176.22m
2G
-1, mean pore size is 10.13nm.
Embodiment 4
Step 1, material dissolution: under nitrogen protection, in the 50ml container of magnetic stir bar is housed, add successively iron nitrate 3.232g under the room temperature, Iron nitrate 1.152g, dehydrated alcohol 12ml fully stir until solution mixes;
The formation of step 2, gel: under whipped state, to the molysite mixed solution and dripping 8.88g epoxy chloropropane of step 1 gained, dropwise and stop to stir, leave standstill to gel formation;
Step 3, aging: the gel of step 2 gained is left standstill aging 7d;
Step 4, solvent exchange: the gel behind the 7d that will wear out is dipped in the acetone, changes acetone one time every 5h, continues displacement 1d;
Step 5, drying: the gel behind the solvent exchange of step 4 gained is carried out the supercritical co drying, temperature 60 C, pressure 15MPa, carbonic acid gas flow velocity 10mL/min, time of drying, 12h obtained granular ferroferric oxide aerogel particle.Obtain crystal grain with the SEM observation and be about 60nm, recording saturation magnetization with vibrating sample magnetometer is 14.28emug
-1, density is 1.25gcm
-1, specific surface area is 229.6m
2G
-1, mean pore size is 13.74nm.
Embodiment 5
Step 1, material dissolution: under nitrogen protection, in the 50ml container of magnetic stir bar is housed, add successively iron(ic) chloride 1.894g under the room temperature, ferrous sulfate 1.112g, dehydrated alcohol 9ml, deionized water 2ml fully stir until solution mixes;
The formation of step 2, gel: under whipped state, to the molysite mixed solution and dripping 2.44g propylene oxide of step 1 gained, dropwise and stop to stir, leave standstill to gel formation;
Step 3, aging: the gel of step 2 gained is left standstill aging 7d;
Step 4, solvent exchange: the gel behind the 7d that will wear out is dipped in the acetone, changes acetone one time every 5h, continues displacement 1d;
Step 5, drying: the gel behind the solvent exchange of step 4 gained is carried out constant pressure and dry, and 80 ℃ of temperature obtain granular ferroferric oxide aerogel particle.Obtain crystal grain with the SEM observation and be about 50nm, recording saturation magnetization with vibrating sample magnetometer is 46.58emug
-1, density is 2.81gcm
-1, specific surface area is 151.43m
2G
-1, mean pore size is 11.07nm.
The present invention includes but be not limited to above embodiment, every any being equal to of carrying out under the principle of spirit of the present invention, replace or local improvement, all will be considered as within protection scope of the present invention.
Claims (4)
1. the preparation method of a ferroferric oxide aerogel, it is characterized in that: concrete steps are as follows:
Step 1, material dissolution: under nitrogen protection, divalent iron salt and trivalent iron salt be dissolved in respectively obtain corresponding solution in organic solvent or the water, get respectively divalent iron salt and ferric salt solution, mix, obtain mixed molysite solution, wherein Fe
3+With Fe
2+Mol ratio be 1:1-2.5:1;
The formation of step 2, gel: the molysite mixed solution and dripping gel promotor to the step 1 gained obtains gel;
Step 3, aging: leave standstill the gel of step 2 gained aging;
Step 4, solvent exchange: the gel after will wearing out is dipped into and carries out solvent exchange among the solvent a, until solvent is replaced by solvent a fully in the gel, obtains containing the gel of solvent a;
Step 5, drying: the gel that contains solvent a of step 4 gained is carried out obtaining ferroferric oxide aerogel after the drying.
2. the preparation method of a kind of ferroferric oxide aerogel as claimed in claim 1, it is characterized in that: the described gel promotor of step 2 is organic Lewis base, is preferably small molecules epoxy compounds, the derivative of 1 α position electrophilic substitution, Racemic glycidol ether compound.
3. the preparation method of a kind of ferroferric oxide aerogel as claimed in claim 1, it is characterized in that: the described solvent a of step 4 is organic solvent, is preferably acetone or alcohol.
4. such as the preparation method of claim 1 or 3 described a kind of ferroferric oxide aerogels, it is characterized in that: the described drying mode of step 5 can be supercritical drying, constant pressure and dry, lyophilize.
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| CN102923788B CN102923788B (en) | 2014-07-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107619092A (en) * | 2017-07-18 | 2018-01-23 | 南京工业大学 | A kind of preparation method of magnetic aeroge |
| WO2020149818A1 (en) * | 2019-01-14 | 2020-07-23 | Massachusetts Institute Of Technology | Salt-aided hydrogel/aerogel growth |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060009370A1 (en) * | 2000-05-04 | 2006-01-12 | Lars Zuechner | Use of nanoscale particles for improving dirt removal |
| CN101485969B (en) * | 2008-06-23 | 2010-09-29 | 南京工业大学 | Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process |
| CN101851009B (en) * | 2010-06-10 | 2012-03-07 | 南京工业大学 | Method for preparing lobate ferroferric oxide aerogel particle |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060009370A1 (en) * | 2000-05-04 | 2006-01-12 | Lars Zuechner | Use of nanoscale particles for improving dirt removal |
| CN101485969B (en) * | 2008-06-23 | 2010-09-29 | 南京工业大学 | Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process |
| CN101851009B (en) * | 2010-06-10 | 2012-03-07 | 南京工业大学 | Method for preparing lobate ferroferric oxide aerogel particle |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107619092A (en) * | 2017-07-18 | 2018-01-23 | 南京工业大学 | A kind of preparation method of magnetic aeroge |
| WO2020149818A1 (en) * | 2019-01-14 | 2020-07-23 | Massachusetts Institute Of Technology | Salt-aided hydrogel/aerogel growth |
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| CN102923788B (en) | 2014-07-02 |
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