CN107416909A - A kind of preparation method of iron-based oxide silica aerogel - Google Patents
A kind of preparation method of iron-based oxide silica aerogel Download PDFInfo
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- CN107416909A CN107416909A CN201710753800.4A CN201710753800A CN107416909A CN 107416909 A CN107416909 A CN 107416909A CN 201710753800 A CN201710753800 A CN 201710753800A CN 107416909 A CN107416909 A CN 107416909A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 230000005291 magnetic effect Effects 0.000 claims abstract description 34
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 23
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000000376 reactant Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002485 combustion reaction Methods 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 23
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 8
- 229910002518 CoFe2O4 Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008246 gaseous mixture Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002771 BaFe12O19 Inorganic materials 0.000 claims description 2
- 229910017163 MnFe2O4 Inorganic materials 0.000 claims description 2
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims description 2
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 230000005611 electricity Effects 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- 239000011358 absorbing material Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 47
- 230000003595 spectral effect Effects 0.000 description 16
- 238000001228 spectrum Methods 0.000 description 15
- 229910003321 CoFe Inorganic materials 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910001960 metal nitrate Inorganic materials 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 3
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 3
- 239000004964 aerogel Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
Classifications
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
-
- 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
-
- 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
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of iron-based oxide silica aerogel, it is related to the preparation method of oxide silica aerogel.It is to solve existing oxide silica aerogel preparation method energy consumption it is big, complex operation, the technical problem of long preparation period.This method：The nitrate of various metallic elements in iron-based oxide and pore-creating reactant are prepared into solution, is then heated in solution after moisture evaporating completely and self-propagating combustion reaction occurs, obtain iron-based oxide silica aerogel.This method equipment is simple and convenient to operate, quickly, energy consumption it is low, raw material is easy to get, the purity of iron-based oxide is high in the aeroge of the present invention, available for the field such as sewage disposal, catalyst, high energy battery, sensitive material, absorbing material and optics, electricity, magnetics.
Description
Technical field
The present invention relates to the preparation method of oxide silica aerogel, belongs to special appearance and functional inorganic nano-material field.
Background technology
Because iron-based oxide has the physical properties such as good electricity, magnetics, optics, and chemically stable and biofacies
The advantages that appearance, make it in ferromagnetic material, ferroelectric material, photoelectric material, battery, catalysis, targeted drug, sewage disposal and microwave
The fields such as absorption are widely used.
Aerogel material is gassiness material in a kind of space net structure, with density is low, specific surface area is big, hole
The features such as gap rate is high, adsorptivity is strong, is widely used in fields such as absorption, catalysis, insulations.
Iron-based oxide silica aerogel combines the advantages of above two material, with density is small, specific surface area is big, surface is inhaled
The outstanding features such as attached property is strong.Therefore, iron-based oxide silica aerogel magnetic material, photoelectric material, energy storage material, absorption, catalysis,
The field such as biomedical, sensor and insulation has a good application prospect.
The preparation method of existing oxide silica aerogel is using supercritical drying, freeze-drying, collosol and gel re-dry
Method, it is big energy consumption to be present in these methods, the shortcomings that complex operation, long preparation period, can not mass produce.
The content of the invention
The present invention is to solve the preparation method energy consumption of existing oxide silica aerogel is big, complex operation, long preparation period
Technical problem, and provide a kind of preparation method of iron-based oxide silica aerogel.
The preparation method of the iron-based oxide silica aerogel of the present invention, is carried out according to the following steps：
First, various metallic element nitrate are weighed by the stoichiometric proportion of various metallic elements in iron-based oxide, then claimed
Pore-creating reactant is taken, wherein pore-creating reactant is glycine (NH2CH2COOH) or citric acid, whole metallic element nitrate are with making
The mol ratio (M/G) of hole reactant is 1：(0.5~1.5)；
2nd, whole metallic element nitrate and pore-creating reactant are added in appropriate deionized water, magnetic agitation makes it
Dissolving, obtains precursor liquid；
3rd, under agitation, precursor liquid is heated to temperature as 180 DEG C~220 DEG C until being sent out after moisture evaporating completely
Propagating combustion reaction is born from, obtains iron-based oxide silica aerogel.
Utilize Fe2O3Aeroge can also prepare magnetic Fe3O4Aeroge, its method are：Fe2O3Aeroge is put into tubular type
In stove, under conditions of the mixed atmosphere of nitrogen and hydrogen, 350 DEG C~500 DEG C are heated to 5~10 DEG C/min heating rate
Reduction reaction is carried out, after reaction terminates, that is, obtains magnetic Fe3O4Aeroge；Wherein in the gaseous mixture of nitrogen and hydrogen shared by hydrogen
Percent by volume be 5%~8%.
In the present invention, metal nitrate and NH2CH2COOH (or citric acid) solution steams in heating process with moisture
Hair becomes gel, and further heating causes metal nitrate and NH2CH2Combustion reaction occurs for COOH (or citric acid), and moment produces
Substantial amounts of vapor, CO2、CO、NO2, the gas such as NO, control the ratio of different metal nitrates and pore-creating reactant (M/G) energy
Different product purities and pattern are obtained, appropriate M/G ratios can obtain the iron-based oxide silica aerogel of high-purity.The present invention is also
By Fe2O3Aeroge is by controlling hydrogen flowing quantity, reaction temperature and time selectivity to be reduced to magnetic Fe3O4, reduction product Fe3O4
Still remain loose porous aerogel structure.
The present invention prepares iron-based oxide silica aerogel using self-propagating combustion, and the preparation method device therefor is simple, behaviour
Facilitate, raw material is easy to get, it is possible to achieve industrial mass production.Iron-based oxide silica aerogel purity height, the knot of this method preparation
The advantages that crystalline substance is good, density is small, specific surface area is big, property is stable, in sewage disposal, catalyst, high energy battery, sensitive material
The field such as material, absorbing material and optics, electricity, magnetics has a good application prospect.
Brief description of the drawings
Fig. 1 is iron-based oxide Fe prepared by experiment 1,2 and 32O3The XRD spectrum of aeroge；
Fig. 2 is iron-based oxide Fe prepared by experiment 1,2 and 33O4The XRD spectrum of aeroge；
Fig. 3 is iron-based oxide Fe prepared by experiment 12O3The SEM spectrum of aeroge；
Fig. 4 is iron-based oxide Fe prepared by experiment 13O4The SEM spectrum of aeroge；
Fig. 5 is iron-based oxide Fe prepared by experiment 23O4Magnetic phenomenon photo of the aeroge under external magnetic field；
Fig. 6 is iron-based oxide Fe prepared by experiment 32O3Aeroge photo；
Fig. 7 is iron-based oxide CoFe prepared by experiment 4,5 and 62O4The XRD spectrum of aeroge；
Fig. 8 is iron-based oxide CoFe prepared by experiment 42O4The SEM spectrum of aeroge.
Fig. 9 is iron-based oxide CoFe prepared by experiment 42O4Magnetic phenomenon photo of the aeroge under external magnetic field.
Embodiment
Embodiment one：The preparation method of the iron-based oxide silica aerogel of present embodiment, is carried out according to the following steps：
First, various metallic element nitrate are weighed by the stoichiometric proportion of various metallic elements in iron-based oxide, then claimed
Pore-creating reactant is taken, wherein pore-creating reactant is glycine (NH2CH2COOH) or citric acid, whole metallic element nitrate are with making
The mol ratio (M/G) of hole reactant is 1：(0.5~1.5)；Whole metallic element nitrate and pore-creating reactant are added appropriate
Deionized water in, magnetic agitation makes its dissolving, obtains precursor liquid；
2nd, under agitation, precursor liquid is heated into temperature to keep to moisture evaporating completely for 180 DEG C~220 DEG C
Generation self-propagating combustion reacts, and obtains iron-based oxide silica aerogel.
Embodiment two：Present embodiment is Fe from iron-based oxide unlike embodiment one2O3、
CoFe2O4、NiFe2O4、MnFe2O4、BaFe12O19Or MnxZn1-xFe2O4(x=0~1)；It is other with the phase of embodiment one
Together.
Embodiment three：Whole metals in present embodiment step 1 unlike embodiment one or two
The mol ratio (M/G) of element nitrate and pore-creating reactant is 1：0.6；It is other identical with embodiment one or two.
Embodiment four：Whole metals in present embodiment step 1 unlike embodiment one or two
The mol ratio (M/G) of element nitrate and pore-creating reactant is 1：0.8；It is other identical with embodiment one or two.
Embodiment five：Whole metals in present embodiment step 1 unlike embodiment one or two
The mol ratio (M/G) of element nitrate and pore-creating reactant is 1：1；It is other identical with embodiment one or two.
Embodiment six：It is preceding in step 1 unlike one of present embodiment and embodiment one to five
The concentration for driving whole metal ions in body fluid is 0.1~0.3mol/L；It is other identical with one of embodiment one to five.
Embodiment seven：Utilize Fe2O3Aeroge prepares magnetic Fe3O4The method of aeroge, it is specially：Fe2O3
Aeroge is put into tube furnace, under conditions of the mixed atmosphere of nitrogen and hydrogen, is heated with 5~10 DEG C/min heating rate
To 350 DEG C~500 DEG C progress reduction reactions, after reaction terminates, that is, magnetic Fe is obtained3O4Aeroge；Wherein nitrogen and hydrogen is mixed
It is 5%~8% to close the percent by volume in gas shared by hydrogen.
Embodiment eight：Present embodiment and reduction reaction time unlike embodiment seven be 0.5h~
1.5h；It is other identical with one of embodiment one to five.
Beneficial effects of the present invention are verified using tests below：
Experiment 1：The Fe of this experiment2O3The preparation method of aeroge follows the steps below：
First, 2.02g Fe (NO are weighed3)3·9H2O and 0.2252g NH2CH2COOH is in 100ml beakers, Fe
(NO3)3·9H2O and NH2CH2COOH mol ratio (M/G) is 1:0.6,50ml deionized waters are added, magnetic agitation 10min makes it
Dissolving, obtains precursor liquid；
2nd, the precursor liquid for obtaining step 1 is placed on heating magnetic stirring apparatus, while magnetic agitation, is heated to temperature
For 200 DEG C of holdings, until self-propagating combustion reaction occurs after moisture evaporating completely, Fe is obtained2O3Aeroge；
The Fe for recycling this experiment 1 to obtain2O3Aeroge prepares magnetic Fe3O4Aeroge, specific steps are carried out as follows：
Fe2O3Aeroge is put into tube furnace, under conditions of the mixed atmosphere of nitrogen and hydrogen, is added with 5 DEG C/min heating rate
Hot to 450 DEG C carry out reduction reaction 1 hour, after reaction terminates, that is, obtain magnetic Fe3O4Aeroge；Wherein nitrogen and hydrogen is mixed
It is 5% to close the percent by volume in gas shared by hydrogen.
The Fe that this experiment 1 obtains2O3The XRD spectrum of aeroge, can be with from the spectral line a in Fig. 1 as shown in the spectral line a in Fig. 1
Find out, the composition in aeroge is α-Fe2O3With γ-Fe2O3；Fe3O4The XRD spectrum of aeroge as shown in the spectral line a in Fig. 2,
It is Fe that the composition in aeroge is can be seen that from the spectral line a in Fig. 23O4。
Fig. 3 is this experiment product Fe2O3The SEM of aeroge schemes, as can be seen from Figure 3 Fe2O3Aeroge is irregular thin-walled
Loose structure；Fig. 4 this experiment product magnetic Fes3O4The SEM of aeroge schemes, as can be seen from Figure 4 magnetic Fe3O4Aeroge is fluffy
The coralliform structure of pine.
The equipment of this experiment is simple and convenient to operate, and raw material is easy to get, short preparation period, and energy consumption is low.
Experiment 2：The Fe of this experiment2O3The preparation method of aeroge follows the steps below：
First, 2.02g Fe (NO are weighed3)3·9H2O and 0.3003g NH2CH2COOH is in 100ml beakers, Fe
(NO3)3·9H2O and NH2CH2COOH mol ratio (M/G) is 1:0.8,50ml deionized waters are added, magnetic agitation 10min makes it
Dissolving, obtains precursor liquid；
2nd, the precursor liquid of step 1 is placed on heating magnetic stirring apparatus and is heated to temperature as 220 DEG C, while magnetic force stirs
Mix, until self-propagating combustion reaction occurs after moisture evaporating completely, obtain Fe2O3Aeroge；
The Fe for recycling this experiment 2 to obtain2O3Aeroge prepares magnetic Fe3O4Aeroge, specific steps are carried out as follows：
The Fe that experiment 2 is obtained2O3Aeroge is put into tube furnace, is being passed through the atmosphere bar of the gaseous mixture of nitrogen and hydrogen
Under part, it is heated to 450 DEG C with 5 DEG C/min heating rate and carries out reduction reaction 1 hour, after reaction terminates, that is, obtain magnetic
Fe3O4Aeroge；Percent by volume wherein in the gaseous mixture of nitrogen and hydrogen shared by hydrogen is 5%.
The product Fe of this experiment 22O3The XRD spectrum of aeroge is as shown in the spectral line b in Fig. 1, it can be seen that can
To find out, the composition in aeroge is α-Fe2O3With γ-Fe2O3；The product Fe of this experiment 23O4The XRD spectrum of aeroge such as Fig. 2
In spectral line b shown in, as can be seen from the figure the composition in aeroge is Fe3O4.Matched completely with corresponding product.
Fig. 5 is the product Fe of this experiment 23O4Magnetic phenomenon of the aeroge under external magnetic field.It can be seen that
Fe3O4Aeroge can be by magnet adsorption.
The equipment of this experiment is simple and convenient to operate, and raw material is easy to get, short preparation period, and energy consumption is low.
Experiment 3：The Fe of this experiment2O3The preparation method of aeroge follows the steps below：
First, 2.02g Fe (NO are weighed3)3·9H2O and 0.3754g NH2CH2COOH is in 100ml beakers, Fe
(NO3)3·9H2O and NH2CH2COOH mol ratio (M/G) is 1:1,50ml deionized waters are added, magnetic agitation 10min makes its molten
Solution, obtains precursor liquid；
2nd, the precursor liquid of step 1 is placed on heating magnetic stirring apparatus and is heated to temperature as 200 DEG C, while magnetic force stirs
Mix, until self-propagating combustion reaction occurs after moisture evaporating completely, obtain Fe2O3Aeroge；
The Fe for recycling this experiment 3 to obtain2O3Aeroge prepares magnetic Fe3O4Aeroge, specific steps are carried out as follows：
The Fe that experiment 3 is obtained2O3Aeroge is put into tube furnace, is being passed through the atmosphere bar of the gaseous mixture of nitrogen and hydrogen
Under part, 440 DEG C of progress reduction reaction 1.5h are heated to 5 DEG C/min heating rate, after reaction terminates, that is, obtain magnetic Fe3O4
Aeroge；Percent by volume wherein in the gaseous mixture of nitrogen and hydrogen shared by hydrogen is 5%.
The iron-based oxide Fe that this experiment 3 obtains2O3The photo in kind of aeroge is as shown in Figure 6.It macroscopically shows as dredging
Loose macroporous structure.The product Fe of this experiment 32O3The XRD spectrum of aeroge is as shown in the spectral line c in Fig. 1, from the spectral line c in Fig. 1
As can be seen that the composition in aeroge is α-Fe2O3With γ-Fe2O3；Fe3O4The XRD spectrum of aeroge such as the spectral line c institutes in Fig. 2
Show, it is Fe that the composition in aeroge is can be seen that from the spectral line c in Fig. 23O4.Corresponding product matches completely.
The equipment of this experiment is simple and convenient to operate, and raw material is easy to get, short preparation period, and energy consumption is low.
Experiment 4：The CoFe of this experiment2O4The preparation method of aeroge follows the steps below：
First, 1.3467g Fe (NO are weighed3)3·9H2O, 0.4850g Co (NO3)2·6H2O's and 0.3003g
NH2CH2COOH is in 100ml beakers, Co (NO3)2·6H2O and Fe (NO3)3·9H2O mol ratio is 1:2, total metal ion
Fe3+And Co2+With NH2CH2COOH mol ratio (M/G) is 1:0.8th, 50ml deionized waters are added, magnetic agitation 10min makes its molten
Solution, obtains precursor liquid；
2nd, the precursor liquid of step 1 is placed on heating magnetic stirring apparatus and is heated to temperature as 200 DEG C, while magnetic force stirs
Mix, until self-propagating combustion reaction occurs after moisture evaporating completely, obtain CoFe2O4Aeroge.
The product CoFe of this experiment 42O4The XRD spectrum of aeroge, can be with from Fig. 7 spectral line a as shown in the spectral line a in Fig. 7
Find out, the CoFe of aeroge2O4With CoFe2O4PDF standard card perfect matchings.
Fig. 8 is the product CoFe of this experiment 42O4The SEM pictures of aeroge, from figure 8, it is seen that aeroge is loose structure.
Fig. 9 is the product CoFe of this experiment 42O4Magnetic phenomenon of the aeroge under external magnetic field.From fig. 9, it can be seen that should
CoFe2O4Aeroge can be by magnet adsorption.
The equipment of this experiment is simple and convenient to operate, and raw material is easy to get, short preparation period, and energy consumption is low.
Experiment 5：Fe (the NO for being distinguished as weighing 1.3467g in step 1 of this experiment and experiment 43)3·9H2O、0.4850g
Co (NO3)2·6H2O and 0.3754g NH2CH2COOH is in 100ml beakers, Co (NO3)2·6H2O and Fe (NO3)3·9H2O
Mol ratio be 1:2, total metal cations Fe3+And Co2+With NH2CH2COOH mol ratio (M/G) is 1:1.Other and experiment 4
It is identical.
The product CoFe of this experiment 52O4The XRD spectrum of aeroge, can be with from Fig. 7 spectral line b as shown in the spectral line b in Fig. 7
Find out, the CoFe of aeroge2O4With CoFe2O4PDF standard card perfect matchings.
Experiment 6：Fe (the NO for being distinguished as weighing 1.3467g in step 1 of this experiment and experiment 43)3·9H2O、0.4850g
Co (NO3)2·6H2O and 0.4504g NH2CH2COOH is in 100ml beakers, Co (NO3)2·6H2O and Fe (NO3)3·9H2O
Mol ratio be 1:2, total metal cations Fe3+And Co2+With NH2CH2COOH mol ratio (M/G) is 1:1.2.Other and experiment
4 is identical.
The product CoFe of this experiment 62O4The XRD spectrum of aeroge, can be with from Fig. 7 spectral line c as shown in the spectral line c in Fig. 7
Find out, the CoFe of aeroge2O4With CoFe2O4PDF standard card perfect matchings.
Claims (9)
1. a kind of preparation method of iron-based oxide silica aerogel, it is characterised in that this method is carried out according to the following steps：
First, various metallic element nitrate are weighed by the stoichiometric proportion of various metallic elements in iron-based oxide, then weighs and make
Hole reactant, wherein pore-creating reactant are mole of glycine or citric acid, whole metallic element nitrate and pore-creating reactant
It is 1 than (M/G)：(0.5~1.5)；Whole metallic element nitrate and pore-creating reactant are added in appropriate deionized water, magnetic
Power stirring makes its dissolving, obtains precursor liquid；
2nd, under agitation, precursor liquid is heated into temperature to keep to moisture evaporating completely occurring for 180 DEG C~220 DEG C
Self-propagating combustion reacts, and obtains iron-based oxide silica aerogel.
A kind of 2. preparation method of iron-based oxide silica aerogel according to claim 1, it is characterised in that described iron-based
Oxide is Fe2O3、CoFe2O4、NiFe2O4、MnFe2O4、BaFe12O19Or MnxZn1-xFe2O4(x=0~1).
3. the preparation method of a kind of iron-based oxide silica aerogel according to claim 1 or 2, it is characterised in that in step 1
The mol ratio (M/G) of whole metallic element nitrate and pore-creating reactant is 1：0.6.
4. the preparation method of a kind of iron-based oxide silica aerogel according to claim 1 or 2, it is characterised in that in step 1
The mol ratio (M/G) of whole metallic element nitrate and pore-creating reactant is 1：0.8.
5. the preparation method of a kind of iron-based oxide silica aerogel according to claim 1 or 2, it is characterised in that complete in rapid one
The mol ratio (M/G) of portion's metallic element nitrate and pore-creating reactant is 1：1.
6. the preparation method of a kind of iron-based oxide silica aerogel according to claim 1 or 2, it is characterised in that in step 1
The mol ratio (M/G) of whole metallic element nitrate and pore-creating reactant is 1：1.2.
A kind of 7. preparation method of iron-based oxide silica aerogel according to claim 1 or 2, it is characterised in that step 1
In, the concentration of whole metal ions is 0.1~0.3mol/L in precursor liquid.
8. utilize the Fe described in claim 22O3Aeroge prepares magnetic Fe3O4The method of aeroge, it is characterised in that this method
Carry out according to the following steps：Fe2O3Aeroge is put into tube furnace, under conditions of the mixed atmosphere of nitrogen and hydrogen, with 5~
10 DEG C/min heating rate is heated to 350 DEG C~500 DEG C progress reduction reactions, after reaction terminates, that is, obtains magnetic Fe3O4Gas
Gel；Percent by volume wherein in the gaseous mixture of nitrogen and hydrogen shared by hydrogen is 5%~8%.
9. according to claim 8 utilize Fe2O3Aeroge prepares magnetic Fe3O4The method of aeroge, it is characterised in that also
The former reaction time is 0.5h~1.5h.
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