CN106607095A - Method for preparing magnetic hierarchical pore structure composite material through evaporation-induced self assembly - Google Patents
Method for preparing magnetic hierarchical pore structure composite material through evaporation-induced self assembly Download PDFInfo
- Publication number
- CN106607095A CN106607095A CN201710002560.4A CN201710002560A CN106607095A CN 106607095 A CN106607095 A CN 106607095A CN 201710002560 A CN201710002560 A CN 201710002560A CN 106607095 A CN106607095 A CN 106607095A
- Authority
- CN
- China
- Prior art keywords
- structure composite
- evaporation
- magnetic
- porous structure
- hierarchical porous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000802 evaporation-induced self-assembly Methods 0.000 title claims abstract description 14
- 239000002149 hierarchical pore Substances 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 26
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 230000002269 spontaneous effect Effects 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 239000006184 cosolvent Substances 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000002638 heterogeneous catalyst Substances 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000010919 dye waste Substances 0.000 abstract 1
- 239000004973 liquid crystal related substance Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 9
- 230000000694 effects Effects 0.000 description 4
- 150000002823 nitrates Chemical class 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- LITYQKYYGUGQLY-UHFFFAOYSA-N iron nitric acid Chemical compound [Fe].O[N+]([O-])=O LITYQKYYGUGQLY-UHFFFAOYSA-N 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 239000002122 magnetic nanoparticle Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000005405 multipole Effects 0.000 description 1
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for preparing a magnetic hierarchical pore structure composite material through evaporation-induced self assembly. The innovation points and the characteristics of the preparation method are as follows: (1) a surfactant P123 or F127 is dissolved into an organic solvent ethanol, and certain ferric nitrate is intruded into the system to be complexed with the ethanol; (2) the system innovatively introduces normal octane as a cosolvent and a pore-enlarging agent and utilizes that the normal octane and the ethanol have the same volatilizing property; (3) ferrocence is introduced, and the ferrocence only can be dissolved in the nonpolar normal octane solvent and is integrated into a surfactant hydrophobic liquid crystal phase to serve as an iron source in the pore and a pore-enlarging agent; and (4) oxygen atmosphere calcination is adopted to effectively remove the organic molecular chain from the pore, so that the magnetic iron oxide is distributed on the inner surface of the magnetic hierarchical pore structure composite material uniformly. The magnetic hierarchical pore structure composite material prepared by the method has high catalytic property and can serve as a heterogeneous catalyst for dye waste water degradation.
Description
Technical field
The present invention relates to environmental catalysis field of material technology, and in particular to it is multistage that a kind of evaporation-induced self-assembly prepares magnetic
The method of pore structure composite.
Background technology
At present, preparing the technology of magnetic hierarchical porous structure composite mainly has area load and limit threshold to grow two kinds of sides
Method, area load is the method for most traditional preparation magnetic hierarchical porous structure composite, and the shortcoming of this kind of preparation method is to make
Active component dispersion is uneven, causes its catalysis activity to be easy to run off, and application is subject to certain restrictions.Limit threshold is grown with luxuriant iron long-chain
Surfactant is that template prepares iron content hierarchical porous structure composite for representative, and the shortcoming of this kind of method is long-chain containing metal
Surfactant preparation flow is loaded down with trivial details, lasts length, yields poorly, and causes its industrialization difficulty big.The present inventor is through grinding
Study carefully discovery, these preparation methods all have some shortcomings, how to prepare magnetic hierarchical porous structure composite, strengthen its catalysis and live
Property, become technical problem urgently to be resolved hurrily at present.
The content of the invention
For the technical problem that prior art is present, the present invention provides a kind of evaporation-induced self-assembly and prepares magnetic multi-stage porous
The method of structural composite material, magnetic hierarchical porous structure composite catalytic performance made by the method is high, can be used as heterogeneous
Catalyst is used for dye wastewater degradation.
In order to solve above-mentioned technical problem, following technical scheme is present invention employs：
A kind of method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite, methods described includes following step
Suddenly：
(1) P123 the or F127 surfactants for, weighing 2.3～4.6g are dissolved in the absolute ethyl alcohol of 15～30ml, will be contained
The beaker for having absolute ethyl alcohol is put on temperature constant magnetic stirring machine, and normal temperature sealing 0.5～1h of stirring is added to after being completely dissolved
0.148～5.2g ferric nitrates；
(2) normal octane for, measuring 2.28～4.56ml is added drop-wise in the solution of step (1), normal temperature sealing 2～4h of stirring,
And the P123 or F127 and the mol ratio of normal octane are 0.028～0.030；
(3), weigh 1.602～3.204g ferrocene to be dissolved in the mixed solution of step (2), normal temperature sealing 2～4h of stirring,
And the ferric nitrate and the ratio of the amount of the material of iron in ferrocene are 0～70；
(4), in the mixed solution of step (3) add 4.5～9ml tetraethyl orthosilicate, normal temperature sealing stirring 12～
Silicon in 24h, and the tetraethyl orthosilicate is 50 with the ratio of the amount of the material of iron in ferrocene and ferric nitrate：1～5：7；
(5), take out beaker the reactant liquor in step (4) to be proceeded in the culture dish of 90ml, 3～4d of room temprature evaporation；
(6), culture dish is put in the constant temperature blast drying oven in 60～80 DEG C and is dried 3～24h；
(7), dried sample is placed in Muffle furnace, under oxygen atmosphere, 300～550 DEG C is heated to, heating
The speed of intensification is 11 DEG C/min, and the roasting 6h at a temperature of 300～550 DEG C, i.e., effectively gone using oxygen atmosphere calcination
Except the organic molecule chain in hole, magnetic iron oxide is set to be evenly distributed on the inner surface of magnetic multipole pore structure composite；
(8), grinding obtains sample after spontaneous combustion cooling, is put in standby in drying box.
Further, surfactant is P123 in the step (1), and the magnetic hierarchical porous structure composite of preparation is six
Square duct structure.
Further, surfactant is F127 in the step (1), and the magnetic hierarchical porous structure composite of preparation is vertical
Square duct structure.
Compared with prior art, the evaporation-induced self-assembly that the present invention is provided prepares magnetic hierarchical porous structure composite
Method, adds ferric nitrate to be complexed with ethanol in the absolute ethyl alcohol of dissolving P123 or F127 surfactants, and adds normal octane
Used as cosolvent and expanding agent, ferrocene plays certain reaming effect, ferric nitrate iron as the source of iron and expanding agent in hole
Source is uniformly distributed in hierarchical porous structure composite inner, it is thus possible to form different pore passage structures, such as hexagonal hole road structure
With a cube pore passage structure, the magnetic nano-particle such as iron ion of different content is embedded or is embedded in hierarchical porous structure composite
Inner surface or outer surface, make the magnetic hierarchical porous structure composite of catalytic active component high degree of dispersion, thus the method
Made by magnetic hierarchical porous structure composite catalytic performance it is high, dye wastewater degradation can be used for as heterogeneous catalysis.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, enter below
One step illustrates the present invention.
Embodiment 1：
A kind of method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite, methods described includes following step
Suddenly：
(1) the P123 surfactants for, weighing 2.3g are dissolved in 15 absolute ethyl alcohol, and the beaker for filling absolute ethyl alcohol is put
On temperature constant magnetic stirring machine, normal temperature sealing stirring 0.5h adds 0.148g ferric nitrates to after being completely dissolved；
(2) normal octane for, measuring 2.28ml is added drop-wise in the solution of step (1), normal temperature sealing stirring 2h, and the P123
It is 0.028 with the mol ratio of normal octane；
(3), weigh 1.602g ferrocene to be dissolved in the mixed solution of step (2), normal temperature sealing stirring 2h, and the nitric acid
Iron is 1 with the ratio of the amount of the material of iron in ferrocene：3；
(4) tetraethyl orthosilicate (TEOS) of 4.5ml, is added in the mixed solution of step (3), 12h is stirred in normal temperature sealing,
And the silicon in the tetraethyl orthosilicate and the ratio of the amount of the material of iron in ferrocene and ferric nitrate are 9：1；
(5), take out beaker the reactant liquor in step (4) to be proceeded in the culture dish of 90ml, room temprature evaporation 3d；
(6), culture dish is put in the constant temperature blast drying oven in 60 DEG C and is dried 3h；
(7), dried sample is placed in Muffle furnace, under oxygen atmosphere, 300 DEG C is heated to, heat temperature raising
Speed be 11 DEG C/min, and the roasting 6h at a temperature of 300 DEG C；
(8), grinding obtains sample after spontaneous combustion cooling, and the sample is hexagonal hole road magnetic hierarchical porous structure composite,
And be put in the sample standby in drying box.
Embodiment 2：
A kind of method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite, methods described includes following step
Suddenly：
(1) the F127 surfactants for, weighing 2.3g are dissolved in the absolute ethyl alcohol of 20ml, will fill the beaker of absolute ethyl alcohol
It is put on temperature constant magnetic stirring machine, normal temperature sealing stirring 0.8h adds 0.914g ferric nitrates to after being completely dissolved；
(2) normal octane for, measuring 2.28ml is added drop-wise in the solution of step (1), normal temperature sealing stirring 3h, and the F127
It is 0.029 with the mol ratio of normal octane；
(3), weigh 1.602g ferrocene to be dissolved in the mixed solution of step (2), normal temperature sealing stirring 3h, and the nitric acid
Iron is 1 with the ratio of the amount of the material of iron in ferrocene：2；
(4) tetraethyl orthosilicate of 4.5ml, is added in the mixed solution of step (3), 12h is stirred in normal temperature sealing, and described
Silicon in tetraethyl orthosilicate is 8 with the ratio of the amount of the material of iron in ferrocene and ferric nitrate：2；
(5), take out beaker the reactant liquor in step (4) to be proceeded in the culture dish of 90ml, room temprature evaporation 3.5d；
(6), culture dish is put in the constant temperature blast drying oven in 70 DEG C and is dried 12h；
(7), dried sample is placed in Muffle furnace, under oxygen atmosphere, 450 DEG C is heated to, heat temperature raising
Speed be 11 DEG C/min, and the roasting 6h at a temperature of 450 DEG C；
(8), grinding obtains sample after spontaneous combustion cooling, and the sample is cube duct magnetic hierarchical porous structure composite,
And be put in the sample standby in drying box.
Embodiment 3：
A kind of method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite, methods described includes following step
Suddenly：
(1) the F127 surfactants for, weighing 4.6g are dissolved in the absolute ethyl alcohol of 30ml, will fill the beaker of absolute ethyl alcohol
It is put on temperature constant magnetic stirring machine, normal temperature sealing stirring 1h adds 1.602g ferric nitrates to after being completely dissolved；
(2) normal octane for, measuring 4.56ml is added drop-wise in the solution of step (1), normal temperature sealing stirring 4h, and the F127
It is 0.030 with the mol ratio of normal octane；
(3), weigh 3.204g ferrocene to be dissolved in the mixed solution of step (2), normal temperature sealing stirring 4h, and the nitric acid
Iron is 2 with the ratio of the amount of the material of iron in ferrocene：3；
(4), in the mixed solution of step (3) add 9ml tetraethyl orthosilicate, normal temperature sealing stirring 24h, and it is described just
Silicon in silester is 5 with the ratio of the amount of the material of iron in ferrocene and ferric nitrate：7；
(5), take out beaker the reactant liquor in step (4) to be proceeded in the culture dish of 90ml, room temprature evaporation 4d；
(6), culture dish is put in the constant temperature blast drying oven in 80 DEG C and is dried 24h；
(7), dried sample is placed in Muffle furnace, under oxygen atmosphere, 550 DEG C is heated to, heat temperature raising
Speed be 11 DEG C/min, and the roasting 6h at a temperature of 550 DEG C；
(8), grinding obtains sample after spontaneous combustion cooling, and the sample is cube duct magnetic hierarchical porous structure composite,
And be put in the sample standby in drying box.
Compared with prior art, the evaporation-induced self-assembly that the present invention is provided prepares magnetic hierarchical porous structure composite
Method, adds ferric nitrate to be complexed with ethanol in the absolute ethyl alcohol of dissolving P123 or F127 surfactants, and adds normal octane
Used as cosolvent and expanding agent, ferrocene plays certain reaming effect, ferric nitrate iron as the source of iron and expanding agent in hole
Source is uniformly distributed in hierarchical porous structure composite inner, it is thus possible to form different pore passage structures, such as hexagonal hole road structure
With a cube pore passage structure, the magnetic nano-particle such as iron ion of different content is embedded or is embedded in hierarchical porous structure composite
Inner surface or outer surface, make the magnetic hierarchical porous structure composite of catalytic active component high degree of dispersion, thus the method
Made by magnetic hierarchical porous structure composite catalytic performance it is high, dye wastewater degradation can be used for as heterogeneous catalysis.
The present invention is when magnetic hierarchical porous structure composite catalyst is prepared：It is just pungent in organic solvent ethanol solution
Alkane can be dissolved each other with any ratio with ethanol, therefore not play a part of reaming.And ferrocene and ethanol indissoluble, according to " phase
Patibhaga-nimitta is molten " principle, it is easier to it is dissolved in normal octane.Therefore, the addition of ferrocene, can form an Emulsions with normal octane
System, can play a role to reaming.Meanwhile, normal octane has similar volatility, in self assembling process, table to ethanol
Face activating agent can be evenly dispersed in ethanol solution, and normal octane also easily can be dispersed in ethanol solution, and two
Luxuriant iron is not uniformly dispersed in ethanol solution, and ferrocene can be evenly dispersed in normal octane system.In evaporation induction
Self assembly is prepared in magnetic hierarchical porous structure composite material, by evaporation, the aggregation of surfactant hydrophobic group, hydrophilic group
Reunite and collect, ferrocene is dissolved in normal octane system, it is easier to and hydrophobic grouping is combined, and away from hydrophilic radical；By evaporation
Induction self assembly, the magnetic hierarchical porous structure composite aperture of preparation is adjustable, forms the different magnetic multi-stage porous of pore passage structure
Structural composite material, thus ferrocene is also acted on reaming.
Finally illustrate, above example is only unrestricted to illustrate technical scheme, although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, it all should cover at this
In the middle of the right of invention.
Claims (3)
1. the method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite, it is characterised in that methods described includes
Following steps：
(1) P123 the or F127 surfactants for, weighing 2.3～4.6g are dissolved in the absolute ethyl alcohol of 15～30ml, will fill nothing
The beaker of water-ethanol is put on temperature constant magnetic stirring machine, and normal temperature sealing stirs 0.5～1h to after being completely dissolved, and addition 0.148～
5.2g ferric nitrate；
(2) normal octane for, measuring 2.28～4.56ml is added drop-wise in the solution of step (1), normal temperature sealing 2～4h of stirring, and institute
It is 0.028～0.030 that P123 or F127 is stated with the mol ratio of normal octane；
(3), weigh 1.602～3.204g ferrocene to be dissolved in the mixed solution of step (2), normal temperature sealing 2～4h of stirring, and institute
It is 0～70 that ferric nitrate is stated with the ratio of the amount of the material of iron in ferrocene；
(4) tetraethyl orthosilicate of 4.5～9ml, is added in the mixed solution of step (3), 12～24h is stirred in normal temperature sealing, and
Silicon in the tetraethyl orthosilicate is 50 with the ratio of the amount of the material of iron in ferrocene and ferric nitrate：1～5：7；
(5), take out beaker the reactant liquor in step (4) to be proceeded in the culture dish of 90ml, 3～4d of room temprature evaporation；
(6), culture dish is put in the constant temperature blast drying oven in 60～80 DEG C and is dried 3～24h；
(7), dried sample is placed in Muffle furnace, under oxygen atmosphere, 300～550 DEG C is heated to, heat temperature raising
Speed be 11 DEG C/min, and the roasting 6h at a temperature of 300～550 DEG C；
(8), grinding obtains sample after spontaneous combustion cooling, is put in standby in drying box.
2. the method that evaporation-induced self-assembly according to claim 1 prepares magnetic hierarchical porous structure composite, it is special
Levy and be, surfactant is P123 in the step (1), and the magnetic hierarchical porous structure composite of preparation is hexagonal hole road knot
Structure.
3. the method that evaporation-induced self-assembly according to claim 1 prepares magnetic hierarchical porous structure composite, it is special
Levy and be, surfactant is F127 in the step (1), and the magnetic hierarchical porous structure composite of preparation is a cube duct knot
Structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710002560.4A CN106607095B (en) | 2017-01-03 | 2017-01-03 | The method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710002560.4A CN106607095B (en) | 2017-01-03 | 2017-01-03 | The method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106607095A true CN106607095A (en) | 2017-05-03 |
| CN106607095B CN106607095B (en) | 2019-03-01 |
Family
ID=58636978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710002560.4A Expired - Fee Related CN106607095B (en) | 2017-01-03 | 2017-01-03 | The method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106607095B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195164A (en) * | 2020-09-17 | 2022-03-18 | 中国石油天然气股份有限公司 | Composite material with step pore structure distribution and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837988A (en) * | 2010-03-12 | 2010-09-22 | 重庆理工大学 | Method for preparing iron modified SBA-15 mesoporous molecular sieve |
| CN102041584A (en) * | 2010-12-16 | 2011-05-04 | 中南大学 | Magnetic self-assembled mesoporous fiber and preparation method thereof |
| CN103285908A (en) * | 2013-06-21 | 2013-09-11 | 黑龙江大学 | Co-SBA-16 mesoporous molecule sieve synthesis method |
| CN106219604A (en) * | 2016-07-26 | 2016-12-14 | 北京科技大学 | A kind of preparation method preparing hierarchical porous structure titanium dioxide and photocatalytic applications thereof |
-
2017
- 2017-01-03 CN CN201710002560.4A patent/CN106607095B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837988A (en) * | 2010-03-12 | 2010-09-22 | 重庆理工大学 | Method for preparing iron modified SBA-15 mesoporous molecular sieve |
| CN102041584A (en) * | 2010-12-16 | 2011-05-04 | 中南大学 | Magnetic self-assembled mesoporous fiber and preparation method thereof |
| CN103285908A (en) * | 2013-06-21 | 2013-09-11 | 黑龙江大学 | Co-SBA-16 mesoporous molecule sieve synthesis method |
| CN106219604A (en) * | 2016-07-26 | 2016-12-14 | 北京科技大学 | A kind of preparation method preparing hierarchical porous structure titanium dioxide and photocatalytic applications thereof |
Non-Patent Citations (2)
| Title |
|---|
| CHUNGUANG GAO ET AL.: "Bridged-ferrocene functionalized mesoporous SBA-15 material prepared via evaporation-induced self-assembly", 《J POROUS MATER》 * |
| HUANLING XIE ET AL.: "Synthesis for Magnetic Mesoporous Fe3O4-SiO2 Composites and Heterogeneous Fenton Degradation of Methyl Blue", 《INTERNATIONAL JOURNAL OF NANOSCIENCE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195164A (en) * | 2020-09-17 | 2022-03-18 | 中国石油天然气股份有限公司 | Composite material with step pore structure distribution and preparation method thereof |
| CN114195164B (en) * | 2020-09-17 | 2023-09-26 | 中国石油天然气股份有限公司 | Composite material with step hole structure distribution and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106607095B (en) | 2019-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102643513B (en) | Preparation method of meta-aminophenol-formaldehyde resin spheres and preparation method of carbon spheres | |
| CN105344368B (en) | A kind of preparation method and application of transition metal phosphide for hydrogenation-dechlorination reaction | |
| CN105271431B (en) | Method for preparing ferriferrous oxide magnetic material and composite material thereof | |
| CN108128774A (en) | A kind of preparation method of high-purity porous charcoal | |
| CN105566589B (en) | Amino functional ordered mesoporous phenolic resin material and preparation method thereof | |
| CN104692344A (en) | Preparation method of mesoporous graphite-phase carbon nitride material | |
| CN107096564B (en) | A kind of SAPO-34 supporting Pt and the catalyst of WOx and preparation method thereof | |
| CN109482185A (en) | A kind of high dispersive stable type copper-based catalysts and preparation method thereof | |
| CN106824069B (en) | For handling the preparation method of the rear-earth-doped iron Carbon Materials of arsenic-containing waste water | |
| CN107651660A (en) | A kind of preparation method and application of grade macropore mesoporous carbon spheres | |
| CN108285162B (en) | Silicon modified alumina and preparation method and application thereof | |
| CN104479978A (en) | White spirit aging accelerating agent, aging hastening method and aging tank | |
| CN106607095A (en) | Method for preparing magnetic hierarchical pore structure composite material through evaporation-induced self assembly | |
| CN107512712B (en) | A kind of multi-stage porous Carbon Materials and preparation method thereof | |
| CN106236605A (en) | Porous microsphere and preparation method thereof, application | |
| CN111056543A (en) | Preparation method of low-specific-surface high-compaction iron phosphate | |
| CN104891539A (en) | Chambering method for spherical aluminum oxide particles | |
| CN104399514B (en) | Preparation method for boric-acid-modified microporous molecular sieve shape-selective catalyst | |
| CN104148116B (en) | The preparation method of low cost bigger serface cerium oxide | |
| CN104624234A (en) | Mesoporous phenolic resin/copper nano particle heterogeneous catalyst, and preparation method and application of catalyst | |
| CN112569927A (en) | Preparation method of mesoporous silica-coated cobalt manganese oxide, product and application thereof | |
| CN109482184B (en) | Preparation method of catalyst for synthesizing ethylene glycol by dimethyl oxalate hydrogenation | |
| CN107555413A (en) | A kind of preparation method of the regulatable nitrating ordered mesoporous carbon of nitrogen content | |
| CN106006661A (en) | Preparation method of magnetic SBA-15 mesoporous molecular sieve | |
| CN105712366A (en) | Neodymium-doped SBA-15 mesoporous molecular sieve and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190301 Termination date: 20200103 |