CN105214664A - A kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and its preparation method and application - Google Patents

A kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and its preparation method and application Download PDF

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CN105214664A
CN105214664A CN201510719181.8A CN201510719181A CN105214664A CN 105214664 A CN105214664 A CN 105214664A CN 201510719181 A CN201510719181 A CN 201510719181A CN 105214664 A CN105214664 A CN 105214664A
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copper
composite nano
aluminum bar
cladding aluminum
magnetic composite
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CN105214664B (en
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陈逢喜
谢圣龙
邱心泓
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Wuhan Institute of Technology
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Abstract

The invention discloses a kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and its preparation method and application, belongs to magnetic nano-particle and water treatment research field.The present invention for raw material, adopts the hot method of ion with source of iron, copper source and alkali source, in ionic eutectic solvent, carries out reacting obtained described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material (Cu-Fe 3o 4).The Cu-Fe of preparation 3o 4can be used as multiphase-fenton fenton catalyst, excellent degradation capability is shown to the organic matter (as dyestuff etc.) in waste water, and be easy to that Magnetic Isolation reclaims, repeat performance stablizes and (as still reaches 85%, k to the room temperature degradation and decolorization rate of conventional industrial dye rhodamine B solution after reusing 8 times 1=0.0132min -1), for a kind of cost is low, it is quick and convenient to operate, successful, the novel magnetic environment-friendly materials that have a extensive future.

Description

A kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and its preparation method and application
Technical field
The invention belongs to synthesis and the application field of water treatment of magnetic Nano material, be specifically related to a kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and its preparation method and application.
Background technology
Chemical oxidization method is particularly the high-level oxidation technology of representative with Fenton reagent, is the important method of the organic pollution administering difficult for biological degradation.But there is a lot of problem in actual applications in conventional homogeneous Fenton reaction system, as narrower in pH value range of application (~ 3), H 2o 2utilization rate is not high, easily forms iron mud secondary pollution etc.With Fe 3o 4magnetic nanoparticle is the deficiency that the heterogeneous Fenton system of representative is expected to make up conventional homogeneous Fenton reaction, particularly reduces the leaching content of iron ion in the aqueous solution, eliminates the secondary pollution to environment, and realizes the cycling and reutilization to catalyst.Research shows common Fe 3o 4magnetic nanoparticle activation H 2o 2ability very limited, in order to make organic pollution that degraded to a certain degree occur, often need in system to add excessive H 2o 2(as usually exceeded 2-4 the order of magnitude than pollutant levels 0.02-3mM), and reaction time longer (3-6h), be therefore necessary to improve Fe further 3o 4catalytic performance (Chemosphere2008,73, the 1524-1528 of magnetic nanoparticle; JournalofHazardousMaterials2009,167,560-566; AppliedCatalysisB:Environmental2009,89,432-440; JournalofMolecularCatalysisA:Chemical2011,349,71-79; JournalofMolecularCatalysisA:Chemical2013,371,94-103).
Be expected to improve Fe by doping 3o 4catalytic performance.At Fe 3o 4the catalytic performance of the metallic elements such as middle doping Cr, V, Mn, Co, Bi, Ti has bibliographical information (JournalofHazardousMaterials2006,129,171-178; AppliedCatalysisB:Environmental2008,84,468-473; AppliedCatalysisB:Environmental2010,97,151-159), but to Copper-cladding Aluminum Bar Fe 3o 4the catalytic performance report of magnetic composite seldom.Only have a small amount of about Copper-cladding Aluminum Bar Fe 3o 4magnetic composite to the report of arsenic-adsorbing, as patent CN104437344A adopts solvent structure Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material, shows excellent absorption and regenerative adsorption performance to the pentavalent arsenic in water body and trivalent arsenic.But adopt solvent structure Copper-cladding Aluminum Bar Fe 3o 4usually select the ethylene glycol with reproducibility as solvent during magnetic composite nano material, make Cu 2+very difficult doping enters Fe 3o 4lattice, and be deposited on Fe after being more easily reduced into copper simple substance 3o 4particle surface.
Summary of the invention
The object of this invention is to provide a kind of Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material, its preparation method is simple, cost is low, is conducive to Copper-cladding Aluminum Bar and enters Fe 3o 4lattice; The Fe of preparation 3o 4magnetic composite nano material room temperature catalytic degradation organic wastewater ability is strong, and reaction rate is fast, consumption is few, and is easy to that Magnetic Isolation reclaims, repeat performance is stablized, and is applicable to applying.
For achieving the above object, the technical solution used in the present invention is:
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, it comprises the following steps:
1) urea and hydrogen bond receptor preparation ionic eutectic solvent is adopted;
2) ferrous salt and the alkali source that accounts for total addition level 1/3 ~ 2/3 are added step 1) in described ionic eutectic solvent, stir, obtain mixed liquor;
3) mantoquita and residue alkali source are added step 2) in gained mixed liquor, stir, obtain reactant liquor;
4) by step 3) gained reactant liquor is placed in baking oven and heating is reacted, and then carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, drying, obtains described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Preferably, the mol ratio of described hydrogen bond receptor and urea is 1:2.
In such scheme, described hydrogen bond receptor is Choline Chloride or betaine.
In such scheme, described ferrous salt is ferrous sulfate or frerrous chloride; Described mantoquita is copper sulphate or copper chloride.
In such scheme, the mol ratio of described ferrous salt and hydrogen bond receptor is (0.04 ~ 0.3): 1; The mol ratio of mantoquita and ferrous salt is (2.5 ~ 10): 100.
In such scheme, described alkali source is one or more in KOH, NaOH, NaOAc.
In such scheme, the OH that the total addition level of described alkali source is introduced with it -be as the criterion, OH -be (2.6 ~ 3.2) with the mol ratio of ferrous salt: 1.
In such scheme, described step 4) in reaction temperature be 80 ~ 200 DEG C, the reaction time is 2 ~ 12h.
In such scheme, described step 4) in preferred reaction temperature be 110 ~ 170 DEG C, the reaction time is 4 ~ 8h.
Copper-cladding Aluminum Bar Fe is prepared into according to such scheme 3o 4magnetic composite nano material.
According to Copper-cladding Aluminum Bar Fe prepared by such scheme 3o 4magnetic composite nano material can be applicable to catalytic degradation organic wastewater.
According to such scheme, the Copper-cladding Aluminum Bar Fe of preparation 3o 4magnetic composite nano material can be used as multiphase-fenton fenton catalyst, excellent degradation capability is shown to the organic matter (as dyestuff etc.) in waste water, and be easy to Magnetic Isolation reclaim, repeat performance stablize, after it reuses 8 times, still 85%, k is reached to the room temperature degradation and decolorization rate of conventional industrial dye rhodamine B solution 1=0.0132min -1.
Beneficial effect of the present invention is:
1) the present invention adopts the hot legal system of ion for Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material, the raw material related to is simple, cost is low, preparation technology and reaction condition simple, and requires low to consersion unit, and operation is easy to control, and is conducive to batch production.
2) the present invention prepares Copper-cladding Aluminum Bar Fe 3o 4the hot method of ion of magnetic composite nano material for solvent with ionic liquid (ionic eutectic solvent), avoids and uses reproducibility organic solvent.Mantoquita is deposited on Fe be more easily reduced into copper simple substance in reproducibility organic solvent after 3o 4particle surface, and be that solvent is conducive to Cu with ionic liquid 2+doping enters Fe 3o 4lattice.
3) Copper-cladding Aluminum Bar Fe provided by the invention 3o 4magnetic composite nano material is particularly useful for the common industrial dyestuff in catalytic degradation waste water.Room temperature catalytic degradation ability is strong, and reaction rate is fast, and catalyst amount is few, good stability, be easy to carry out Magnetic Isolation recovery, can realize recycled for multiple times.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 products therefrom.
Fig. 2 is the Cu2pXPS figure of the embodiment of the present invention 1 products therefrom.
Fig. 3 is the TEM figure of the embodiment of the present invention 1 products therefrom.
Fig. 4 is the magnetization curve figure of the embodiment of the present invention 1 products therefrom.
Fig. 5 is the embodiment of the present invention 1 gained Copper-cladding Aluminum Bar Fe 3o 4the loop test figure of magnetic composite nano material catalyzes rhodamine B degradation.
Detailed description of the invention
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but the present invention is not only confined to the following examples.
As no specific instructions, the reagent of employing is commercially available chemical reagent or industrial products to following examples.
Embodiment 1
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are added thermal agitation at 50 DEG C of temperature and is mixed with ionic eutectic solvent; 3mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 5.2mmolKOH, stirs, and obtains mixed liquor, continues to add 3.75mmolKOH and 0.15mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 110 DEG C of baking ovens react 4h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain end product.
The X-ray diffraction analysis of the present embodiment products therefrom the results are shown in Figure characteristic peak in 1, Fig. 1 and Fe 3o 4standard diagram consistent (JCPDSNo.65-3107), show that product particles has inverse spinel phase structure; The Cu2pXPS spectrum of the present embodiment products therefrom is shown in Fig. 2, and in figure, two macroseisms swash peak respectively with S mark, show copper in the product with Cu 2+form exists; The present embodiment products therefrom is carried out TEM observation (see Fig. 3), result shows that products therefrom is based on spheric granules, and average grain diameter is about 10nm.
The above results shows that products therefrom is described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
The magnetization curve of the present embodiment products therefrom is shown in Fig. 4.Fig. 4 shows that the saturation magnetization of products therefrom is 48.0emu/g, and remanent magnetism is 5.6emu/g, and coercivity is 51.8Oe.
Application examples
Copper-cladding Aluminum Bar Fe prepared by the present embodiment 3o 4magnetic composite nano materials application, in rhodamine B degradation (RhB), comprises the following steps:
By 0.025g the present embodiment gained Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material and 50mLRhB (~ 10 -5m) solution mixing, adds 0.23gH after pre-absorption 15min 2o 2(30%) under 25 DEG C and pH are the condition of 6.4, there is the degradation and decolorization reaction of RhB.
After degradation and decolorization reaction 2h, the present embodiment gained Copper-cladding Aluminum Bar Fe 3o 4the percent of decolourization of magnetic composite nano material to RhB solution reaches 95%, and under room temperature, reaction rate reaches 0.0247min -1.
After RhB solution degradation decoloring reaction completes, under additional magnet effect, the water sample after process is drained from flask, then to the Copper-cladding Aluminum Bar Fe that recovery obtains 3o 4magnetic composite nano material adds 50mLRhB (~ 10 -5m) solution, carries out degradation experiment next time according to above-mentioned degradation step.Circulation like this (circulation Degrading experiment), gained circulation degradation results is shown in Fig. 5.
In Fig. 5, (under room temperature, RhB solution 2h percent of decolourization still reaches 85%, and reaction rate is 0.0132min to use catalyst still to keep high catalytic activity the 8th time -1).
Embodiment 2
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are carried out adding thermal agitation at 50 DEG C of temperature and is mixed with to obtain ionic eutectic solvent; 6mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 10.4mmolKOH, stirs, and obtains mixed liquor, continues to add 7.5mmolKOH and 0.15mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 110 DEG C of baking ovens react 4h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Embodiment 3
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are carried out adding thermal agitation at 50 DEG C of temperature and is mixed with to obtain ionic eutectic solvent; 0.8mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 1mmolKOH, stirs, and obtains mixed liquor, continues to add 1.4mmolKOH and 0.08mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 110 DEG C of baking ovens react 6h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Embodiment 4
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are carried out adding thermal agitation at 50 DEG C of temperature and is mixed with to obtain ionic eutectic solvent; 3mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 5.2mmolKOH, stirs, and obtains mixed liquor, continues to add 3.75mmolKOH and 0.15mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 198 DEG C of baking ovens react 4h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Embodiment 5
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are carried out adding thermal agitation at 50 DEG C of temperature and is mixed with to obtain ionic eutectic solvent; 3mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 5.2mmolKOH, stirs, and obtains mixed liquor, continues to add 3.75mmolKOH and 0.075mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 80 DEG C of baking ovens react 8h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Embodiment 6
A kind of Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, comprises the following steps:
20mmol Choline Chloride and 40mmol urea are carried out adding thermal agitation at 50 DEG C of temperature and is mixed with to obtain ionic eutectic solvent; 3mmolFeSO is added in gained ionic eutectic solvent 47H 2o and 5.2mmolKOH, stirs, and obtains mixed liquor, continues to add 3.75mmolKOH and 0.3mmolCuCl in gained mixed liquor 22H 2o, continues to stir, obtains reactant liquor; Gained reactant liquor is placed in after 110 DEG C of baking ovens react 4h, carries out annealing cooling and Magnetic Isolation collects gained solid particle, finally by washing, dry, obtain described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
Above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.

Claims (10)

1. a Copper-cladding Aluminum Bar Fe 3o 4the preparation method of magnetic composite nano material, is characterized in that, comprises the following steps:
1) urea and hydrogen bond receptor preparation ionic eutectic solvent is adopted;
2) ferrous salt and the alkali source that accounts for total addition level 1/3 ~ 2/3 are added step 1) in gained ionic eutectic solvent, stir, obtain mixed liquor;
3) mantoquita and residue alkali source are added step 2) in gained mixed liquor, stir, obtain reactant liquor;
4) by step 3) heating of gained reactant liquor carries out the cooling of reaction after annealing, and Magnetic Isolation collects gained solid particle, finally by washing, drying, obtains described Copper-cladding Aluminum Bar Fe 3o 4magnetic composite nano material.
2. preparation method according to claim 1, is characterized in that, the mol ratio of described hydrogen bond receptor and urea is 1:2.
3. preparation method according to claim 1, is characterized in that, described hydrogen bond receptor is Choline Chloride or betaine.
4. preparation method according to claim 1, is characterized in that, described ferrous salt is ferrous sulfate or frerrous chloride; Mantoquita is copper sulphate or copper chloride; Alkali source is one or more in KOH, NaOH, NaOAc.
5. preparation method according to claim 1, is characterized in that, the mol ratio of described ferrous salt and hydrogen bond receptor is (0.04 ~ 0.3): 1; The mol ratio of described mantoquita and ferrous salt is (2.5 ~ 10): 100.
6. preparation method according to claim 4, is characterized in that, the OH that the total addition level of described alkali source is introduced with it -be as the criterion, OH -be (2.6 ~ 3.2) with the mol ratio of ferrous salt: 1.
7. preparation method according to claim 1, is characterized in that, described step 4) in reaction temperature be 80 ~ 200 DEG C, the reaction time is 2 ~ 12h.
8. preparation method according to claim 1, is characterized in that, described step 4) in reaction temperature be 110 ~ 170 DEG C, the reaction time is 4 ~ 8h.
9. the Copper-cladding Aluminum Bar Fe that obtains of preparation method described in any one of claim 1 ~ 8 3o 4magnetic composite nano material.
10. Copper-cladding Aluminum Bar Fe described in claim 9 3o 4the application of magnetic composite nano material in catalytic degradation organic wastewater.
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CN105921152A (en) * 2016-05-06 2016-09-07 武汉工程大学 Aluminum modified Fe3O4 magnetic material and preparing method and application thereof
CN108176401A (en) * 2018-01-10 2018-06-19 扬州工业职业技术学院 A kind of preparation method of the nano ferriferrous oxide Fenton catalyst of selenium doping
CN108404942A (en) * 2018-02-02 2018-08-17 武汉工程大学 A kind of fluorine richness Fe3O4Magnetic Nano material and its preparation method and application

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CN104437344A (en) * 2014-10-13 2015-03-25 中南大学 Copper doped composite magnetic nano-material and preparation and application thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105665028A (en) * 2016-03-08 2016-06-15 哈尔滨工业大学 Nano heterogeneous Fenton catalyst with alginate core coated with copper/magnetic Fe3O4 and preparation method of Nano heterogeneous Fenton catalyst
CN105665028B (en) * 2016-03-08 2018-07-13 哈尔滨工业大学 A kind of alginic acid salt core outer cladding copper/magnetic Fe3O4The heterogeneous class fenton catalyst of nanometer and preparation method thereof
CN105921152A (en) * 2016-05-06 2016-09-07 武汉工程大学 Aluminum modified Fe3O4 magnetic material and preparing method and application thereof
CN105921152B (en) * 2016-05-06 2018-05-01 武汉工程大学 A kind of aluminium MODIFIED Fe3O4Magnetic material and its preparation method and application
CN108176401A (en) * 2018-01-10 2018-06-19 扬州工业职业技术学院 A kind of preparation method of the nano ferriferrous oxide Fenton catalyst of selenium doping
CN108404942A (en) * 2018-02-02 2018-08-17 武汉工程大学 A kind of fluorine richness Fe3O4Magnetic Nano material and its preparation method and application

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