CN105214664B - A kind of Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material and its preparation method and application - Google Patents
A kind of Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material and its preparation method and application Download PDFInfo
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- CN105214664B CN105214664B CN201510719181.8A CN201510719181A CN105214664B CN 105214664 B CN105214664 B CN 105214664B CN 201510719181 A CN201510719181 A CN 201510719181A CN 105214664 B CN105214664 B CN 105214664B
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Abstract
The invention discloses a kind of Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material and its preparation method and application, belong to magnetic nano-particle and water process research field.The present invention, using ionothermal synthesis, in ionic eutectic solvent, carries out the Copper-cladding Aluminum Bar Fe that reaction is made described using source of iron, copper source and alkali source as raw material3O4Magnetic composite nano material (Cu Fe3O4).The Cu Fe of preparation3O4It can be used as multiphase-fenton fenton catalyst, excellent degradation capability is shown to the organic matter (such as dyestuff) in waste water, and it is easy to Magnetic Isolation recovery, repeat performance stabilization (to commonly using the room temperature degradation and decolorization rate of industrial dye rhodamine B solution still up to 85%, k after such as reusing 8 times1=0.0132min‑1), it is that a kind of cost is low, operates quick and convenient, positive effect, the novel magnetic environment-friendly materials having a extensive future.
Description
Technical field
The invention belongs to the synthesis of magnetic Nano material and application field of water treatment, and in particular to a kind of Copper-cladding Aluminum Bar Fe3O4Magnetic
Property composite nano materials and its preparation method and application.
Background technology
Chemical oxidization method, the high-level oxidation technology particularly using Fenton reagent as representative, it is to administer difficult for biological degradation
The important method of organic pollution.But there are many problems, such as pH value in conventional homogeneous Fenton reaction systems in actual applications
Application is narrower (~3), H2O2Utilization rate is not high, easily forms iron cement secondary pollution etc..With Fe3O4Magnetic nanoparticle is
The multiphase Fenton systems of representative are expected to make up the deficiency of conventional homogeneous Fenton reactions, particularly reduce iron ion in the aqueous solution
Leaching content, eliminate the secondary pollution to environment, and realize the cycling and reutilization to catalyst.Research shows common Fe3O4Magnetic
Nanoparticulate activated H2O2Ability it is very limited, in order that a certain degree of degraded occurs for organic pollution, often needed in system
Add excessive H2O2(as being generally higher by the 2-4 order of magnitude than pollutant concentration 0.02-3mM), and the reaction time is longer
(3-6h), it is therefore necessary to further improve Fe3O4Magnetic nanoparticle catalytic performance (Chemosphere 2008,73,
1524-1528；Journal of Hazardous Materials 2009,167,560-566；Applied Catalysis
B:Environmental 2009,89,432-440；Journal of Molecular Catalysis A:Chemical
2011,349,71-79；Journal of Molecular Catalysis A:Chemical 2013,371,94-103).
It is expected to improve Fe by doping3O4Catalytic performance.In Fe3O4The metal members such as middle doping Cr, V, Mn, Co, Bi, Ti
Existing document report (the Journal of Hazardous Materials 2006,129,171-178 of the catalytic performance of element；
Applied Catalysis B:Environmental 2008,84,468-473；Applied Catalysis B:
Environmental 2010,97,151-159), but to Copper-cladding Aluminum Bar Fe3O4The catalytic performance report of magnetic composite is seldom.
Only on a small quantity on Copper-cladding Aluminum Bar Fe3O4Magnetic composite is to the report of arsenic-adsorbing, as patent CN104437344A uses solvent heat
Method has synthesized Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material, the pentavalent arsenic in water body and trivalent arsenic are shown excellent absorption and
Regenerative adsorption performance.But using solvent structure Copper-cladding Aluminum Bar Fe3O4Generally being selected during magnetic composite nano material has reproducibility
Ethylene glycol as solvent, make Cu2+It is difficult to adulterate into Fe3O4Lattice, and be easier to be deposited on after being reduced into copper simple substance
Fe3O4Particle surface.
The content of the invention
It is an object of the invention to provide a kind of Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material, its preparation method is simple, cost
It is low, be advantageous to Copper-cladding Aluminum Bar and enter Fe3O4Lattice；The Fe of preparation3O4Magnetic composite nano material room temperature catalytic degradation organic wastewater energy
Power is strong, and reaction rate is fast, dosage is few, and is easy to Magnetic Isolation recovery, repeat performance stabilization, is adapted to popularization and application.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, it comprises the following steps：
1) ionic eutectic solvent is prepared using urea and hydrogen bond receptor；
2) ferrous salt is added in step 1) the ionic eutectic solvent with the alkali source for accounting for total addition level 1/3~2/3,
Stir, obtain mixed liquor；
3) mantoquita and remaining alkali source are added in mixed liquor obtained by step 2), stirs, obtain reaction solution；
4) reaction solution obtained by step 3) is placed in baking oven and heated and reacted, then carry out annealing cooling and magnetic point
It is last scrubbed, dry from collection gained solid particle, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Preferably, the mol ratio of the hydrogen bond receptor and urea is 1:2.
In such scheme, the hydrogen bond receptor is Choline Chloride or glycine betaine.
In such scheme, the ferrous salt is ferrous sulfate or frerrous chloride；The mantoquita is copper sulphate or copper chloride.
In such scheme, the mol ratio of the ferrous salt and hydrogen bond receptor is (0.04~0.3):1；Mantoquita and ferrous salt
Mol ratio is (2.5~10):100.
In such scheme, the alkali source is the one or more in KOH, NaOH, NaOAc.
In such scheme, OH that the total addition level of the alkali source is introduced with it-It is defined, OH-Mol ratio with ferrous salt is
(2.6~3.2):1.
In such scheme, the reaction temperature in the step 4) is 80~200 DEG C, and the reaction time is 2~12h.
In such scheme, preferable reaction temperature is 110~170 DEG C in the step 4), and the reaction time is 4~8h.
Copper-cladding Aluminum Bar Fe is prepared into according to such scheme3O4Magnetic composite nano material.
The Copper-cladding Aluminum Bar Fe prepared according to such scheme3O4Magnetic composite nano material can be applied to catalytic degradation organic wastewater.
According to such scheme, the Copper-cladding Aluminum Bar Fe of preparation3O4Magnetic composite nano material can be used as multiphase-fenton fenton catalyst,
Excellent degradation capability is shown to the organic matter (such as dyestuff) in waste water, and is easy to Magnetic Isolation recovery, reusability
Can be stable, its reuse 8 times after to commonly using the room temperature degradation and decolorization rate of industrial dye rhodamine B solution still up to 85%, k1=
0.0132min-1。
Beneficial effects of the present invention are：
1) present invention prepares Copper-cladding Aluminum Bar Fe using ionothermal synthesis3O4Magnetic composite nano material, the raw material being related to is simple, into
This low, preparation technology and reaction condition are simple, and require low to consersion unit, and operation is easily controllable, is advantageous to produce in batches.
2) present invention prepares Copper-cladding Aluminum Bar Fe3O4(ionic is low common with ionic liquid for the ionothermal synthesis of magnetic composite nano material
Molten solvent) it is solvent, avoid using reproducibility organic solvent.Mantoquita is easier to be reduced into copper in reproducibility organic solvent
Fe is deposited on after simple substance3O4Particle surface, and be advantageous to Cu by solvent of ionic liquid2+Doping enters Fe3O4Lattice.
3) Copper-cladding Aluminum Bar Fe provided by the invention3O4Magnetic composite nano material is particularly suitable for use in normal in catalytic degradation waste water
See industrial dye.Room temperature catalytic degradation ability is strong, and reaction rate is fast, and catalyst amount is few, stability is good, is easy to carry out magnetic
Separation and recovery, recycled for multiple times can be achieved.
Brief description of the drawings
Fig. 1 is the XRD of the products therefrom of the embodiment of the present invention 1.
Fig. 2 is that the Cu2p XPS of the products therefrom of the embodiment of the present invention 1 scheme.
Fig. 3 is that the TEM of the products therefrom of the embodiment of the present invention 1 schemes.
Fig. 4 is the magnetization curve figure of the products therefrom of the embodiment of the present invention 1.
Fig. 5 is the gained Copper-cladding Aluminum Bar Fe of the embodiment of the present invention 13O4The circulation of magnetic composite nano material catalytic degradation rhodamine B
Test chart.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
Unless specific instructions, the reagent used is commercially available chemical reagent or industrial products to following examples.
Embodiment 1
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
By 20mmol Choline Chlorides and 40mmol urea, to be configured to ionic eutectic molten for heating stirring at a temperature of 50 DEG C
Agent；3mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 5.2mmol KOH, stir, and must mix
Liquid, 3.75mmol KOH and 0.15mmol CuCl are continuously added into gained mixed liquor2·2H2O, continue to stir, obtain instead
Answer liquid；Gained reaction solution is placed in 110 DEG C of baking ovens after reacting 4h, carries out annealing cooling and Magnetic Isolation collects gained solid
Grain, it is last scrubbed, dry, produce final product.
The X-ray diffraction analysis result of the present embodiment products therefrom is shown in Fig. 1, characteristic peak and Fe in Fig. 13O4Standard drawing
Spectrum is consistent (JCPDS No.65-3107), shows that product particles have inverse spinel phase structure；The present embodiment products therefrom
Cu2pXPS, which is composed, sees Fig. 2, and two macroseisms swash peak and marked respectively with S in figure, show copper in the product with Cu2+Form is present；By this reality
Apply a products therefrom and carry out TEM observations (see Fig. 3), the results showed that products therefrom is based on spheric granules, average grain diameter about 10nm.
The above results show that products therefrom is described Copper-cladding Aluminum Bar Fe3O4Magnetic 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, remanent magnetism 5.6emu/g, coercivity 51.8Oe.
Application examples
By Copper-cladding Aluminum Bar Fe manufactured in the present embodiment3O4Magnetic composite nano materials application in rhodamine B degradation (RhB), including
Following steps：
By Copper-cladding Aluminum Bar Fe obtained by 0.025g the present embodiment3O4Magnetic composite nano material and 50mL RhB (~10-5M) solution
Mixing, pre- addition 0.23g H after adsorbing 15min2O2(30%) degraded that RhB occurs under conditions of being, 6.4 at 25 DEG C and pH takes off
Colour response.
After degradation and decolorization reaction 2h, Copper-cladding Aluminum Bar Fe obtained by the present embodiment3O4Magnetic composite nano material takes off to RhB solution
Color rate reaches 0.0247min up to 95%, at room temperature reaction rate-1。
After the completion of RhB solution degradation decoloring reactions, the water sample after processing is drained from flask under the effect of additional magnet,
The Copper-cladding Aluminum Bar Fe obtained again to recovery3O4Magnetic composite nano material adds 50mL RhB (~10-5M) solution, according to above-mentioned drop
Solve step and carry out degradation experiment next time.So circulation (circulation Degrading experiment), gained circulation degradation results are shown in Fig. 5.
In Fig. 5, still kept using catalyst for the 8th time high catalytic activity (RhB solution 2h percent of decolourizations are still up to 85% at room temperature,
Reaction rate is 0.0132min-1)。
Embodiment 2
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
20mmol Choline Chlorides and 40mmol urea are carried out at a temperature of 50 DEG C heating stirring be configured to ionic is low
Congruent melting solvent；6mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 10.4mmol KOH, stir,
Mixed liquor is obtained, 7.5mmol KOH and 0.15mmol CuCl are continuously added into gained mixed liquor2·2H2O, continue to stir,
Obtain reaction solution；Gained reaction solution is placed in 110 DEG C of baking ovens after reacting 4h, carries out annealing cooling and Magnetic Isolation collection gained is solid
Body particle, it is last scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Embodiment 3
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
20mmol Choline Chlorides and 40mmol urea are carried out at a temperature of 50 DEG C heating stirring be configured to ionic is low
Congruent melting solvent；0.8mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 1mmol KOH, stir,
Mixed liquor is obtained, 1.4mmol KOH and 0.08mmol CuCl are continuously added into gained mixed liquor2·2H2O, continue to stir,
Obtain reaction solution；Gained reaction solution is placed in 110 DEG C of baking ovens after reacting 6h, carries out annealing cooling and Magnetic Isolation collection gained is solid
Body particle, it is last scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Embodiment 4
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
20mmol Choline Chlorides and 40mmol urea are carried out at a temperature of 50 DEG C heating stirring be configured to ionic is low
Congruent melting solvent；3mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 5.2mmol KOH, stir,
Mixed liquor is obtained, 3.75mmol KOH and 0.15mmol CuCl are continuously added into gained mixed liquor2·2H2O, it is equal to continue stirring
It is even, obtain reaction solution；Gained reaction solution is placed in 198 DEG C of baking ovens after reacting 4h, carries out annealing cooling and Magnetic Isolation collects institute
Solid particle is obtained, it is last scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Embodiment 5
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
20mmol Choline Chlorides and 40mmol urea are carried out at a temperature of 50 DEG C heating stirring be configured to ionic is low
Congruent melting solvent；3mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 5.2mmol KOH, stir,
Mixed liquor is obtained, 3.75mmol KOH and 0.075mmol CuCl are continuously added into gained mixed liquor2·2H2O, it is equal to continue stirring
It is even, obtain reaction solution；Gained reaction solution is placed in 80 DEG C of baking ovens after reacting 8h, carries out annealing cooling and Magnetic Isolation collects gained
Solid particle, it is last scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Embodiment 6
A kind of Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, comprises the following steps：
20mmol Choline Chlorides and 40mmol urea are carried out at a temperature of 50 DEG C heating stirring be configured to ionic is low
Congruent melting solvent；3mmol FeSO are added into gained ionic eutectic solvent4·7H2O and 5.2mmol KOH, stir,
Mixed liquor is obtained, 3.75mmol KOH and 0.3mmol CuCl are continuously added into gained mixed liquor2·2H2O, continue to stir,
Obtain reaction solution；Gained reaction solution is placed in 110 DEG C of baking ovens after reacting 4h, carries out annealing cooling and Magnetic Isolation collection gained is solid
Body particle, it is last scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material.
Above example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that for this skill
For the those of ordinary skill in art field, under the premise without departing from the principles of the invention, some change can also be carried out to the present invention
Enter and modify, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
Claims (8)
- A kind of 1. Copper-cladding Aluminum Bar Fe3O4The preparation method of magnetic composite nano material, it is characterised in that comprise the following steps：1) ionic eutectic solvent is prepared using urea and hydrogen bond receptor；2) ferrous salt is added in ionic eutectic solvent obtained by step 1) with the alkali source for accounting for total addition level 1/3~2/3, stirring Uniformly, mixed liquor is obtained；3) mantoquita and remaining alkali source are added in mixed liquor obtained by step 2), stirs, obtain reaction solution；4) reaction solution heating obtained by step 3) is carried out reacting after annealing cooling, Magnetic Isolation collects gained solid particle, finally It is scrubbed, dry, produce described Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material；Reaction temperature in the step 4) is 110~170 DEG C, and the reaction time is 4~8h.
- 2. preparation method according to claim 1, it is characterised in that the mol ratio of the hydrogen bond receptor and urea is 1:2.
- 3. preparation method according to claim 1, it is characterised in that the hydrogen bond receptor is Choline Chloride or glycine betaine.
- 4. preparation method according to claim 1, it is characterised in that the ferrous salt is ferrous sulfate or frerrous chloride； Mantoquita is copper sulphate or copper chloride；Alkali source is the one or more in KOH, NaOH, NaOAc.
- 5. preparation method according to claim 1, it is characterised in that the mol ratio of the ferrous salt and hydrogen bond receptor is (0.04~0.3):1；The mol ratio of the mantoquita and ferrous salt is (2.5~10):100.
- 6. preparation method according to claim 4, it is characterised in that the OH that the total addition level of the alkali source is introduced with it-For Standard, OH-Mol ratio with ferrous salt is (2.6~3.2):1.
- 7. Copper-cladding Aluminum Bar Fe made from any one of claim 1~6 preparation method3O4Magnetic composite nano material.
- 8. Copper-cladding Aluminum Bar Fe described in claim 73O4Application of the magnetic composite nano material in catalytic degradation organic wastewater.
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| CN109704417A (en) * | 2019-02-19 | 2019-05-03 | 中国科学院兰州化学物理研究所 | It is a kind of alkalinity eutectic solvent preparation and synthesis transition metal oxide nano-material in application |
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| 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 |
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| CN102921422B (en) * | 2012-11-06 | 2015-01-21 | 常州大学 | Preparation of magnetic nano Cu-Fe3O4/grapheme composite catalyst and application of composite catalyst in reduction of nitro-compounds |
| CN104437344B (en) * | 2014-10-13 | 2016-08-24 | 中南大学 | A kind of Copper-cladding Aluminum Bar composite magnetic nano material and preparation thereof and application |
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