CN103990463A - Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material - Google Patents

Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material Download PDF

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CN103990463A
CN103990463A CN201410217944.4A CN201410217944A CN103990463A CN 103990463 A CN103990463 A CN 103990463A CN 201410217944 A CN201410217944 A CN 201410217944A CN 103990463 A CN103990463 A CN 103990463A
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张彦中
袁卉华
李碧云
易兵成
娄向新
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Donghua University
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Abstract

The invention relates to a preparation method of a NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material. The preparation method comprises the following steps: (1) preparing an aluminum salt/nickel salt mixed solution; (2) preparing an aluminum salt/nickel salt/spinnable high polymer mixed spinning solution; (3) carrying out electrostatic spinning on the spinning solution, so as to obtain precursor composite nanofibers; and (4) calcining products obtained in the step (3), so as to obtain the NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material. The preparation method has the beneficial effects that the prepared composite ceramic nanofiber has high photocatalytic activity, the diameter distribution of the fiber is uniform, the length-diameter ratio is high, the process is simple, and the method is suitable for large-scale preparation; besides, the method has the advantages of easiness in separation, recovery and recycling and wide market prospect, and more chances are provided for the selection of the photocatalytic materials for the air and water pollution treatment.

Description

A kind of NiO/ γ-Al 2o 3the preparation method of composite ceramics nanofiber catalysis material
Technical field
The invention belongs to composite nano fiber field, particularly a kind of NiO/ γ-Al 2o 3the preparation method of composite ceramics nanofiber catalysis material.
Background technology
Along with the fast development of China's economy and improving constantly of industrialization rate, problem of environmental pollution is day by day serious.Compare with traditional organic contamination substance treating method, photocatalysis technology is a kind of brand-new energy-conserving and environment-protective green oxidation technology, the advantages such as, environmental friendliness low with its processing cost, sustainable recovery use, are attracting wide attention aspect environmental improvement and new energy field.Conductor photocatalysis material is exactly a kind of new functional material that development in recent years is got up, can by most of organic chlorides, multiple pesticide, surfactant and to cause color base group exhaustive oxidation be CO 2thereby with non-toxic products complete oxidation degradable organic pollutants such as water.In numerous conductor photocatalysis materials, so far, ceramic-like nano-powder (as NiO, TiO 2) because it has, specific area is large, catalytic activity advantages of higher, be widely used, but have the problems such as difficult, specific area utilization rate is low that reclaim.
Electrostatic spinning technique is a kind ofly to utilize high voltage to prepare fibre fineness to reach nano level superfine fibre technology of preparing.The nano-fiber material of being prepared by electrostatic spinning technique generally has the features such as high-specific surface area (than high 1～2 order of magnitude of traditional fibre), loose structure, low-density, small-bore, very applicable photocatalytic applications.Static Spinning ceramic nanofibers is compared with traditional nano particle catalysis material as catalysis material, has following advantage: the specific area of (1) material is large, the more organic pollution of can degrading equally under the catalysis material of equivalent; (2) the material degree of crystallinity obtaining is high, and without agglomeration, granularity is large and even, has improved its photocatalytic activity; (3) while being directly used in wastewater treatment with fibers form, than traditional nano-powder or particle, be easier to separated recovery, reduced operating cost.Therefore, the nano-powder of tool photocatalytic activity is prepared into nanofiber and will be the effective way addressing the above problem.In the past few years, increasing research is found electrostatic spinning technique to be prepared to the composite material nanometer fiber of organic-inorganic hybrid in conjunction with sol-gel chemistry method, then obtains functionality ceramic nanofiber for photocatalysis by the method removal organic component of heat treatment or roasting.
NiO is a kind of conventional catalysis material, Ni 2+there is 3d track, polyelectron oxygen is had to the preferentially tendency of absorption, reducing gas is had to activation, in the processes such as dimerization of water decomposition hydrogen manufacturing, organic matter degradation, gasoline hydrocracking, methane oxidation reformation, ethene, all show good catalytic activity.In light-catalyzed reaction process, still there is the defects such as quantum efficiency is low, sunshine utilizes rate variance, photo-generated carrier recombination probability is high, be difficult for reclaiming, recycling rate of waterused is low in NiO, has limited its process of industrialization.At present, adopting electrostatic spinning to prepare NiO nanofiber is one of important method improving NiO photocatalysis performance, and adopts on this basis semiconductor carrier compound (as: ZnO, TiO 2deng) and the method such as non-metal carrier (as: PVA) doping change its level structure, be the effective ways that further improve its photocatalysis efficiency.Al 2o 3being a kind of conventional catalyst carrier, is phase time in its crystalline state, shows as mesoporous type, has higher specific area.If be prepared into mesoporous type NiO/ γ-Al by itself and NiO are compound 2o 3nanofiber can improve the photocatalytic activity of NiO greatly.Adopt at present electrostatic spinning technique can prepare NiO[Guan H.Y., et al.Preparation and characterization of NiO nanofibres via an electrospinning technique.Inorg.Chem.Commun.2003, 6:1302-1303], γ-Al2O3[Wang Y., et al.Electrospinning preparation and adsorption properties of mesoporous alumina fibers.J.Mater.Chem.A2013, 1:10720-10726] and both nanofiber [Shao C.L.s compound with other inorganic material respectively, Electrospun nanofibers ofNiO/ZnO composite.Inorg.Chem.Commun.2004, 7:625-627, Lotus A.F., et al.Characterization of TiO2-Al2O3composite fibers formed by electrospinning a sol-gel and polymer mixture.Mater.Sci.Eng.B2010,167:55-59], but the research work that up to now the two is prepared into composite nano fiber have not been reported, more there is no the research report of photocatalytic applications.
Summary of the invention
The object of the invention is to develop a kind of by conjunction with sol-gel chemistry method and electrostatic spinning technique for the preparation of light-catalysed NiO/ γ-Al 2o 3the preparation method of composite nano inoganic fiber catalysis material, the method technique is simple, is convenient to preparation and is easy to reclaim.
The invention provides a kind of preparation method for light-catalysed high-activity nano fiber catalyst, step is as follows:
(1) preparation aluminum salt solution, joins nickel salt in aluminum salt solution, fully stirs to obtain aluminium salt/nickel salt mixed solution;
(2) preparation can be spun the solution of high polymer, and gained solution is joined in above-mentioned aluminium salt/nickel salt mixed solution, obtains aluminium salt/nickel salt/can spin high polymer blend spinning liquid;
(3) above-mentioned spinning solution is carried out to electrostatic spinning, obtain presoma composite nano fiber;
(4) step (3) products obtained therefrom is calcined in air atmosphere, in air atmosphere, naturally cooled to room temperature, obtain NiO/ γ-Al 2o 3composite ceramics nanofiber catalysis material.
The described aluminium salt of above-mentioned steps (1) is aluminium chloride, aluminum sulfate, aluminum nitrate, alumina silicate or aluminium sulfide.
The described nickel salt of above-mentioned steps (1) is nickel acetate, nickelous sulfate, nickel nitrate, nickel chloride, nickelous carbonate or amino acid nickel.
The described aluminum salt solution solvent used of above-mentioned steps (1) is methyl alcohol, ethanol or propyl alcohol.
The aluminum salt solution that above-mentioned steps (1) is described, the weight ratio of aluminium salt and solvent is 1: 1-40.
Preferably, the weight ratio of aluminium salt and solvent is 1: 20.
Aluminium salt/nickel salt mixed solution that above-mentioned steps (1) is described, the weight ratio of aluminium salt and nickel salt is 1: 1-9.
Preferably, the weight ratio of aluminium salt and nickel salt is 1: 4.
The solution solvent used of the spun high polymer that above-mentioned steps (2) is described is methyl alcohol, ethanol or propyl alcohol.
The solution of the spun high polymer that above-mentioned steps (2) is described, can spin high polymer is poly, PPTA, cellulose acetate, polyaniline, PEO, polyethylene glycol oxide, polystyrene, polyacrylonitrile, polycaprolactone, polyvinylpyrrolidone, polymethyl methacrylate, polyethylene glycol oxalate, Merlon, nylon 6, polyvinyl alcohol, PLA, poly butyric ester, poly-valeric acid butyrate, poly-3-hydroxybutyrate or 3-hydroxycaproic acid copolymer.
The solution of the spun high polymer that above-mentioned steps (2) is described, the weight ratio that can spin high polymer and solvent is 1: 1-18.
Preferably, the weight ratio that can spin high polymer and solvent is 1: 9.
The weight ratio that above-mentioned steps (2) can be spun the solution of high polymer and aluminium salt/nickel salt mixed solution of step (1) gained is 1-4: 1.
Preferably, can to spin the weight ratio of the solution of high polymer and aluminium salt/nickel salt mixed solution of step (1) gained be 2: 1 to step (2).
The electrostatic spinning that above-mentioned steps (3) is described, its process conditions are voltage 5-50kv.
The electrostatic spinning that above-mentioned steps (3) is described, its process conditions are that the distance in the device for spinning using between receiving system and spinning head is 10-30cm.
The electrostatic spinning that above-mentioned steps (3) is described, its process conditions are that the spinning solution flow velocity of step (2) gained is 0.1-3ml/h.
The electrostatic spinning that above-mentioned steps (3) is described, its process conditions are, environment temperature 10-50 ℃.
The electrostatic spinning that above-mentioned steps (3) is described, its process conditions are that ambient humidity is 20%-80%.
The calcining that above-mentioned steps (4) is described, its process conditions are, from room temperature, are warmed up to 800-1000 ℃.
The calcining that above-mentioned steps (4) is described, its process conditions are, heating rate 0.8-1.2 ℃/min.
The calcining that above-mentioned steps (4) is described, calcination time is 12-24h.
The present invention proposes to be mixed with the precursor solution of proper viscosity and electrostatic spinning and roasting technique with sol-gel and develops a kind of for the preparation of high activity NiO/ γ-Al 2o 3the preparation method of composite nano fiber catalysis material.
beneficial effect
1) the present invention adopts traditional electrostatic spinning technique indirectly to prepare inorganic nano-fiber, and distribution of fiber diameters is even, and draw ratio is high, and technique simple possible is applicable to a large amount of preparations;
2) the present invention can obtain the NiO/ γ-Al of mesoporous type 2o 3, there is higher specific area and photocatalytic activity;
3) the prepared material of the present invention is as catalysis material, and its cost is low, catalytic efficiency is suitable with conventional titania nanoparticles, but it can conveniently recycle, for photocatalysis field provides a brand-new selection.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of precursor nano-composite fiber;
Fig. 2 is 800 ℃ of spinning scanning electron microscope (SEM) photographs after calcining;
Fig. 3 is 1000 ℃ of spinning scanning electron microscope (SEM) photographs after calcining;
Fig. 4 is the XRD spectra of 800,1000 ℃ of calcining afterproducts;
Fig. 5 NiO/ γ-Al 2o 3the curve map of composite nano fiber photocatalytic degradation rhodamine B.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
By 0.3g aluminum acetate (Al (CH 3cOO) 3) join in 6g methyl alcohol (the two weight ratio is 1: 20) solvent, mix and blend fully dissolves component and obtains Al (CH 3cOO) 3solution; By 4g nickel acetate (Ni (CH 3cOO) 2) solid joins Al (CH above 3cOO) 3in solution, fully stir and obtain finely dispersed Ni (CH 3cOO) 2/ Al (CH 3cOO) 3mixed solution; 2g PVP (PVP) solid is joined to 18 gin ethanol (the two weight ratio is 1: 9), fully dissolve and obtain PVP solution; By PVP solution, be to join above-mentioned Ni (CH at 2: 1 in mass ratio 3cOO) 2/ Al (CH 3cOO) 3mixed solution in, then stir and obtain Ni (CH 3cOO) 2/ Al (CH 3cOO) 3/ PVP precursor solution.
(electrospinning parameter is: voltage 9kV to carry out electrostatic spinning, silk liquid delivery rate is 1.0ml/h, spinning head is 15cm to the distance between dash receiver, environment temperature is 25 ℃ of left and right, ambient humidity is 30%), obtain precursor nano-composite fiber film as shown in Figure 1, finally by 800 ℃ of calcining 12h, obtain ceramic nanofibers as shown in Figure 2.XRD detects as shown in Figure 4, and the ceramic nanofibers that shows to prepare gained is NiO/ γ-Al 2o 3ceramic nanofibers.
By 0.01gNiO/ γ-Al 2o 3ceramic nanofibers sample adds to the rhodamine B (1.0 * 10 that volume is about the new preparation of 100mL -5mol/L), in the aqueous solution, lucifuge stirs 0.5h at ambient temperature, then under the photocatalytic reaction device of 50W high-pressure sodium lamp, reacts 10min, the rhodamine B of degradable 19.11% (as shown in Figure 5).
Case study on implementation 2
By 0.3g aluminum acetate (Al (CH 3cOO) 3) join in 6g methyl alcohol (both weight ratios are 1: 20) solvent, mix and blend fully dissolves component and obtains Al (CH 3cOO) 3solution; By 4g nickel acetate (Ni (CH 3cOO) 2) solid joins Al (CH above 3cOO) 3in solution, fully stir and obtain finely dispersed Ni (CH 3cOO) 2/ Al (CH 3cOO) 3mixed solution; The PVP of 2g (PVP) solid is joined in the ethanol (both weight ratios are 1: 10) of 20g, fully dissolve and obtain PVP solution; By PVP solution, be to join above-mentioned Ni (CH at 2: 1 in mass ratio 3cOO) 2/ Al (CH 3cOO) 3mixed solution in, then stir and obtain Ni (CH 3cOO) 2/ Al (CH 3cOO) 3/ PVP precursor solution.
(electrospinning parameter is: voltage 10kV to carry out electrostatic spinning, silk liquid delivery rate is 1.0ml/h, spinning head is 15cm to the distance between dash receiver, environment temperature is 25 ℃ of left and right, ambient humidity is 40%), obtain precursor nano-composite fiber film, finally by 800 ℃ of calcining 12h, obtain NiO/ γ-Al2O3 ceramic nanofibers.
By 0.01gNiO/ γ-Al 2o 3ceramic nanofibers sample adds to the rhodamine B (1.0 * 10 that volume is about the new preparation of 100mL -5mol/L), in the aqueous solution, lucifuge stirs 0.5h at ambient temperature, then under the photocatalytic reaction device of 50W high-pressure sodium lamp, reacts 30min, the rhodamine B of degradable 47.39% (as shown in Figure 5).
Embodiment 3
By 0.15g aluminum acetate (Al (CH 3cOO) 3) join in 3g methyl alcohol (both weight ratios are 1: 20) solvent, mix and blend fully dissolves component and obtains Al (CH 3cOO) 3solution; By 2g nickel acetate (Ni (CH 3cOO) 2) solid joins Al (CH above 3cOO) 3in solution, fully stir and obtain finely dispersed Ni (CH 3cOO) 2/ Al (CH 3cOO) 3mixed solution; The PVP of 1g (PVP) solid is joined in the ethanol (both weight ratios are 1: 9) of 9g, fully dissolve and obtain PVP solution; By PVP solution, be to join above-mentioned Ni (CH at 2: 1 in mass ratio 3cOO) 2/ Al (CH 3cOO) 3mixed solution in, then stir and obtain Ni (CH 3cOO) 2/ Al (CH 3cOO) 3/ PVP precursor solution.
(electrospinning parameter is: voltage 11kV to carry out electrostatic spinning, silk liquid delivery rate is 1.0ml/h, spinning head is 15cm to the distance between dash receiver, environment temperature is 25 ℃ of left and right, ambient humidity is 50%), obtain precursor nano-composite fiber film, finally by 800 ℃ of calcining 12h, obtain NiO/ γ-Al2O3 ceramic nanofibers.
By 0.01gNiO/ γ-Al 2o 3ceramic nanofibers sample adds to volume and is about in new rhodamine B (1.0 * 10-5mol/L) aqueous solution of preparing of 100mL, lucifuge stirs 0.5h at ambient temperature, then under the photocatalytic reaction device of 50W high-pressure sodium lamp, react 50min, the rhodamine B of degradable 72.91% (as shown in Figure 5).
Embodiment 4
By 1g aluminum acetate (Al (CH 3cOO) 3) join in 18g methyl alcohol (both weight ratios are 1: 18) solvent, mix and blend fully dissolves component and obtains Al (CH 3cOO) 3solution, by 2g nickel acetate (Ni (CH 3cOO) 2) solid joins Al (CH above 3cOO) 3in solution, fully stir and obtain finely dispersed Ni (CH 3cOO) 2/ Al (CH 3cOO) 3mixed solution; The PVP of 1g (PVP) is joined in the ethanol (both weight ratios are 1: 9) of 9g, fully dissolve and obtain PVP solution; By PVP solution, be to join above-mentioned Ni (CH at 2: 1 in mass ratio 3cOO) 2/ Al (CH 3cOO) 3mixed solution in, then stir and obtain Ni (CH 3cOO) 2/ Al (CH 3cOO) 3/ PVP precursor solution.
(electrospinning parameter is: voltage 12kv to carry out electrostatic spinning, silk liquid delivery rate is 1.0ml/h, spinning head is 15cm to the distance between dash receiver, environment temperature is 25 ℃ of left and right, ambient humidity is 60%), obtain precursor nano-composite fiber film, finally by 1000 ℃ of calcinings, obtain ceramic nanofibers as shown in Figure 3, fibre diameter attenuates and is coarse.As shown in Figure 4, that show to prepare gained is NiO/ γ-Al to XRD 2o 3composite ceramics nanofiber, and degree of crystallinity increases.
By 0.01gNiO/ γ-Al 2o 3ceramic nanofibers sample adds to volume and is about in new rhodamine B (1.0 * 10-5mol/L) aqueous solution of preparing of 100mL, lucifuge stirs 0.5h at ambient temperature, then under the photocatalytic reaction device of 50W high-pressure sodium lamp, react 60min, the rhodamine B of degradable 85.57% (as shown in Figure 5).

Claims (10)

1. a NiO/ γ-Al 2o 3the preparation method of composite ceramics nanofiber catalysis material, comprises the steps:
(1) preparation aluminum salt solution, joins nickel salt in aluminum salt solution, fully stirs to obtain aluminium salt/nickel salt mixed solution; Wherein, the weight ratio of aluminium salt and nickel salt is 1: 1-9;
(2) preparation can be spun the solution of high polymer, and gained solution is joined in above-mentioned aluminium salt/nickel salt mixed solution, obtains aluminium salt/nickel salt/can spin high polymer blend spinning liquid;
(3) above-mentioned spinning solution is carried out to electrostatic spinning, obtain presoma composite nano fiber;
(4) step (3) products obtained therefrom is calcined in air atmosphere, in air atmosphere, naturally cooled to room temperature, obtain NiO/ γ-Al 2o 3composite ceramics nanofiber catalysis material.
2. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the described aluminium salt of step (1) is aluminium chloride, aluminum sulfate, aluminum nitrate, alumina silicate or aluminium sulfide.
3. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the described nickel salt of step (1) is nickel acetate, nickelous sulfate, nickel nitrate, nickel chloride, nickelous carbonate or amino acid nickel.
4. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the solution solvent used of the spun high polymer that the aluminum salt solution that step (1) is described and step (2) are described is methyl alcohol, ethanol or propyl alcohol.
5. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the aluminum salt solution that step (1) is described, and the weight ratio of aluminium salt and solvent is 1: 1-40.
6. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, it is characterized in that, the solution of the spun high polymer that step (2) is described, can spin high polymer is poly, PPTA, cellulose acetate, polyaniline, PEO, polyethylene glycol oxide, polystyrene, polyacrylonitrile, polycaprolactone, polyvinylpyrrolidone, polymethyl methacrylate, polyethylene glycol oxalate, Merlon, nylon 6, polyvinyl alcohol, PLA, poly butyric ester, poly-valeric acid butyrate, poly-3-hydroxybutyrate or 3-hydroxycaproic acid copolymer.
7. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the solution of the spun high polymer that step (2) is described, and the weight ratio that can spin high polymer and solvent is 1: 1-18.
8. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the weight ratio that step (2) can be spun the solution of high polymer and aluminium salt/nickel salt mixed solution of step (1) gained is 1-4: 1.
9. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, it is characterized in that, the electrostatic spinning that step (3) is described, its process conditions are, voltage 5-50kv, the distance in the device for spinning using between receiving system and spinning head is 10-30cm, spinning solution flow velocity is 0.1-3ml/h, environment temperature 10-50 ℃, ambient humidity is 20%-80%.
10. a kind of NiO/ γ-Al according to claim 1 2o 3the preparation method of composite ceramics nanofiber catalysis material, is characterized in that, the calcining that step (4) is described, and its process conditions are, from room temperature, are warmed up to 800-1000 ℃, heating rate 0.8-1.2 ℃/min, calcination time is 12-24h.
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CN105002599A (en) * 2015-06-30 2015-10-28 宁波工程学院 Preparation method of high-purity N-doped TiO2 mesoporous nanofiber
CN108085784A (en) * 2017-12-29 2018-05-29 济南大学 A kind of synthetic method and products obtained therefrom of NiO multistages micro nanometer fiber
CN109759080A (en) * 2019-01-18 2019-05-17 湖北工业大学 Oxidation of formaldehyde composite catalyzing material and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104324742A (en) * 2014-11-13 2015-02-04 武汉钢铁(集团)公司 Nickel carbonate-supported titanium dioxide ultraviolet light catalyst and preparation method thereof
CN105002599A (en) * 2015-06-30 2015-10-28 宁波工程学院 Preparation method of high-purity N-doped TiO2 mesoporous nanofiber
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CN108085784A (en) * 2017-12-29 2018-05-29 济南大学 A kind of synthetic method and products obtained therefrom of NiO multistages micro nanometer fiber
CN108085784B (en) * 2017-12-29 2020-02-07 济南大学 Synthetic method of NiO multi-stage micro-nano fiber and obtained product
CN109759080A (en) * 2019-01-18 2019-05-17 湖北工业大学 Oxidation of formaldehyde composite catalyzing material and preparation method thereof

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Application publication date: 20140820