CN109926053A - A kind of NiO/NiTiO3Composite nano-fiber membrane catalysis material - Google Patents
A kind of NiO/NiTiO3Composite nano-fiber membrane catalysis material Download PDFInfo
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Abstract
The invention discloses a kind of NiO/NiTiO3Composite nano-fiber membrane catalysis material and preparation method thereof belongs to catalysis material technical field.The present invention uses electrostatic spinning technique, using nickel acetate, four fourth rouge of metatitanic acid as nickel, titanium source, nickel acetate is dissolved in acetic acid and obtains solution A, polyvinylpyrrolidone is dissolved in ethyl alcohol and obtains solution B, solution A addition solution B is stirring evenly and then adding into butyl titanate, continues to stir to get precursor solution.It is prepared under specific operating voltage, receiving distance, pump fltting speed with NiO/NiTiO using electrostatic spinning process3Composite fibre film precursor obtains NiO/NiTiO after being heat-treated to fiber film precursor3Composite nano-fiber membrane catalysis material.The product has the structure features such as porous, self-supporting, and photocatalysis performance is excellent and environmental-friendly, and is easier to realize the separation with degraded solutions, there is important practical application potentiality.
Description
Technical field
The present invention relates to catalysis material technical fields, and in particular to a kind of NiO/NiTiO3Composite nano-fiber membrane light is urged
Change material and preparation method thereof.
Background technique
Water is material base for the survival of mankind, but recently as industrial expansion, the environmental problems such as water pollution
It gets worse, especially organic pollutant difficult to degrade in water, it causes very big influence to the mankind and nature.Semiconductor
Light-catalyzed reaction refers to that under certain illumination condition, photochemical catalyst, which is excited, generates photohole-electronics pair, generates Strong oxdiative
Free love base, so that organic matter degradation be made to ultimately become the small organic molecule of no environmental hazard or the chemistry of inorganic molecules substance
Reaction process, purification of waste water and in terms of have great potential.
In photocatalysis field, the catalysis material of most practical value is TiO at present2, forbidden bandwidth 3.2eV, because
This can only utilize ultraviolet light in light-catalyzed reaction, but ultraviolet light only accounts for 4% or so of solar energy, therefore it is in nature
Light-catalyzed reaction efficiency and quantum yield under sunlight is not high, therefore develops with full spectrum or visible light-responded a large amount
The photochemical catalyst of sub- yield is the direction of area research person effort always.In recent years, researcher has found novel urge successively
Agent, such as oxide (ZnO, SnO2), sulfide (such as CdS, ZnIn2S4、CdxZn1-x) and nitrogen (oxygen) compound (such as Ta S3N5、
TaON) etc., but photocatalysis performance still have it is to be hoisted.For the principle and process of light-catalyzed reaction, to photocatalysis to be improved
The performance of agent must just be modified catalysis material, and main method is as follows: first is adjustment band gap width, extends photocatalysis
The visible absorption and response region of agent；Second is the position for adjusting valence band and conduction band, so that current potential more matches；Third is
Promote the separation of electron hole, inhibit the compound of electronics and hole, the fourth is that form composite heterogenous junction by preparation to improve light
Catalyst system.
Nickel titanate (NiTiO3) it is a kind of typical perovskite structure, titanium atom and nickle atom compartment of terrain are arranged in octahedron
The cationic layer of coordination belongs to n-type semiconductor.It is anti-that neutron-diffraction study and sensibility measurement to powder show that nickel titanate has
Ferromagnetic structure, forbidden bandwidth 2.18eV, research shows that the NiTiO being prepared3Nanostructure often has well
Photocatalysis performance.Nickel oxide (NiO) is p-type semiconductor, forbidden bandwidth 3.5eV, the position difference of valence band and conduction band
Below the valence band of NiTiO3 and above conduction band.In conjunction with its band gap characteristic, this project is proposed NiTiO3It is carried out with NiO compound
NiO/NiTiO is prepared3Composite photo-catalyst forms p-n heterojunction structure using the characteristic of semiconductor of the two, is made by collaboration
Inhibit the quick compound raising photohole of photo-generated carrier with the response wave length and built in field of expanding wide band gap semiconducter
With mechanism the effects of the utilization efficiency of electronics, preferable photocatalysis effect is obtained.
Electrostatic spinning technique is that using high-voltage electrostatic field the breakdown effects of precursor solution are prepared with a wiener micron fibre
The method for tieing up material, corpus fibrosum can directly obtain the tunica fibrosa with porous pattern in the unordered accumulation in receiving end in practice
Structure, if being always maintained at independent membrane structure in the treatment process in later period, constant to obtain stablizing self-existent semiconductor multiple
Condensating fiber membrane material has important theoretical significance and practical application value in the practical application of photochemical catalyst.
Therefore NiO/ is prepared in the use electrostatic spinning process combination situ heat treatment one-step method of the invention
NiTiO3Composite nano-fiber membrane material adjusts its performance by material rate regulation and technology controlling and process, and leads using two and half
Formed between oxide body it is heterogeneous obtain more excellent photocatalysis performance, become a kind of novel photocatalysis material for potential
Material, it may have important application value and technological innovation meaning.
Summary of the invention
A kind of NiO/NiTiO of the present invention3Composite nano-fiber membrane catalysis material be designed to provide a kind of high efficiency,
Segregative catalysis material improves photocatalysis efficiency, realizes catalysis material to solve the environmental problems such as existing water pollution
Easily separated reusable target.
To achieve the above object, the invention proposes NiO and NiTiO that a kind of object phase composition obtains for reaction in-situ3's
Compound, pattern are by NiO/NiTiO3The high-performance optical for the perforated membrane composite nano-fiber membrane that nanofiber is formed is catalyzed material
Material and preparation method thereof can satisfy the condition of degradation sewage, and be conducive to back with excellent photocatalysis performance and environmental-friendly
Receipts processing, has broad application prospects.
The object phase composition of this product is the NiO and NiTiO that reaction in-situ obtains3Compound, wherein NiO and NiTiO3's
Molar ratio is 0.01:1 to 0.4:1；Its pattern is by NiO/NiTiO3The perforated membrane that nanofiber is formed, wherein nanofiber is straight
Diameter is 100-400nm.
A kind of NiO/NiTiO of the present invention3The preparation method of composite nano-fiber membrane catalysis material, feature exist
In:
(1) with butyl titanate (C16H36O4, nickel acetate (Ni (CH Ti, purity: 99.5%)3COO)2, purity 99.5%)
Respectively as titanium, nickel source, by NiO and NiTiO3Molar ratio be 0.01:1 to 0.4:1 carry out ingredient, nickel acetate is dissolved in one
Solution A is obtained in quantitative acetic acid, using ethyl alcohol as solvent and polyvinylpyrrolidone (PVP) (1%-10%) is added to adjust it viscous
Butyl titanate is uniformly added to obtain the solution B for meeting spinning requirement, by solution A addition solution B magnetic agitation in degree afterwards, continues
Stir to get precursor solution.
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, voltage
(10kv-20kv), distance (10cm-20cm), spinning solution propulsion rate are received to be spun under (0.4mL/h-2.0mL/h)
Silk, obtains the NiO/NiTiO for having nanometer fibrous3Composite fibre film precursor.
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed in the Muffle furnace that beginning temperature is room temperature, in temperature
For (400 DEG C -1200 DEG C) heat treatment time (0.5h-4.0h), heating rate and rate of temperature fall (1 DEG C/min-10 DEG C/min) into
Row heat treatment obtains the stable NiO/NiTiO of morphosis3Composite nano-fiber membrane.
The present invention has the advantage that
(1) there is excellent photocatalysis performance；
(2) separation easily with liquid after processing；
(3) recycling process still keeps stable photocatalysis performance.
Detailed description of the invention
Fig. 1 is the NiO/NiTiO for the technique preparation that embodiment 1 provides3The SEM of composite nano-fiber membrane schemes.It can be with by figure
Find out, obtains nano fibrous membrane and be made of continuous uniform nanofiber.
Fig. 2 is the NiO/NiTiO for the technique preparation that embodiment 1 provides3The XRD spectrum of composite nano-fiber membrane, comparison mark
Quasi- card data shows that the object of sample is mutually NiO and NiTiO3。
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
(1) using nickel acetate as nickel source, 1.10mmol nickel acetate is dissolved in 2ml acetic acid and obtains solution A, with 10ml second
Alcohol is solvent and polyvinylpyrrolidone (PVP) 0.6g is added adjusts its viscosity to obtain the solution B for meeting spinning requirement, will be molten
Liquid A is added solution B magnetic agitation and butyl titanate 1.00mmol is uniformly added afterwards, continues to stir to get precursor solution.
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, voltage
17.5kv, distance 20cm, spinning solution propulsion rate are received to carry out spinning under 1mL/h, obtains having nanometer fibrous
NiO/NiTiO3Composite fibre film precursor.
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed in the Muffle furnace that beginning temperature is room temperature, and room temperature is
20 DEG C, the organic principle that 1 DEG C/min heating rate is kept the temperature in 0.5h burn-up tunica fibrosa to 400 DEG C, then with 1 DEG C/min heating rate
Object phase reaction is carried out to 800 DEG C of heat preservation 0.5h, then room temperature is dropped to 1 DEG C/min rate of temperature fall, it is stable to obtain morphosis
NiO/NiTiO3Composite nano-fiber membrane.
(4) it using the rhodamine B of 5mg/L as organic pollutant, is separated simultaneously using a set of photochemical catalyst and pollutant solution
The uninterrupted equipment for carrying out photocatalytic degradation reaction can be recycled.Equipment reactor is divided into two parts, and upper and lower two parts are with frosted
Mouth connection, it is ensured that rhodamine B solution is not spilt over.Take NiO/NiTiO3Composite nano-fiber membrane sample 30mg is placed in the reactor
Between it is fixed, it is ensured that mix with pollutant solution, avoiding needs the process for separating catalyst with solution after reacting；Light source uses
Parallel light source is capable of providing stable photon energy, and photochemical catalyst is made to generate light induced electron and hole；Right side adds a recirculated water
Pump controls pollutant solution circulation rate by flow control valve, keeps the catalyst among rhodamine B solution and reactor anti-
It answers.Dark treatment 30min is first carried out to equipment, opens full spectrum light source, rhodamine B solution is all degraded after 60min.
Embodiment 2
(1) using nickel acetate as nickel source, 1.15mmol nickel acetate is dissolved in 2ml acetic acid and obtains solution A, with 10ml second
Alcohol is solvent and polyvinylpyrrolidone (PVP) 0.6g is added adjusts its viscosity to obtain the solution B for meeting spinning requirement, will be molten
Liquid A is added solution B magnetic agitation and butyl titanate 1.00mmol is uniformly added afterwards, continues to stir to get precursor solution.
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, voltage
17.5kv, distance 20cm, spinning solution propulsion rate are received to carry out spinning under 1mL/h, obtains having nanometer fibrous
NiO/NiTiO3Composite fibre film precursor.
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed in the Muffle furnace that beginning temperature is room temperature, and room temperature is
20 DEG C, the organic principle that 1 DEG C/min heating rate is kept the temperature in 0.5h burn-up tunica fibrosa to 400 DEG C, then with 1 DEG C/min heating rate
Object phase reaction is carried out to 800 DEG C of heat preservation 0.5h, then room temperature is dropped to 1 DEG C/min rate of temperature fall, it is stable to obtain morphosis
NiO/NiTiO3Composite nano-fiber membrane.
(4) it using the rhodamine B of 5mg/L as organic pollutant, is separated simultaneously using a set of photochemical catalyst and pollutant solution
The uninterrupted equipment for carrying out photocatalytic degradation reaction can be recycled.Equipment reactor is divided into two parts, and upper and lower two parts are with frosted
Mouth connection, it is ensured that rhodamine B solution is not spilt over.Take NiO/NiTiO3Composite nano-fiber membrane sample 30mg is placed in the reactor
Between it is fixed, it is ensured that mix with pollutant solution, avoiding needs the process for separating catalyst with solution after reacting；Light source uses
Parallel light source is capable of providing stable photon energy, and photochemical catalyst is made to generate light induced electron and hole；Right side adds a recirculated water
Pump controls pollutant solution circulation rate by flow control valve, keeps the catalyst among rhodamine B solution and reactor anti-
It answers.Dark treatment 30min is first carried out to equipment, opens full spectrum light source, rhodamine B solution is all degraded after 60min.
Embodiment 3
(1) using nickel acetate as nickel source, 1.10mmol nickel acetate is dissolved in 2ml acetic acid and obtains solution A, with 10ml second
Alcohol is solvent and polyvinylpyrrolidone (PVP) 0.6g is added adjusts its viscosity to obtain the solution B for meeting spinning requirement, will be molten
Liquid A is added solution B magnetic agitation and butyl titanate 1.00mmol is uniformly added afterwards, continues to stir to get precursor solution.
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, voltage
17.5kv, distance 20cm, spinning solution propulsion rate are received to carry out spinning under 1mL/h, obtains having nanometer fibrous
NiO/NiTiO3Composite fibre film precursor.
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed in the Muffle furnace that beginning temperature is room temperature, and room temperature is
20 DEG C, the organic principle that 1 DEG C/min heating rate is kept the temperature in 0.5h burn-up tunica fibrosa to 400 DEG C, then with 1 DEG C/min heating rate
Object phase reaction is carried out to 900 DEG C of heat preservation 0.5h, then room temperature is dropped to 1 DEG C/min rate of temperature fall, it is stable to obtain morphosis
NiO/NiTiO3Composite nano-fiber membrane.
(4) it using the rhodamine B of 5mg/L as organic pollutant, is separated simultaneously using a set of photochemical catalyst and pollutant solution
The uninterrupted equipment for carrying out photocatalytic degradation reaction can be recycled.Equipment reactor is divided into two parts, and upper and lower two parts are with frosted
Mouth connection, it is ensured that rhodamine B solution is not spilt over.Take NiO/NiTiO3Composite nano-fiber membrane sample 30mg is placed in the reactor
Between it is fixed, it is ensured that mix with pollutant solution, avoiding needs the process for separating catalyst with solution after reacting；Light source uses
Parallel light source is capable of providing stable photon energy, and photochemical catalyst is made to generate light induced electron and hole；Right side adds a recirculated water
Pump controls pollutant solution circulation rate by flow control valve, keeps the catalyst among rhodamine B solution and reactor anti-
It answers.Dark treatment 30min is first carried out to equipment, opens full spectrum light source, rhodamine B solution is all degraded after 60min.
Embodiment 4
(1) using nickel acetate as nickel source, 1.15mmol nickel acetate is dissolved in 2ml acetic acid and obtains solution A, with 10ml second
Alcohol is solvent and polyvinylpyrrolidone (PVP) 0.6g is added adjusts its viscosity to obtain the solution B for meeting spinning requirement, will be molten
Liquid A is added solution B magnetic agitation and butyl titanate 1.00mmol is uniformly added afterwards, continues to stir to get precursor solution.
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, voltage
17.5kv, distance 20cm, spinning solution propulsion rate are received to carry out spinning under 1mL/h, obtains having nanometer fibrous
NiO/NiTiO3Composite fibre film precursor.
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed in the Muffle furnace that beginning temperature is room temperature, and room temperature is
20 DEG C, the organic principle that 1 DEG C/min heating rate is kept the temperature in 0.5h burn-up tunica fibrosa to 400 DEG C, then with 1 DEG C/min heating rate
Object phase reaction is carried out to 900 DEG C of heat preservation 0.5h, then room temperature is dropped to 1 DEG C/min rate of temperature fall, it is stable to obtain morphosis
NiO/NiTiO3Composite nano-fiber membrane.
(4) it using the rhodamine B of 5mg/L as organic pollutant, is separated simultaneously using a set of photochemical catalyst and pollutant solution
The uninterrupted equipment for carrying out photocatalytic degradation reaction can be recycled.Equipment reactor is divided into two parts, and upper and lower two parts are with frosted
Mouth connection, it is ensured that rhodamine B solution is not spilt over.Take NiO/NiTiO3Composite nano-fiber membrane sample 30mg is placed in the reactor
Between it is fixed, it is ensured that mix with pollutant solution, avoiding needs the process for separating catalyst with solution after reacting；Light source uses
Parallel light source is capable of providing stable photon energy, and photochemical catalyst is made to generate light induced electron and hole；Right side adds a recirculated water
Pump controls pollutant solution circulation rate by flow control valve, keeps the catalyst among rhodamine B solution and reactor anti-
It answers.Dark treatment 30min is first carried out to equipment, opens full spectrum light source, rhodamine B solution is all degraded after 60min.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (3)
1. a kind of NiO/NiTiO3Composite nano-fiber membrane catalysis material, it is characterised in that:
Its object phase composition is the NiO and NiTiO that reaction in-situ obtains3Compound, wherein NiO and NiTiO3Molar ratio range
For 0.01:1 to 0.4:1；Its pattern is by NiO/NiTiO3Nanofiber formed perforated membrane, wherein nanofiber diameter be
100-400nm。
2. a kind of NiO/NiTiO described in claim 13Composite nano-fiber membrane catalysis material preparation method mainly includes nickel
Source, titanium source, configuration precursor solution, electrostatic spinning are at NiO/NiTiO3Composite nano-fiber membrane presoma, high-temperature heat treatment obtain
To NiO/NiTiO3Composite nano-fiber membrane catalysis material and etc., it is characterised in that:
(1) using butyl titanate and nickel acetate as titanium source, nickel source, by NiO and NiTiO3Molar ratio be 0.01:1 extremely
0.4:1 carries out ingredient, and nickel acetate is dissolved in a certain amount of acetic acid and obtains solution A, by polyvinylpyrrolidone (1%-10%)
It is added to alcohol solvent and obtains solution B, then solution A addition solution B is stirred evenly, butyl titanate is added, continues to stir
It mixes to obtain precursor solution；
(2) take suitable precursor sol in the glass liquid storage device of traditional single spinning head electrostatic spinning apparatus, in voltage
(10kV-20kV), reception distance (10cm-20cm), spinning solution carry out under the conditions of promoting rate (0.4mL/h-2.0mL/h) etc.
Spinning obtains the NiO/NiTiO for having nanometer fibrous3Composite fibre film precursor；
(3) by NiO/NiTiO3Composite nano-fiber membrane presoma is placed into Muffle furnace, at certain temperature (400 DEG C -1200 DEG C)
Lower heat treatment 0.5-4.0h, heating rate and rate of temperature fall are 1-10 DEG C/min, obtain the stable NiO/NiTiO of morphosis3
Composite nano-fiber membrane.
3. a kind of NiO/NiTiO described in claim 13Composite nano-fiber membrane catalysis material, it is characterised in that:
Simulated solar irradiation light source irradiation under, can within 60min the simulating pollutions object such as degradable rhodamine B, after separation
NiO/NiTiO3Composite nano-fiber membrane is still able to maintain stable photocatalysis performance during recycling.
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Cited By (6)
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| CN110560066A (en) * | 2019-09-25 | 2019-12-13 | 齐鲁工业大学 | NiO/CuO composite material and preparation method and application thereof |
| CN110813298A (en) * | 2019-11-06 | 2020-02-21 | 齐鲁工业大学 | Cobalt titanate @ nickel oxide core-shell photocatalytic material and preparation method and application thereof |
| CN111111681A (en) * | 2019-12-26 | 2020-05-08 | 东莞东阳光科研发有限公司 | NiO/WO with multi-stage nano structure3Photocatalyst and preparation method and application thereof |
| CN114632536A (en) * | 2022-04-01 | 2022-06-17 | 吉林化工学院 | NiCo with photocatalytic properties2O4/NiO/g-C3N4Nanotube preparation method and application |
| CN115155606A (en) * | 2022-06-21 | 2022-10-11 | 蚌埠学院 | Bi 2 MO 6 /NiTiO 3 Preparation method and application of heterojunction photocatalytic film material |
| CN117599834A (en) * | 2024-01-23 | 2024-02-27 | 河海大学 | Photocatalytic nanofiber membrane and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560066A (en) * | 2019-09-25 | 2019-12-13 | 齐鲁工业大学 | NiO/CuO composite material and preparation method and application thereof |
| CN110813298A (en) * | 2019-11-06 | 2020-02-21 | 齐鲁工业大学 | Cobalt titanate @ nickel oxide core-shell photocatalytic material and preparation method and application thereof |
| CN110813298B (en) * | 2019-11-06 | 2023-03-17 | 齐鲁工业大学 | Cobalt titanate @ nickel oxide core-shell photocatalytic material and preparation method and application thereof |
| CN111111681A (en) * | 2019-12-26 | 2020-05-08 | 东莞东阳光科研发有限公司 | NiO/WO with multi-stage nano structure3Photocatalyst and preparation method and application thereof |
| CN114632536A (en) * | 2022-04-01 | 2022-06-17 | 吉林化工学院 | NiCo with photocatalytic properties2O4/NiO/g-C3N4Nanotube preparation method and application |
| CN114632536B (en) * | 2022-04-01 | 2023-10-20 | 吉林化工学院 | NiCo with photocatalytic properties 2 O 4 /NiO/g-C 3 N 4 Nanotube preparation method and application |
| CN115155606A (en) * | 2022-06-21 | 2022-10-11 | 蚌埠学院 | Bi 2 MO 6 /NiTiO 3 Preparation method and application of heterojunction photocatalytic film material |
| CN115155606B (en) * | 2022-06-21 | 2023-07-04 | 蚌埠学院 | Bi (Bi) 2 MoO 6 /NiTiO 3 Preparation method and application of heterojunction photocatalytic film material |
| CN117599834A (en) * | 2024-01-23 | 2024-02-27 | 河海大学 | Photocatalytic nanofiber membrane and preparation method and application thereof |
| CN117599834B (en) * | 2024-01-23 | 2024-05-07 | 河海大学 | Photocatalytic nanofiber membrane and preparation method and application thereof |
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Application publication date: 20190625 |
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