CN109926063A - A kind of preparation method of copper tungstate nanofiber photocatalyst - Google Patents
A kind of preparation method of copper tungstate nanofiber photocatalyst Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of copper tungstate nanofiber photocatalyst, belong to photocatalysis technology field.The one-dimensional copper tungstate nanofiber is prepared by electrostatic spinning technique, and the fibre diameter is uniform, large specific surface area, and photo-generated carrier transmission range is short, can effectively improve the catalytic activity of its Visible Light Induced Photocatalytic organic matter.The preparation method of the photochemical catalyst, which mainly comprises the steps that, is dissolved in inorganic tungsten salt and inorganic mantoquita in ethyl alcohol or DMF solution, PAN or PVP is added, obtains spinning solution, composite fibre is obtained by electrostatic spinning apparatus, high-temperature calcination is to get porous copper tungstate nanofiber.The preparation process is easy to operate, low in cost, is expected to realize the large scale preparation of copper tungstate nanofiber, have broad application prospects in environment and energy field.
Description
Technical field
The present invention relates to a kind of preparation methods of copper tungstate nanofiber photocatalyst, belong to photocatalysis technology field, more
Add particularly that the present invention provides a kind of copper tungstate nanofibers with highlight catalytic active, high surface area and high stability
The preparation method of photochemical catalyst.
Background technique
With the rapid growth of China's economy and the development of global industry, environmental pollution is getting worse.Find one
The green common technology of item low cost, administers have great importance to environmental pollutants.Photocatalitic Technique of Semiconductor can be straight
It connects using the oxygen in solar energy and air, is at normal temperatures and pressures nontoxic CO by the organic pollutant mineralising in solution2Point
Son, the technical treatment is at low cost, it is easy to operate, secondary pollution will not be generated, be with a wide range of applications.In numerous semiconductors
In photochemical catalyst, TiO2It is most widely used, but TiO2Band gap is larger, can only absorb the ultraviolet portion of solar spectral, cause
Solar energy utilization ratio is low, limits its practical application.
CuWO4It is a kind of n-type semiconductor, the sun below of 550nm in solar spectral can be absorbed in band gap 2.25eV
Light absorbs the concern of more and more researchers in recent years.But copper tungstate itself that there is specific surface areas is small, conductivity is low,
The problems such as carrier recombination velocity is fast and charge transmission range is short, causes its solar conversion efficiency low, is unable to satisfy reality
Application demand.It develops one-dimensional copper tungstate nanofiber to be expected to eliminate some defects existing for copper tungstate itself, increases its surface area,
Its surface-active number of sites is improved, reduces photogenerated charge transmission range, and then improve copper tungstate photocatalytic degradation environmental contaminants
Activity.Electrostatic spinning technique is the strong means for synthesizing nano-fiber material, but copper tungstate nano-fiber material is always
It has not been reported, is primarily due to lack copper tungstate spinning formula of liquid and the relevant technical solution of copper tungstate spinning technology parameter,
It is unfavorable for the preparation of copper tungstate nano-fiber material.In the present invention, we successfully mix the spinning of copper tungstate nanofiber
Formula of liquid has synthesized the uniform copper tungstate nanofiber of diameter by electrostatic spinning apparatus, and the fiber is under visible light illumination, right
Dye molecule in solution has good degradation effect.In short, the preparation method is easy to operate, and it is low in cost, it is expected to realize
The large-scale production of copper tungstate, and promote it in the extensive use of field of environmental improvement.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of copper tungstate nanofiber photocatalyst, the purpose of the present invention
It is realized by following operating procedure:
1) a certain amount of inorganic tungsten salt is weighed, is dissolved in ethyl alcohol or n,N-Dimethylformamide (DMF), then, is added one
Quantitative inorganic mantoquita, copper and the control of tungsten molar ratio are 1:1, stirring and dissolving；A certain amount of polyethylene pyrrole is added into the solution
Pyrrolidone (PVP) or polyacrylonitrile (PAN) stir 2-72h, obtain homogeneous spinning solution；
2) above-mentioned spinning solution is added in electrostatic spinning apparatus, adjusting syringe fltting speed is 0.5-15mm/h, is spun
It is 5-20cm, drum rotation speed 300-500r/min that filament voltage 10-30kV, syringe needle and roller, which receive distance, is obtained cured compound
Fiber, it is dry in 100-150 DEG C of baking oven；
3) composite fibre after drying is put into Muffle furnace, 0.5-5h is calcined at 400-800 DEG C, heating rate control is
0.5-10 DEG C/min, the cooling inorganic copper tungstate nanofiber to get porous structure.
The technical solution is easy to operate, low in cost, is suitable for large scale preparation copper tungstate nano-porous fiber material；Institute
The copper tungstate nanofiber diameter obtained is uniform, and pore-size distribution is wider, effectively increases the specific surface area of copper tungstate photochemical catalyst.It can
Under light-exposed irradiation, compared with the copper tungstate powder of hydro-thermal method synthesis, nanofiber improves the removal efficiency of dye molecule.It is heavier
It wants, the copper tungstate nanofiber recycling of preparation is convenient, it can be achieved that recycled for multiple times.These advantages make copper tungstate Nanowire
Dimension has broad application prospects in future source of energy and environmental area.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of the copper tungstate nanofiber prepared in embodiment one.
Fig. 2 is the UV-vis DRS map of the copper tungstate nanofiber prepared in embodiment two；
Fig. 3 is the graph of pore diameter distribution of the copper tungstate nanofiber prepared in embodiment three；
Fig. 4 is the scanning electron microscope (SEM) photograph of the copper tungstate nanofiber prepared in example IV；
Fig. 5 is the scanning electron microscope (SEM) photograph of the copper tungstate nanofiber prepared in embodiment five；
Fig. 6 is the scanning electron microscope (SEM) photograph of the copper tungstate nanofiber prepared in embodiment six.
Fig. 7 is that the copper tungstate nanofiber for preparing and copper tungstate powder are degraded methyl under visible light illumination in embodiment seven
The time plot of orange.
Specific embodiment
In order to better understand the present invention, below with reference to the embodiment and attached drawing content that the present invention is furture elucidated, but this
The content of invention is not limited solely to the following examples.
Embodiment one
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
By 1g WCl6It is dissolved in the DMF of 10mL, stirring and dissolving, 0.5g copper acetate is then added, stirring and dissolving adds 1g
PAN is stirred overnight, and obtains spinning liquid as precursor；Above-mentioned spinning solution is poured into 10ml syringe, spinning technology parameter is adjusted are as follows:
Spinning voltage 15kV, syringe fltting speed are 2mm/h, and it is 10cm, drum rotation speed 300r/min that syringe needle and roller, which receive distance,
Room temperature control is 25 DEG C；Composite fibre after drying is put into Muffle furnace, 1h, heating rate control are calcined at 600 DEG C
It is cooling to get porous copper tungstate nanofiber for 1 DEG C/min.
Fig. 1 gives the X ray diffracting spectrum of copper tungstate nanofiber, as seen from the figure, the crystal form of copper tungstate good
With for anorthic system, and do not occur the crystal phase of other substances in XRD diagram, shows that the copper tungstate of synthesis is pure phase.
Embodiment two
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
By 1g WCl6It is dissolved in the DMF of 10mL, stirs 20 minutes, 0.5g copper acetate is then added, stirring and dissolving is added
1g PVP, is stirred overnight, and obtains spinning solution；Above-mentioned spinning solution is poured into 10ml syringe, adjusts spinning technology parameter are as follows: spinning
Voltage 16kV, syringe fltting speed are 3mm/h, and it is 10cm that syringe needle and roller, which receive distance, drum rotation speed 350r/min to get
Composite nano fiber, 120 DEG C of constant temperature 6h；Composite fibre after drying is put into Muffle furnace, 1h, heating speed are calcined at 650 DEG C
Rate control is 1 DEG C/min, cooling to get porous copper tungstate nanofiber.
Fig. 2 is the UV-vis DRS spectrum of the copper tungstate nanofiber of preparation, in 550nm hereinafter, the suction of copper tungstate
Receipts sharply increase, and show that copper tungstate is a kind of visible-light photocatalyst, band gap is about 2.25eV.
Embodiment three
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
0.61g ammonium tungstate is dissolved in the DMF of 12mL, then 0.44g copper acetate is added in ultrasonic dissolution, stirring and dissolving is added
1.5g PVP is dissolved by heating, is stirred overnight, obtains spinning solution；Above-mentioned spinning solution is poured into 10ml syringe, spinning technique is adjusted
Parameter are as follows: spinning voltage 17kV, syringe fltting speed are 6mm/h, and it is 10cm, drum rotation speed that syringe needle and roller, which receive distance,
380r/min is to get porous nano-fibre, 150 DEG C of constant temperature 10h；Composite fibre after drying is put into Muffle furnace, at 550 DEG C
1h is calcined, heating rate control is 5 DEG C/min, cooling to get yellow wolframic acid copper nano particles.
Fig. 3 is the graph of pore diameter distribution of the copper tungstate measured using specific surface area and pore analysis instrument, as seen from the figure, copper tungstate
Pore size distribution range it is wider (2.4-106nm), but mainly based on aperture.And its specific surface area (Asp) use Brunauer-
Emmett-Teller (BET) adsorption isotherm equation carries out being calculated as 13.58m2/g。
Example IV
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
0.08g sodium tungstate is dissolved in the DMF of 12mL, then 0.6g copper nitrate is added in ultrasonic dissolution, stirring and dissolving is added
1g PVP is dissolved by heating, is stirred overnight, obtains spinning solution；Above-mentioned spinning solution is poured into 10ml syringe, spinning technique ginseng is adjusted
Number are as follows: spinning voltage 18kV, syringe fltting speed are 6mm/h, and it is 10cm, drum rotation speed that syringe needle and roller, which receive distance,
400r/min is to get composite nano fiber, 150 DEG C of constant temperature 10h；Composite fibre after drying is put into Muffle furnace, at 550 DEG C
2h is calcined, heating rate control is 2 DEG C/min to get yellow wolframic acid copper nano particles.
Fig. 4 is the scanning electron microscope (SEM) photograph before the calcining of copper tungstate nanofiber, it can be seen that copper tungstate calcining front surface is very smooth,
For fibre diameter in 200nm or so, length is mutually overlapping between fiber up to tens microns, forms reticular structure.
Embodiment five
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
By 1.2g WCl6It is dissolved in the ethyl alcohol of 10mL, stirs half an hour, then addition 0.6g copper acetate, stirring and dissolving,
0.5g PVP is added, is stirred overnight, spinning solution is obtained；Above-mentioned spinning solution is poured into 10ml syringe, spinning technology parameter is adjusted
Are as follows: spinning voltage 15kV, syringe fltting speed are 4mm/h, and it is 12cm, drum rotation speed 450r/ that syringe needle and roller, which receive distance,
Min is to get composite nano fiber, 150 DEG C of constant temperature 8h；Composite fibre after drying is put into Muffle furnace, is calcined at 550 DEG C
2h, heating rate control are 1 DEG C/min, cooling to get copper tungstate nanofiber.
Fig. 5 is the scanning electron microscope (SEM) photograph of calcined copper tungstate nanofiber, and as seen from the figure, the diameter of fiber is 250nm left
It is right.At high temperature, organic matter is thermally decomposed, and nanofiber surface is no longer smooth, but is made of many tiny nano particles,
These little particles can effectively increase the specific surface area of copper tungstate.
Embodiment six
A kind of preparation method of copper tungstate nanofiber photocatalyst, the specific steps are as follows:
By 0.5g WCl6It is dissolved in the DMF of 5mL, stirs half an hour, 0.3g copper acetate is then added, stirring and dissolving is mended
Add 0.5g PAN, be stirred overnight, obtains spinning solution；Above-mentioned spinning solution is poured into 10ml syringe, spinning technology parameter is adjusted are as follows:
Spinning voltage 14kV, syringe fltting speed are 2mm/h, and it is 15cm, drum rotation speed 500r/min that syringe needle and roller, which receive distance,
It up to composite nano fiber, being transferred in Muffle furnace later, 1h is calcined at 550 DEG C, heating rate control is 2 DEG C/min, it is cooling,
Up to copper tungstate nanofiber.
Fig. 6 is the scanning electron microscope (SEM) photograph of the copper tungstate nanofiber that is prepared using this method after firing, as seen from the figure, the party
The copper tungstate nanofiber of method preparation is in bone shape, and diameter is in 120nm or so.Since organic matter is thermally decomposed, fibrous inside is produced
Raw a large amount of holes, and fiber surface generates some fine particles, effectively increases the specific surface area of copper tungstate.
Embodiment seven
Fig. 7 is to synthesize copper tungstate powder visible light with hydro-thermal method using copper tungstate nanofiber prepared by embodiment three to urge
The curve graph for changing degradation of methylene blue dyestuff, copper tungstate nanofiber reaches 90% or so to the degradation rate of dyestuff after 4h, and water
The copper tungstate powder of thermal method synthesis is only 50% or so to dyestuff degradation rate, show the photocatalytic activity of copper tungstate nanofiber compared with
It is more excellent on the powder characteristic of hydro-thermal method synthesis.
The experiment of simulated visible light degradation of methylene blue, concrete operations are as follows:
(1) compound concentration is 10mg/L methylene blue solution；
(2) the copper tungstate powder of 25mg copper tungstate nanofiber and hydrothermal synthesis is added into quartz ampoule respectively, then distinguishes
The methylene blue solution of 50mL is added；
(3) above-mentioned reaction solution is transferred in photo catalysis reactor, the xenon lamp of 500W is removed as light source using optical filter
420nm wavelength light below carrys out simulated visible light catalytic condition with this；
(4) xenon lamp is opened after darkroom air agitation 1h, is carried out photocatalytic degradation, is taken from above-mentioned quartz ampoule respectively every 1h
Sample is then centrifuged for, and takes its supernatant liquor；The absorbance of methylene blue solution is measured at 664nm using spectrophotometer, is calculated
Degradation rate.
Claims (7)
1. a kind of preparation method of copper tungstate nanofiber photocatalyst, it is characterised in that the following steps are included:
1) it using inorganic tungsten salt and inorganic mantoquita as raw material, is dissolved in ethyl alcohol or n,N-Dimethylformamide (DMF), is added certain
The organic high molecular polymer of amount stirs 2-72h, obtains spinning solution；
2) above-mentioned spinning solution is added in 10ml syringe, by electrostatic spinning apparatus, certain spinning technology parameter is set,
Cured composite fibre, 100-150 DEG C of drying are received on the roller for be covered with aluminium-foil paper；
3) above-mentioned composite fibre is transferred in Muffle furnace, controls certain heating rate calcining to get copper tungstate nanofiber.
2. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, it is characterised in that described
The inorganic tungsten salt that step 1 uses is one or more of wolframic acid, sodium tungstate, ammonium tungstate, tungsten hexachloride.
3. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, it is characterised in that described
The inorganic mantoquita that step 1 uses is one or more of copper nitrate, copper acetate, copper chloride, copper sulphate.
4. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, which is characterized in that step
1 organic high molecular polymer is polyvinylpyrrolidone (PVP) or polyacrylonitrile (PAN).
5. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, which is characterized in that step
The Cu:W molar ratio in 1 copper source and tungsten source is that the mass fraction of 1:1, ethyl alcohol or DMF and organic high molecular polymer is 5:1-
30:1。
6. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, it is characterised in that described
The technological parameter of step 2 electrostatic spinning are as follows: syringe fltting speed 0.5-15mm/h, spinning voltage 10-30kV receive distance 5-
20cm, drum rotation speed 300-500r/min.
7. a kind of preparation method of copper tungstate nanofiber photocatalyst according to claim 1, which is characterized in that step
3 calcination temperatures are 400-800 DEG C, and heating rate is 0.5-10 DEG C/min, calcination time 0.5-5h.
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| CN115634686B (en) * | 2022-09-09 | 2024-04-16 | 齐鲁工业大学 | Photocatalytic material MWO capable of responding to visible light and near infrared light and selectively degrading 4 Preparation method and application thereof |
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