CN109759147A - A kind of preparation that the molybdenum disulfide of core-shell structure coats polypyrrole nanocomposite and the application in dye wastewater treatment - Google Patents
A kind of preparation that the molybdenum disulfide of core-shell structure coats polypyrrole nanocomposite and the application in dye wastewater treatment Download PDFInfo
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Abstract
A kind of preparation method and dye wastewater degradation application of molybdenum disulfide cladding polypyrrole core-shell photocatalyst, are related to a kind of light-catalysed preparation method and applications of nanoparticle.Method: one, using pyrroles as raw material, polyvinyl alcohol is protective agent, Fe3+For catalyst, the synthetic solvent A by way of oxidation polymerization；It two, is that raw material is placed in polytetrafluoroethylene (PTFE) and is, then polytetrafluoroethylene (PTFE) pyroreaction kettle is put into baking oven and reacts to obtain solution B by solution A, sodium molybdate, thiocarbamide, hydroxylamine hydrochloride and F127 in the reaction kettle of liner by using a step hydro-thermal and oxidative polymerization method；Three, the solution for obtaining step 2 is fitted into centrifuge tube and is centrifuged 3 times, and removal supernatant leaves residue.Four, solution B is put into sample bottle, obtains the organic wastewater contaminant degradation material with photo-catalysis function.Cost of the invention is low, and catalyst is reusable, and low energy consumption, and secondary pollution is few, and degradation efficiency is close to 99.3%.The present invention is used for waste water from dyestuff contaminant degradation field.
Description
Technical field
Molybdenum disulfide of the present invention coats the preparation of the photochemical catalyst of polypyrrole core-shell structure and its in dye wastewater degradation
Application.
Background technique
Water is the important component of natural resources, is indispensable important substance money during the mankind depend on for existence and development
One of source.Said from global range, water is the tie for connecting all ecosystems, natural ecosystems not only can control the flowing of water but also
The purification and circulation of water can constantly be promoted.Therefore water in the natural environment, has for the existence of biology and the mankind and determines
The meaning of property.Currently, the freshwater resources total amount in China is 28000 billion cubic meters, the 6% of global water resources, water resource of per capita are accounted for
Only 2300 cubic metres, only the 1/4 of world average level, and China is the country that water consumption is most in the world, this causes
The water resource in China there is a serious shortage of.China realizes whole quickly development from after reforming and opening up to the outside world in national economy, however
In recent years, as dyestuff textile industry rapidly develops, the kind and quantity of dyestuff also increasingly increase, and various new dyes constantly go out
Existing, dyeing waste water has become one of important source of water pollution.Dyeing waste water water quality complexity, color are compared with deep, discharge amount is big, harm
Property it is strong and be difficult to degrade therefore very urgent for the improvement of Dying Wastewater Treatment &.
Pollution to natural water body, after dyeing waste water is discharged into natural water body, the water temperature of dyeing waste water is higher, usually 30~
40 DEG C, sometimes up to 50 DEG C or more, and large amount of organic can consume rapidly the dissolved oxygen in water body in water, produce river because of anoxic
Raw anaerobic digestion, the H released2S further consumes the dissolved oxygen in water body, dissolved oxygen sharp fall in water body.Waste water
Middle total phosphorus, total nitrogen content increase, and water eutrophication is made after discharge.Free chlorine in bleaching effluent may destroy or reduce river
Self-purification capacity.Heavy metal usually will form bed mud, endanger the growth of animals and plants in water.Dyeing waste-water colours river water, seriously
The natural ecology chain of water body is destroyed, while being greatly reduced the economic value of water body.Such chroma in waste water depth, organic pollutant
Content height, complicated components, change of water quality and the big difficult for biological degradation of bio-toxicity, the anti-light solution of dyestuff, inoxidizability are strong, and containing more
Kind has bio-toxicity or leads to the organic matter of " three cause " (carcinogenic, teratogenesis, mutagenesis) performance, is difficult to carry out with conventional method
Dirt brings serious pollution to environment.And dyeing waste water contains a large amount of organic pollutant, and dissolved oxygen will be consumed by being discharged into water body,
Ecology balance is destroyed, the existence of fish and other aquatiles is jeopardized.Demersal organic matter can be produced because of anaerobic digestion
The pernicious gases such as raw hydrogen sulfide, adverse condition.The most of all meta-alkalescences of dyeing waste water can make saline Land into farmland, into
Enter water body, the balance of water body but will be influenced.
Molybdenum disulfide has important application in the fields such as photoelectric conversion and catalysis as stratiform transient metal sulfide
Prospect.After the discovery and application of nano material based on by graphene, two-dimentional (2D) stratiform filtering metal sulfide due to
Their unique performances and wide potential application cause research interest in industry and scientific domain.At these two-dimentional (2D)
In stratified nano materials, molybdenum disulfide is sandwiched between two layers of six side's solid matter sulphur atoms by molybdenum atom and is formed, and is had many excellent
Performance, such as very high unsaturation, reactivity height.And many fields can be widely used in, for example are being catalyzed
It agent, hydrogen storage, solid super strong lubricant and solid field of lithium ion secondary and is gone as hydrodesulfurization, sulphur removal in petroleum
The catalyst of nitrogen.Therefore, a large amount of research for making great efforts be dedicated to molybdenum disulfide always.A large amount of two sulphur with different-shape
Change molybdenum nanostructure (nano particle, tiny balloon, nanotube, nanometer rods, nano wire, nano flower) by various methods, including
It is prepared by vapor- phase synthesis, electrochemical deposition, thermal decomposition, biochemical synthesis and hydro-thermal method.In these methods, due to hydrothermal synthesis
Route is at low cost, high-efficient and product well-crystallized, so it has been considered as one of most promising synthetic route so far
Until, the molybdenum disulfide nano material of the various forms prepared by hydro-thermal method is forward-looking in terms of photochemical catalyst to answer
With, but obtained molybdenum disulfide nano structure is usually irregular aggregated nanoparticles.Therefore, facing challenges still have
It is prepared in heterogeneous photochemical catalyst aspect in the molybdenum disulfide nano material with enhancing photocatalytic activity is foundation.
Summary of the invention
The present invention is to solve existing waste water from dyestuff pollutant deep purifying is expensive, it is difficult to recycle, deviate from efficiency
Low problem problem provides the preparation of the photochemical catalyst of molybdenum disulfide cladding polypyrrole core-shell structure and its in dye wastewater degradation
In application.
The preparation method of the photochemical catalyst of molybdenum disulfide cladding polypyrrole core-shell structure of the present invention, it is characterised in that this method
The following steps are included:
One, a certain amount of polyvinyl alcohol is dissolved in 30-50 ml deionized water, iron chloride is dissolved in 3-8 ml deionized water
In and ultrasonic dissolution mixing respectively, form uniform mixed solution, then pyrroles is instilled in mixed solution and stirs to get solution A；
Two, solution A and sodium molybdate, thiocarbamide, hydroxylamine hydrochloride and F127 that step 1 obtains are mixed in a certain proportion and are dissolved in 10-
25 ml deionized water ultrasonic dissolutions.The sample is placed in reaction kettle, certain time is reacted at a certain temperature and obtains solution B；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, after high speed centrifugation 3-5 times, removes supernatant to get to two sulphur
Change molybdenum and coats polypyrrole core-shell photocatalyst.
Further, ultrasonic power is 60 ~ 80 W in step 1.
Further, centrifugation rate described in step 3 is the r/min of 2000 r/min ~ 15000.
The photochemical catalyst of the molybdenum disulfide cladding polypyrrole core-shell structure of above method preparation is in dye wastewater degradation
Using.
The present invention can be achieved waste water from dyestuff contaminant degradation, and degradation efficiency is close to 99.3%.
The principle of the present invention:
The photochemical catalyst of molybdenum disulfide cladding polypyrrole core-shell structure mainly exists in dye wastewater degradation working principle in the present invention
Under the action of visible light luminous energy, molybdenum disulfide electronics from ground state transition to excitation state, shift electronics into polypyrrole core effectively
Prevent electronics-hole pair compound.Polypyrrole is met in air when coating molybdenum disulfide photocatalytic degradation methylene blue solution
Oxygen, oxygen is reduced into oxygen radical, and methylene blue solution is degraded by catalytic to carbon dioxide and water, nontoxic
It is discharged into air.This illustrates the core-shell structure prepared by us, the polypyrrole cladding two with dye wastewater degradation function
Molybdenum sulfide nanoparticle has high visible light catalysis activity, using methylene blue as the dye wastewater treatment application of representative
In, show very high degradation efficiency, degradation efficiency may be up to 99.3%.
Beneficial effects of the present invention:
For the method for the present invention using pyrroles as raw material, polyvinyl alcohol is protective agent, Fe3+For catalyst, the system by way of oxidation polymerization
Standby place's polypyrrole nanoparticle.Polypyrrole nanoparticle is coated by the molybdenum disulfide of the method synthesis core shell structure of hydrothermal synthesis
Son.Therefore, it can use the photochemical catalyst of molybdenum disulfide cladding polypyrrole core-shell structure of the invention to dye wastewater degradation.
The present invention is synthesized by one step hydro thermal method and oxidative polymerization method, and preparation method is simple, cost of material is low and source is wide
It is general, it is easy to operate.Since using pyrroles as raw material, polyvinyl alcohol is protective agent, Fe3+For catalyst, by way of oxidation polymerization
Polypyrrole nanoparticle at preparation.Using the polypyrrole nanoparticle prepared as raw material, pass through the method synthetic kernel of hydrothermal synthesis
The polypyrrole of shell structure coats molybdenum disulfide core-shell photocatalyst, and generating polypyrrole cladding molybdenum disulfide photochemical catalyst has
Good photocatalysis performance, therefore there is preferable degradation capability, degradation efficiency is up to 99.3%.Molybdenum disulfide packet indicated above
Polypyrrole core-shell photocatalyst is covered with good practicability and in wide application prospect.
Molybdenum disulfide prepared by this method coats the photochemical catalyst size uniformity of polypyrrole core-shell structure, dispersibility,
Synthetic method is simple, and raw material is cheap and easy to get, at low cost, and product obtained is nontoxic, has preferable photocatalysis performance, to environment
Waste water from dyestuff, which pollutes object, has degradation function.It has broad application prospects in environmental monitoring and improvement, technical field of material chemistry.
Detailed description of the invention
Fig. 1 is the TEM image for the photochemical catalyst that molybdenum disulfide prepared by embodiment 1 coats polypyrrole core-shell structure；
Fig. 2 is the XRD spectra for the photochemical catalyst that molybdenum disulfide prepared by embodiment 1 coats polypyrrole core-shell structure；
Fig. 3 is the FTIR spectrum figure for the photochemical catalyst that molybdenum disulfide prepared by embodiment 1 coats polypyrrole core-shell structure；
Fig. 4 is that molybdenum disulfide prepared by embodiment 1 coats the photochemical catalyst of polypyrrole core-shell structure in methylene blue dye wastewater
Photo in kind in processing；
Fig. 5 is the photochemical catalyst uv absorption spectra that molybdenum disulfide prepared by embodiment 1 coats polypyrrole core-shell structure.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: the preparation side of the photochemical catalyst of present embodiment molybdenum disulfide cladding polypyrrole core-shell structure
Method, it is characterised in that method includes the following steps:
One, a certain amount of polyvinyl alcohol is dissolved in 30-50 ml deionized water, iron chloride is dissolved in 3-8 ml deionized water
In and ultrasonic dissolution mixing respectively, form uniform mixed solution, then pyrroles is instilled in mixed solution and stirs to get solution A；
Two, solution A and sodium molybdate, thiocarbamide, hydroxylamine hydrochloride and F127 that step 1 obtains are mixed in a certain proportion and are dissolved in 10-
25 ml deionized water ultrasonic dissolutions, which is placed in reaction kettle, is reacted certain time at a certain temperature and is obtained solution B；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, after high speed centrifugation 3-5 times, removes supernatant to get to two sulphur
Change molybdenum and coats polypyrrole core-shell photocatalyst.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: oxidant species in step 1
Including iron chloride, ammonium persulfate, H2O2。
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: ultrasonic function in step 1
Rate is 60 ~ 100 W.Other are other the same as one or two specific embodiments.
Specific embodiment 4: present embodiment is unlike specific embodiment one to three: being mixed described in step 1
3-8 h, which is stirred at room temperature, in solution terminates.It is other identical as specific embodiment one to three.
Specific embodiment 5: present embodiment is unlike specific embodiment one to four: polyethylene in step 1
Alcohol and iron chloride mass ratio (1-5)；1.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: chlorine in step 1
Change iron and pyrroles mass ratio 1:(8-12).It is other identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: molybdenum in step 2
Sour sodium, thiocarbamide, hydroxylamine hydrochloride and F127 mass ratio (2-5)；(5-8)；(1-3)；1 it is other with specific embodiment one to six it
One is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: in step 2
15-48 h is reacted in 200 DEG C of heating.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: institute in step 2
Stating centrifugation rate is the r/min of 2000 r/min ~ 15000.It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: the photochemical catalyst of present embodiment polypyrrole cladding molybdenum disulfide core-shell structure is useless in dyestuff
Application in water degradation
It elaborates below to the embodiment of the present invention, following embodiment carries out reality under the premise of the technical scheme of the present invention
It applies, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1:
One, 0.5 g polyvinyl alcohol is dissolved in 35 ml deionized waters, 0.25 g iron chloride is dissolved in 5 ml deionized waters
And difference ultrasonic dissolution.It takes 5 ml ferric chloride solutions to be slowly dropped into poly-vinyl alcohol solution, forms uniform mixed solution, then will
2.7 ml pyrroles instill mixed solution, and 5 h of magnetic agitation obtains polypyrrole solution together；
Two, the solution A for obtaining step 1 takes 2.1 ml, with 0.03 g sodium molybdate, 0.06 g thiocarbamide, 0.02 g hydroxylamine hydrochloride with
And 0.01 g F127 be dissolved in 18 ml deionized water dissolvings, by the sample be placed in polytetrafluoroethylene (PTFE) be liner reaction kettle in, then
Reaction kettle is put into reaction synthesis polypyrrole cladding molybdenum disulfide core-shell nano in baking oven；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, and at 10000 r/min high speed centrifugation 3 times, removal supernatant is left
Residue；
Four, the solution B for obtaining step 2 takes 0.05ml, is dissolved in 10 ml deionized waters with 10 ml methylene blue solutions and prepares 12
It is carried out illumination observation methylene blue wastewater degradation situation by bottle under different time.
Fig. 1 is the images of transmissive electron microscope that molybdenum disulfide manufactured in the present embodiment coats polypyrrole core-shell photocatalyst；
As shown in Figure 2, the particle size of prepared molybdenum disulfide cladding polypyrrole core-shell nano is about 80 nm, and size compares
It is uniform, favorable dispersibility.
The XRD spectra of Fig. 2 molybdenum disulfide cladding polypyrrole core-shell photocatalyst manufactured in the present embodiment, it can be seen that
Prepared molybdenum disulfide cladding polypyrrole core-shell nano is almost the same with the peak of molybdenum disulfide, and the peak of polypyrrole is not examined
It measures.Illustrate that polypyrrole nanoparticle is coated completely by molybdenum disulfide.
Fourier's infrared spectrum of Fig. 3 molybdenum disulfide cladding polypyrrole core-shell photocatalyst manufactured in the present embodiment.
It can be seen that the infrared spectroscopy of molybdenum disulfide cladding polypyrrole core-shell nano is in 3423 cm-1With 3223 cm-For curing
The N-H stretching vibration of molybdenum, in 1640 cm-1With 1407 cm-1Place is the basic vibration of asymmetrical pyrrole ring and symmetrical pyrrole ring
It is dynamic, 1120 cm-1For the stretching vibration of C-N, 910 cm-1For C-N out-of-plane bending vibration.
The photochemical catalyst of Fig. 4 molybdenum disulfide cladding polypyrrole core-shell structure manufactured in the present embodiment is useless in methylene blue dye
Photo in kind in water process, it can be seen that with the increase of light application time, the color of sample bottle Methylene Blue (MB) solution
It is gradually becoming shallower as, when illumination reaches 60 minutes, methylene blue solution is degradable.
Fig. 5 the present embodiment prepares the uv absorption spectra of molybdenum disulfide cladding polypyrrole core-shell photocatalyst.It can
With find out the absorbance of methylene blue (MB) dyestuff in the corresponding absorbing wavelength of maximum for 675 nm, when different visible light illumination
Between under methylene blue (MB) dyestuff maximum absorption wavelength it is constant, and absorbance with the increase of photocatalytic degradation time and
It is gradually reduced.
Molybdenum disulfide cladding polypyrrole core-shell photocatalyst manufactured in the present embodiment has preferable degradation capability, drop
Efficiency is solved up to 99.3%.
Embodiment 2:
One, 0.3g polyvinyl alcohol is dissolved in 50 ml deionized waters, 0.1 g ammonium persulfate is dissolved in 8 ml deionized waters
And difference ultrasonic dissolution, it takes 5 ml ammonium persulfate solutions to be slowly dropped into poly-vinyl alcohol solution, forms uniform mixed solution, then
1 ml pyrroles is instilled mixed solution, and 4 h of magnetic agitation obtains polypyrrole solution together；
Two, the solution A for obtaining step 1 takes 2.1 ml, with 0.05 g sodium molybdate, 0.07 g thiocarbamide, 0.02 g hydroxylamine hydrochloride with
And 0.01 g F127 be dissolved in 15 ml deionized water dissolvings, by the sample be placed in polytetrafluoroethylene (PTFE) be liner reaction kettle in, then
Reaction kettle is put into baking oven and reacts to obtain molybdenum disulfide cladding polypyrrole core-shell nano；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, and at 8000 r/min high speed centrifugation 3 times, removal supernatant is left
Residue；
Four, the solution B for obtaining step 2 takes 0.03 ml, is dissolved in 10 ml deionized waters with 10 ml methylene blue solutions and prepares
12 bottles, it is carried out to illumination observation methylene blue wastewater degradation situation under different time.
The photochemical catalyst that the present embodiment prepares molybdenum disulfide cladding polypyrrole core-shell structure can realize waste water from dyestuff pollutant
Degradation, degradation efficiency is close to 99.1%.
Embodiment 3:
One, 0.4 g polyvinyl alcohol is dissolved in 30 ml deionized waters, 0.2 g H2O2It is dissolved in 6 ml deionized waters simultaneously
Ultrasonic dissolution respectively.Take 5 ml H2O2Solution is slowly dropped into poly-vinyl alcohol solution, forms uniform mixed solution, then by 2.1
Ml pyrroles instills mixed solution, and 6 h of magnetic agitation obtains polypyrrole solution together；
Two, the solution A for obtaining step 1 takes 2.1 ml, with 0.08 g sodium molybdate, 0.06 g thiocarbamide, 0.04 g hydroxylamine hydrochloride with
And 0.02 g F127 be dissolved in 20 ml deionized water dissolvings, by the sample be placed in polytetrafluoroethylene (PTFE) be liner reaction kettle in, then
Reaction kettle is put into baking oven and reacts to obtain molybdenum disulfide cladding polypyrrole core-shell nano；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, and at 13000 r/min high speed centrifugation 3 times, removal supernatant is left
Residue；
Four, the solution B for obtaining step 2 takes 0.05 ml, is dissolved in 10 ml deionized waters with 10 ml methylene blue solutions and prepares
12 bottles, it is carried out to illumination observation methylene blue wastewater degradation situation under different time.
The photochemical catalyst that the present embodiment prepares molybdenum disulfide cladding polypyrrole core-shell structure can realize waste water from dyestuff pollutant
Degradation, degradation efficiency is close to 99.2%.
Claims (10)
1. a kind of preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst, it is characterised in that this method include with
Lower step:
One, a certain amount of polyvinyl alcohol is dissolved in 30-50 ml deionized water, iron chloride is dissolved in 3-8 ml deionized water
In and ultrasonic dissolution mixing respectively, form uniform mixed solution, then pyrroles is instilled in mixed solution and stirs to get solution A；
Two, solution A and sodium molybdate, thiocarbamide, hydroxylamine hydrochloride and F127 that step 1 obtains are mixed in a certain proportion and are dissolved in 10-
25 ml deionized water ultrasonic dissolutions, which is placed in reaction kettle, is reacted certain time at a certain temperature and is obtained solution B；
Three, the solution for obtaining step 2 is fitted into centrifuge tube, after high speed centrifugation 3-5 times, removes supernatant to get to two sulphur
Change molybdenum and coats polypyrrole core-shell photocatalyst.
2. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
Be: oxidant species described in step 1 include iron chloride, ammonium persulfate, H2O2。
3. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
Be: ultrasonic power is 60 ~ 100 W in step 1.
4. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
Be: mixed solution is stirred at room temperature 3-8 h and terminates in step 1.
5. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
It is: polyvinyl alcohol and iron chloride mass ratio (1-5) in step 1: 1.
6. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
It is: iron chloride and pyrroles's mass ratio 1 in step 1；(8-12).
7. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
It is: the mass ratio (2-5) of sodium molybdate, thiocarbamide, hydroxylamine hydrochloride and F127 in step 2: (5-8): (1-3): 1.
8. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
It is: reacts 15-48 h in 200 DEG C of heating in step 2.
9. the preparation method of molybdenum disulfide cladding polypyrrole core-shell photocatalyst according to claim 1, feature
Be: centrifugation rate described in step is the r/min of 2000 r/min ~ 15000.
10. the molybdenum disulfide cladding polypyrrole core-shell photocatalyst of method preparation as described in claim 1 is in waste water from dyestuff
Application in degradation.
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Application publication date: 20190517 |