CN104353469B - A kind of preparation method and application of nano composite material photocatalyst - Google Patents
A kind of preparation method and application of nano composite material photocatalyst Download PDFInfo
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Abstract
The invention belongs to technical field of environmental material preparation, a kind of preparation method and applications of nano composite material photocatalyst are refered in particular to.Weigh graphene oxide to be placed in a certain amount of deionized water, be added separately in graphene oxide solution for caddy and zinc chloride to being completely dissolved by ultrasonic vibration, L cysteines are added after stirring and dissolving and continues to stir to being completely dissolved；Then pH=7 is adjusted with sodium hydroxide solution, adds vulcanized sodium then to lead to the 15min of nitrogen gas stirring 10, above-mentioned solution is poured into autoclave, natural cooling is taken out after being subsequently placed to high temperature oven insulation；To reacted solution centrifugal, washing, grinding obtains CdS/ZnS nano composite materials load graphene oxide photochemical catalyst after drying.CdS/ZnS nano composite materials that the present invention is prepared load graphene oxide photochemical catalyst, effectively can be degraded tetracycline using visible ray in antibiotic waste water.
Description
Technical field
The invention belongs to technical field of environmental material preparation, it is related to the synthesis of graphene oxide and hydro-thermal method synthesis CdS/
ZnS nano composite materials load redox graphene photochemical catalyst and its application.
Background technology
Antibiotic (Antibiotics) is the chemical substance produced by certain micro-organisms or animals and plants, can suppress microorganism
The material bred with other cells, is widely used in the various bacterium infections for the treatment of or suppresses the medicine of pathogenic microorganism infection.Due to
The irrational utilization of antibiotic medicine, larger harm is generated to environment, by taking tetracycline antibiotic as an example, many research reports
Show that antibiotic has been widely present in soil, surface water, underground water, deposit, municipal sewage and animal excrements oxidation pond；
Therefore, it has been that researcher is compeled to eliminate the problems such as environmental pollution for bringing of antibiotic residue and food chain product safety in environment
Be essential the significant problem to be solved, and the means of current wastewater treatment mainly have Physical, chemical method, biochemical process etc., but many
Many wastewater processing technologies or to there is operating cost high or the shortcomings of with secondary pollution so that treatment effect is unsatisfactory.
Conductor photocatalysis degradation technique is a kind of high-level oxidation technology, is a kind of most possible using nature sunshine
The environmentally-friendly technique of cleaning decontamination is realized, people has been turned at present and has been paid close attention to more method of wastewater treatment；In numerous photocatalysis
With TiO in semi-conducting material2Photochemical catalyst has the advantages that cheap, non-secondary pollution, is described as environment-friendly pollution treatment
Material, is widely paid close attention in environmental protection and the application prospect of energy-conservation, its be mainly used in waste water, exhaust-gas treatment and antibacterial, oneself
The fields such as the exploitation of cleaning products；But TiO2Itself there is also limitation, and such as its light absorbs threshold value is confined to ultraviolet region, light
Quantum efficiency lacks selectivity etc. than relatively low, photocatalytic degradation, therefore, in recent years with visible light-responded ability is strong, photocatalysis
The focus for being developed into research of the novel photocatalyst of high, the selective degradation capability of activity.
Graphene oxide (Graphene Oxide), is the derivative of graphene functionalized, it may also be said to be graphite oxide
The mono-layer graphite oxide thin slice obtained by mechanical stripping, the structure of graphene oxide is similar with Graphene, close to plane and is in
Existing two-dimensional network structure, except that, surface of graphene oxide has various oxy radicals, such as C=O, C-OOH, C-OH etc.,
These groups appear in surface and the interlayer of graphite flake, wherein substantial amounts of hydroxyl and epoxy after flaky graphite is oxidized treatment
Group is present in plane, and has a small amount of carboxyl, carbonyl, phenylol, ester group and quinonyl to be distributed in the edge of lamella；By
In having substantial amounts of oxy radical on surface, graphene oxide has more preferable hydrophily than Graphene, can permitted well
Dispersion is particularly in water in many solution, thus can be used to carry out load matrix.
Cadmium sulfide (CdS) is a kind of more typical II-VI piezoelectric semiconductor of race and semiconductor photosensitive material, with larger
Band gap width (about 2.45eV), is also a kind of good solar cell window material and nonlinear optical material, because it has
Excellent optics, electrical properties, be widely used in various luminescent devices, photovoltaic device, optical detector, light sensor with
And the field such as photocatalysis, but the photoetches that have of CdS in itself limit its and apply；ZnS is II-VI group wide bandgap semiconductor
Compound-material, its Emission in Cubic energy gap 3.7eV, hexagonal phase energy gap is 3.8eV.
Obtained CdS/ZnS nano composite materials load redox graphene photochemical catalyst catalyst, side in the present invention
Method is simple to operate, effectively reduces photoetch, and have preferable degradation effect to Fourth Ring while to improve catalyst steady
It is qualitative, and prepared photochemical catalyst have good degradation effect to Fourth Ring.
The content of the invention
The present invention includes two parts, is respectively that the synthesis and the load of CdS/ZnS nano composite materials of graphene oxide are gone back
The synthesis of former graphene oxide photochemical catalyst.
The present invention is carried out according to the following steps；
(1) synthesis of graphene oxide：Delay under stirring condition to native graphite and sodium nitrate, ice bath is added in the concentrated sulfuric acid
It is slow to add potassium permanganate, it is kept stirring for 2h at 0-20 DEG C；Then 35 DEG C of stirrings of heating water bath, set to distilled water is added in solution
Water bath heating temperature is 98 DEG C of holding 40min；It is slowly anti-to distilled water termination is continuously added in solution while stirring after end
Should, the aqueous hydrogen peroxide solution that mass concentration is 30% is subsequently adding, stand, supernatant is outwelled, press 1 with concentrated hydrochloric acid and water：10
Volume ratio mixing mixed liquor washing, stir 20-40min, stand, outwell supernatant, and be washed with distilled water to neutrality, put
It is placed in vacuum drying oven and is dried to obtain graphene oxide.
(2) CdS/ZnS nano composite materials load the synthesis of redox graphene photochemical catalyst：Weigh graphene oxide
It is placed in a certain amount of deionized water, be added separately to for caddy and zinc chloride to aoxidize stone to being completely dissolved by ultrasonic vibration
In black alkene solution, Cys are added after stirring and dissolving and continues to stir to being completely dissolved；Then adjusted with sodium hydroxide solution
Section pH=7, adds vulcanized sodium then to lead to nitrogen gas stirring 10-15min, and above-mentioned solution is poured into autoclave, is subsequently placed with
Natural cooling is taken out after high temperature oven is incubated；To reacted solution centrifugal, washing, grinding obtains CdS/ZnS and receives after drying
Nano composite material loads redox graphene photochemical catalyst.
The mass ratio of potassium permanganate, aqueous hydrogen peroxide solution, the concentrated sulfuric acid, sodium nitrate and native graphite in step (1) is
4:10:30:2.5:1, the distilled water for adding for the first time is 10 with the mass ratio of potassium permanganate:1, second distilled water for adding with
The mass ratio of potassium permanganate is 35:1.
The consumption of deionized water described in step (2) is so that caddy, zinc chloride, Cys, graphene oxide, sulphur
Change sodium to be completely dissolved.
Optimal graphene oxide, caddy, zinc chloride, Cys, vulcanized sodium mass ratio are 6.5- in step (2)
26.25:104:62:439:219, preferred proportion 19.75：104:62:439:219.
Sodium hydroxide solution described in step (2) is that concentration is 1mol/L.
It is positioned over after being incubated in high temperature oven to take out described in step (2) and refers to and be incubated 1h in 180 DEG C.
Washing described in step (2) refer to respectively with deionized water and absolute ethanol washing twice.
Drying described in step (2) is 50 DEG C of drying 6h.
The CdS/ZnS nano composite materials obtained according to preparation method of the present invention load redox graphene light
Catalyst, and its degraded tetracycline antibiotic application.
Chemicals used is and analyzes pure in the present invention, wherein graphite powder, and sodium nitrate, potassium permanganate, the concentrated sulfuric acid is purchased
In traditional Chinese medicines chemical reagent Co., Ltd；Caddy, zinc chloride, vulcanized sodium is purchased from Aladdin chemical reagent Co., Ltd；Tetracycline
Antibiotic is mark product, is purchased from Shanghai along vigorous bioengineering Co., Ltd.
Beneficial effects of the present invention：
It is catalyst degradation antibiotic that the present invention is realized with CdS/ZnS nano composite materials load redox graphene
The purpose of waste water.Semi-conducting material is used as photochemical catalyst, it is seen that light as exciting, by the interface phase interaction with contaminant molecule
With special catalysis or conversion effet is realized, the oxygen of surrounding and hydrone is set to be excited into the free anion of great oxidizing force,
So as to reach the purpose of harmful organic substances in degraded environment, the method does not result in the formation of the wasting of resources and additional pollution,
And it is easy to operate, it is a kind of efficient process technology of environmental protection.
Brief description of the drawings
Fig. 1 is graphene oxide, CdS, ZnS, CdS/ZnS and CdS/ZnS nano composite material load oxygen reduction fossil
The XRD of black alkene photochemical catalyst.
Fig. 2 schemes for the TEM of redox graphene-CdS/ZnS；A, graphene oxide TEM scheme；B, c, reduction-oxidation graphite
The TEM figures of alkene-CdS/ZnS；E, d, are the HRTEM figures of redox graphene-CdS/ZnS.
Fig. 3 is graphene oxide, redox graphene-CdS/ZnS, the fluorescence emission spectrum of CdS/ZnS.
Fig. 4 is the contrast schematic diagram of the degraded tetracycline of the redox graphene of CdS/ZnS load different contents.
Fig. 5 is contrast schematic diagram of the different photochemical catalysts to tetracycline degradation behavior.
Fig. 6 is redox graphene-CdS/ZnS photochemical catalyst recovery experiment schematic diagrames.
Specific embodiment
Photocatalytic activity evaluation：Carried out in DW-01 type photochemical reactions instrument (being purchased from city Co., Ltd of Yangzhou University), can
See light light irradiation, by 100mL tetracyclines simulated wastewater add reactor in and determine its initial value, be subsequently adding composite photocatalyst
Agent, magnetic agitation and open aerator be passed through air maintain the catalyst in suspension or afloat, in During Illumination be spaced
10min sampling analyses, take supernatant liquor in spectrophotometer λ after centrifugationmaxMensuration absorbance at=278nm, and by public affairs
Formula：
DR=[(A0-Ai)/A0] × 100%
Calculate degradation rate, wherein A0To reach the absorbance of occrycetin solution during adsorption equilibrium, AiFor timing sampling is surveyed
The absorbance of fixed occrycetin solution.
With reference to specific implementation example, the present invention will be further described.
Embodiment 1：
The preparation of graphene oxide：
1g native graphites and 2.5g sodium nitrate, ice bath, under stirring condition are added in the there-necked flask for filling the 30g concentrated sulfuric acids
4g potassium permanganate is slowly added to, 2h is kept under conditions of 15 DEG C.Then 35 DEG C of stirring 30min solution of heating water bath are changed into blackish green
Color has bubble formation simultaneously, in solution add 40ml distilled water and set water bath heating temperature for 98 DEG C keep 40min, solution
It is changed into khaki；After end, while stirring slowly in solution add 140ml distilled water terminating reactions, be subsequently adding 10g,
30% aqueous hydrogen peroxide solution, solution is changed into golden yellow, stands, and outwells supernatant, and 1 is pressed with concentrated hydrochloric acid and water:10 volume
Than the mixed liquor washing for mixing, 30min is stirred, stood, outwell supernatant, and be washed with distilled water to neutrality, be positioned over vacuum
Oven drying obtains graphene oxide.
Embodiment 2：
(1) weigh obtained graphene oxide 0.0026g in embodiment 1 and add deionized water ultrasonic vibration to completely molten
Solution, forms uniform solution；0.0416g caddies and 0.0248g zinc chloride are added, is stirred to after being completely dissolved, add 0.1756g
Cys are stirred to being completely dissolved, and adjust the pH=7 of solution with the sodium hydroxide solution of 1mol/L after being sufficiently stirred for, then
0.0876g vulcanized sodium is added in above-mentioned solution, nitrogen gas stirring 15min is passed through, 180 DEG C of guarantors in 50mL autoclaves are poured into
Warm 1h, takes out natural cooling, by the solution centrifugal after cooling, washs and is put into vacuum drying chamber and ground in after 6h drying in 50 DEG C
Mill obtains CdS/ZnS nano composite materials load redox graphene photochemical catalyst.
(2) sample carries out photocatalytic degradation experiment in 0.05g photochemical reaction instrument in taking (1), measures the photochemical catalyst
Degradation rate to 10mg/L tetracycline antibiotics reaches 79.89% in 60min.
Embodiment 3：
By the step in embodiment 2, unlike choose amount 0.0053g of graphene oxide in (1), wherein caddy,
Zinc chloride, Cys, the mass conservation of vulcanized sodium, reaction take out natural cooling after terminating, by the solution centrifugal after cooling,
Wash and be put into and obtain photochemical catalyst after drying grinding in vacuum drying chamber.
(2) sample 0.05g carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures obtained light and urges
Agent reaches 82.06% to the degradation rate of 10mg/L tetracycline antibiotics in 60min.
Embodiment 4：
By the step in embodiment 2, the difference is that graphene oxide 0.0079g is chosen in (1) prepares catalyst, take out certainly
So cooling, by the solution centrifugal after cooling, to wash and is put into and obtain photochemical catalyst after drying grinding in vacuum drying chamber.
(2) sample 0.05g carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures obtained light and urges
Agent reaches 87.08% to the degradation rate highest of 10mg/L tetracycline antibiotics in 60min.
Embodiment 5：
By the step in embodiment 2, unlike in (1) graphene oxide be 0.0105g, photocatalytic synthesis into and it is other
Condition does not change.
(2) sample 0.05g carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures the photochemical catalyst
Degradation rate to 15mg/L tetracycline antibiotics reaches 74.97% in 60min.
Embodiment 6：
By the step in embodiment 2, unlike be not added with graphene oxide in (1), photocatalytic synthesis into and other condition
Do not change.
(2) sample 0.05g carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures the photochemical catalyst
69.59% is reached in 60min to the degradation rate to 10mg/L tetracycline antibiotics.
Embodiment 7：
(1) 0.08332g caddies are added in deionized water, are stirred to after being completely dissolved, add 0.1756g L- half
Cystine adjusts the pH=7 of solution with the sodium hydroxide solution of 1mol/L after being sufficiently stirred for, then add 0.0876g vulcanized sodium
To in above-mentioned solution, nitrogen gas stirring 15min is passed through, pours into 180 DEG C of insulation 1h in 50mL autoclaves, take out natural cooling,
By the solution centrifugal after cooling, wash and be put into and dried in 6h in 50 DEG C in vacuum drying chamber, obtain CdS photochemical catalysts.
(2) sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures and deserves photochemical catalyst consumption
Degradation rate during for 0.05g to 10mg/L tetracycline antibiotics reaches 60.74% in 60min.
Embodiment 8：
(1) by 0.0497g zinc chloride addition deionized water, stir to after being completely dissolved, add the Guangs of 0.1756g L- half
Propylhomoserin adjusts the pH=7 of solution with the sodium hydroxide solution of 1mol/L after being sufficiently stirred for, be then added to 0.0876g vulcanized sodium
In above-mentioned solution, nitrogen gas stirring 15min is passed through, pours into 180 DEG C of insulation 1h in 50mL autoclaves, take out natural cooling, will
Solution centrifugal after cooling, washs and is put into and dried in 6h in 50 DEG C in vacuum drying chamber, obtains ZnS photochemical catalysts.
(2) sample 0.05g carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (1), measures the photochemical catalyst
Degradation rate to 10mg/L tetracycline antibiotics reaches 17.86% in 60min.
Fig. 1 is graphene oxide, CdS, ZnS, CdS/ZnS and CdS/ZnS nano composite material load oxygen reduction fossil
The XRD of black alkene photochemical catalyst, the characteristic peak for presenting each material that be will be apparent that in figure；As shown in Figure 1, resulting CdS/
The characteristic peak of ZnS heterojunction structures is fairly obvious, and peak sharply has no any miscellaneous peak explanation product crystallinity and purity is all higher, and goes back
Disappear at the peak that former graphene oxide-CdS/ZnS characteristic peaks substantially weaken even GO, it may be possible to going back in due to course of reaction
Former agent and water-heat process, promote graphene oxide to be changed into redox graphene, while also causing the peak of CdS/ZnS to weaken.
The TEM figure .a. graphene oxides TEM figure b of Fig. 2 redox graphenes-CdS/ZnS, c. redox graphenes-
The TEM figures e, d. of CdS/ZnS schemes for the HRTEM of redox graphene-CdS/ZnS；It can be seen that graphene oxide from a figures
Slabbing structure, and the presence of pleated structure illustrates that graphene oxide has preferable elasticity, be can be seen that from b figures
CdS/ZnS is evenly distributed on redox graphene surface, and granular size is homogeneous, and HRTEM shows CdS/ZnS hetero-junctions
Substantially, (101) crystal face of wherein CdS and (111) crystal face of ZnS overlap the spacing of lattice of structure, it was demonstrated that the presence of heterojunction structure.
Fig. 3 is graphene oxide, redox graphene-CdS/ZnS, the fluorescence emission spectrum of CdS/ZnS；Can from figure
To find out the fluorescence intensity reduction due to the presence CdS/ZnS heterojunction structures of redox graphene, oxygen reduction fossil is illustrated
Black alkene prevents the compound of wherein electron hole pair to a certain extent, improves the ability of the anti-light corrosion of photochemical catalyst.
Fig. 4 is the degraded tetracycline spectrogram of the graphene oxide of CdS/ZnS load different contents；As can be seen from the figure with
The increase of graphene oxide amount in preparation process, degradation efficiency first increases and subtracts afterwards, wherein being 0.0079g in graphene oxide content
When, degradation effect is best.
Fig. 5 is degradation behavior contrast schematic diagram of the different catalysts to tetracycline；Known by figure, CdS/ZnS nano materials pair
The degradation efficiency of tetracycline apparently higher than CdS, ZnS, and with graphene oxide in preparation process addition degradation efficiency more
Height, while also illustrate that the formation of the CdS/ZnS heterojunction structures of non-composite reduction graphene oxide.
Fig. 6 is redox graphene-CdS/ZnS photochemical catalyst recovery experiment schematic diagrames；By 5 circulation and stress realities
Test, the efficiency of photochemical catalyst illustrates that the stability of redox graphene-CdS/ZnS photochemical catalysts is preferable without substantially reduction.
Claims (11)
1. a kind of preparation method of nano composite material photocatalyst, it is characterised in that step is as follows：Graphene oxide is weighed to put
In a certain amount of deionized water, caddy and zinc chloride are added separately to graphene oxide by ultrasonic vibration to being completely dissolved
Cys are added in solution, after stirring and dissolving to continue to stir to being completely dissolved；Then pH is adjusted with sodium hydroxide solution
=7, add vulcanized sodium then to lead to nitrogen gas stirring 10-15min, above-mentioned solution is poured into autoclave, it is subsequently placed to height
Natural cooling is taken out after warm baking oven insulation；To reacted solution centrifugal, washing, grinding obtains CdS/ZnS nanometers again after drying
Condensation material loads redox graphene photochemical catalyst.
2. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：The oxidation
The synthetic method of Graphene is as follows：To native graphite and sodium nitrate, ice bath is added in the concentrated sulfuric acid height is slowly added under stirring condition
Potassium manganate, 2h is kept stirring at 0-20 DEG C；Then 35 DEG C of stirrings of heating water bath, heating water bath is set to distilled water is added in solution
Temperature is 98 DEG C of holding 40min；After end, while stirring slowly to continuously adding distilled water terminating reaction, Ran Houjia in solution
Enter the aqueous hydrogen peroxide solution that mass concentration is 30%, stand, outwell supernatant, 1 is pressed with concentrated hydrochloric acid and water：10 volume ratio is mixed
The mixed liquor washing of conjunction, stirs 20-40min, stands, and outwells supernatant, and is washed with distilled water to neutrality, is positioned over vacuum baking
Case is dried to obtain graphene oxide.
3. a kind of preparation method of nano composite material photocatalyst as claimed in claim 2, it is characterised in that：The Gao Meng
The mass ratio of sour potassium, aqueous hydrogen peroxide solution, the concentrated sulfuric acid, sodium nitrate and native graphite is 4:10:30:2.5:1, add for the first time
The mass ratio of distilled water and potassium permanganate be 10:1, the distilled water and the mass ratio of potassium permanganate that second adds are 35:1.
4. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：It is described go from
The consumption of sub- water is so that caddy, zinc chloride, Cys, graphene oxide, vulcanized sodium are completely dissolved.
5. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：Graphite oxide
Alkene, caddy, zinc chloride, Cys, vulcanized sodium mass ratio are 6.5-26.25:104:62:439:219.
6. a kind of preparation method of nano composite material photocatalyst as claimed in claim 5, it is characterised in that：Graphite oxide
Alkene, caddy, zinc chloride, Cys, vulcanized sodium mass ratio are 19.75：104:62:439:219.
7. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：The hydrogen-oxygen
The concentration for changing sodium solution is 1mol/L.
8. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：The placement
Taken out after being incubated in high temperature oven and referred in 180 DEG C of insulation 1h.
9. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：Described washes
Wash finger and use deionized water and absolute ethanol washing twice respectively.
10. a kind of preparation method of nano composite material photocatalyst as claimed in claim 1, it is characterised in that：Described
It is 50 DEG C of drying 6h to dry.
Nano composite material photocatalyst prepared by 11. preparation methods as claimed in claim 1 is in tetracycline antibiotic of degrading
Application.
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| US20140174905A1 (en) * | 2012-12-20 | 2014-06-26 | Sunpower Technologies Llc | Photo-catalytic systems for the production of hydrogen |
| CN103316694A (en) * | 2013-07-11 | 2013-09-25 | 吉林大学 | Preparation method of composite material of Zn0.8Cd0.2S and graphene |
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| CN108686681A (en) * | 2018-05-14 | 2018-10-23 | 南昌航空大学 | A kind of graphene/ZnS-MoS with visible light catalysis activity2Nano Solid Solution photochemical catalyst |
| CN108686681B (en) * | 2018-05-14 | 2021-05-28 | 南昌航空大学 | graphene/ZnS-MoS with visible light catalytic activity2Nano solid solution photocatalyst |
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