CN106540717A - A kind of hydro-thermal method synthesizes recyclable CdS/CoFe2O4The preparation method and its usage of/rGO composite photo-catalysts - Google Patents
A kind of hydro-thermal method synthesizes recyclable CdS/CoFe2O4The preparation method and its usage of/rGO composite photo-catalysts Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 16
- 229910002518 CoFe2O4 Inorganic materials 0.000 claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002351 wastewater Substances 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 30
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 229910003321 CoFe Inorganic materials 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000004098 Tetracycline Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 229960002180 tetracycline Drugs 0.000 claims description 4
- 229930101283 tetracycline Natural products 0.000 claims description 4
- 235000019364 tetracycline Nutrition 0.000 claims description 4
- 150000003522 tetracyclines Chemical class 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 4
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 3
- 239000004201 L-cysteine Substances 0.000 claims description 3
- 235000013878 L-cysteine Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 abstract description 15
- 230000015556 catabolic process Effects 0.000 abstract description 12
- 238000006731 degradation reaction Methods 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 14
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 10
- 239000003643 water by type Substances 0.000 description 10
- 238000006552 photochemical reaction Methods 0.000 description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 7
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229960003405 ciprofloxacin Drugs 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- -1 Caddy (Cleary) Chemical compound 0.000 description 1
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 1
- 150000008538 L-cysteines Chemical class 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000002223 anti-pathogen Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/049—Sulfides with chromium, molybdenum, tungsten or polonium with iron group metals or platinum group metals
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a kind of hydro-thermal method synthesizes recyclable CdS/CoFe2O4The preparation method and its usage of/rGO composite photo-catalysts, the preparation method include：Step 1, prepare graphite oxide GO；Step 2, preparation CoFe2O4；Step 3, preparation CdS/CoFe2O4/ rGO composite photo-catalysts.Present invention achieves with CdS/CoFe2O4Purposes of/the rGO for catalyst degradation antibiotic waste water.
Description
Technical field
The invention belongs to technical field of environmental material preparation, is related to a kind of hydro-thermal method and synthesizes recyclable CdS/CoFe2O4/rGO
The preparation method and its usage of composite photo-catalyst.
Background technology
Antibiotic (Antibiotics) is that had by antibacterial, mycete or other microorganisms are produced in life process
One class material of antipathogen or other activity, is widely used in the various bacterium infections for the treatment of or suppresses the medicine of pathogenic microorganism infection
Thing.In recent years, the species of antibiotic, yield and consumption are continuously increased, serious to the irrational utilization phenomenon of antibiotic medicine, give
Environment brings larger harm.By taking Ciprofloxacin as an example, many research reports show that antibiotic has been widely present soil, earth's surface
In water, subsoil water, deposit, municipal sewage and animal excrements oxidation pond.Therefore, in eliminating environment, antibiotic remainss bring
Environmental pollution and be researcher significant problem in the urgent need to address the problems such as food chain product safety.
CdS can directly absorb ripple as a kind of most important its energy gap of semi-conducting material about 2.4eV of II-VI group
The long visible ray less than 550nm, is widely used in preparing many fields such as photocell, photoconductive resistance and solaode.Together
When, it has fabulous photocatalysis performance, in visible ray of the wavelength less than 500nm, it is possible to use CdS produce a large amount of electronics and
There is redox reaction in hole, Some Organic Pollutants can be oxidized to carbon dioxide, water and inorganic salt etc..But due to electronics
The quick of hole pair is combined so as to which application is restricted.In order to solve the problems, such as that carrier is easily compound, CdS is partly led with other
It is a kind of effective solution that body is combined.Existing report (Huo P W, Tang Y F, Zhou M J et
al.Fabrication of ZnWO4-CdS heterostructure photocatalysts for visible light
induced degradation of ciprofloxacin antibiotics.J.Ind.Eng.Chem.,2016,37:340-
346), by hydro-thermal method by CdS and ZnWO4Heterojunction structure is formed, effectively control electron-hole pair is compound, improves light
Catalysis activity；(Zhou P P,Le Z G,Xie Y et al.Studies on facile synthesis and
properties of mesoporous CdS/TiO2composites for photocatalysis
applications.J.Alloy.Compd.,2017,692:170-177), CdS is synthesized by simple two steps sol-gal process
With TiO2Hetero-junctions effectively inhibits the compound of electron-hole pair while decreasing the photoetch of CdS.But due to TiO2Forbidden band
Width can not make full use of solar energy greatly, and research finds CoFe2O4With suitable energy gap, and there is good magnetic to have
Beneficial to the recycling of photocatalyst, it is most important that CdS and CoFe2O4Hetero-junctions can be formed and effectively reduce carrier
Compound raising photocatalytic activity.We as the receiver of electronics and pass loser by the use of rGO, have been greatly reduced electron hole
To recombination rate.Therefore, CdS/CoFe2O4The waste water that/rGO composite photo-catalysts come in processing environment is a kind of more satisfactory
Material.
The content of the invention
The purpose of the present invention is to prepare CdS/CoFe by technological means of hydro-thermal method2O4/ rGO composite photo-catalysts.
The present invention is achieved through the following technical solutions：
A kind of hydro-thermal method synthesizes recyclable CdS/CoFe2O4The preparation method of/rGO composite photo-catalysts, in accordance with the following steps
Carry out：
Step 1, prepare graphite oxide GO；
Step 2, preparation CoFe2O4：
By Fe (NO3)3·9H2O、Co(NO3)2.6H2O is stirred in being added to ethylene glycol, stirs to after being completely dissolved addition
PVP is uniformly mixing to obtain mixed liquor A, and solution is transferred in reactor carries out constant temperature thermal response；After reaction terminates, room is dropped to
Temperature, then solid matter with deionized water, washing with alcohol dry, CoFe is obtained2O4, it is standby；
Step 3, preparation CdS/CoFe2O4/ rGO composite photo-catalysts (rGO is redox graphene)：
By CdCl2·2.5H2O and L-Cysteine dissolving in deionized water and are stirred to being completely dissolved and obtain mixed liquor
B；Adjust the pH of mixed liquid B again with sodium hydroxide solution, then GO, CoFe are added in mixed liquid B2O4Continue to stir, then
Add Na2S·9H2O is simultaneously uniformly mixing to obtain mixed liquor C, and subsequently, solution is transferred in reactor carries out constant temperature thermal response；Instead
After should terminating, with Magnet by precipitate and solution separating, washing with alcohol precipitate is used, dry in being put into vacuum drying oven, obtain
CdS/CoFe2O4/ rGO composite photo-catalysts.
In step 2, when preparing mixed liquor A, the Fe (NO for being used3)3·9H2O、Co(NO3)2.6H2O, ethylene glycol and PVP
Amount ratio be 0.0646g：0.0233g：40mL：0.005g.
In step 2, the temperature of described constant temperature thermal response is 240 DEG C, and the response time is 24h.
In step 3, when preparing mixed liquid B, the CdCl for being used2·2.5H2O, L-Cysteine, the consumption of deionized water
Than for 0.1833g：0.1756g：40mL.
In step 3, the concentration of the sodium hydroxide solution for being used is 0.1mol/L, and the pH for being adjusted is 5～8.
In step 3, when preparing mixed liquor C, GO, the CoFe for being used2O4With Na2S·9H2O mass ratioes are 2～10：10～
30：9.
In step 3, the temperature of described constant temperature thermal response is 180 DEG C, and the response time is 2h.
Prepared CdS/CoFe2O4In/rGO composite photo-catalysts, the mass fraction of rGO is 10～50%, CoFe2O4/
The mass fraction of rGO is 20～90%.
Prepared CdS/CoFe2O4/ rGO composite photo-catalysts, for the tetracycline in degrading waste water.
Photocatalytic activity evaluation：Carry out in DW-01 type photochemical reaction instrument (being purchased from Educational Instrument Factory of Yangzhou University), can
See light light irradiation, 100mL Ciprofloxacin simulated wastewater is added in reactor and its initial value is determined, complex light is subsequently adding and is urged
Agent, magnetic agitation and open aerator be passed through air maintain the catalyst in suspension or afloat, in the middle of During Illumination
Every 10min sample analysis, the supernatant is taken after centrifugation in spectrophotometer λmaxMensuration absorbance at=358nm, and pass through
Formula：DR=[(A0-Ai)/A0] × 100% calculates degradation rate, wherein A0To reach the extinction of tetracycline during adsorption equilibrium
Degree, AiThe absorbance of the tetracycline determined for timing sampling.
Cabaltous nitrate hexahydrate used in the present invention, Fe(NO3)39H2O, nine hydrated sulfuric acid sodium, sodium acetate, sodium hydroxide,
Caddy (Cleary), PVP, L-Cysteine salt is analyzes pure, is purchased from traditional Chinese medicines chemical reagent company limited；Tetracycline antibiotic is mark
Product, are purchased from Shanghai along vigorous biological engineering company limited.
Beneficial effect：
Present invention achieves with CdS/CoFe2O4Purposes of/the rGO for catalyst degradation antibiotic waste water.Semi-conducting material is made
For photocatalyst, it is seen that light realizes special catalysis or conversion by the interfacial interaction with contaminant molecule as exciting
Effect, makes the oxygen and hydrone of surrounding be excited into the free anion of great oxidizing force, is harmful in degraded environment so as to reach
The purpose of organic substance, the method do not result in the formation of the wasting of resources and additional pollution, and easy to operate, are a kind of green rings
The efficient process technology of guarantor.
Description of the drawings
Fig. 1 is CdS/CoFe2O4/ rGO composite photo-catalyst photocatalysis fluorograms, wherein figure A is Solid fluorescene spectrum,
Figure B is transient state fluorescence spectrum, and illustration is solid fluorescence decaying kinetics zoomed-in view；
Fig. 2 is CdS/CoFe2O4The hysteresis curve figure of/rGO composite photo-catalysts, illustration is CdS/CoFe2O4/ rGO successes
Schematic diagram is separated by external magnetic field；
Fig. 3 is CdS/CoFe2O4The stability degraded figure of/rGO composite photo-catalysts.
Specific embodiment
With reference to example is embodied as, the present invention will be further described.
Embodiment 1：
(1) preparation of GO：
GO is synthesized using natural graphite powder according to Hummer methods.By 1g graphite powders, 2.5g NaNO3Add with 30ml concentrated sulphuric acids
Enter in 250ml three-neck flasks, and three-neck flask is put into into magnetic agitation in ice bath.Stir slow to being completely dissolved in backward suspension
It is slow to add 0.4g KMnO4, 2h is persistently stirred until mixture becomes green, mixture is cooled to into 0 DEG C now.Subsequently, by which
Remove ice bath, 30min reacted under the conditions of 35 DEG C, then in mixture plus 40ml deionized waters, then under the conditions of 98 DEG C it is anti-
Answer 40min.When solution reaction is into dark-brown, 10ml 30%H are added to which respectively2O2, 40ml deionized waters are with terminating reaction.
Finally, product is washed 3～4 times with 30%HCl, precipitation, centrifugation dry 10h in 50 DEG C of vacuum.
(2)CoFe2O4Preparation：
By 0.0646g Fe (NO3)3·9H2O、0.0233g Co(NO3)2.6H2O is stirred in being added to 40mL ethylene glycol, is stirred
Mix to after being completely dissolved and add 0.005g PVP, stir, solution is transferred in 240 DEG C of reactors carries out 24h constant temp. heatings
Reaction；After reaction terminates, room temperature is dropped to, then solid matter with deionized water, washing with alcohol is dried under the conditions of 60 DEG C
12h, obtains CoFe2O4。
(3)CdS/CoFe2O4The preparation of/rGO composite photo-catalysts：
By 0.1833g CdCl2·2.5H2During O and 0.1756g L-Cysteine is dissolved in 40mL deionized waters and stir
To being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts the pH=7 of above-mentioned solution, then wherein add 0.05g GO and
0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs, and subsequently, solution is shifted
2h constant temperature thermal responses are carried out into 180 DEG C of reactors；After reaction terminates, with Magnet by precipitate and solution separating, washed with ethanol
Precipitate is washed, is dried in being put into vacuum drying oven, is obtained CdS/CoFe2O4/ rGO composite photo-catalysts.
(4) in taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 86.3% in 90min.
Embodiment 2：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=5, then wherein add 0.05g GO and 0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
In taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst husky to ring third
The degradation rate of star antibiotic reaches 40.56% in 90min.
Embodiment 3：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=6, then wherein add 0.05g GO and 0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
In taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst husky to ring third
The degradation rate of star antibiotic reaches 54.26% in 90min.
Embodiment 4：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=8, then wherein add 0.05g GO and 0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
In taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst husky to ring third
The degradation rate of star antibiotic reaches 38.25% in 90min.
Embodiment 5：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=7, then wherein add 0.025g GO and 0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
(4) in taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 56.39% in 90min.
Embodiment 6：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=7, then wherein add 0.010g GO and 0.05g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
(4) in taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 49.25% in 90min.
Embodiment 7：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=7, then wherein add 0.05g GO and 0.10g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
(4) in taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 66.75% in 90min.
Embodiment 8：
By the step in embodiment 1, except for the difference that (3) are by 0.1833g CdCl2·2.5H2Half Guang ammonia of O and 0.1756g L-
During acid is dissolved in 40mL deionized waters and stir to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=7, then wherein add 0.05g GO and 0.15g CoFe2O4Continue to stir, be subsequently adding 0.045g Na2S·
9H2O simultaneously stirs, and subsequently, solution is transferred in 180 DEG C of reactors carries out 2h constant temperature thermal responses；After reaction terminates, magnetic is used
Precipitate and solution separating are used washing with alcohol precipitate by ferrum, dry, obtain CdS/CoFe in being put into vacuum drying oven2O4/rGO
Composite photo-catalyst.
(4) in taking (3), sample carries out photocatalytic degradation test in photochemical reaction instrument, measures the photocatalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 79.32% in 90min.
With regard to the sign of the present invention, Fig. 1 is CdS/Fe3O4/ rGO composite photo-catalyst photocatalysis fluorograms；It is very clear in figure
Chu presents CdS/Fe3O4/ rGO has good catalysis activity.Fig. 2 is CdS/CoFe2O4The magnetic of/rGO composite photo-catalysts
Hysteresis line chart；As can be seen from the figure photocatalyst has good magnetic.Fig. 3 is CdS/CoFe2O4/ rGO composite photo-catalysts
Stability degraded figure.As can be seen from the figure CdS/CoFe2O4/ rGO has good stability.
Claims (9)
1. a kind of hydro-thermal method synthesizes recyclable CdS/CoFe2O4The preparation method of/rGO composite photo-catalysts, it is characterised in that press
Carry out according to following steps：
Step 1, prepare graphite oxide GO；
Step 2, preparation CoFe2O4：
By Fe (NO3)3·9H2O、Co(NO3)2.6H2O is stirred in being added to ethylene glycol, is stirred to after being completely dissolved and is added PVP to stir
Mix, solution is transferred in reactor carries out constant temperature thermal response；After reaction terminates, room temperature is dropped to, will be solid
Body product deionized water, washing with alcohol, then dry, obtain CoFe2O4, it is standby；
Step 3, preparation CdS/CoFe2O4/ rGO composite photo-catalysts：
By CdCl2·2.5H2O and L-Cysteine dissolving in deionized water and are stirred to being completely dissolved and obtain mixed liquid B；Again
The pH of mixed liquid B is adjusted with sodium hydroxide solution, then GO, CoFe are added in mixed liquid B2O4Continue to stir, be subsequently adding
Na2S·9H2O is simultaneously uniformly mixing to obtain mixed liquor C, and subsequently, solution is transferred in reactor carries out constant temperature thermal response；Reaction knot
Shu Hou, with Magnet by precipitate and solution separating, uses washing with alcohol precipitate, dries, obtain CdS/ in being put into vacuum drying oven
CoFe2O4/ rGO composite photo-catalysts.
2. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 2, when preparing mixed liquor A, the Fe (NO for being used3)3·9H2O、Co(NO3)2.6H2O, second two
The amount ratio of alcohol and PVP is 0.0646g：0.0233g：40mL：0.005g.
3. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 2, the temperature of described constant temperature thermal response is 240 DEG C, and the response time is 24h.
4. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 3, when preparing mixed liquid B, the CdCl for being used2·2.5H2O, L-Cysteine, deionization
The amount ratio of water is 0.1833g：0.1756g：40mL.
5. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 3, the concentration of the sodium hydroxide solution for being used is 0.1mol/L, the pH for being adjusted is 5～
8。
6. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 3, when preparing mixed liquor C, GO, the CoFe for being used2O4With Na2S·9H2O mass ratioes are 2
～10：10～30：9.
7. a kind of hydro-thermal method according to claim 1 synthesizes recyclable CdS/CoFe2O4The preparation of/rGO composite photo-catalysts
Method, it is characterised in that in step 3, the temperature of described constant temperature thermal response is 180 DEG C, and the response time is 2h.
8. a kind of hydro-thermal method described in claim 1 synthesizes recyclable CdS/CoFe2O4The preparation method of/rGO composite photo-catalysts
The CdS/CoFe of preparation2O4/ rGO composite photo-catalysts, it is characterised in that prepared CdS/CoFe2O4/ rGO composite photocatalysts
In agent, the mass fraction of rGO is 10～50%, CoFe2O4The mass fraction of/rGO is 20～90%.
9. a kind of hydro-thermal method described in claim 1 synthesizes recyclable CdS/CoFe2O4The preparation method of/rGO composite photo-catalysts
The CdS/CoFe of preparation2O4The purposes of/rGO composite photo-catalysts, it is characterised in that prepared CdS/CoFe2O4/ rGO is combined
Photocatalyst, for the tetracycline in degrading waste water.
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