CN104003557B - Method for carrying out photocatalytic degradation on sulfamethoxazole - Google Patents
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- 229960005404 sulfamethoxazole Drugs 0.000 title claims abstract description 79
- JLKIGFTWXXRPMT-UHFFFAOYSA-N sulphamethoxazole Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 JLKIGFTWXXRPMT-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 77
- 239000010439 graphite Substances 0.000 claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 75
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000002131 composite material Substances 0.000 claims abstract description 40
- 239000002086 nanomaterial Substances 0.000 claims abstract description 30
- 239000002351 wastewater Substances 0.000 claims abstract description 15
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- 230000015556 catabolic process Effects 0.000 claims abstract description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 8
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 8
- 239000011733 molybdenum Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 32
- 239000000725 suspension Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910021382 natural graphite Inorganic materials 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000012216 screening Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The invention relates to a method for carrying out photocatalytic degradation on sulfamethoxazole. The problem of waste water treatment of the sulfamethoxazole hard to biodegraded can be effectively solved. The method comprises the steps that elements of iron, molybdenum and bismuth are adopted to be doped with expanded graphite to prepare a Fe/Bi/Mo-expanded graphite composite nano material, the Fe/Bi/Mo-expanded graphite composite nano material is added to waste water with the sulfamethoxazole, the pH value is adjusted to be 5.5-8.5 through alkaline matter, irradiation is carried out under visible light for 170 minutes to 190 minutes, the Fe/Bi/Mo-expanded graphite composite nano material is utilized, the waste water with the sulfamethoxazole with the concentration of 5 mg/L to 10 mg/L is directly oxidized through the single Fe/Bi/Mo-expanded graphite composite nano material without adding other promoters, and the adding amount of the Fe/Bi/Mo-expanded graphite composite nano material is 1 g/L to 2 g/L; finally, the degradation rate of the sulfamethoxazole is measured. Acidic materials do not need to be added manually, the solution of the sulfamethoxazole is acidic, a photocatalytic reaction can be carried out conveniently, after the photocatalytic reaction, the sulfamethoxazole is degraded, even part of the sulfamethoxazole is mineralized, the removal rate of the sulfamethoxazole is more than 90 percent, energy conservation and environmental protection are achieved, and great economic and social benefits are achieved.
Description
Technical field
The present invention relates to environmental protection field, particularly a kind of method of photocatalytic degradation Sulfamethoxazole.
Background technology
Since microbiotic self-discovery, in disease prevention and treatment, make great contribution.Current antibiotic is mainly used in agriculture production and medical treatment, and the microbiotic used at present is mainly tetracyclines, amides, Macrolide and sulfamido.The annual whole world has at least the microbiotic of more than 50% to be for animal husbandry and aquaculture at present according to statistics.Investigation display, at present, all detect that antibiotic medicine pollutes in the soil and water in global many areas, kind is more, and concentration is also in rising trend.Detected 4 class microbiotic medicines in 5 sewage effluentses of such as Sweden, comprise 3 kinds of quinolone antibiotics and a kind of tetracycline antibiotics, maximum concentration reaches 1.34 μ g/mL.In the Inlet and outlet water of Pekinese of China Gaobeidian City's Sewage Plant, also detected 8 kinds of quinolone antibiotics, concentration range is between 5 ~ 18 μ g/mL.
The microbiotic of Environmental Trace can cause water pollution, has a negative impact to people and animals and plants, threatens the balance of the ecosystem.Although antibiotic concentration is lower in environment, but strong, the difficult volatilization of most of antibiotic substance polarity, not easily escape from water body environment, hydrobiont is subject to antibiotic permanence and exposes, easily cause the biological accumulation effect that food chain transmission causes, thus human body is produced to the disadvantageous effect being difficult to predict.Such as, microbiotic residual in food, may cause crowd's anaphylaxis; Part has the physiological function of medicine energy severe jamming people of carcinogenic, teratogenesis, mutagenesis; Some Hormones class medicine and some makeup can cause organism endocrine regulation, cause sex entanglement or deformity.In view of microbiotic is to the potential hazard of environment and human health, part microbiotic is listed in the short-list of priority monitoring and control polluted articles by Environmental Protection Agency (EPA) and " EU Water framework directive/guide ".European Union, for antibiotic use, has promulgated relevant laws and regulations, prohibites in herding and aquaculture and uses the microbiotic of non-drug character as animal growth promoter.In China, although the parties concerned have noticed that antibiotic a large amount of production and abuse can cause potential ecological hazard, regrettably ensure that the laws and regulations of microbiotic safe handling are also fewer, caused the situation of abuse of antibiotics still to exist.
For reducing or eliminating antibiotic ecological hazard, lot of domestic and international scientist has carried out antibiotic removal research in water surrounding, minimizing technology mainly comprises the following aspects: coagulation and flocculation, sand filtration, charcoal absorption, active sludge treatment, artificial wetland treatment, advanced oxidation process, the chlorination in advanced oxidation, ozone oxidation, photochemical catalytic oxidation, Fenton oxidation, Oxone/Co
2+oxidation, wet air oxidation and x ray irradiation x etc. all can be used for antibiotic removal.But aforesaid method all has certain defect, such as coagulation and absorption can not change the molecular structure of antibiotic substance, just microbiotic are transferred to solid phase from liquid phase, easily cause secondary pollution; Different sorts is different with the processing requirement of structure microbiotic to active sludge; Artificial wetland treatment then needs big area soil.
In sum, more or less all there is certain defect in existing antibiotic treatment method.In the long run, reduction antibiotic usage amount or Sources controlling turnout are the most effectual ways preventing microbiotic from polluting, but are difficult in a short time accomplish, especially China.The antibiotic turnout of current China about 210,000 t/, consumption is about 138g year per capita, is 10 times of the U.S..Therefore, finding out technique microbiotic removal technology that is simple, efficient, non-secondary pollution is technical problem urgently to be resolved hurrily.
Summary of the invention
For above-mentioned situation, for overcoming the defect of prior art, the object of the present invention is just to provide a kind of method of photocatalytic degradation Sulfamethoxazole, effectively can solve and be difficult to biodegradable Sulfamethoxazole waste water handling problem.
The technical scheme that the present invention solves is, adopt iron, molybdenum, bismuth element doping expanded graphite prepares Fe/Bi/Mo-expanded graphite composite nano materials, add in the waste water containing Sulfamethoxazole, be 5.5-8.5 by alkaline matter adjust pH, irradiate 170-190 minute under visible light, utilize Fe/Bi/Mo-expanded graphite composite nano materials, when not adding other promotor, be directly the Sulfamethoxazole waste water of 5-10mg/L by single Fe/Bi/Mo-expanded graphite composite nano materials oxide treatment concentration, Fe/Bi/Mo-expanded graphite composite nano materials add-on is 1-2g/L, finally measure the degradation rate of Sulfamethoxazole, its degradation rate formula is:
wherein C
0for the starting point concentration of Sulfamethoxazole waste water, C
tfor the residual concentration of Sulfamethoxazole in final solution,
Described alkaline matter is the one of sodium hydroxide, potassium hydroxide or saleratus;
The mass ratio of described iron, molybdenum, bismuth, expanded graphite is 7.5-8.5 ︰ 45-55 ︰ 190-210 ︰ 4.8-5.2, is preferably 8 ︰ 50 ︰ 200 ︰ 5;
Described Fe/Bi/Mo-expanded graphite composite nano materials is, take natural graphite as raw material, be less than at 4 DEG C, natural graphite 9-11g slowly being joined concentration is in the vitriol oil 50-70mL of 98%, rapid stirring 30min, slowly add 18-22g potassium permanganate again and stir 10min, vibrate after 1h under 30 DEG C of constant temperature, add the warm water dilution of 90-110mL40-50 DEG C, obtain suspension, the hydrogen peroxide adding 28-32mL concentration 30% in suspension is oxidized natural graphite further, reaction 5min, filter to obtain graphite oxide, 3-5 graphite oxide is rinsed respectively with the dilute hydrochloric acid of mass concentration 5% and rare saleratus of mass concentration 5%, dry under 80 DEG C of constant temperature again, pass through microwave, graphite oxide is expanded, obtain expanded graphite, by expanded graphite 0.04-0.06g and Fe
3o
4nano powder 0.009-0.011g joins in 90-110mL distilled water, and ultrasonic disperse 1h must be oxidized expanded graphite suspension, by the Bi (NO of 4.5-5.0g
3)
35H
2o slowly joins in expanded graphite suspension (or claiming dispersion liquid), stirred at ambient temperature 1h, then by (the NH of 0.8-1.0g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, stirred at ambient temperature 2h, and regulator solution, to neutral, obtains mixing suspension, after mixing suspension is reacted 2h under 100 DEG C of constant temperature, filter, obtain screening, screening washing 3-5 time, at 75-85 DEG C, dry 2h, grinding, obtains the Fe/Bi/Mo-expanded graphite composite nano materials that magnetic is visible light-responded.
The present invention artificially need not add acidic substance, and Sulfamethoxazole solution itself is aobvious acid, is conducive to light-catalyzed reaction and carries out.After light-catalyzed reaction, Sulfamethoxazole is degraded, and even part is by mineralising, and Sulfamethoxazole clearance is up to more than 90%, and energy-conserving and environment-protective, economic and social benefit is huge.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is elaborated.
Embodiment 1
The present invention, in concrete enforcement, is realized by following methods:
First Fe/Bi/Mo-expanded graphite composite nano materials is prepared, method is, adopt electrooptical balance precise 10g natural graphite, at the vitriol oil 60mL that the beaker centerbody volume concentrations of 500mL is 98%, being less than under 4 DEG C of ice wash one's hair, natural graphite is slowly joined in beaker, after vigorous stirring 30min, slowly add 20g potassium permanganate and stir 10min, beaker being placed in constant temperature 30 DEG C of vibrators and vibrating after 1h, add 100mL warm water and dilute.After this in above-mentioned suspension, the hydrogen peroxide adding 30mL volumetric concentration 30% is oxidized natural graphite further, after reaction 5min, filter out graphite oxide, graphite oxide is rinsed 3-5 time with volumetric concentration 5% dilute hydrochloric acid and the rare saleratus of volumetric concentration 5%, fully dry in 80 DEG C of thermostatic drying chambers, after its steady quality, by 1kw microwave, expand graphite oxide obtained expanded graphite; Get 0.05g expanded graphite and 0.01gFe
3o
4nano-powder joins in the beaker that 100mL distilled water is housed, and ultrasonic disperse 1h obtains oxidation expanded graphite suspension; By the Bi (NO of 4.85g
3)
35H
2o slowly joins in expanded graphite suspension, stirred at ambient temperature 1h, then by (the NH of 0.9g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, stirred at ambient temperature 2h, regulator solution is to neutral, mixing suspension, mixing suspension is moved into constant temperature in reactor and to react 2h, filter, obtain screening, screening washes 5 times, 80 DEG C dries 2h, and grinding, obtains the Fe/Bi/Mo-expanded graphite composite nano materials that magnetic is visible light-responded;
Adopt Fe/Bi/Mo-expanded graphite composite nano materials again, the Sulfamethoxazole under natural light irradiation in the catalyzed degradation aqueous solution, first in photo catalysis reactor, add starting point concentration (C
0) be the Sulfamethoxazole solution 100mL of 10mg/L, the Fe/Bi/Mo-expanded graphite composite nano materials of 2g/L is added in Sulfamethoxazole solution, in dark surrounds, with the constant temperature oscillator vibration 40min that frequency is 150Hz, the Sulfamethoxazole in solution is made to be adsorbed to Fe/Bi/Mo-expanded graphite composite nano materials surface, then reactor is moved to irradiation 3h under natural light, catalyzed degradation Sulfamethoxazole, every 30min, the solution (sample) of 1mL containing the catalyzed degraded of Sulfamethoxazole is got with liquid-transfering gun, after 0.45 μm of membrane filtration, with the residual concentration (C of Sulfamethoxazole in efficient liquid phase chromatographic analysis solution
t), the clearance of Sulfamethoxazole at the end of reaction
if desired, also after photoresponse 3h, by HLPC-MS test analysis, the Photodegradation Products (determine what degraded product is, not in the scope of request protection of the present invention, therefore be not described further) of Sulfamethoxazole can be confirmed.
The present invention is through experiment and test, its add-on on the degradation rate of Sulfamethoxazole and Fe/Bi/Mo-expanded graphite composite nano materials, the concentration of Sulfamethoxazole solution and the pH value of solution have direct impact, and obtain sufficient proof through test, related tests data is as follows:
In the present invention, the Optimum of Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material is determined by following test.Be in the Sulfamethoxazole solution of 10mg/L in concentration, add different amounts (0,0.25,0.5,1.0,1.5,2g/L) Fe/Bi/Mo-exfoliated-graphite composite, after dark surrounds absorption 40min, adopt visible radiation 3h, analyze the impact that different amounts Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material is degraded on Sulfamethoxazole, test-results is as shown in the table.As can be seen from the table, when Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material is more than 1g/L, to 10mg/L Sulfamethoxazole, there is good removal effect.
In the present invention, the effect of Sulfamethoxazole solution to photocatalytic degradation of different starting point concentration has certain influence.Configure respectively starting point concentration be 5,10, three parts of Sulfamethoxazole solution of 15mg/L, the Fe/Bi/Mo-exfoliated-graphite composite of 2g/L is all added in every part of solution, whip attachment 40min in dark surrounds, optical radiation 3h, adopt high performance liquid chromatograph to measure radiation and terminate remaining Sulfamethoxazole concentration in rear solution, and calculate its clearance.When starting point concentration is 5mg/L, after photochemical catalysis 3h, the clearance of Sulfamethoxazole can reach 95.78%; When starting point concentration is 10mg/L, after photochemical catalysis 3h, the clearance of Sulfamethoxazole can reach 93.56%; When starting point concentration is 15mg/L, after photochemical catalysis 3h, the clearance of Sulfamethoxazole can reach 90.12%.This shows that the starting point concentration of Sulfamethoxazole has impact to its degradation process, and as its concentration lower (5 ~ 10mg/L), the light-catalyzed reaction of short period of time (3h) just can obtain the clearance of more than 90%.
In the present invention, the degraded of solution ph on Sulfamethoxazole has impact.Be 2g/L when the concentration of Sulfamethoxazole solution is 10mg/L, Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material consumption, dark adsorption time is 40min, and light application time is under 3h condition, and when pH value of solution is 5.5, the clearance of Sulfamethoxazole is 98.87%; When pH value of solution is 6.1, the clearance of Sulfamethoxazole is 95.78%; When pH value of solution is 7.0, the clearance of Sulfamethoxazole is 93.26%; When pH value of solution is 8.5, the clearance of Sulfamethoxazole is 90.14%; When pH value of solution is 9.0, the clearance of Sulfamethoxazole is 86.72%.This shows in sour environment, and the clearance of Sulfamethoxazole is higher, and reason is in sour environment, and the content of the oxidative free radical of light reaction procedure is higher, and its catalytic activity is strong.Need not be artificial in present method add acidic substance again, Sulfamethoxazole solution itself presents slightly acidic.
After adopting the method degraded Sulfamethoxazole in the present invention, analyzed by HPLC-MS, find that Sulfamethoxazole is degraded, be degraded to small-molecule substance by macromolecular substance, and part Sulfamethoxazole is by mineralising, illustrates that this kind of method is feasible.
From the above, the present invention adopts iron, molybdenum, bismuth element doping expanded graphite prepares Fe/Bi/Mo-expanded graphite composite nano materials, with the Sulfamethoxazole in its wastewater by photocatalysis, under natural light (visible ray) irradiates, make full use of the characteristic of this composite Nano luminescent material, direct oxidation process is containing the Sulfamethoxazole waste water of different concns, other promotor is no longer added in treating processes, technique is simple, cost is low, due in Fe/Bi/Mo-expanded graphite composite nano materials doped with ferro element, the composite Nano luminescent material of preparation is made to have magnetic, fundamentally can solve the problem that photocatalyst is difficult to reclaim, and then realize its recycling.Sulfamethoxazole waste water can be processed rapidly, can light-catalyzed reaction be completed in 3h, and efficiency be high, the efficiency of degraded Sulfamethoxazole, higher than 90%, does not add promotor in treating processes, such as metal ion, too much acidity and alkaline matter, avoid secondary pollution, energy-conserving and environment-protective; The expanded graphite base composite nano photocatalyst material process Sulfamethoxazole waste water particularly adopting iron, molybdenum, bismuth to adulterate, do not need the concentration regulating Sulfamethoxazole waste water, by regulating the consumption of Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material, the Sulfamethoxazole waste water of concentration range 5 ~ 15mg/L is processed, equal can obtain more than 90% high clearance, therefore have very strong practicality, economic and social benefit is huge.
Claims (4)
1. the method for a photocatalytic degradation Sulfamethoxazole, it is characterized in that, adopt iron, molybdenum, bismuth element doping expanded graphite prepares Fe/Bi/Mo-expanded graphite composite nano materials, add in the waste water containing Sulfamethoxazole, be 5.5-8.5 by alkaline matter adjust pH, irradiate 170-190 minute under visible light, utilize Fe/Bi/Mo-expanded graphite composite nano materials, when not adding other promotor, be directly the Sulfamethoxazole waste water of 5-10mg/L by single Fe/Bi/Mo-expanded graphite composite nano materials oxide treatment concentration, Fe/Bi/Mo-expanded graphite composite nano materials add-on is 1-2g/L, finally measure the degradation rate of Sulfamethoxazole, its degradation rate formula is:
wherein C
0for the starting point concentration of Sulfamethoxazole waste water, C
tfor the residual concentration of Sulfamethoxazole in final solution,
Described alkaline matter is the one of sodium hydroxide, potassium hydroxide or saleratus;
Described Fe/Bi/Mo-expanded graphite composite nano materials is, take natural graphite as raw material, be less than at 4 DEG C, natural graphite 9-11g slowly being joined concentration is in the vitriol oil 50-70mL of 98%, rapid stirring 30min, slowly add 18-22g potassium permanganate again and stir 10min, vibrate after 1h under 30 DEG C of constant temperature, add the warm water dilution of 90-110mL 40-50 DEG C, obtain suspension, the hydrogen peroxide adding 28-32mL concentration 30% in suspension is oxidized natural graphite further, reaction 5min, filter to obtain graphite oxide, 3-5 graphite oxide is rinsed respectively with the dilute hydrochloric acid of mass concentration 5% and rare saleratus of mass concentration 5%, dry under 80 DEG C of constant temperature again, pass through microwave, graphite oxide is expanded, obtain expanded graphite, by expanded graphite 0.04-0.06g and Fe
3o
4nano powder 0.009-0.011g joins in 90-110mL distilled water, and ultrasonic disperse 1h must be oxidized expanded graphite suspension, by the Bi (NO of 4.5-5.0g
3)
35H
2o slowly joins in expanded graphite suspension, stirred at ambient temperature 1h, then by (the NH of 0.8-1.0g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, stirred at ambient temperature 2h, and regulator solution, to neutral, obtains mixing suspension, after mixing suspension is reacted 2h under 100 DEG C of constant temperature, filter, obtain screening, screening washing 3-5 time, at 75-85 DEG C, dry 2h, grinding, obtains the Fe/Bi/Mo-expanded graphite composite nano materials that magnetic is visible light-responded.
2. the method for photocatalytic degradation Sulfamethoxazole according to claim 1, is characterized in that, the mass ratio of described iron, molybdenum, bismuth, expanded graphite is 7.5-8.5 ︰ 45-55 ︰ 190-210 ︰ 4.8-5.2.
3. the method for photocatalytic degradation Sulfamethoxazole according to claim 1 and 2, is characterized in that, the mass ratio of described iron, molybdenum, bismuth, expanded graphite is 8 ︰ 50 ︰ 200 ︰ 5.
4. the method for photocatalytic degradation Sulfamethoxazole according to claim 1, is characterized in that, realized by following methods:
First Fe/Bi/Mo-expanded graphite composite nano materials is prepared, method is, adopt electrooptical balance precise 10g natural graphite, at the vitriol oil 60mL that the beaker centerbody volume concentrations of 500mL is 98%, be less than under 4 DEG C of ice wash one's hair, natural graphite is slowly joined in beaker, after vigorous stirring 30min, slowly add 20g potassium permanganate and stir 10min, beaker being placed in constant temperature 30 DEG C of vibrators vibrates after 1h, add 100mL warm water to dilute, after this in above-mentioned suspension, the hydrogen peroxide adding 30mL volumetric concentration 30% is oxidized natural graphite further, after reaction 5min, filter out graphite oxide, graphite oxide is rinsed 3-5 time with volumetric concentration 5% dilute hydrochloric acid and the rare saleratus of volumetric concentration 5%, fully dry in 80 DEG C of thermostatic drying chambers, after its steady quality, by 1kw microwave, expand graphite oxide obtained expanded graphite, get 0.05g expanded graphite and 0.01gFe
3o
4nano-powder joins in the beaker that 100mL distilled water is housed, and ultrasonic disperse 1h obtains oxidation expanded graphite suspension, by the Bi (NO of 4.85g
3)
35H
2o slowly joins in expanded graphite suspension, stirred at ambient temperature 1h, then by (the NH of 0.9g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, stirred at ambient temperature 2h, regulator solution is to neutral, mixing suspension, mixing suspension is moved into constant temperature in reactor and to react 2h, filter, obtain screening, screening washes 5 times, 80 DEG C dries 2h, and grinding, obtains the Fe/Bi/Mo-expanded graphite composite nano materials that magnetic is visible light-responded,
Adopt Fe/Bi/Mo-expanded graphite composite nano materials again, the Sulfamethoxazole under natural light irradiation in the catalyzed degradation aqueous solution, first in photo catalysis reactor, add starting point concentration C
0for the Sulfamethoxazole solution 100mL of 10mg/L, the Fe/Bi/Mo-expanded graphite composite nano materials of 2g/L is added in Sulfamethoxazole solution, in dark surrounds, with the constant temperature oscillator vibration 40min that frequency is 150Hz, the Sulfamethoxazole in solution is made to be adsorbed to Fe/Bi/Mo-expanded graphite composite nano materials surface, then reactor is moved to irradiation 3h under natural light, catalyzed degradation Sulfamethoxazole, every 30min, the solution of 1mL containing the catalyzed degraded of Sulfamethoxazole is got with liquid-transfering gun, after 0.45 μm of membrane filtration, with the residual concentration C of Sulfamethoxazole in efficient liquid phase chromatographic analysis solution
t, the clearance of Sulfamethoxazole at the end of reaction
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