CN104003557A - Method for carrying out photocatalytic degradation on sulfamethoxazole - Google Patents
Method for carrying out photocatalytic degradation on sulfamethoxazole Download PDFInfo
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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 27
- 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 31
- 239000000725 suspension Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910021382 natural graphite Inorganic materials 0.000 claims description 12
- 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
- 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
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000011858 nanopowder Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
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- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical compound C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 2
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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 microbiotic is mainly used in agriculture production and medical treatment, and the microbiotic using is at present mainly tetracyclines, amides, Macrolide and sulfamido.At present to have more than 50% microbiotic at least be for animal husbandry and aquaculture in the annual whole world according to statistics.Investigation shows, at present, all detects that antibiotic medicine pollutes in the soil and water in global many areas, and kind is more, and concentration is also rising trend.In 5 sewage effluentses such as Sweden, detected 4 class microbiotic medicines, comprised 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, and people and animals and plants are had a negative impact, and threatens the balance of the ecosystem.Although antibiotic concentration is lower in environment, but strong, the difficult volatilization of most of antibiotic substance polarity, be difficult for escaping from water body environment, hydrobiont is subject to antibiotic permanence and exposes, the biological accumulation effect that easily causes food chain transmission to cause, thus human body is produced to the disadvantageous effect that is difficult to prediction.Such as, residual microbiotic in food, may cause crowd's anaphylaxis; Part has the medicine energy severe jamming people's of carcinogenic, teratogenesis, mutagenesis physiological function; Some Hormones class medicine and some makeup can cause organism endocrine regulation, cause sex entanglement or deformity.In view of the potential hazard of microbiotic to environment and human health, Environmental Protection Agency (EPA) and " EU Water framework directive/guide " have been listed part microbiotic in priority monitoring and have been controlled the short-list of pollutent.European Union, for antibiotic use, has promulgated relevant laws and regulations, prohibites in herding and aquaculture and uses the microbiotic of non-medication matter as animal growth promoter.In China, although having noticed antibiotic a large amount of production and abuse, the parties concerned can cause potential ecological hazard, regrettably ensure that the laws and regulations of microbiotic safe handling are also fewer, cause 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, removal method mainly comprises the following aspects: coagulation and flocculation, sand filtration, charcoal absorption, active sludge treatment, artificial swamp processing, advanced oxidation processing, the chlorination in advanced oxidation, ozone oxidation, photochemical catalytic oxidation, Fenton oxidation, Oxone/Co
2+oxidation, wet type 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 is transferred to solid phase from liquid phase, easily cause secondary pollution; Different sorts is different to the processing requirement of active sludge with structure microbiotic; Artificial swamp is processed needs big area soil.
In sum, more or less all there is certain defect in existing antibiotic treatment method.In the long run, reducing microbiotic usage quantity or source production control amount is the most effectual way that prevents that microbiotic from polluting, but is difficult in a short time accomplish, especially China.At present China antibiotic turnout approximately 210,000 t/, year about 138g of consumption per capita, is 10 times of the U.S..Therefore, finding out technique microbiotic removal technology 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 present invention's object is just to provide a kind of method of photocatalytic degradation Sulfamethoxazole, can effectively 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 is prepared Fe/Bi/Mo-expanded graphite composite nano materials, add in the waste water that contains Sulfamethoxazole, be 5.5-8.5 by alkaline matter adjust pH, under visible ray, irradiate 170-190 minute, utilize Fe/Bi/Mo-expanded graphite composite nano materials, in the situation that not adding other promotor, the Sulfamethoxazole waste water that is directly 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, taking natural graphite as raw material, be less than at 4 DEG C, it is in 98% vitriol oil 50-70mL that natural graphite 9-11g is slowly joined to concentration, rapid stirring 30min, slowly add again 18-22g potassium permanganate to stir 10min, under 30 DEG C of constant temperature, vibrate after 1h, add the warm water dilution of 90-110mL40-50 DEG C, obtain suspension, in suspension, add the hydrogen peroxide of 28-32mL concentration 30% to be further oxidized natural graphite, reaction 5min, filter to obtain graphite oxide, rinse respectively graphite oxide 3-5 time 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 dispersion 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), under room temperature, stirs 1h, then by (the NH of 0.8-1.0g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, under room temperature, stirs 2h, and regulator solution, to neutral, obtains mixing suspension, mixing suspension is reacted after 2h under 100 DEG C of constant temperature, filter, obtain screening, screening washing 3-5 time is dried 2h at 75-85 DEG C, grinds, and obtains the visible light-responded Fe/Bi/Mo-expanded graphite composite nano materials of magnetic.
The present invention need not artificially 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%, energy-conserving and environment-protective, and 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 prepare Fe/Bi/Mo-expanded graphite composite nano materials, method is, adopt electrooptical balance accurately to weigh 10g natural graphite, the vitriol oil 60mL that is 98% at the beaker centerbody volume concentrations of 500mL, being less than under 4 DEG C of ice wash one's hair, slowly joins natural graphite in beaker, after vigorous stirring 30min, slowly add 20g potassium permanganate and stir 10min, beaker being placed in to 30 DEG C of vibrators of constant temperature and vibrating after 1h, adding 100mL warm water to dilute.After this in above-mentioned suspension, add the hydrogen peroxide of 30mL volumetric concentration 30% to be further oxidized natural graphite, after reaction 5min, filter out graphite oxide, rinse graphite oxide 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, graphite oxide is expanded and makes 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 dispersion 1h obtains being oxidized expanded graphite suspension; By the Bi (NO of 4.85g
3)
35H
2o slowly joins in expanded graphite suspension, under room temperature, stirs 1h, then by (the NH of 0.9g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, under room temperature, stir 2h, regulator solution is to neutral, mixing suspension, mixing suspension is moved in reactor to the constant temperature 2h that reacts, filter, obtain screening, 5 times, 80 DEG C oven dry 2h of screening washing, grind, and obtain the visible light-responded Fe/Bi/Mo-expanded graphite composite nano materials of magnetic;
Adopt Fe/Bi/Mo-expanded graphite composite nano materials, the Sulfamethoxazole under natural light irradiation in the catalyzed degradation aqueous solution first adds starting point concentration (C in photo catalysis reactor again
0) be the Sulfamethoxazole solution 100mL of 10mg/L, to the Fe/Bi/Mo-expanded graphite composite nano materials that adds 2g/L in Sulfamethoxazole solution, in dark surrounds, the constant temperature oscillator that is 150Hz by frequency vibration 40min, make the Sulfamethoxazole in solution 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, get 1mL containing the solution (sample) of the catalyzed degraded of Sulfamethoxazole with liquid-transfering gun, after 0.45 μ m membrane filtration, with the residual concentration (C of Sulfamethoxazole in efficient liquid phase chromatographic analysis solution
t), the clearance of Sulfamethoxazole when reaction finishes
if desired, also can, after photoresponse 3h, by HLPC-MS test analysis, confirm the Photodegradation Products (determine what degraded product is, the scope of not protecting in request of the present invention, therefore be not described further) of Sulfamethoxazole.
The present invention is through experiment and test, its degradation rate on Sulfamethoxazole and add-on, the concentration of Sulfamethoxazole solution and the pH value of solution of Fe/Bi/Mo-expanded graphite composite nano materials have direct impact, and obtained 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.In the Sulfamethoxazole solution that is 10mg/L in concentration, add the Fe/Bi/Mo-exfoliated-graphite composite of different amounts (0,0.25,0.5,1.0,1.5,2g/L), after dark surrounds absorption 40min, adopt visible radiation 3h, analyze the impact of different amounts Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material on Sulfamethoxazole degraded, test-results is as shown in the table.As can be seen from the table, Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material is 1g/L when above, the removal effect good to having of 10mg/L Sulfamethoxazole.
In the present invention, the Sulfamethoxazole solution of different starting point concentrations has certain influence to the effect of photocatalytic degradation.Configure respectively starting point concentration and be 5,10, three parts of Sulfamethoxazole solution of 15mg/L, in every part of solution, all add the Fe/Bi/Mo-exfoliated-graphite composite of 2g/L, whip attachment 40min in dark surrounds, optical radiation 3h, adopt high performance liquid chromatograph to measure radiation and finish 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 starting point concentration that shows Sulfamethoxazole has impact to its degradation process, and when its concentration lower (5～10mg/L), the light-catalyzed reaction of short period of time (3h) just can obtain more than 90% clearance.
In the present invention, pH has impact to the degraded of Sulfamethoxazole.When the concentration of Sulfamethoxazole solution is 10mg/L, Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material consumption is 2g/L, and dark adsorption time is 40min, and light application time is under 3h condition, and pH value of solution is 5.5 o'clock, and the clearance of Sulfamethoxazole is 98.87%; In the time that pH value of solution is 6.1, the clearance of Sulfamethoxazole is 95.78%; In the time that pH value of solution is 7.0, the clearance of Sulfamethoxazole is 93.26%; In the time that pH value of solution is 8.5, the clearance of Sulfamethoxazole is 90.14%; In the time that 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 again acidic substance, Sulfamethoxazole solution itself presents slightly acidic.
Adopt after the method degraded Sulfamethoxazole in the present invention, analyze 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 is prepared 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, the Sulfamethoxazole waste water containing different concns is processed in direct oxidation, in treating processes, no longer add other promotor, technique is simple, cost is low, due in Fe/Bi/Mo-expanded graphite composite nano materials doped with ferro element, make the composite Nano luminescent material of preparation there is magnetic, can fundamentally solve photocatalyst and be difficult to the problem reclaiming, and then realize its recycling.Can process rapidly Sulfamethoxazole waste water, in 3h, can complete light-catalyzed reaction, and efficiency be high, the efficiency of degraded Sulfamethoxazole, higher than 90%, is not added promotor, such as metal ion in treating processes, too much acidity and alkaline matter, avoided secondary pollution, energy-conserving and environment-protective; Particularly adopt the expanded graphite base composite nano photocatalyst material of iron, molybdenum, bismuth doping to process Sulfamethoxazole waste water, do not need to regulate the concentration of Sulfamethoxazole waste water, by regulating the consumption of Fe/Bi/Mo-expanded graphite composite Nano photocatalyst material, Sulfamethoxazole waste water to concentration range 5～15mg/L is processed, all 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 is prepared Fe/Bi/Mo-expanded graphite composite nano materials, add in the waste water that contains Sulfamethoxazole, be 5.5-8.5 by alkaline matter adjust pH, under visible ray, irradiate 170-190 minute, utilize Fe/Bi/Mo-expanded graphite composite nano materials, in the situation that not adding other promotor, the Sulfamethoxazole waste water that is directly 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, taking natural graphite as raw material, be less than at 4 DEG C, it is in 98% vitriol oil 50-70mL that natural graphite 9-11g is slowly joined to concentration, rapid stirring 30min, slowly add again 18-22g potassium permanganate to stir 10min, under 30 DEG C of constant temperature, vibrate after 1h, add the warm water dilution of 90-110mL40-50 DEG C, obtain suspension, in suspension, add the hydrogen peroxide of 28-32mL concentration 30% to be further oxidized natural graphite, reaction 5min, filter to obtain graphite oxide, rinse respectively graphite oxide 3-5 time 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 dispersion 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), under room temperature, stirs 1h, then by (the NH of 0.8-1.0g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, under room temperature, stirs 2h, and regulator solution, to neutral, obtains mixing suspension, mixing suspension is reacted after 2h under 100 DEG C of constant temperature, filter, obtain screening, screening washing 3-5 time is dried 2h at 75-85 DEG C, grinds, and obtains the visible light-responded Fe/Bi/Mo-expanded graphite composite nano materials of magnetic.
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, is realized by following methods:
First prepare Fe/Bi/Mo-expanded graphite composite nano materials, method is, adopt electrooptical balance accurately to weigh 10g natural graphite, the vitriol oil 60mL that is 98% at the beaker centerbody volume concentrations of 500mL, being less than under 4 DEG C of ice wash one's hair, slowly joins natural graphite in beaker, after vigorous stirring 30min, slowly add 20g potassium permanganate and stir 10min, beaker being placed in to 30 DEG C of vibrators of constant temperature and vibrating after 1h, adding 100mL warm water to dilute.After this in above-mentioned suspension, add the hydrogen peroxide of 30mL volumetric concentration 30% to be further oxidized natural graphite, after reaction 5min, filter out graphite oxide, rinse graphite oxide 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, graphite oxide is expanded and makes 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 dispersion 1h obtains being oxidized expanded graphite suspension; By the Bi (NO of 4.85g
3)
35H
2o slowly joins in expanded graphite suspension, under room temperature, stirs 1h, then by (the NH of 0.9g
4)
6mo
7o
244H
2o slowly adds in expanded graphite suspension, under room temperature, stir 2h, regulator solution is to neutral, mixing suspension, mixing suspension is moved in reactor to the constant temperature 2h that reacts, filter, obtain screening, 5 times, 80 DEG C oven dry 2h of screening washing, grind, and obtain the visible light-responded Fe/Bi/Mo-expanded graphite composite nano materials of magnetic;
Adopt Fe/Bi/Mo-expanded graphite composite nano materials, the Sulfamethoxazole under natural light irradiation in the catalyzed degradation aqueous solution first adds starting point concentration C in photo catalysis reactor again
0for the Sulfamethoxazole solution 100mL of 10mg/L, to the Fe/Bi/Mo-expanded graphite composite nano materials that adds 2g/L in Sulfamethoxazole solution, in dark surrounds, the constant temperature oscillator that is 150Hz by frequency vibration 40min, make the Sulfamethoxazole in solution 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, get 1mL containing the solution of the catalyzed degraded of Sulfamethoxazole with liquid-transfering gun, after 0.45 μ m membrane filtration, with the residual concentration C of Sulfamethoxazole in efficient liquid phase chromatographic analysis solution
t, the clearance of Sulfamethoxazole when reaction finishes
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| CN106124659A (en) * | 2016-06-23 | 2016-11-16 | 井冈山大学 | The method of prediction sulfa antibiotics rate of photocatalytic oxidation |
| CN106442818A (en) * | 2015-08-04 | 2017-02-22 | 中国水产科学研究院 | Magnetic separation based method for rapidly determining residual amount of sulfonamide antibiotics in animal muscle tissue |
| CN115350729A (en) * | 2022-07-13 | 2022-11-18 | 润赢科技(郑州)有限公司 | Novel efficient environment-friendly photocatalytic formaldehyde scavenger and preparation method thereof |
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| CN102784626A (en) * | 2012-08-08 | 2012-11-21 | 江苏大学 | Temperature-sensitive magnetic sulfadimidine molecular imprinted adsorbent as well as preparation method and application thereof |
| CN103007882A (en) * | 2012-12-13 | 2013-04-03 | 同济大学 | Preparation method of Fe3O4@MnO2/active carbon magnetic compound adsorption material |
| CN103111258A (en) * | 2013-02-22 | 2013-05-22 | 山东大学 | Reaction column filled with river-sand loaded graphene oxide/titanium dioxide (GO/TiO2) filler |
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| US20040108274A1 (en) * | 2002-12-09 | 2004-06-10 | Dirk Schulze-Makuch | Removal of biological pathogens using surfactant-modified zeolite |
| CN102784626A (en) * | 2012-08-08 | 2012-11-21 | 江苏大学 | Temperature-sensitive magnetic sulfadimidine molecular imprinted adsorbent as well as preparation method and application thereof |
| CN103007882A (en) * | 2012-12-13 | 2013-04-03 | 同济大学 | Preparation method of Fe3O4@MnO2/active carbon magnetic compound adsorption material |
| CN103111258A (en) * | 2013-02-22 | 2013-05-22 | 山东大学 | Reaction column filled with river-sand loaded graphene oxide/titanium dioxide (GO/TiO2) filler |
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| CN106442818A (en) * | 2015-08-04 | 2017-02-22 | 中国水产科学研究院 | Magnetic separation based method for rapidly determining residual amount of sulfonamide antibiotics in animal muscle tissue |
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| CN106124659A (en) * | 2016-06-23 | 2016-11-16 | 井冈山大学 | The method of prediction sulfa antibiotics rate of photocatalytic oxidation |
| CN115350729A (en) * | 2022-07-13 | 2022-11-18 | 润赢科技(郑州)有限公司 | Novel efficient environment-friendly photocatalytic formaldehyde scavenger and preparation method thereof |
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