CN103657590A - Adsorption and degradation of sulfated graphene-TiO2 composite material to amide and organophosphorus pesticides - Google Patents
Adsorption and degradation of sulfated graphene-TiO2 composite material to amide and organophosphorus pesticides Download PDFInfo
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Abstract
The invention relates to adsorption-degradation action of a sulfated graphene-titanium dioxide composite material which is capable of simultaneously carrying out adsorption and photocatalytic degradation on pesticide residue in water to five amide herbicides (alachlor, acetochlor, pretilachlor, metolachlor and butachlor) and seven organophosphorus insecticides (phorate, ethoprophos, pirimiphos-methyl, chlorpyrifos, malathion, fenthion, and methidathion) in water. The sulfated graphene-titanium dioxide composite material has the advantages that the sulfated graphene-titanium dioxide composite material has better adsorption effect on the amide herbicides and the organophosphorus insecticides, and meanwhile, has good photocatalytic degradation effect under the simulative sunlight; compared with the graphene-titanium dioxide composite material, the sulfated graphene-titanium dioxide composite material has better photocatalytic degradation effect on the amide herbicides and the organophosphorus insecticides.
Description
Technical field
The present invention relates to sulfonated Graphene/Graphene-TiO
2the absorption of composite and the method for Researches on Photocatalytic Degradation of Pesticide Using, belong to photocatalysis technology and degradation of pesticide technical field.
Technical background
Since the middle and later periods eighties 20th century, the usable floor area of China's herbicide, use amount all increases substantially, and its growth rate has been sure to occupy first of agricultural chemicals (pesticide, bactericide, herbicide and other class agricultural chemicals).Acetamide-group herbicides are one of a large amount of herbicides that use of China.Organophosphorus insecticides, through development, becomes one of main Types in main pesticide.The toxicity of these agricultural chemicals is large, environment release rate is large, influence surface is also wider, due to various in style and considerable output and use amount, brought harm significantly to human health and environment, as force soil quality decline, the deterioration of the ecological environment, cause that water pollution, Pesticide Residues exceed standard etc.The people and animals' injures and deaths and the tremendous economic loss that due to pollution by pesticides and intoxication accident, cause every year, brought serious negative effect to the agro based economic development of China.According to statistics, the pesticide producing amount in China's later stage nineties 20th century reaches 760,000 tons, and use amount is up to 50～600,000 tons, and wherein, nearly 80% agricultural chemicals is through in various approach entered environments, and most of agricultural chemicals finally collects and enters in water body, causes the pollution of various water bodys.
Literature survey discovery, KexinLi etc. [J.Hazard.Mater., 2013,250:19-28] utilize nonionic surface active agent and hydro-thermal method one-step synthesis TiO
2-graphene nano ion, is successfully used in the lasting pollutant rhodamine B of degradation water dissolubility, phonamiphos and Norfloxacin.Khalid etc. [Curr.Appl.Phys., 2012,12:1485-1492] with hydrothermal reaction at low temperature by nitrogen doped Ti O
2nanoparticle Modified, on Graphene, has synthesized GR-N/TiO
2compound, it is raw material that YanyanGao etc. [Carbon, 2012,50:4093-4101] be take graphene oxide (GO), urea and titanyl nitrate, by combustion method one-step synthesis TiO
2-GO nano material, with pure TiO
2compare, these two kinds of nano materials are higher to the light degradation property of methyl orange dye (MO).But above resulting product is not all reported its application of photocatalytic degradation to agricultural chemicals.Sulfonated Graphene-TiO
2the hydro-thermal method of composite is synthesized and the degraded of agricultural chemicals is not reported yet.
Therefore, set up the effectively method of degraded water body Pesticide Residues and play important realistic meaning for water conservation.
Summary of the invention
In view of this, the object of the invention is to propose a kind of composite, can adsorb and separate acetamide-group herbicides and organophosphorus insecticides, under simulated solar photocatalysis, can degrade again acetamide-group herbicides and organophosphorus insecticides simultaneously.
The technical solution adopted in the present invention be take sulfonated Graphene, graphene oxide and titanium tetrachloride solution as raw material, utilizes hydro-thermal reaction one step to prepare sulfonated Graphene-TiO
2composite photocatalyst material and Graphene-TiO
2composite photocatalyst material, makes it to acetamide-group herbicides, have good suction-operated, under simulated solar illumination, acetamide-group herbicides and organophosphorus insecticides is had to photocatalytic Degradation simultaneously, and its concrete preparation method's step is:
Sulfonated graphene/graphene oxide is soluble in water, mix.Titanium tetrachloride solution is added drop-wise in sulfonated graphene/graphene oxide suspension, mix and blend 1h, wherein the quality of sulfonated graphene/graphene oxide suspension is 5.347g, 6.684g, 13.369g, 33.420g, 66.840g, and titanium tetrachloride is 6.127mL, and concentration is 1.46M.And heating make it reaction, obtain sulfonated Graphene-titanium dioxide/graphene-composite titania material suspension.
Absorption of the present invention and light degradation process are divided into following steps:
(1) enrichment: get the sulfonated Graphene-TiO of 9mL
2/ Graphene-TiO
2join in the water sample that 20mL contains amide-type/organophosphorus insecticide, then vortex 2min, makes object be adsorbed on graphene composite material;
(2) separation: the water sample that contains amide-type/organophosphorus insecticide of step (1) is centrifugal, discard water layer, be precipitated thing;
(3) illumination: in gained sediment, add 4mL water, vortex or concussion several seconds, pipette 2mL, be placed in solar simulator (photodissociation instrument) illumination, control experiment is set;
(4) extract: illumination finishes, and with the ultrasonic extraction of 4mL ethyl acetate, is adsorbed on Graphene-TiO
2in undegradable agricultural chemicals, get 1mL upper strata organic layer, dewater, cross the organic mesentery of 0.22 μ L, wait for sample introduction;
(5) detect: the sample after mistake film is entered to GC-MS (acetamide-group herbicides)/GC-FPD (organophosphorus insecticides) and detect.
It is simple, with low cost, easy to operate that beneficial effect of the present invention is mainly reflected in step, has good application prospect in water body aspect the absorption of acetamide-group herbicides and organophosphorus insecticides and photocatalytic degradation.
Accompanying drawing explanation
Fig. 1 is sulfonated Graphene-TiO
2the degradation effect block diagram of composite to five kinds of acetamide-group herbicides mixtures (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor).
Fig. 2 is sulfonated Graphene-TiO
2the degradation effect block diagram of composite to seven kinds of organophosphorus insecticides mixtures (containing phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex, methidathion).
Fig. 3 is Graphene-TiO
2the adsorption effect figure of composite to five kinds of acetamide-group herbicides mixtures (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor).
Fig. 4 is Graphene-TiO
2the degradation effect block diagram of composite to five kinds of acetamide-group herbicides mixtures (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor).
Fig. 5 is Graphene-TiO
2the degradation effect block diagram of composite to seven kinds of organophosphorus insecticides mixtures (containing phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex, methidathion).
The specific embodiment
Below in conjunction with specific embodiment, the present invention is conducted further description, but protection domain of the present invention is not limited in this:
Embodiment 1:
According to the synthetic sulfonated Graphene of bibliographical information (Chem.Mater., 1998,10,718-722).
Take sulfonated Graphene as raw material, according to list of references, prepare sulfonated Graphene-TiO
2composite (Int.J.HydrogenEnerg, 2008,37,811-815).Wherein the quality of sulfonated Graphene is 13.369g, and titanium tetrachloride is 6.127mL.
Prepared sulfonated Graphene-TiO
2composite deionized water is washed to neutrality, is diluted to the suspension that concentration is 3000mg/L, ultrasonic it is mixed.
The suspension of 9mL configuration is joined in the water sample that is added with acetamide-group herbicides, vortex 2min, centrifugal 5min, discards water layer, then adds heartily water of 4mL, and vortex 30s mixes it.Get 2mL suspension and be placed under simulated solar irradiation, difference illumination 1h, 2h, 4h and 5h, and control experiment is set.
Illumination finishes to add in backward suspension 4mL ethyl acetate, ultrasonic 5min.Standing 5min, gets 1mL upper strata organic layer, after dewatering, crosses 0.22 μ m organic phase filter membrane, enters GC-MS and detects.
Result shows sulfonated Graphene-TiO
2composite is fine to the photocatalytic degradation effect of five kinds of acetamide-group herbicides (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor), reaches degradation amount and reach 53.4%～75.5% after illumination 4h.
Embodiment 2:
According to the synthetic sulfonated Graphene of bibliographical information (Chem.Mater., 1998,10,718-722).
Take sulfonated Graphene as raw material, according to list of references, prepare sulfonated Graphene-TiO
2composite (Int.J.HydrogenEnerg, 2008,37,811-815).Wherein the quality of sulfonated Graphene is 13.369g, and titanium tetrachloride is 6.127mL.
Prepared sulfonated Graphene-TiO
2composite deionized water is washed to neutrality, is diluted to the suspension that concentration is 3000mg/L, ultrasonic it is mixed.
The suspension of 9mL configuration is joined in the water sample that is added with organophosphorus insecticides, vortex 2min, centrifugal 5min, discards water layer, then adds heartily water of 4mL, and vortex 30s mixes it.Get 2mL suspension and be placed under simulated solar irradiation, difference illumination 1h, 2h, 4h and 5h, and control experiment is set.
Illumination finishes to add in backward suspension 4mL acetonitrile, ultrasonic 5min.Standing 5min, gets 1mL upper strata organic layer, after dewatering, crosses 0.22 μ m organic phase filter membrane, enters GC-FPD and detects.
Result shows, result shows that sulfonated Graphene-TiO2 composite has certain photocatalytic degradation effect to seven kinds of organophosphorus insecticideses (containing phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex, methidathion), after illumination 5h, degradation amount reaches 27.0%～39.9%.
Embodiment 3:
According to the method for bibliographical information prepare Graphene-TiO2 composite (Int.J.HydrogenEnerg, 2008,37,811-815).Wherein the quality of graphene oxide is 13.369g, and titanium tetrachloride is 6.127mL.
Prepared Graphene-TiO
2composite deionized water is washed to neutrality, is diluted to the suspension that concentration is 3000mg/L, ultrasonic it is mixed.
The suspension of 9mL configuration is joined in the water sample that is added with acetamide-group herbicides, vortex 2min, centrifugal 5min, discards water layer, add again 10mL ethyl acetate, 3g sodium chloride, vortex 2min, centrifugal, after getting 1mL supernatant and dewatering, cross 0.22 μ m organic phase filter membrane, enter GC-MS and detect.
Result shows Graphene-TiO
2composite is all fine to the adsorption effect of five kinds of acetamide-group herbicides (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor), and adsorption rate is all between 97.0%～100%.
Embodiment 4:
By the Graphene-TiO of 9mL configuration
2composite suspension joins in the water sample that is added with acetamide-group herbicides, vortex 2min, and centrifugal 5min, discards water layer, then adds heartily water of 4mL, and vortex 30s mixes it.Get 2mL suspension and be placed under simulated solar irradiation, difference illumination 1h, 2h, 4h and 5h, and control experiment is set.
Illumination finishes to add in backward suspension 4mL ethyl acetate, ultrasonic 5min.Standing 5min, gets 1mL upper strata organic layer, after dewatering, crosses 0.22 μ m organic phase filter membrane, enters GC-MS and detects.
Result shows that Graphene-TiO2 composite has certain photocatalytic degradation effect to five kinds of acetamide-group herbicides (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor), photocatalytic degradation effect to isopropyl methoxalamine is best, reaches degradation amount and reach 50.9% after illumination 4h.
Embodiment 5:
Graphene-TiO2 composite suspension of 9mL configuration is joined in the water sample that is added with organophosphorus insecticides, vortex 2min, centrifugal 5min, discards water layer, then adds heartily water of 4mL, and vortex 30s mixes it.Get 2mL suspension and be placed under simulated solar irradiation, difference illumination 1h, 2h, 4h and 5h, and control experiment is set.
Illumination finishes to add in backward suspension 4mL acetonitrile, ultrasonic 5min.Standing 5min, gets 1mL upper strata organic layer, after dewatering, crosses 0.22 μ m organic phase filter membrane, enters GC-FPD and detects.
Result shows Graphene-TiO
2composite has certain photocatalytic degradation effect to seven kinds of organophosphorus insecticideses (containing phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex, methidathion) except chlopyrifos, wherein best to the photocatalytic degradation effect of thimet.
Complex chart 1, Fig. 2, Fig. 4, Fig. 5 can find out, sulfonated Graphene-TiO
2composite to the photocatalytic degradation effect of five kinds of acetamide-group herbicides (containing alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine, butachlor) and seven kinds of organophosphorus insecticideses (containing phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex, methidathion) than Graphene-TiO
2the photocatalysis effect of composite is good.
Claims (8)
1. a sulfonated Graphene-TiO
2composite material photocatalyst, is characterized in that: described composite has good adsorption effect to acetamide-group herbicides and organophosphorus insecticides, under simulated solar irradiation to acetamide-group herbicides and the good degradation effect of organophosphorus insecticides.
2. acetamide-group herbicides according to claim 1 are alachlor, Acetochlor, the third careless amine, isopropyl methoxalamine and butachlor.
3. organophosphorus insecticides according to claim 1 is phonamiphos, thimet, pirimiphos-methyl, chlopyrifos, malathion, Entex and methidathion.
4. sulfonated Graphene-TiO according to claim 1
2the preparation method of composite, is characterized in that comprising the following steps:
A) utilize native graphite, by chemical oxidization method, prepare sulfonated Graphene;
B) sulfonated Graphene is scattered in the aqueous solution, dropwise adds 1.46M titanium tetrachloride solution, stir 1 hour;
C) gained mixed solution in reactor 180 ℃ stir 6 hours, gained suspension washs with deionized water, dilutes to obtain the suspension of 3000mg/L.
5. according to claim 1, composite is as follows to the absorption of acetamide-group herbicides and organophosphorus insecticides and degradation experiment method:
A) enrichment: get the sulfonated Graphene-TiO2 of 9mL composite and join in the water sample that 20mL contains amide-type/organophosphorus insecticide, then vortex 2min, makes object be adsorbed on graphene composite material;
B) separation: the step water sample that contains amide-type/organophosphorus insecticide a) is centrifugal, discard water layer, be precipitated thing;
C) illumination: in gained sediment, add 4mL water, vortex or concussion several seconds, pipette 2mL, be placed in solar simulator illumination, and control experiment is set;
D) extract: illumination finishes, and with the ultrasonic extraction of 4mL ethyl acetate, is adsorbed on sulfonated Graphene-TiO
2on undegradable agricultural chemicals, get 1mL upper strata organic layer, dewater, cross the organic mesentery of 0.22 μ L, wait for sample introduction;
E) detect: the sample after mistake film is entered respectively to GC-MS (acetamide-group herbicides)/GC-FPD (organophosphorus insecticides) and detect.
6. method according to claim 4, is also applicable to Graphene-TiO
2the preparation of composite.
7. Graphene-TiO according to claim 6
2the preparation method of composite, is characterized in that:
A) graphene oxide is scattered in the aqueous solution, dropwise adds 1.46M titanium tetrachloride solution, stir 1 hour;
B) gained mixed solution in reactor 180 ℃ stir 6 hours, gained suspension washs with deionized water, dilutes to obtain the suspension of 3000mg/L.
8. Graphene-TiO according to claim 6
2composite also has adsorption-photocatalytic degradation effect to acetamide-group herbicides and organophosphorus insecticides.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815616A (en) * | 2015-05-05 | 2015-08-05 | 河海大学 | Preparation method of layered sulfonated graphene/titanium dioxide composite material and application of the material in the field of sewage treatment |
| CN107308909A (en) * | 2017-05-16 | 2017-11-03 | 江苏城工建设科技有限公司 | The preparation method of sulfonated graphene and its application for handling antibiotic water body |
| CN110327853A (en) * | 2019-07-08 | 2019-10-15 | 浙江工业大学 | A kind of sulfonated graphene aeroge and its preparation method and application of titanium dioxide quantum dot load |
| CN110404519A (en) * | 2019-09-04 | 2019-11-05 | 安徽省聚科石墨烯科技股份公司 | A kind of graphene aerogel adsorbent detected for phenylurea analog herbicide in water |
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| CN101474899A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
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2013
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Patent Citations (2)
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| CN101474899A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
| US20110121240A1 (en) * | 2009-11-23 | 2011-05-26 | Khalil Amine | Coated electroactive materials |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815616A (en) * | 2015-05-05 | 2015-08-05 | 河海大学 | Preparation method of layered sulfonated graphene/titanium dioxide composite material and application of the material in the field of sewage treatment |
| CN107308909A (en) * | 2017-05-16 | 2017-11-03 | 江苏城工建设科技有限公司 | The preparation method of sulfonated graphene and its application for handling antibiotic water body |
| CN110327853A (en) * | 2019-07-08 | 2019-10-15 | 浙江工业大学 | A kind of sulfonated graphene aeroge and its preparation method and application of titanium dioxide quantum dot load |
| CN110327853B (en) * | 2019-07-08 | 2021-09-07 | 浙江工业大学 | Sulfonated graphene aerogel loaded with titanium dioxide quantum dots as well as preparation method and application of sulfonated graphene aerogel |
| CN110404519A (en) * | 2019-09-04 | 2019-11-05 | 安徽省聚科石墨烯科技股份公司 | A kind of graphene aerogel adsorbent detected for phenylurea analog herbicide in water |
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Application publication date: 20140326 |