CN100342784C - Method for organochlorine pesticide photocatalytic degradation on nano titania - Google Patents
Method for organochlorine pesticide photocatalytic degradation on nano titania Download PDFInfo
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- CN100342784C CN100342784C CNB2006100708627A CN200610070862A CN100342784C CN 100342784 C CN100342784 C CN 100342784C CN B2006100708627 A CNB2006100708627 A CN B2006100708627A CN 200610070862 A CN200610070862 A CN 200610070862A CN 100342784 C CN100342784 C CN 100342784C
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Abstract
The present invention provides a method for the lustring catalytic degradation of organochlorine pesticide on nano TiO2, which relates to organochlorine pesticide, particularly to a method for degradating and converting the organochlorine pesticide in contamination. The present invention provides a rapid and simple conversion method for organochlorine pesticide in normal temperature with low cost. The present invention takes pesticide standard which is prepared by acetone, the acetone can be weathered via the air blast sweep of N2, and nano TiO2 powder and water can be added so as to attain the mixing suspending liquid of the TiO2 and the pesticide. After ultrasonic oscillation, air can be led into the mixing suspension liquid of the TiO2 and the pesticide, the mixing suspension liquid can be directly irradiated by an ultraviolet sterilizing lamp, and the TiO2 powder can be filtered by a filter after photocatalytic degradation. The filtered solutions can be extracted by hexane so as to remove water phase, and remaining organic phase is the target product. The present invention has the advantages of environmental protection, low cost, simple entire degradation process and low time consumption, the present invention can satisfy the requirements of the pesticide degradation of organochlorine in 30 min, and the present invention can be used for processing organochlorine pesticide in waste water or other aspects.
Description
Technical field
The present invention relates to a kind of organo-chlorine pesticide, especially relate to a kind of method of degraded and the conversion applicable to organo-chlorine pesticide in the pollutant.
Background technology
In agricultural chemicals family, organic chlorine agriculture chemicals occupies suitable ratio.The organo-chlorine pesticide acute toxicity is little, but because its chemical property is stable, in environment degraded very slow, residual easily and enter human body by the effect of accumulating with food chain in the animal and plant body, cause harm to health.Particularly hexachlorcyclohexane and dichlorodiphenyl trichloroethane agricultural chemicals, these two kinds of agricultural chemicals do not resemble and are easy to decompose and transform other organic pollutants, but extended residual is in environment, and can enter human body by food chain, and health is caused great harm.China has forbidden the use of this type of agricultural chemicals in nineteen eighty-three, use chloride or produce the phenomenon of chloride metabolite agricultural chemicals but still have in vegetables, tealeaves cultivation and production at present.Except that hexachlorcyclohexane and these two kinds of common organo-chlorine pesticides of dichlorodiphenyl trichloroethane, also having dieldrin, aldrin, endrin and heptachlor etc. all is to have highly toxic material.Therefore significant to the Degradation and Transformation of organo-chlorine pesticide.
Set up a kind of method that can transform organo-chlorine pesticide fast, not only help protecting environment, and our growth in the living standard is provided safeguard.The biodegrading process of at present common organo-chlorine pesticide is degraded (kingdom's favour, the screening of organo-chlorine pesticide efficient degrading bacteria and the research of degradation capability thereof, environmental protection, 2004,8:12-14 such as kingdom's favour to organo-chlorine pesticide for utilizing microorganism; Fang Ling, the microbial strains separation screening and the effect of degraded organo-chlorine pesticide, Chinese Journal of Applied Ecology, 2000,11 (2): 249-252) utilize the organic chlorine degradation bacterium to realize to organochlorine weed killer herbicide 2, the degraded of 4-D, but this bacterial classification can only be to single organo-chlorine pesticide degraded, and organo-chlorine pesticide when being in higher concentration the activity of bacterial classification can be suppressed, culture of strains bothers very much simultaneously, bacterial classification requirement to temperature when degraded is relatively stricter, only under its best temperature higher degradation rate is arranged.(Zhang Shaoyuan etc. such as Zhang Shaoyuan, the application of ozone oxidation organic pollutant in degrading waste water, external environmental science and technology, 1997,2:32-34) utilize pollutant in the ozone oxidation degrading waste water, utilize ozone oxidation degrading pesticide waste water, though also can degrade to Multiple Pesticides, but degradation time is long, 3～5h, and the manufacturing expense of ozone is than higher.Dechlorinating process also is to eliminate organo-chlorine pesticide, reduces a kind of method of its toxicity.(Annegret K.Hall, et al, Mechanochemical reaction of DDT with calcium oxide, Environmentalscience ﹠amp such as Annegret K.Hall; Technology, 1996,30 (12): 3401-3407) utilize the mechanical ball milling technology, CaO and DDT (dichlorodiphenyl trichloroethane) are mixed, in argon atmosphere, ball milling in steel cylinder, through behind the 12h, DDT dechlorination substantially has higher dechlorination rate.But the method is consuming time long, and will be in the argon atmosphere, and expense is relatively more expensive.Therefore develop a kind of quick, easy, organo-chlorine pesticide method for transformation cheaply, make its research that is degraded to little molecule or hypotoxic material be subjected to people's attention.
In the last few years, existing both at home and abroad much relevant for using oxide to come the bibliographical information of photocatalytic degradation organochlorine material, PtO is arranged
2, SiO
2, TiO
2And the catalyzer of some multiple oxide-bonded uses, because nano-TiO
2Have nontoxic and the catalytic efficiency advantages of higher, therefore use TiO
2It is in the majority to do Photodegradation catalyst.(E.Moctezuma, et al.Photocatalytic degradation of the herbicide " paraquat ", Chemoshere, 1999,39 (3): 511-517) use TiO such as E.Moctezuma
2Paraquat (two chloro-1 of under UV, degrading, 1 '-dimethyl-4.4 '-pyridine), (M.H ü g ü l such as M.H ü g ü l, et al.Photocatalytic decomposition of 4-chlorophenol over oxide catalysts, Journal of HazardousMaterial B, 1999,64:313-322) use PtO
2/ TiO
2Degraded 4-chlorophenol under UV, and the catalysis time ratio is shorter.(Alessandra Bianco Prevot such as Alessandra Bianco Prevot, et al.Analytical monitoring ofphotocatalytic treatments.Degradationof 2,3,6-trichlorobenzoic acid in aqueous TiO2 dispersions, Talanta, 1999,48:847-857) use TiO
2The aqueous-phase suspending system is catalytic degradation 2,3 under visible light, and the 6-trichlorobenzoic acid is converted into the inorganic chlorine ion.
Summary of the invention
The objective of the invention is to the deficiency that exists at the existing method that organic oxygen agricultural chemicals is degraded, provide a kind of fast and convenient, low-cost, just can realize method at normal temperatures the quick conversion of organo-chlorine pesticide.
Step of the present invention is:
1) takes the standard sample of pesticide that acetone is prepared, place reaction unit, at N
2Air-blowing is swept down solvent acetone is dried up;
2) in reaction unit, add nano-TiO
2Powder and water, mix TiO
2With the agricultural chemicals mixing suspension, control TiO
2Concentration be 0.25～1.0mg/mL, the concentration of standard sample of pesticide is 0.1～1.0 μ g/mL, with TiO
2With agricultural chemicals mixing suspension sonic oscillation, make TiO
2Particle is uniformly dispersed, described nano-TiO
2The diameter of powder is 20～50nm, described nano-TiO
2Can select anatase for use;
3) with TiO
2With agricultural chemicals mixing suspension bubbling air, use the ultraviolet germicidal direct irradiation at TiO
2On the agricultural chemicals mixing suspension, through photocatalytic degradation, the flow velocity of air is preferably 80～150mL/min, and the photocatalysis time is preferably 15～90min;
4) will be through the TiO of photocatalytic degradation
2With the agricultural chemicals mixing suspension, remove by filter powder TiO with filter
2, with the solution n-hexane extraction after filtering, aqueous phase discarded, gained organic facies are target product, described filter preferably adopts≤and the syringe filters of 0.45 μ m.
The gained target product can be after testing, analyze, handle and calculate, and obtains its degradation rate.
Compare with the existing method that organo-chlorine pesticide is degraded, outstanding advantage of the present invention is: (1) photocatalytic degradation organo-chlorine pesticide is environmentally friendly, and cost is low; (2) whole degradation process method is easy, and weak point consuming time can satisfy the requirement of organo-chlorine pesticide degraded substantially within 30min, is expected to be applied to sewage or otherwise organo-chlorine pesticide and handles; (3) the present invention can carry out Degradation and Transformation to multiple organo-chlorine pesticide.
Description of drawings
Fig. 1 and 2 is organo-chlorine pesticide degradation rate and light degradation time relation.In Fig. 1 and 2, abscissa is represented photocatalytic degradation time t/min, and ordinate is represented the light degradation rate n/% of various agricultural chemicals.
Fig. 3 is the degradation rates of various agricultural chemicals under photocatalysis and illumination condition.In Fig. 3, abscissa is represented photocatalytic degradation time t/min, and ordinate is represented the light degradation rate n/% of various agricultural chemicals.
Fig. 4 is TiO
2The relation of concentration and organo-chlorine pesticide degradation rate.In Fig. 4, abscissa is represented TiO
2Concentration mg/mL, ordinate represent the light degradation rate n/% of various organo-chlorine pesticides.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Embodiment 1
Organo-chlorine pesticide is expelled to contains the Powdered nano-TiO that diameter is 35nm
2In the distilled water, the concentration that makes organo-chlorine pesticide in the solution is 100ppb, nano-TiO
2Concentration is 0.50mg/mL, feeding flow velocity is the air of 100mL/min, after the ultrasonic mixing of this solution, strong agitation on magnetic stirring apparatus, and with ultra violet lamp photocatalytic degradation 30min, ultraviolet source is the ultraviolet germicidal of 30W, and its radiation wavelength is 254nm, and uviol lamp places 9～10cm place, solution top.Reacted solution is crossed the syringe filters of 0.45 μ m to remove powder TiO
2With the solution n-hexane extraction after filtering, aqueous phase discarded, the product of gained organic facies after GC-ECD check and analysis degraded, the most organo-chlorine pesticide in surface its degraded productive rate after reacting can reach more than 90%, and other difficult degradations as β-BHC (β-hexachlorcyclohexane), 5-BHC (δ-hexachlorcyclohexane), its degradation rate also reaches more than 40%.The degradation rate of α-BHC, β-BHC, γ-BHC, δ-BHC, aldrin, dieldrin and endrin is referring to Fig. 1.The nano-TiO that is adopted
2Be anatase.
Embodiment 2
With 12 kinds of organo-chlorine pesticides such as α-BHC, β-BHC, γ-BHC, δ-BHC, aldrin, dieldrin, endrin, Biphenthrin, betacyfluthrin, cypermethrin, sumicidin and heptachlor and the chrysanthemum ester that contains the chlorine element, wherein betacyfluthrin concentration is 400ppb, other are 100ppb, TiO
2Consumption is 0.50mg/mL, and diameter is 50nm, and air mass flow is 90mL/min, and the selective light degradation time is respectively 15,30, and 60min carries out photocatalytic degradation.Reacted solution is crossed the syringe filters of 0.45 μ m to remove powder TiO
2, with the solution n-hexane extraction after filtering, aqueous phase discarded, the product of the organic facies of gained after GC-ECD check and analysis degraded.With α-BHC (α-hexachlorcyclohexane) is example, and by analysis and calculate, 15,30, the degradation rate of 60min is respectively 83.67%, 90.17%, 97.19%, is respectively 41.87%, 84.14% for the dieldrin degradation rate, 86.47%; And to the β-BHC of difficult degradation, the growth of its degradation rate is more obvious, and degradation rate is respectively 12.52%, 37.67%, 75.02%; For the material that chrysanthemum ester, heptachlor, aldrin etc. are degraded extremely easily, its degradation rate just reaches more than 90% when 15min, and it is very little to increase its degradation rate variation with light application time.The relation of degradation of pesticide rate and light application time is referring to Fig. 1 and 2.
Embodiment 3
With above-mentioned 12 kinds of organo-chlorine pesticides and the chrysanthemum ester that contains the chlorine element, wherein betacyfluthrin concentration is for being 160ppb, and other are 40ppb, and air mass flow is 120mL/min, and carrying out illumination (does not have nano-TiO
2) and photocatalytic degradation (TiO
2Consumption is 0.25mg/mL) comparison, degradation time 30min.Solution n-hexane extraction after direct sunshine shines.The photocatalytic degradation reacted solution is crossed the syringe filters of 0.45 μ m to remove powder TiO
2, with the solution n-hexane extraction after filtering, aqueous phase discarded, the product of the organic facies of gained after GC-ECD check and analysis degraded.The most obvious with dieldrin and endrin, their degradation rates under illumination condition are respectively 6.57% and 2.90%, and degradation rate can reach 94.08% and 93.57% respectively in photocatalytic degradation, and therefore explanation has TiO
2The photocatalytic degradation that participates in is highly beneficial to degradation of pesticide, and this mainly is because the oxidation of active hydroxyl radical free radical and superoxide ion radical pair agricultural chemicals causes.This has very strong absorption spectrum in the ultra-violet (UV) band owing to these agricultural chemicals simultaneously, and the main radiation wavelength of ultraviolet germicidal just in time drops on this absorption region at 254nm, and during therefore even without catalyzer, the degraded of chrysanthemum ester and aldrin etc. is also apparent in view.The degradation rate of various agricultural chemicals under photocatalysis and illumination condition seen Fig. 3.
Embodiment 4
With above-mentioned 12 kinds of organo-chlorine pesticides and the chrysanthemum ester that contains the chlorine element, wherein betacyfluthrin concentration is 400ppb, and other are 100ppb, and air mass flow is 100mL/min, and the light degradation time is respectively 30min, selects TiO
2Consumption is respectively and is 0.25mg/mL, 0.50mg/mL, and 1.0mg/mL carries out photocatalytic degradation.Reacted solution is crossed the syringe filters of 0.45 μ m to remove powder TiO
2, with the solution n-hexane extraction after filtering, aqueous phase discarded, the product of the organic facies of gained after GC-ECD check and analysis degraded.As calculated, be example with α-BHC, at TiO
2Consumption is 0.25mg/mL, 0.50mg/mL, and during 1.0mg/mL, its degraded productive rate is respectively 85.40%, 90.17%, 93.83%; For β-BHC, the degraded productive rate is respectively 22.93%, 37.67%, 47.86%; To endrin, the degraded productive rate is respectively 83.71%, 84.21%, 92.92%; For heptachlor, aldrin and chrysanthemum ester class, TiO
2Concentration little to the influence of its degradation rate, in selected several concentration, its degradation rate substantially all reaches more than 90%, sumicidin can be degraded fully.Various agricultural chemicals are at the TiO of variable concentrations
2Degradation rate under the condition is seen Fig. 4.
Embodiment 5
Similar to Example 1, its difference is that the flow velocity of air is 80mL/min, Powdered nano-TiO
2Diameter be 40nm, ultra violet lamp photocatalytic degradation 80min.
Embodiment 6
Similar to Example 1, its difference is that the flow velocity of air is 150mL/min, Powdered nano-TiO
2Diameter be 20nm, ultra violet lamp photocatalytic degradation 90min.
The nano-TiO of the said Detitanium-ore-type of the present invention
2Can be synthetic voluntarily by Hydrolyze method.Nano-TiO
2Building-up process is: with TiCl
4As presoma, at ice-water bath with under stirring, with TiCl
4Dropwise slowly splash in the distilled water, the aqueous solution that will be dissolved with ammonium sulfate and concentrated hydrochloric acid then is added drop-wise to the TiCl of gained
4In the aqueous solution, stir, temperature is controlled at 0～15 ℃ in the mixed process.After mixture is warming up to boiling water bath and is incubated 1～2h, add concentrated ammonia liquor and regulate pH value to 8～9.Ageing 10～20h, filtering the back can influence the chlorion of experimental result (with the AgNO of 0.1mol/L with the distilled water flush away
3The solution check) after, more than one time, filters under the room temperature condition of back and will precipitate vacuum drying, with the calcining under 700～900 ℃ of the powder after the vacuum drying, promptly obtain needed nano-titanium oxide powder at last, experiment control TiCl with absolute ethanol washing
4With the volume ratio of distilled water and dense salt be 1: 8: 0.4～1: 12: 0.6, TiCl
4With ammonium sulfate be 1: 1.8～1: 2.0 according to the ratio of amount of substance.
Claims (7)
1, organo-chlorine pesticide photocatalytic degradation method on nano titanium oxide is characterized in that the steps include:
1) takes the organo-chlorine pesticide that acetone is prepared, place reaction unit, at N
2Air-blowing is swept down solvent acetone is dried up;
2) in reaction unit, add nano-TiO
2Powder and water get TiO
2With the organo-chlorine pesticide mixing suspension, control TiO
2Concentration be 0.25～1.0mg/mL, the concentration of organo-chlorine pesticide is 0.1～1.0 μ g/mL;
3) with TiO
2With organo-chlorine pesticide mixing suspension bubbling air, use the ultraviolet germicidal direct irradiation at TiO
2On the organo-chlorine pesticide mixing suspension, through photocatalytic degradation;
4) will be through the TiO of photocatalytic degradation
2With the organo-chlorine pesticide mixing suspension, remove by filter powder TiO with filter
2, with the solution n-hexane extraction after filtering, aqueous phase discarded, gained organic facies are target product.
2, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide is characterized in that in step 2) in, in reaction unit, add nano-TiO
2Behind powder and the water, with TiO
2With organo-chlorine pesticide mixing suspension sonic oscillation, make TiO
2Particle is uniformly dispersed.
3, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide is characterized in that described nano-TiO
2The diameter of powder is 20～50nm.
4, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide is characterized in that described nano-TiO
2Be anatase.
5, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide, the flow velocity that it is characterized in that bubbling air is 80～150mL/min.
6, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide is characterized in that the photocatalysis time is 15～90min.
7, organo-chlorine pesticide as claimed in claim 1 photocatalytic degradation method on nano titanium oxide is characterized in that described filter adopts the syringe filters of≤0.45 μ m.
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| CN100591626C (en) * | 2008-09-08 | 2010-02-24 | 北京联合大学生物化学工程学院 | Method for degrading subaqueous organochlorine pesticide in water by photocatalysis |
| CN102120631B (en) * | 2010-12-07 | 2012-07-18 | 北京联合大学生物化学工程学院 | Photocatalytic degradation method of pyrethroid pesticide in water |
| CN102764758A (en) * | 2012-08-02 | 2012-11-07 | 大连民族学院 | DDT (dichloro-diphenyl-trichloroethane) contaminated soil combined remediation method by ultraviolet rays, alfalfa and DDT degrading bacteria |
| CN104055198A (en) * | 2014-06-10 | 2014-09-24 | 湖南省农产品加工研究所 | Method for degrading pesticide residues on fruit and vegetables |
| CN104042626A (en) * | 2014-07-01 | 2014-09-17 | 李绍明 | Bactericidal and bacteriostatic agent |
| CN104287063A (en) * | 2014-09-17 | 2015-01-21 | 中国人民解放军总后勤部军需装备研究所 | Fruit and vegetable deep cleaning and processing device |
| CN105851000A (en) * | 2016-04-27 | 2016-08-17 | 贺州学院 | Nano titanium dioxide compound abamectin pesticide and preparation method thereof |
| CN105815330A (en) * | 2016-04-27 | 2016-08-03 | 贺州学院 | Nanometer titanium dioxide composite cypermethrin pesticide and preparation method thereof |
| CN105851001A (en) * | 2016-04-27 | 2016-08-17 | 贺州学院 | Nano titanium dioxide compound chlorpyrifos pesticide and preparation method thereof |
| CN112400868A (en) * | 2020-12-01 | 2021-02-26 | 南京拓呗新材料科技有限公司 | Nano pesticide and preparation method thereof |
| CN115067313A (en) * | 2022-06-29 | 2022-09-20 | 广西壮族自治区农业科学院 | Method for fumigating and killing soil-dwelling termites by smoke |
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| WO2005105304A2 (en) * | 2004-04-30 | 2005-11-10 | Leibniz-Institut Für Neue Materialien Gemeinnützige Gmbh | Use of photocatalytic tio2 layers for functionalizing substrates |
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| CN1504555A (en) * | 2002-11-29 | 2004-06-16 | 深圳市永吉实业有限公司 | Purpose for modified photocatalyst nanometer composite material |
| JP2005218957A (en) * | 2004-02-05 | 2005-08-18 | Japan Atom Energy Res Inst | Visible light-responsive titanium dioxide photocatalyst thin film and manufacturing method therefor |
| WO2005105304A2 (en) * | 2004-04-30 | 2005-11-10 | Leibniz-Institut Für Neue Materialien Gemeinnützige Gmbh | Use of photocatalytic tio2 layers for functionalizing substrates |
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