CN103058446A - Method for removing pesticide residues in water body by using magnetic titanium oxide micellar system - Google Patents
Method for removing pesticide residues in water body by using magnetic titanium oxide micellar system Download PDFInfo
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- CN103058446A CN103058446A CN2013100268839A CN201310026883A CN103058446A CN 103058446 A CN103058446 A CN 103058446A CN 2013100268839 A CN2013100268839 A CN 2013100268839A CN 201310026883 A CN201310026883 A CN 201310026883A CN 103058446 A CN103058446 A CN 103058446A
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Abstract
The invention discloses a method for removing pesticide residues in a water body by using a magnetic titanium oxide micellar system and relates to a method of removing the pesticide residues in the water body. The method aims to solve the problems that the technology of removing the pesticide residues in the water body is complicated in technology, high in treatment cost and low in removal efficiency. The method comprises the following steps of: firstly, preparing Fe2O4 magnetic fluid; secondly, preparing magnetic titanium oxide nanoparticles; and thirdly, removing the pesticide residues, i.e. finishing the removal of the pesticide residues in the water body to be treated, thereby obtaining the treated water body. The method for removing the pesticide residues in the water body by using the magnetic titanium oxide micellar system is mainly used for removing the pesticide residues in the water body.
Description
Technical field
The present invention relates to a kind of method of removing the water body Pesticide Residues.
Background technology
Along with the development of modern agriculture, the pesticide species that uses in the world wide is more and more, and consumption constantly increases, and pesticide residue cause environmental pollution, cause the destruction of ecosystem structure and function, are subject to already extensive concern both domestic and external.According to relevant report, chemical pesticide is in application, and only having an appointment 20% directly remains on the crop, and remaining then enters soil, underground water by natural subsidence, precipitation, and quite a few is entering lake, river with the earth's surface runoff.For a long time, after a large amount of all kinds of agricultural chemicals that use enter water surrounding, the series of problems such as many water environment pollutions, ecosystem destruction, food safety have been caused.Therefore the removal method of studying simple and convenient efficiently water surrounding Pesticides is all very necessary with human health existence for preserving the ecological environment.At present, the removal method of insecticide pollution mainly contains active carbon adsorption, biological degradation method and oxidation style etc.Yet these methods exist mostly that treatment process is loaded down with trivial details, processing cost is high and remove the shortcomings such as efficient is low.
The in recent years ionogenic surfactant self-assembly behavior that is adsorbed on metal oxide surface is paid close attention to by the physical chemist, ionogenic surfactant can form the mixed micelle self-assembly system on the surface of the metal oxides such as aluminum oxide, silicon-dioxide, ferric oxide, generally has very strong adsorptive power about studies show that the solid phase extraction based on this unit molecule/bimolecular mixed micelle absorption system is set up for hydrophobic type, amphiphilic and ionic organic compound.
In sum, the pesticide residue removal technology in the existing environmental water sample exists that technique is loaded down with trivial details, processing cost is high and remove inefficient problem.
Summary of the invention
The objective of the invention is to solve pesticide residue removal technology in the water body and have that technique is loaded down with trivial details, processing cost is high and remove inefficient problem, and a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues is provided.
A kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues is specifically finished: one, preparation Fe according to the following steps
3O
4Magnetic fluid: at first with FeCl
24H
2O and FeCl
36H
2O is dissolved in the distilled water fully, and low whipping speed is to be warming up to 80 ℃～90 ℃ from room temperature under 400rmp～600rmp, then adds NH
3H
2O, and be that 80 ℃～90 ℃ and stirring velocity are to react 0.5h～1.5h under 400rmp～600rmp condition in temperature, then utilize magnet to carry out magnetic resolution, obtain the black solid product, adopt distilled water wash black solid product, the wastewater pH after washing is extremely washed is till the neutrality, namely obtains Fe
3O
4Magnetic fluid; FeCl described in the step 1
24H
2O and FeCl
36H
2The mol ratio of O is 1:(1.9～2); FeCl described in the step 1
24H
2O and NH
3H
2The mol ratio of O is 1:(8～9);
Two, the magnetic oxygenated titanium nano particle of preparation: at first with Fe
3O
4Magnetic fluid joins in the distilled water, then adds TiCl
4And low whipping speed is to stir 10min～20min under 400rmp～600rmp, add again aqueous sodium hydroxide solution the pH value is adjusted to 8.5～9.5, continuing low whipping speed is to stir 5min～15min under 400rmp～600rmp, then be 140 ℃～160 ℃ lower reaction 5h～8h in temperature, namely obtain the brown solid product, adopt distilled water wash brown solid product, wastewater pH after washing is extremely washed is till the neutrality, obtain washing rear brown solid product, then be under 80 ℃～100 ℃ brown solid product after washing to be dried in temperature, dry to constant weight and namely obtain magnetic oxygenated titanium nano particle; Fe described in the step 2
3O
4The quality of magnetic fluid and the volume ratio of distilled water are 1g:(30mL～80mL); Fe described in the step 2
3O
4The quality of magnetic fluid and TiCl
4Volume ratio be 1g:(1mL～2mL);
Three, remove pesticide residue: at first magnetic oxygenated titanium nano particle and tensio-active agent are joined in the staying water, then low whipping speed is to stir 1min～40min under 300rmp～600rmp, then utilize magnet to carry out magnetic resolution, draw supernatant liquor, adopt 0.2 μ m filter membrane that supernatant liquor is filtered, namely finish the removal of staying water Pesticide Residues after the filtration, obtain processing rear water body; Described magnetic oxygenated titanium nano particle and tensio-active agent mass ratio are 1:(0.5～1.5); The quality of described magnetic oxygenated titanium nano particle and the volume ratio of staying water are 1g:(2L～10L).
Advantage of the present invention: one, the present invention prepares that the method for magnetic oxygenated titanium nano particle is simple, condition is easy to control, and the magnetic oxygenated titanium nano particle of the present invention's preparation has good superparamagnetism, and its saturation magnetization can arrive 20emug
-1～35emug
-1Two, magnetic oxygenated titanium nano particle and the tensio-active agent of the present invention's preparation carry out combination, form magnetic oxygenated titanium micellar system, magnetic oxygenated titanium micellar system is a kind of novel remover, the got both bigger serface of nano material of this remover, the superparamagnetism of magneticsubstance, TiO
2Good stability and the ability of removing more by force of mixed micelle, when being used for removing the pesticide residue of water body, at short notice, clearance can reach more than 95%, and the method is simple to operate, processing cost is low, and the condition such as the concentration by optimal control option table surface-active agent, pH value of solution, can be used for the removal of different sorts pesticide residue.
Description of drawings
Fig. 1 is the magnetic oxygenated titanium nano particle SEM figure of test one step 2 preparation; Fig. 2 is the Fourier infrared spectrum figure of the magnetic oxygenated titanium nano particle of test one step 2 preparation; Fig. 3 tests the magnetic hysteresis loop of the magnetic oxygenated titanium nano particle of step 2 preparation; Fig. 4 is liquid chromatogram, and A represents to test the liquid chromatogram of ten described staying waters among the figure, and B represents to test the liquid chromatogram of water body after the ten described processing among the figure, and a represents the absorption peak of cyhalothrin among the figure; Fig. 5 is for testing six to the 11 magnetic oxygenated titanium mixed micelle systems that form to the kinetics adsorption curve of agricultural chemicals cyhalothrin; Fig. 6 is the first order kinetics matched curve of the magnetic oxygenated titanium micellar system absorption cyhalothrin of test six to 11 formation; Fig. 7 is the second-order kinetics matched curve of the magnetic oxygenated titanium micellar system absorption cyhalothrin of test six to 11 formation.
Embodiment
Embodiment one: present embodiment is a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues, specifically finishes according to the following steps: one, preparation Fe
3O
4Magnetic fluid: at first with FeCl
24H
2O and FeCl
36H
2O is dissolved in the distilled water fully, and low whipping speed is to be warming up to 80 ℃～90 ℃ from room temperature under 400rmp～600rmp, then adds NH
3H
2O, and be that 80 ℃～90 ℃ and stirring velocity are to react 0.5h～1.5h under 400rmp～600rmp condition in temperature, then utilize magnet to carry out magnetic resolution, obtain the black solid product, adopt distilled water wash black solid product, the wastewater pH after washing is extremely washed is till the neutrality, namely obtains Fe
3O
4Magnetic fluid;
Two, the magnetic oxygenated titanium nano particle of preparation: at first with Fe
3O
4Magnetic fluid joins in the distilled water, then adds TiCl
4And low whipping speed is to stir 10min～20min under 400rmp～600rmp, add again aqueous sodium hydroxide solution the pH value is adjusted to 8.5～9.5, continuing low whipping speed is to stir 5min～15min under 400rmp～600rmp, then be 140 ℃～160 ℃ lower reaction 5h～8h in temperature, namely obtain the brown solid product, adopt distilled water wash brown solid product, wastewater pH after washing is extremely washed is till the neutrality, obtain washing rear brown solid product, then be under 80 ℃～100 ℃ brown solid product after washing to be dried in temperature, dry to constant weight and namely obtain magnetic oxygenated titanium nano particle;
Three, remove pesticide residue: at first magnetic oxygenated titanium nano particle and tensio-active agent are joined in the staying water, then low whipping speed is to stir 1min～40min under 300rmp～600rmp, then utilize magnet to carry out magnetic resolution, draw supernatant liquor, adopt 0.2 μ m filter membrane that supernatant liquor is filtered, namely finish the removal of staying water Pesticide Residues after the filtration, obtain processing rear water body.
FeCl described in the present embodiment step 1
24H
2O and FeCl
36H
2The mol ratio of O is 1:(1.9～2); FeCl described in the present embodiment step 1
24H
2O and NH
3H
2The mol ratio of O is 1:(8～9).
Fe described in the present embodiment step 2
3O
4The quality of magnetic fluid and the volume ratio of distilled water are 1g:(30mL～80mL); Fe described in the present embodiment step 2
3O
4The quality of magnetic fluid and TiCl
4Volume ratio be 1g:(1mL～2mL).
Magnetic oxygenated titanium nano particle described in the present embodiment step 3 and tensio-active agent mass ratio are 1:(0.5～1.5); The quality of the magnetic oxygenated titanium nano particle described in the present embodiment step 3 and the volume ratio of staying water are 1g:(2L～10L).
The method that present embodiment prepares magnetic oxygenated titanium nano particle is simple, condition is easy to control, and the magnetic oxygenated titanium nano particle of present embodiment preparation has good superparamagnetism, and its saturation magnetization can arrive 20emug
-1～35emug
-1
Embodiment two: the difference of present embodiment and embodiment one is: low whipping speed is to be warming up to 80 ℃～88 ℃ from room temperature under 450rmp～550rmp in the step 1.Other are identical with embodiment one.
Embodiment three: present embodiment and one of embodiment one or two difference are: being 80 ℃～88 ℃ in temperature in the step 1 is to react 0.8h～1.2h under 450rmp～550rmp condition with stirring velocity.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: in the step 2 with Fe
3O
4Magnetic fluid joins in the distilled water, then adds TiCl
4, and low whipping speed is to stir 12min～18min under 450rmp～550rmp.Other are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: add aqueous sodium hydroxide solution in the step 2 pH value is adjusted to 8.6～9.4, continuing low whipping speed is to stir 8min～12min under 450rmp～550rmp, then be 145 ℃～155 ℃ lower reaction 5.5h～7.5h in temperature, namely obtain the brown solid product.Other are identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five difference is: the magnetic oxygenated titanium nano particle described in the step 3 and tensio-active agent mass ratio are 1:(0.8～1.2).Other are identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six difference is: the tensio-active agent described in the step 3 is cetyl trimethylammonium bromide, sodium lauryl sulphate or Cetyltrimethylammonium bromide.Other are identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: low whipping speed is to stir 10min～30min under 300rmp～600rmp.Other are identical with embodiment one to seven.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues, specifically finish according to the following steps: one, preparation Fe
3O
4Magnetic fluid: at first with the FeCl of 10mmol
24H
2The FeCl of O and 20mmol
36H
2O is dissolved in the distilled water fully, and low whipping speed is to be warming up to 80 ℃ from room temperature under the 500rmp, then adds the NH of 80mmol
3H
2Then O, and be that 80 ℃ and stirring velocity are to react 1h under the 500rmp condition in temperature utilizes magnet to carry out magnetic resolution, obtains the black solid product, adopts distilled water wash black solid product, and the wastewater pH of washing to the washing is till the neutrality, namely obtains Fe
3O
4Magnetic fluid;
Two, the magnetic oxygenated titanium nano particle of preparation: at first with the Fe of 1g
3O
4Magnetic fluid joins in the distilled water of 50mL, then adds the TiCl of 1mL
4And low whipping speed is to stir 10min under the 500rmp, add again aqueous sodium hydroxide solution the pH value is adjusted to 9 ± 0.1, continuing low whipping speed is to stir 10min under the 500rmp, then be 150 ℃ of lower reaction 6h in temperature, namely obtain the brown solid product, adopt distilled water wash brown solid product, wastewater pH after washing is extremely washed is till the neutrality, obtain washing rear brown solid product, then be under 100 ℃ brown solid product after washing to be dried in temperature, dry to constant weight and namely obtain magnetic oxygenated titanium nano particle;
Three, remove pesticide residue: at first the magnetic oxygenated titanium nano particle of 100mg and the cetyl trimethylammonium bromide of 100mg are joined in the staying water of 500mL, then low whipping speed is to stir 30min under the 500rmp, utilize magnet to carry out magnetic resolution, draw supernatant liquor, adopt 0.2 μ m filter membrane that supernatant liquor is filtered, namely finish the removal of staying water Pesticide Residues after the filtration, obtain processing rear water body.
Staying water described in this testing sequence three is the concentration 0.1mgL of cyhalothrin
-1Water sample.
Magnetic oxygenated titanium nano particle and cetyl trimethylammonium bromide described in this testing sequence three carry out combination, form magnetic oxygenated titanium micellar system, this magnetic oxygenated titanium micellar system is a kind of novel remover, the got both bigger serface of nano material of this remover, the superparamagnetism of magneticsubstance, TiO
2Good stability and the ability of removing more by force of mixed micelle.
Adopt sem observation to test the magnetic oxygenated titanium nano particle of step 2 preparation, detected result as shown in Figure 1, Fig. 1 is the magnetic oxygenated titanium nano particle SEM figure of test one step 2 preparation, the magnetic oxygenated titanium nano particle of testing as shown in Figure 1 step 2 preparation is nano level, thereby having large specific surface area, adsorptive power also can strengthen thereupon.
Adopt Fourier infrared spectrograph to detect the magnetic oxygenated titanium nano particle of test one step 2 preparation, detected result as shown in Figure 2, Fig. 2 is for the Fourier infrared spectrum figure of the magnetic oxygenated titanium nano particle of test one step 2 preparation, as shown in Figure 2 at 580cm
-1There is the absorption peak of Fe-O in the place, at 1390cm
-1There is the absorption peak of Ti-O key in the place, at 3430cm
-1There is the absorption peak of O-H in the place, therefore tests as can be known TiO in the magnetic oxygenated titanium nano particle of step 2 preparation
2Success and Fe
3O
4In conjunction with.
Adopt vibrating sample magnetometer to detect the magnetic oxygenated titanium nano particle of test one step 2 preparation, detected result as shown in Figure 3, Fig. 3 tests the magnetic hysteresis loop of the magnetic oxygenated titanium nano particle of step 2 preparation, and the saturation magnetic field intensity of testing as shown in Figure 3 the magnetic oxygenated titanium nano particle of step 2 preparation is 28.6emug
-1, thereby the magnetic oxygenated titanium nano particle of testing step 2 preparation can be realized sharp separation under the effect of externally-applied magnetic field.
Water body behind the employing high performance liquid chromatography Check processing is processed the concentration of cyhalothrin in the rear water body as can be known for being almost 0mgL
-1, the clearance of cyhalothrin is 100% by calculating as can be known.
Test two: this test with the difference of test one is: the staying water described in the step 3 is the concentration 0.5mgL of cyhalothrin
-1Water sample.Other are identical with test one.
Water body behind the employing high performance liquid chromatography Check processing is processed the concentration of cyhalothrin in the rear water body as can be known for being almost 0mgL
-1, the clearance of cyhalothrin is 100% by calculating as can be known.
Test three: this test with the difference of test one is: the staying water described in the step 3 is the concentration 1.0mgL of cyhalothrin
-1Water sample.Other are identical with test one.
Water body behind the employing high performance liquid chromatography Check processing, the concentration of processing as can be known cyhalothrin in the rear water body is 0.007mgL
-1, the clearance of cyhalothrin is 99.3% by calculating as can be known.
Test four: this test with the difference of test one is: the staying water described in the step 3 is the concentration 5.0mgL of cyhalothrin
-1Water sample.Other are identical with test one.
Water body behind the employing high performance liquid chromatography Check processing, the concentration of processing as can be known cyhalothrin in the rear water body is 0.145mgL
-1, the clearance of cyhalothrin is 97.1% by calculating as can be known.
Test five: this test with the difference of test one is: the staying water described in the step 3 is the concentration 10.0mgL of cyhalothrin
-1Water sample.Other are identical with test one.
Water body behind the employing high performance liquid chromatography Check processing, the concentration of processing as can be known cyhalothrin in the rear water body is 0.460mgL
-1, the clearance of cyhalothrin is 95.4% by calculating as can be known.
Test six: a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues, specifically finish according to the following steps: one, preparation Fe
3O
4Magnetic fluid: the prime minister is with the FeCl of 10mmol
24H
2The FeCl of O and 20mmol
36H
2O is dissolved in the distilled water fully, and low whipping speed is to be warming up to 80 ℃ from room temperature under the 500rmp, then adds the NH of 80mmol
3H
2Then O, and be that 80 ℃ and stirring velocity are to react 1h under the 500rmp condition in temperature utilizes magnet to carry out magnetic resolution, obtains the black solid product, adopts distilled water wash black solid product, and the wastewater pH of washing to the washing is till the neutrality, namely obtains Fe
3O
4Magnetic fluid;
Two, the magnetic oxygenated titanium nano particle of preparation: at first with the Fe of 1g
3O
4Magnetic fluid joins in the distilled water of 50mL, then adds the TiCl of 1mL
4And low whipping speed is to stir 10min under the 500rmp, add again aqueous sodium hydroxide solution the pH value is adjusted to 9 ± 0.1, continuing low whipping speed is to stir 10min under the 500rmp, then be 150 ℃ of lower reaction 6h in temperature, namely obtain the brown solid product, adopt distilled water wash brown solid product, wastewater pH after washing is extremely washed is till the neutrality, obtain washing rear brown solid product, then be under 100 ℃ brown solid product after washing to be dried in temperature, dry to constant weight and namely obtain magnetic oxygenated titanium nano particle;
Three, remove pesticide residue: at first the magnetic oxygenated titanium nano particle of 100mg and the cetyl trimethylammonium bromide of 100mg are joined in the staying water of 500mL, then low whipping speed is to stir 1min under the 500rmp, utilize magnet to carry out magnetic resolution, draw supernatant liquor, adopt 0.2 μ m filter membrane that supernatant liquor is filtered, namely finish the removal of staying water Pesticide Residues after the filtration, obtain processing rear water body.
Staying water described in this testing sequence three is the concentration 2.0mgL of cyhalothrin
-1Water sample.
Magnetic oxygenated titanium nano particle and cetyl trimethylammonium bromide described in this testing sequence three carry out combination, form magnetic oxygenated titanium micellar system, this magnetic oxygenated titanium micellar system is a kind of novel remover, the got both bigger serface of nano material of this remover, the superparamagnetism of magneticsubstance, TiO
2Good stability and the ability of removing more by force of mixed micelle.
Test seven: this test with the difference of test six is: low whipping speed is to stir 5min under the 500rmp.Other are identical with test six.
Test eight: this test with the difference of test six is: low whipping speed is to stir 10min under the 500rmp.Other are identical with test six.
Test nine: this test with the difference of test six is: low whipping speed is to stir 20min under the 500rmp.Other are identical with test six.
Test ten: this test with the difference of test six is: low whipping speed is to stir 30min under the 500rmp.Other are identical with test six.
Water body after adopting high performance liquid chromatography detection test ten described staying waters and testing ten processing that obtain is 85% acetonitrile solution in moving phase, and flow velocity is 1.0mLmin
-1The detection wavelength is 243nm, temperature is that room temperature condition detects, detected result as shown in Figure 4, Fig. 4 is liquid chromatogram, A represents to test the liquid chromatogram of ten described staying waters among the figure, and B represents to test the liquid chromatogram of water body after the ten described processing among the figure, and a represents the absorption peak of cyhalothrin among the figure; As shown in Figure 4, it is fine that test ten utilizes the method removal effect of magnetic oxygenated titanium micellar system removal water body Pesticide Residues.
Test 11: this test with the difference of test six is: low whipping speed is to stir 40min under the 500rmp.Other are identical with test six.
Water body after employing liquid chromatographic detection test six to 11 processing that obtain is according to formula
Calculate Q
t(magnetic oxygenated titanium micellar system is in the adsorptive capacity of different time to cyhalothrin), wherein C
0Be the starting point concentration of cyhalothrin, C
eBe the equilibrium concentration of cyhalothrin, V is the volume of sample solution, and m is the quality of magnetic oxygenated titanium nano particle, can test as calculated six to 11 Q
tBe respectively 1.67mgg
-1, 8.23mgg
-1, 8.65mgg
-1, 9.61mgg
-1, 9.73mgg
-1And 9.96mgg
-1With Q
tBe depicted as kinetics adsorption curve figure for ordinate zou, take the time as X-coordinate, the result as shown in Figure 5, the magnetic oxygenated titanium mixed micelle systems that Fig. 5 forms for test six to 11 are to the kinetics adsorption curve of agricultural chemicals cyhalothrin.Can learn that by Fig. 5 the synthetic polymkeric substance of this experiment is very fast to the kinetics of adsorption of cyhalothrin, in 20min, can reach adsorption equilibrium.
According to the kinetics First-order equation
Curve of adsorption kinetics among Fig. 5 is carried out match, wherein, Q
eRepresent that magnetic oxygenated titanium micellar system is to the equilibrium adsorption capacity of cyhalothrin, Q
tRepresent that magnetic oxygenated titanium micellar system is at the adsorptive capacity of different time, Q
1calThe theoretical adsorptive capacity of expression kinetics First order reaction, k
1Expression kinetics first order reaction rate constant, t represents the time.With ln(Q
e-Q
t) for ordinate zou, carry out match take the time as X-coordinate, the result as shown in Figure 6, Fig. 6 is the first order kinetics matched curve of the magnetic oxygenated titanium micellar system absorption cyhalothrin of test six to 11 formation, carry out match by the Origin7.5 mapping software, obtain the coefficient R of the linear equation of first order kinetics matched curve
2Be 0.9224.
According to kinetics secondary equation
Curve of adsorption kinetics figure among Fig. 5 is carried out match, wherein, Q
tRepresent that magnetic oxygenated titanium micellar system is at the adsorptive capacity of different time, Q
2calThe theoretical adsorptive capacity of expression kinetics second order reaction equation, k
2Expression kinetics first order reaction rate constant, t represents the time.With t/Q
tCarry out match for ordinate zou, take the time as X-coordinate, the result as shown in Figure 7, Fig. 7 is the second-order kinetics matched curve of the magnetic oxygenated titanium micellar system absorption cyhalothrin of test six to 11 formation, carry out match by the Origin7.5 mapping software, obtain the coefficient R of the linear equation of second-order kinetics matched curve
2Be 0.9902, therefore the present invention utilizes the method for magnetic oxygenated titanium micellar system removal water body Pesticide Residues cyhalothrin to meet the second-order kinetics fitting result as can be known.
Claims (8)
1. method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues is characterized in that the method for utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues finishes according to the following steps:
One, preparation Fe
3O
4Magnetic fluid: at first with FeCl
24H
2O and FeCl
36H
2O is dissolved in the distilled water fully, and low whipping speed is to be warming up to 80 ℃～90 ℃ from room temperature under 400rmp～600rmp, then adds NH
3H
2O, and be that 80 ℃～90 ℃ and stirring velocity are to react 0.5h～1.5h under 400rmp～600rmp condition in temperature, then utilize magnet to carry out magnetic resolution, obtain the black solid product, adopt distilled water wash black solid product, the wastewater pH after washing is extremely washed is till the neutrality, namely obtains Fe
3O
4Magnetic fluid; FeCl described in the step 1
24H
2O and FeCl
36H
2The mol ratio of O is 1:(1.9～2); FeCl described in the step 1
24H
2O and NH
3H
2The mol ratio of O is 1:(8～9);
Two, the magnetic oxygenated titanium nano particle of preparation: at first with Fe
3O
4Magnetic fluid joins in the distilled water, then adds TiCl
4And low whipping speed is to stir 10min～20min under 400rmp～600rmp, add again aqueous sodium hydroxide solution the pH value is adjusted to 8.5～9.5, continuing low whipping speed is to stir 5min～15min under 400rmp～600rmp, then be 140 ℃～160 ℃ lower reaction 5h～8h in temperature, namely obtain the brown solid product, adopt distilled water wash brown solid product, wastewater pH after washing is extremely washed is till the neutrality, obtain washing rear brown solid product, then be under 80 ℃～100 ℃ brown solid product after washing to be dried in temperature, dry to constant weight and namely obtain magnetic oxygenated titanium nano particle; Fe described in the step 2
3O
4The quality of magnetic fluid and the volume ratio of distilled water are 1g:(30mL～80mL); Fe described in the step 2
3O
4The quality of magnetic fluid and TiCl
4Volume ratio be 1g:(1mL～2mL);
Three, remove pesticide residue: at first magnetic oxygenated titanium nano particle and tensio-active agent are joined in the staying water, then low whipping speed is to stir 1min～40min under 300rmp～600rmp, then utilize magnet to carry out magnetic resolution, draw supernatant liquor, adopt 0.2 μ m filter membrane that supernatant liquor is filtered, namely finish the removal of staying water Pesticide Residues after the filtration, obtain processing rear water body; Described magnetic oxygenated titanium nano particle and tensio-active agent mass ratio are 1:(0.5～1.5); The quality of described magnetic oxygenated titanium nano particle and the volume ratio of staying water are 1g:(2L～10L).
2. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that low whipping speed is to be warming up to 80 ℃～88 ℃ from room temperature under 450rmp～550rmp in the step 1.
3. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that being 80 ℃～88 ℃ in temperature in the step 1 is to react 0.8h～1.2h under 450rmp～550rmp condition with stirring velocity.
4. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that in the step 2 Fe
3O
4Magnetic fluid joins in the distilled water, then adds TiCl
4, and low whipping speed is to stir 12min～18min under 450rmp～550rmp.
5. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1, it is characterized in that adding in the step 2 aqueous sodium hydroxide solution pH value is adjusted to 8.6～9.4, continuing low whipping speed is to stir 8min～12min under 450rmp～550rmp, then be 145 ℃～155 ℃ lower reaction 5.5h～7.5h in temperature, namely obtain the brown solid product.
6. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that the magnetic oxygenated titanium nano particle described in the step 3 and tensio-active agent mass ratio are 1:(0.8～1.2).
7. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that the tensio-active agent described in the step 3 is cetyl trimethylammonium bromide, sodium lauryl sulphate or Cetyltrimethylammonium bromide.
8. a kind of method of utilizing magnetic oxygenated titanium micellar system to remove the water body Pesticide Residues according to claim 1 is characterized in that low whipping speed is to stir 10min～30min under 300rmp～600rmp.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310026883 CN103058446B (en) | 2013-01-24 | 2013-01-24 | Method for removing pesticide residues in water body by using magnetic titanium oxide micellar system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201310026883 CN103058446B (en) | 2013-01-24 | 2013-01-24 | Method for removing pesticide residues in water body by using magnetic titanium oxide micellar system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004052533A1 (en) * | 2002-12-12 | 2004-06-24 | Henkel Kommanditgesellschaft Auf Aktien | Production of magnetic titanium dioxide particles |
| CN101816937A (en) * | 2009-07-29 | 2010-09-01 | 兰州理工大学 | Method for manufacturing magnetic loading type nanometer catalyst TiO2/Fe2O4 |
| CN102580783A (en) * | 2012-01-09 | 2012-07-18 | 兰州交通大学 | Method for preparing TiO2/PS/Fe3O4 magnetic nanoparticle photocatalyst |
| CN102580782A (en) * | 2012-01-09 | 2012-07-18 | 兰州交通大学 | Method for preparing magnetically-supported catalyst TiO2/polypyrrole (PPY)/Fe3O4 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004052533A1 (en) * | 2002-12-12 | 2004-06-24 | Henkel Kommanditgesellschaft Auf Aktien | Production of magnetic titanium dioxide particles |
| CN101816937A (en) * | 2009-07-29 | 2010-09-01 | 兰州理工大学 | Method for manufacturing magnetic loading type nanometer catalyst TiO2/Fe2O4 |
| CN102580783A (en) * | 2012-01-09 | 2012-07-18 | 兰州交通大学 | Method for preparing TiO2/PS/Fe3O4 magnetic nanoparticle photocatalyst |
| CN102580782A (en) * | 2012-01-09 | 2012-07-18 | 兰州交通大学 | Method for preparing magnetically-supported catalyst TiO2/polypyrrole (PPY)/Fe3O4 |
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