CN106542607A - It is a kind of to improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation - Google Patents
It is a kind of to improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation Download PDFInfo
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- CN106542607A CN106542607A CN201610918758.2A CN201610918758A CN106542607A CN 106542607 A CN106542607 A CN 106542607A CN 201610918758 A CN201610918758 A CN 201610918758A CN 106542607 A CN106542607 A CN 106542607A
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- isopropyl methoxalamine
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Hydrology & Water Resources (AREA)
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Abstract
The present invention relates to a kind of improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation, the electricity of preparation and isopropyl methoxalamine including the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites helps photocatalytic degradation：With step（1）The obtained photochemical catalyst electrode with isopropyl methoxalamine imprinted sites is working electrode, constructs standard three electrode system, under light irradiation and bias, catalytic degradation pesticide isopropyl methoxalamine.Compared with prior art, the present invention can effectively improve the speed that electricity helps Researches on Photocatalytic Degradation of Pesticide Using isopropyl methoxalamine, and electrode prepares simple, high catalytic efficiency, repeats and utilizes.
Description
Technical field
The present invention relates to the electricity of environmental contaminants helps Photocatalyst field, it is different more particularly, to a kind of raising pesticide
The method that methoxalamine electricity helps rate of photocatalytic oxidation.
Background technology
Isopropyl methoxalamine [2- methyl -6- ethyl-N- (1- methyl -2- methoxyethyls)-N- ChloroacetYl aniline], also known as
All you, is that a kind of activity is high, and the wide amide-type preemergence herbicide of use range is widely used in corn and soybean, Rhizoma Solani tuber osi, cotton
The preventing and treating of the crop weeds such as flower and Sorghum vulgare Pers., its residue have caused to the environmental pollution caused by crop, soil and water body
The common concern of people in worldwide.
Used as a kind of high-level oxidation technology, which undergoes in terms of environmental contaminants degraded and energy conversion photocatalysis technology
Study to very extensive.But at present the practical application of photocatalysis technology is limited by 2 points, first, light induced electron and hole
Recombination rate is high, it is suppressed that the reaction of the pollutant that are processed in hole and solution.Second, light-catalyzed reaction speed is not high so that light
Catalysis time is long, high cost.Conventional photocatalyst is TiO at present2, it has, and cheap, nontoxic, catalysis activity is high, performance is steady
The advantages of determining.But TiO2Granule is difficult to practical application, because the TiO suspended in solution2Granule is difficult recycling.Such as
Really by TiO2It is fixed on appropriate base material and then can not only solves to be difficult to the difficult problem that reclaims but also can be by the side of external biasing voltage
Formula migrates light induced electron to external circuit, i.e. electricity and helps photocatalysis, and it can promote the separation in light induced electron and hole, improves reaction
Treatment effeciency.And pass through the molecular engram site of target contaminant is constructed in catalyst surface, can both increase catalysis material
Specific surface area, the absorbability to target contaminant can be increased again, so as to improve the speed of catalytic degradation.
The content of the invention
To overcome the deficiencies in the prior art, present invention aim at：A kind of pesticide isopropyl methoxalamine electricity that improves is provided and helps light
The method of catalytic degradation speed.
The present invention by titanium dioxide nano-rod growth in situ on electro-conductive glass, and titanium dioxide nano-rod growth it is same
When target environment pollutant isopropyl methoxalamine is embedded in the surface of titanium dioxide nano-rod, by high temperature removal isopropyl first grass
Amine, stays and isopropyl methoxalamine molecular configuration identical imprinted sites on titanium dioxide nano-rod surface, has the two of the site
TiOx nano rod can quickly adsorb isopropyl methoxalamine in Photocatalytic Degradation Process to the surface of electrode, urge so as to improve light
Change degradation rate.
The purpose of the present invention can be achieved through the following technical solutions：
It is a kind of to improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation, it is characterised in that to comprise the following steps：
（1）The preparation of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites：
Weigh concentrated hydrochloric acid to mix with water, add dropwise butyl titanate, stir, add template molecule isopropyl methoxalamine, obtain
To precursor solution；Precursor solution is transferred in sealed reactor, the conduction of pretreated electro-conductive glass is faced down
In immersion precursor solution, hydro-thermal reaction；After the completion of reaction, product is taken out, cleaning, calcining is obtained by with isopropyl first grass
The TiO of amine imprinted sites2Nanometer rods photochemical catalyst electrode；
（2）The electricity of isopropyl methoxalamine helps photocatalytic degradation：
With step（1）The obtained photochemical catalyst electrode with isopropyl methoxalamine imprinted sites is working electrode, constructs standard three electric
Polar body system, under light irradiation and bias, catalytic degradation pesticide isopropyl methoxalamine.
Step（1）The volume ratio of the addition of middle concentrated hydrochloric acid, water, butyl titanate and isopropyl methoxalamine is 100：100：
（1-4）：（0.2-2）, the concentration of concentrated hydrochloric acid is 36.5wt%-38.5wt%；The process conditions of stirring are：Stir under 300-600rpm
Mix 1-3 h；The process conditions of hydro-thermal reaction are：4-10 h are reacted at 140-180 DEG C；The process conditions of calcining are：In 500-
30-50 min are calcined at 700 DEG C.
Step（2）Described in standard three electrode system in, reference electrode is saturated calomel electrode, to electrode be platinum electricity
Pole, the work area of working electrode is 3 cm2, electrolyte solution is the sodium sulfate of 0.1 mol/L（Na2SO4）Electrolyte；Illumination is
Ultraviolet light, bias-voltage are 0.6 V.
Molecular imprinting in situ and electricity are helped Photocatalyst to combine by the present invention, using TiO2Nanorod electrodes
The molecular engram site of surface construction recycles TiO so as to strengthen the absorbability of electrode pair isopropyl methoxalamine2Nanometer rods are subject to
The photohole produced on surface after illumination will adsorb the isopropyl methoxalamine photocatalytic degradation in electrode surface, so as to strengthen isopropyl
Alachlor electricity helps rate of photocatalytic oxidation and degradation efficiency.
Compared with prior art, the present invention has advantages below：
(1) first in TiO2Nanorod surfaces construct isopropyl methoxalamine imprinted sites, improve photochemical catalyst electrode to isopropyl first grass
The absorbability of amine, helps light-catalysed degradation rate and degradation efficiency so as to enhance electrode pair pesticide isopropyl methoxalamine electricity.
(2) TiO with isopropyl methoxalamine imprinted sites prepared in the present invention2Nanorod electrodes, prepare simply, urge
Change efficiency high, repeat and utilize.
Description of the drawings
Drop of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites prepared during Fig. 1 is of the invention to isopropyl methoxalamine
Solution curve figure, █ represent non-trace TiO2Nanometer rods, ● represent non-trace TiO2Nanometer rods；
Degraded of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites prepared during Fig. 2 is of the invention to isopropyl methoxalamine is bent
Line chart, █ represent non-trace TiO2Nanometer rods, ● represent non-trace TiO2Nanometer rods；
Degraded of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites prepared during Fig. 3 is of the invention to isopropyl methoxalamine is bent
Line chart, █ represent non-trace TiO2Nanometer rods, ● represent non-trace TiO2Nanometer rods；
The scanning electron microscope diagram of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites prepared during Fig. 4 is of the invention.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
A kind of photochemical catalyst electrode with isopropyl methoxalamine imprinted sites, including TiO2Nanorod electrodes, and construct in TiO2
The isopropyl methoxalamine imprinted sites on nanorod electrodes surface, are made by following steps：
（1）Weigh concentrated hydrochloric acid to mix with water, add dropwise butyl titanate, stir 3h at 300 rpm, add template molecule
Isopropyl methoxalamine, the volume ratio of the addition of concentrated hydrochloric acid, water, butyl titanate and isopropyl methoxalamine is 100：100：1：0.2, it is dense
The concentration of hydrochloric acid is 36.5wt%, obtains precursor solution；
（2）Precursor solution is transferred in sealed reactor, the conduction of pretreated electro-conductive glass is faced down and is immersed molten
In liquid, 7h is reacted at 160 DEG C；
（3）After the completion of reaction, product is taken out, deionized water is rinsed, and is taken out surface residue, 30min is calcined at 700 DEG C,
TiO of the purpose product with isopropyl methoxalamine imprinted sites is obtained2Nanorod electrodes.
Obtained purpose product is detected, Fig. 4 shows the SEM figures of purpose product, it is found that this reality from figure
Apply the obtained TiO with isopropyl methoxalamine imprinted sites of example2Nanorod electrodes are upright orderly, compact arranged quadrangular knot
Structure, the quadrangular length of side are about 70 nm, about 1.5 μm of column length, and the TiO for preparing2Nanometer rods size it is relatively unified and
It is regular.
Embodiment 2：
A kind of photochemical catalyst electrode with isopropyl methoxalamine imprinted sites, including TiO2Nanorod electrodes, and construct in TiO2
The isopropyl methoxalamine imprinted sites on nanorod electrodes surface, are made by following steps：
（1）Weigh concentrated hydrochloric acid to mix with water, add dropwise butyl titanate, 2 h are stirred under 450 rpm, add template point
Sub- isopropyl methoxalamine, the volume ratio of the addition of concentrated hydrochloric acid, water, butyl titanate and isopropyl methoxalamine is 100：100：2.5：
1.1, the concentration of concentrated hydrochloric acid is 37.5wt%, obtains precursor solution；
（2）Precursor solution is transferred in sealed reactor, the conduction of pretreated electro-conductive glass is faced down and is immersed molten
In liquid, 4 h are reacted at 180 DEG C；
（3）After the completion of reaction, product is taken out, deionized water is rinsed, and is taken out surface residue, 40min is calcined at 600 DEG C,
TiO of the purpose product with isopropyl methoxalamine imprinted sites is obtained2Nanorod electrodes.
Embodiment 3：
A kind of photochemical catalyst electrode with isopropyl methoxalamine imprinted sites, including TiO2Nanorod electrodes, and construct in TiO2
The isopropyl methoxalamine imprinted sites on nanorod electrodes surface, are made by following steps：
（1）Weigh concentrated hydrochloric acid to mix with water, add dropwise butyl titanate, 1 h is stirred under 600 rpm, add template point
Sub- isopropyl methoxalamine, the volume ratio of the addition of concentrated hydrochloric acid, water, butyl titanate and isopropyl methoxalamine is 100：100：4：2, it is dense
The concentration of hydrochloric acid is 38.5wt%, obtains precursor solution；
（2）Precursor solution is transferred in sealed reactor, the conduction of pretreated electro-conductive glass is faced down and is immersed molten
In liquid, 10 h are reacted at 140 DEG C；
（3）After the completion of reaction, product is taken out, deionized water is rinsed, and takes out surface residue, 50 min are calcined at 500 DEG C,
TiO of the purpose product with isopropyl methoxalamine imprinted sites is obtained2Nanorod electrodes.
Embodiment 4：
Standard three electrode system is adopted in the quartzy degraded pond for be connected with constant temperature system, on electrochemical workstation CHI 660, is used
The TiO with isopropyl methoxalamine imprinted sites prepared by embodiment 12Nanorod electrodes are working electrode, saturated calomel electrode
For reference electrode, platinum electrode is, to electrode, under ultraviolet light and bias, to carry out electricity to isopropyl methoxalamine solution and help light
Catalytic degradation.After degraded 6 hours, the clearance of isopropyl methoxalamine is 86.7%, and degradation rate constant is 0.142 h-1, compared to
The degraded clearance of the photochemical catalyst electrode of non-trace（69.0%）17.7% is improve, compared to the drop of the photochemical catalyst electrode of non-trace
Solution speed constant（0.089 h-1）59.6% is improve, as shown in Figure 1.
Embodiment 5：
Standard three electrode system is adopted in the quartzy degraded pond for be connected with constant temperature system, on electrochemical workstation CHI 660, is used
The TiO with isopropyl methoxalamine imprinted sites prepared by embodiment 22Nanorod electrodes are working electrode, saturated calomel electrode
For reference electrode, platinum electrode is, to electrode, under ultraviolet light and bias, to carry out electricity to isopropyl methoxalamine solution and help light
Catalytic degradation.After degraded 6 hours, the clearance of isopropyl methoxalamine is 86.2%, and degradation rate constant is 0.141 h-1, compared to
The degraded clearance of the photochemical catalyst electrode of non-trace（68.3%）17.9% is improve, compared to the drop of the photochemical catalyst electrode of non-trace
Solution speed constant（0.087 h-1）62.1% is improve, as shown in Figure 2.
Embodiment 6：
Standard three electrode system is adopted in the quartzy degraded pond for be connected with constant temperature system, on electrochemical workstation CHI 660, is used
The TiO with isopropyl methoxalamine imprinted sites prepared by embodiment 32Nanorod electrodes are working electrode, saturated calomel electrode
For reference electrode, platinum electrode is, to electrode, under ultraviolet light and bias, to carry out electricity to isopropyl methoxalamine solution and help light
Catalytic degradation.After degraded 6 hours, the clearance of isopropyl methoxalamine is 85.8%, and degradation rate constant is 0.140 h-1, compared to
The degraded clearance of the photochemical catalyst electrode of non-trace（68.5%）17.3% is improve, compared to the drop of the photochemical catalyst electrode of non-trace
Solution speed constant（0.087 h-1）60.9% is improve, as shown in Figure 3.
The photochemical catalyst electrode with isopropyl methoxalamine imprinted sites drawn by above-described embodiment 4-6 is to isopropyl methoxalamine
Degradation curve figure can be seen that the TiO with isopropyl methoxalamine imprinted sites of present invention preparation2Nanorod electrodes are to isopropyl first
The electricity of careless amine helps rate of photocatalytic oxidation and degraded clearance to be all higher than the TiO for not having imprinted sites2Nanorod electrodes.
Claims (3)
1. it is a kind of to improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation, it is characterised in that to comprise the following steps：
（1）The preparation of the photochemical catalyst electrode with isopropyl methoxalamine imprinted sites：
Weigh concentrated hydrochloric acid to mix with water, add dropwise butyl titanate, stir, add template molecule isopropyl methoxalamine, obtain
To precursor solution；Precursor solution is transferred in sealed reactor, the conduction of pretreated electro-conductive glass is faced down
In immersion precursor solution, hydro-thermal reaction；After the completion of reaction, product is taken out, cleaning, calcining is obtained by with isopropyl first grass
The TiO of amine imprinted sites2Nanometer rods photochemical catalyst electrode；
（2）The electricity of isopropyl methoxalamine helps photocatalytic degradation：
With step（1）The obtained photochemical catalyst electrode with isopropyl methoxalamine imprinted sites is working electrode, constructs standard three electric
Polar body system, under light irradiation and bias, catalytic degradation pesticide isopropyl methoxalamine.
2. the method that a kind of raising pesticide isopropyl methoxalamine electricity according to claim 1 helps rate of photocatalytic oxidation, which is special
Levy and be, step（1）The volume ratio of the addition of middle concentrated hydrochloric acid, water, butyl titanate and isopropyl methoxalamine is 100：100：（1-
4）：（0.2-2）, the concentration of concentrated hydrochloric acid is 36.5wt%-38.5wt%；The process conditions of stirring are：Stir under 300-600rpm
1-3 h；The process conditions of hydro-thermal reaction are：4-10 h are reacted at 140-180 DEG C；The process conditions of calcining are：In 500-700
30-50 min are calcined at DEG C.
3. the method that a kind of raising pesticide isopropyl methoxalamine electricity according to claim 1 helps rate of photocatalytic oxidation, which is special
Levy and be, step（2）Described in standard three electrode system in, reference electrode is saturated calomel electrode, to electrode be platinum electrode,
The work area of working electrode is 3 cm2, electrolyte solution is the sodium sulfate of 0.1 mol/L（Na2SO4）Electrolyte；Illumination is ultraviolet
Light, bias-voltage are 0.6 V.
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| CN201610918758.2A CN106542607A (en) | 2016-10-21 | 2016-10-21 | It is a kind of to improve the method that pesticide isopropyl methoxalamine electricity helps rate of photocatalytic oxidation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162097A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The selective light electro-catalysis minimizing technology of the β estradiol of low concentration 17 in system coexists |
| CN107434270A (en) * | 2017-08-08 | 2017-12-05 | 同济大学 | Iron carbon aerogels Fenton negative electrode and its preparation with contaminant molecule trace |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999608A (en) * | 2016-05-06 | 2016-10-12 | 同济大学 | 2,4-dichlorprop chiral pesticide enantiomer selective photoelectrochemical oxidative degradation method |
-
2016
- 2016-10-21 CN CN201610918758.2A patent/CN106542607A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999608A (en) * | 2016-05-06 | 2016-10-12 | 同济大学 | 2,4-dichlorprop chiral pesticide enantiomer selective photoelectrochemical oxidative degradation method |
Non-Patent Citations (1)
| Title |
|---|
| 郑平著: "《分子印迹固相萃取技术及其在食品安全分析中的应用》", 30 November 2011 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162097A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The selective light electro-catalysis minimizing technology of the β estradiol of low concentration 17 in system coexists |
| CN107434270A (en) * | 2017-08-08 | 2017-12-05 | 同济大学 | Iron carbon aerogels Fenton negative electrode and its preparation with contaminant molecule trace |
| CN107434270B (en) * | 2017-08-08 | 2020-08-18 | 同济大学 | Iron-carbon aerogel electro-Fenton cathode with pollutant molecular imprinting and preparation method thereof |
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