CN113018756A - Method for degrading polychlorinated naphthalene on surface of clay mineral by ultraviolet light - Google Patents
Method for degrading polychlorinated naphthalene on surface of clay mineral by ultraviolet light Download PDFInfo
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- CN113018756A CN113018756A CN202110264495.9A CN202110264495A CN113018756A CN 113018756 A CN113018756 A CN 113018756A CN 202110264495 A CN202110264495 A CN 202110264495A CN 113018756 A CN113018756 A CN 113018756A
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- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
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- A—HUMAN NECESSITIES
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- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
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Abstract
The invention discloses a method for degrading polychlorinated naphthalene on the surface of clay mineral by ultraviolet light. Belonging to the field of organic pollutant treatment. Ultraviolet light is used as a catalyst to degrade trichloronaphthalene on the surface of the clay mineral. The method can effectively degrade the trichloronaphthalene which is an organic pollutant, and the degradation rate can reach 82%. The method for degrading the trichloronaphthalene is simple, has low cost and has good social benefit and environmental benefit.
Description
Technical Field
The invention belongs to the field of treatment of organic pollutants, and particularly relates to a degradation method of polychlorinated naphthalene on a solid-phase surface.
Background
Polychlorinated naphthalenes (PCNs), namely polychlorinated naphthalenes, are persistent organic pollutants generated by chlorination of molten naphthalene, are structurally similar to polychlorinated biphenyls, belong to one kind of organic halogenated compounds, and as halogens have strong electron-withdrawing induction effects, the molecular polarity of organic halides is further enhanced, and the fusion of the organic halides and an enzyme system in organisms is promoted, so that adverse reactions are generated on the organisms, and most of the organic halogenated compounds have toxic effects, especially 'three-cause' (carcinogenesis, teratogenesis and mutagenesis) effects, and great harm is caused to the health of the human bodies.
Polychlorinated naphthalenes have been detected in a variety of substrates in the environment, including air, soil, and sediments. Wherein trichloronaphthalene is a typical representation of polychlorinated naphthalene, and is a major isomer in various environmental substrates. Due to its hydrophobicity, trichloronaphthalene in practical environments is more prone to be adsorbed on solid surfaces such as particles, soil and sediments.
Degradation methods for polychlorinated naphthalene on the surface of a solid phase can be divided into three major categories, namely mechanochemical degradation, biodegradation and photochemical degradation, wherein Mechanochemical (MC) treatment is mainly grinding treatment, CaO is often used as an additive, and the CaO is mostly used in octachloronaphthalene. The biodegradation can deduce a detailed degradation process, is mostly used in the degradation of the chloronaphthalene and cannot be put into practical application due to high cost. Photochemistry is also the primary mode of degradation of polychlorinated naphthalenes, since polychlorinated naphthalenes absorb ultraviolet light at wavelengths greater than 300 nm. But the above way ignores the semi-volatile and high background homological group of trichloronaphthalene.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for degrading trichloronaphthalene on the surface of clay mineral by ultraviolet light.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for degrading polychlorinated naphthalene on the surface of clay mineral by ultraviolet light comprises the following steps: placing the clay mineral adsorbed with polychlorinated naphthalene in a climatic chamber for ultraviolet irradiation.
Further, in the method, 8 artificial climate boxes are used, the power is 30W, and the irradiance is 0.15W/m2An ultraviolet lamp having a wavelength of 365nm is used as a light source for ultraviolet irradiation.
Further, the method controls the temperature in the artificial climate box to be 25 ℃ and the relative humidity to be 70%.
Further, in the above method, the clay mineral is kaolin.
Further, in the method, the ultraviolet light source is 10-15cm away from the sample.
Further, in the above method, the polychlorinated naphthalene is trichloronaphthalene.
The invention has the beneficial effects that: the method can effectively degrade the trichloronaphthalene which is an organic pollutant, and the degradation rate can reach 82%. The method for degrading the trichloronaphthalene is simple, has low cost and has good social benefit and environmental benefit.
Drawings
FIG. 1 is a schematic diagram of the light reaction (upper layer) and the dark reaction (lower layer) in the climatic chamber.
Figure 2 is a graph of the photoreaction at different initial concentrations of trichloronaphthalene in the kaolin layer.
FIG. 3 is a graph of dark response at different initial concentrations of trichloronaphthalene in a kaolin layer.
Detailed Description
Artificial climate box: as shown in figure 1, 8 pieces of power are used in the box body, the power is 30W, and the irradiance is 0.15W/m2An ultraviolet lamp having a wavelength of 365nm is used as a light source for ultraviolet irradiation. The interior of the box body is divided into an upper layer and a lower layer by using a partition plate, the upper layer is used for light reaction in the artificial climate box, and the lower layer is used for dark reaction in the artificial climate box.
Example 1
Preparation of a mock sample
Adding 0.5g of kaolin and 5ml of trichloronaphthalene solution (with n-hexane as a solvent) with the concentration of 0.3mg/l into a culture dish with the diameter of 60mm, shaking uniformly to enable the kaolin to be uniformly distributed at the bottom of the culture dish, heating in a 70 ℃ sand bath for 12min, volatilizing the n-hexane to obtain a solid-phase mixture of the trichloronaphthalene and the kaolin, and detecting that the concentration of the trichloronaphthalene in the kaolin is 3 mu g/g to serve as a simulation sample.
(II) degradation
The simulation samples are transferred into a round-bottom centrifuge tube and are divided into two groups to be placed into a climatic chamber for testing, the temperature in the climatic chamber is controlled to be 25 ℃, and the relative humidity is controlled to be 70%. One set was subjected to the UV irradiation experiment and the other set was subjected to the dark reaction. Two groups of samples were taken at reaction times of 0d, 1d, 2d, 3d, 4d, 5d, 6d, and 7d, respectively.
(III) detection
1. And (3) transferring the solid phase mixture in the round-bottom centrifuge tube taken out from the artificial climate box to weighing paper, transferring the solid phase mixture into a 15ml pointed-bottom centrifuge tube, adding 15ml of n-hexane into the pointed-bottom centrifuge tube, screwing a centrifuge tube cover, placing the centrifuge tube under the conditions of 40KHz and 20 ℃ for ultrasonic treatment for 20min, and controlling the temperature by using an ice bag in the process.
2. And after the ultrasonic extraction is finished, taking the centrifugal tube out of the ultrasonic machine, and centrifuging the kaolin phase and the n-hexane phase by using a centrifuge at the rotating speed of 2000r/min at the set temperature of 20 ℃ for 10 min.
3. And (4) taking the normal hexane phase, moving the normal hexane phase to an air centrifugal tube by using a suction tube, shaking up, and then carrying out quantitative test by using a gas chromatograph. The gas chromatography conditions were: the injection port temperature is 260 deg.C, the ECD detector temperature is 300 deg.C, and the chromatographic column is DB-5(30m × 0.250mm) capillary blood column with a thickness of 0.250 μm. The temperature programming condition of the chromatographic column is as follows: keeping at 180 deg.C for 1min, and keeping at 2 deg.C for min-1Heating to 200 deg.C, and keeping for 2min, wherein the time of the whole heating process is 13 min. The sample injection amount is 1 mu L, the split ratio is 9, the carrier gas is high-purity nitrogen (the purity is more than or equal to 99.999 percent), and the flow rate is 1mL min-1The flow rate of tail gas blowing is 40 mL/min.
4. The data analyzed by the gas chromatograph are collated, and as shown in fig. 2 and fig. 3, the conversion rate of trichloronaphthalene in the light reaction group after 7d is 84%, and the conversion rate in the dark reaction group is only 17.8% at most. It can be seen that the conversion rate of the sample irradiated by ultraviolet light is higher than that of the dark reaction sample.
Example 2
Preparation of a mock sample
Adding 0.5g of kaolin and 5ml of trichloronaphthalene solution (with n-hexane as a solvent) with the concentration of 0.6mg/l into a culture dish with the diameter of 60mm, shaking uniformly to enable the kaolin to be uniformly distributed at the bottom of the culture dish, heating in a 70 ℃ sand bath for 12min, volatilizing the n-hexane to obtain a solid-phase mixture of the trichloronaphthalene and the kaolin, and detecting that the concentration of the trichloronaphthalene in the kaolin is 6 mu g/g to serve as a simulation sample.
(II) degradation
The simulation samples are transferred into a round-bottom centrifuge tube and are divided into two groups to be placed into a climatic chamber for testing, the temperature in the climatic chamber is controlled to be 25 ℃, and the relative humidity is controlled to be 70%. One set was subjected to the UV irradiation experiment and the other set was subjected to the dark reaction. Two groups of samples were taken at reaction times of 0d, 1d, 2d, 3d, 4d, 5d, 6d, and 7d, respectively.
(III) detection
The same procedure as in example 1 resulted in the results shown in FIGS. 2 and 3, where the conversion of trichloronaphthalene in the photoreactive group was 82% after 7d, while the conversion in the dark group was only 14.36% at the maximum. It can be seen that the conversion rate of the sample irradiated by ultraviolet light is higher than that of the dark reaction sample.
Example 3
Preparation of a mock sample
Adding 0.5g of kaolin and 5ml of trichloronaphthalene solution (with n-hexane as a solvent) with the concentration of 1.5mg/l into a culture dish with the diameter of 60mm, shaking uniformly to enable the kaolin to be uniformly distributed at the bottom of the culture dish, heating in a 70 ℃ sand bath for 12min, volatilizing the n-hexane to obtain a solid-phase mixture of the trichloronaphthalene and the kaolin, and detecting that the concentration of the trichloronaphthalene in the kaolin is 15 mu g/g to serve as a simulation sample.
(II) degradation
The simulation samples are transferred into a round-bottom centrifuge tube and are divided into two groups to be placed into a climatic chamber for testing, the temperature in the climatic chamber is controlled to be 25 ℃, and the relative humidity is controlled to be 70%. One set was subjected to the UV irradiation experiment and the other set was subjected to the dark reaction. Two groups of samples were taken at reaction times of 0d, 1d, 2d, 3d, 4d, 5d, 6d, and 7d, respectively.
(III) detection
As shown in FIGS. 2 and 3, the conversion of trichloronaphthalene in the photoreactive group after 7d was 76.95%, while that in the dark group was only 13.56% at the maximum. It can be seen that the conversion rate of the sample irradiated by ultraviolet light is higher than that of the dark reaction sample.
Example 4
Preparation of a mock sample
0.5g of kaolin and 5ml of trichloronaphthalene solution (with n-hexane as a solvent) with the concentration of 2.1mg/l are added into a culture dish with the diameter of 60mm, the mixture is shaken uniformly to enable the kaolin to be uniformly distributed at the bottom of the culture dish, then the culture dish is heated in a 70 ℃ sand bath for 12min, the n-hexane is volatilized to obtain a solid-phase mixture of the trichloronaphthalene and the kaolin, and the detected concentration of the trichloronaphthalene in the kaolin is 21 mu g/g, and the solid-phase mixture is used as a simulation sample.
(II) degradation
The simulation samples are transferred into a round-bottom centrifuge tube and are divided into two groups to be placed into a climatic chamber for testing, the temperature in the climatic chamber is controlled to be 25 ℃, and the relative humidity is controlled to be 70%. One set was subjected to the UV irradiation experiment and the other set was subjected to the dark reaction. Two groups of samples were taken at reaction times of 0d, 1d, 2d, 3d, 4d, 5d, 6d, and 7d, respectively.
(III) detection
The same procedure as in example 1 resulted in the results shown in FIGS. 2 and 3, in which the conversion of trichloronaphthalene in the photoreactive group after 7d was 66.34%, while that in the dark group was only 12.07% at the maximum. It can be seen that the conversion rate of the sample irradiated by ultraviolet light is higher than that of the dark reaction sample.
Example 5
Preparation of a mock sample
Adding 0.5g of kaolin and 5ml of trichloronaphthalene solution (with n-hexane as a solvent) with the concentration of 3.0mg/l into a culture dish with the diameter of 60mm, shaking uniformly to enable the kaolin to be uniformly distributed at the bottom of the culture dish, heating in a 70 ℃ sand bath for 12min, volatilizing the n-hexane to obtain a solid-phase mixture of the trichloronaphthalene and the kaolin, and detecting that the concentration of the trichloronaphthalene in the kaolin is 30 mu g/g to serve as a simulation sample.
(II) degradation
The simulation samples are transferred into a round-bottom centrifuge tube and are divided into two groups to be placed into a climatic chamber for testing, the temperature in the climatic chamber is controlled to be 25 ℃, and the relative humidity is controlled to be 70%. One set was subjected to the UV irradiation experiment and the other set was subjected to the dark reaction. Two groups of samples were taken at reaction times of 0d, 1d, 2d, 3d, 4d, 5d, 6d, and 7d, respectively.
(III) detection
As shown in FIGS. 2 and 3, the conversion of trichloronaphthalene in the photoreactive group after 7d was 70.02%, while that in the dark group was only 9.00% at the maximum. It can be seen that the conversion rate of the sample irradiated by ultraviolet light is higher than that of the dark reaction sample.
As can be seen from fig. 2-3, after 7d, the conversion rate of the trichloronaphthalene in the photoreaction group decreases with the increase of the concentration, because the degradation of the trichloronaphthalene concentration is caused by active free radicals, the kaolin generates active free radicals under the irradiation of ultraviolet light, the active free radicals attack the trichloronaphthalene molecules to degrade the trichloronaphthalene molecules, the increase of the trichloronaphthalene concentration in the kaolin requires more active free radicals, but the capability of the kaolin to generate active free radicals under the irradiation of ultraviolet light is limited, and therefore the conversion rate of the trichloronaphthalene in the photoreaction group decreases with the increase of the concentration. The conversion of trichloronaphthalene in the dark reaction group after 7d likewise decreases with increasing concentration, but the dark reaction concentration changes by up to 17.8%, probably because of the semi-volatility of trichloronaphthalene.
Claims (6)
1. A method for degrading polychlorinated naphthalene on the surface of clay mineral by ultraviolet light is characterized by comprising the following steps: placing the clay mineral adsorbed with polychlorinated naphthalene in a climatic chamber for ultraviolet irradiation.
2. The method as claimed in claim 1, characterized in that 8 power supplies of 30W with an irradiance of 0.15W/m are used in the climatic chamber2An ultraviolet lamp having a wavelength of 365nm is used as a light source for ultraviolet irradiation.
3. A method according to claim 1, characterized in that the temperature in the climatic chamber is controlled to 25 ℃ and the relative humidity to 70%.
4. The method of claim 1, wherein the clay mineral is kaolin.
5. The method of claim 1, wherein the ultraviolet light source is 10-15cm from the sample.
6. The method of any one of claims 1-5, wherein the polychlorinated naphthalene is trichloronaphthalene.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1930208A (en) * | 2004-01-17 | 2007-03-14 | 通用电气公司 | Compositions useful as coatings, their preparation, and articles made therefrom |
| US20090155371A1 (en) * | 2007-12-17 | 2009-06-18 | Sojka Milan F | Compositions Comprising Solid Particles Entrapped In Collapsed Polymeric Microspheres, And Methods Of Making The Same |
| CN102258992A (en) * | 2011-06-23 | 2011-11-30 | 浙江大学 | Surface iron modified titanium dioxide photocatalyst as well as preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1930208A (en) * | 2004-01-17 | 2007-03-14 | 通用电气公司 | Compositions useful as coatings, their preparation, and articles made therefrom |
| US20090155371A1 (en) * | 2007-12-17 | 2009-06-18 | Sojka Milan F | Compositions Comprising Solid Particles Entrapped In Collapsed Polymeric Microspheres, And Methods Of Making The Same |
| CN102258992A (en) * | 2011-06-23 | 2011-11-30 | 浙江大学 | Surface iron modified titanium dioxide photocatalyst as well as preparation method and application thereof |
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