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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- 238000000034 method Methods 0.000 title claims abstract description 27
- 150000002790 naphthalenes Chemical class 0.000 title claims abstract description 17
- 239000002734 clay mineral Substances 0.000 title claims abstract description 11
- 230000000593 degrading effect Effects 0.000 title claims abstract description 7
- QEPTXDCPBXMWJC-UHFFFAOYSA-N 1,2,3-trichloronaphthalene Chemical compound C1=CC=C2C(Cl)=C(Cl)C(Cl)=CC2=C1 QEPTXDCPBXMWJC-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000005995 Aluminium silicate Substances 0.000 claims description 28
- 235000012211 aluminium silicate Nutrition 0.000 claims description 28
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 28
- 238000006731 degradation reaction Methods 0.000 abstract description 15
- 230000015556 catabolic process Effects 0.000 abstract description 14
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 33
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 26
- 238000004088 simulation Methods 0.000 description 10
- 239000007790 solid phase Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- RTNLUFLDZOAXIC-UHFFFAOYSA-N 1,2,3,4,5,6,7,8-octachloronaphthalene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C2=C(Cl)C(Cl)=C(Cl)C(Cl)=C21 RTNLUFLDZOAXIC-UHFFFAOYSA-N 0.000 description 1
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical compound C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 description 1
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
- A62D3/176—Ultraviolet radiations, i.e. radiation having a wavelength of about 3nm to 400nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/22—Organic substances containing halogen
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- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
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Abstract
本发明公开了一种紫外光降解黏土矿物表面多氯萘的方法。属于有机污染物的处理领域。采用紫外光为催化剂，降解黏土矿物表面的三氯萘。本方法可以有效降解有机污染物三氯萘，降解率可以达到82％。本发明的方法降解三氯萘，方法简单，成本低廉，具有良好的社会效益和环境效益。The invention discloses a method for degrading polychlorinated naphthalene on the surface of clay minerals by ultraviolet light. It belongs to the field of treatment of organic pollutants. Using UV light as a catalyst to degrade trichloronaphthalene on the surface of clay minerals. The method can effectively degrade the organic pollutant trichloronaphthalene, and the degradation rate can reach 82%. The method of the invention degrades trichloronaphthalene, the method is simple, the cost is low, and the method has good social and environmental benefits.
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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