CN113636618A - Method for degrading organic pollutants by high-energy liquid-phase ion clusters - Google Patents
Method for degrading organic pollutants by high-energy liquid-phase ion clusters Download PDFInfo
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- CN113636618A CN113636618A CN202110940065.4A CN202110940065A CN113636618A CN 113636618 A CN113636618 A CN 113636618A CN 202110940065 A CN202110940065 A CN 202110940065A CN 113636618 A CN113636618 A CN 113636618A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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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
Abstract
The invention relates to a method for degrading organic pollutants by high-energy liquid-phase ion clusters, which comprises the following steps: high-energy liquid-phase ion clusters are generated by energizing a liquid medium with secondary high voltage, the secondary high voltage is applied to a container provided with a conical small hole of a purified water belt, and the high-energy particle clusters are sprayed on the surface of liquid or solid from the conical small hole, so that organic pollutants in the solution and on the surface of the solid are degraded. The method uses common secondary high voltage, and pure water in a capillary is energized through an inert electrode so as to generate vaporous high-energy ions, thereby generating a degradation effect on organic pollutants or solid surface pollutants in a solution contacted with the high-energy ions; in order to improve the degradation capability of organic pollutants, the degradation effect on organic pollutants or solid surface pollutants in a solution contacted with high-energy ions can be improved by adjusting the voltage of a secondary high-voltage power supply, the transmission distance of the high-energy ions and the yield of the high-energy ions.
Description
Technical Field
The invention relates to the technical field of environmental protection, sewage treatment and micro-surface cleaning, in particular to a method for degrading organic pollutants by high-energy liquid-phase ion clusters.
Background
With the development of synthetic chemistry, a great deal of organic pollutants including dyes, pesticides, bactericides, insecticides and the like are used in daily life, and great threats are brought to the environment and human health. As new chemicals are continuously introduced into the environment, environmental pollution caused by refractory organics is becoming a more challenging multidisciplinary problem. Although the development of the technology gradually leads to a plurality of new organic pollutant degradation technologies such as photocatalysis technology, nanotechnology and the like, no other secondary pollution is introduced due to great risk, such as catalytic degradation of nanoparticles, the patent application number is 202011438283.X, the patent name is an invention patent of a method for treating organic pollutants by using a ferrite-gold nano catalyst, and the method is to treat the organic pollutants by using the ferrite-gold nano catalyst; the iron-manganese ferrite-gold nano catalyst comprises iron-manganese ferrite, nano gold particles and negative-valence gold ions, the nano gold particles and the negative-valence gold ions are deposited on the surface of the iron-manganese ferrite together, and the introduction of the nano catalyst can generate a new round of pollution.
When organic pollutants are degraded by adopting high-energy ions, high energy consumption such as laser, X-ray, ultraviolet light and the like is needed, complex equipment matched with the high-energy ions is needed for preparing the high-energy ions, and chemical reagents such as hydrogen peroxide, chlorine dioxide, sodium sulfite, iron dichloride and the like are needed to be added. It is therefore highly desirable to seek a rapid and efficient, especially clean, method for degrading organic contaminants.
Water is one of the most common substances on earth. The earth's surface is 72% covered by water, which is an important resource for all life including inorganic compounds and human beings, and is also the most important component of the organism. The invention generates zero-additive pollution-free fog-shaped high-energy ions at normal temperature and normal pressure by using sub-high-voltage electrically energized pure water, and the fog-shaped high-energy ions are rich in water cluster hydroxyl radicals, water radical cation clusters, negative oxygen ion clusters, hydronium ions and other degradable solutions to neutralize organic pollutants on the solid surface, so that the development of a method for degrading organic pollutants by using high-energy liquid-phase ion clusters is particularly important.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for degrading organic pollutants by using high-energy liquid-phase ion clusters.
The purified water is energized by secondary high voltage electricity to generate vaporous high-energy ions which are rich in water-containing cluster hydroxyl radicals, water-containing cluster cation clusters, negative oxygen ion clusters, hydronium ions and the like, so that organic pollutants in the degradation solution and on the solid surface are degraded.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for degrading organic pollutants by high-energy liquid-phase ion clusters comprises the following steps:
high-energy liquid-phase ion clusters are generated by energizing a liquid medium with secondary high voltage, the secondary high voltage is applied to a container provided with a conical small hole of a purified water belt, and the high-energy particle clusters are sprayed on the surface of liquid or solid from the conical small hole, so that organic pollutants in the solution and on the surface of the solid are degraded.
Further, the high-energy ionic liquid cluster is generated by enabling the liquid through sub-high-voltage electricity, in the process, firstly, electric energy is converted into kinetic energy and surface energy to enable the liquid to be broken into high-speed tiny liquid drops and tiny liquid drops with high kinetic energy and high surface energy, and secondly, the tiny liquid drops with high kinetic energy and high surface energy are in friction collision with an air medium to enable the high-kinetic energy and high surface energy to be converted into chemical energy to generate ions with high chemical energy. The high-energy ions exist in the nanometer micro-droplets to form high-energy liquid clusters, and the high-energy liquid clusters comprise: hydroxyl radical, water radical cation cluster, negative oxygen ion cluster, hydronium ion.
Further, when the organic pollutants are degraded, the high-energy ionic liquid cluster is sprayed in the organic pollutant solution or on the solid surface carrying the organic pollutants, and the initial speed of the high-energy ions is about 250-300 m/s.
Further, the solvent of the organic contaminant solution includes water and various solvents such as methanol, ethanol, acetonitrile, and the like.
Further, the organic pollutants comprise rhodamine B, fluorescein, nai's blue, methylene blue, organophosphorus pesticides, pyrethrin pesticides and insecticide Kechun mite.
Further, the liquid medium comprises tap water, distilled water or alcohol.
Furthermore, the solid is metal, high polymer material (containing glass and fiber material), melon, fruit, vegetable and organism.
Further, the surface of the solid body includes a smooth surface, a rough surface and a narrow micron-scale micro-area surface and a micron-scale narrow micro-area surface of a chip surface of an integrated circuit.
After the process is improved, the applied secondary high voltage is +/-2 kV-10 kV direct current, the tapered small hole container is a container containing one or more tapered small holes, and the diameter of the tapered small holes of the container is 0.1-100 mu m.
The invention has the technical effects that: the invention uses the secondary high voltage, nano-ampere level micro-current (the secondary high voltage range is +/-2 kV-10 kV, the current is about hundreds of nano-amperes (nA) level), so the invention has the characteristics of low energy consumption, high safety and the like, and the high-energy ions can be rapidly prepared by cheap and easily-obtained liquid medium under the conditions of normal temperature and low temperature difference and energy consumption to remove and degrade organic pollutants in liquid and on the surface of solid;
meanwhile, in order to improve the degradation capability of organic pollutants, the action distance of high-energy ions and the yield of high-energy ions can be adjusted by adjusting the voltage of a high-voltage power supply, so that the degradation effect of organic pollutants or solid surface pollutants in a solution contacted with water mist is improved.
Drawings
FIG. 1 is a schematic view of an apparatus for degrading organic pollutants by using high-energy ion water mist according to the present invention;
FIG. 1a is a schematic view of a container with a tapered orifice according to the present invention;
FIG. 1b is another schematic view of a container with a tapered orifice of the present invention;
FIG. 2 is a schematic diagram of the complete degradation of rhodamine B in two hours by using the high-energy ionic water mist prepared in example 1;
FIG. 3 is a time-varying graph of the high-energy ionic water mist degraded rhodamine B prepared in example 1;
FIG. 4a is a mass spectrum of rhodamine b after 30 minutes of degradation in example 1;
FIG. 4b is a mass spectrum of undegraded rhodamine b in example 1;
FIG. 5a is a graph showing the degradation effect of Naerlan, fluorescein and methylene blue in example 2 within 30 minutes of the test experiment;
FIG. 5b is a graph comparing the degradation of Narland in example 2 within 1 hour and 30 minutes of the test experiment;
FIG. 5c is a graph comparing the degradation of fluorescein in example 2 over 1 hour and 30 minutes of the test experiment;
FIG. 5d is a graph showing the degradation effect of methylene blue of example 2 within 1 hour and 30 minutes of the test experiment;
FIG. 6 is a scanning electron micrograph of Escherichia coli which has not been subjected to the action of the high energy ion water mist;
FIG. 7 is a scanning electron micrograph of E.coli treated with a high energy ion water mist.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for degrading organic pollutants by high-energy liquid-phase ion clusters comprises the following steps:
as shown in fig. 1, fig. 1a and fig. 1b, high-energy liquid-phase ion clusters are generated by energizing a liquid medium with secondary high voltage, the secondary high voltage is applied to a container 1 provided with a conical pore of a purified water belt, and the high-energy particle clusters are sprayed on the surface of a liquid or solid 2 from the conical pore, so that organic pollutants in a solution and on the surface of the solid 2 are degraded.
The high-energy ionic liquid cluster is generated by energizing liquid through sub-high voltage electricity, high-energy ions exist in nanometer micro-droplets to form the high-energy liquid cluster, one electric energy of the high-energy ionic liquid cluster is firstly converted into kinetic energy and surface energy to enable the liquid to be broken into high-speed micro-droplets, the micro-droplets with high kinetic energy and high surface energy are subjected to frictional collision with an air medium, and the high-kinetic energy and high surface energy of the micro-droplets are converted into chemical energy to generate high-chemical-energy ions. The high energy liquid cluster comprises: hydroxyl radical, water radical cation cluster, negative oxygen ion cluster, hydronium ion.
The applied high voltage is +/-2 kV-10 kV direct current, the conical small hole container is a container containing one or more conical small holes, and the diameter of the conical small holes of the container is 0.1-100 mu m.
When the organic pollutant is degraded, the high-energy ionic liquid cluster is sprayed in the organic pollutant solution or on the solid surface carrying the organic pollutant. The initial velocity of the high-energy ions is about 250-300 m/s.
The organic pollutant solution contains water solution and various organic solvents, wherein the organic solvents comprise methanol, ethanol and acetonitrile.
The solid is metal, high molecular material, fruits, vegetables and organisms, and contains glass and fiber material.
The liquid medium comprises tap water, distilled water or alcohol. The organic pollutants comprise rhodamine B, fluorescein, Nalron blue, methylene blue, organophosphorus pesticide, pyrethrin pesticide and insecticide Kechun mite.
The surface of the solid comprises a smooth surface, a rough surface and a narrow micron-scale micro-area surface, and is used for the micron-scale narrow micro-area surface of the surface of an integrated circuit or a chip.
The invention is further illustrated by the following specific examples:
example 1
The method for degrading rhodamine b by using high-energy ion water mist comprises the following steps:
firstly, preparing high-concentration rhodamine b aqueous solution 500 ppm, dripping a sample on the surface of a solid, then energizing purified water by adopting sub-high voltage (direct current of +/-2 kV-10 kV), spraying vaporous high-energy ions from a conical pipe orifice (the initial speed is about 250-300 m/s), recording the time, and then disconnecting the high voltage;
dripping 500 ppm (high concentration) rhodamine b aqueous solution samples on the solid surface, keeping out of the sun, drying at room temperature, then energizing purified water by adopting sub-high voltage electricity, spraying vaporous high-energy ions on the rhodamine b stain solid surface on the solid surface through a conical pipe orifice, recording the time, and then disconnecting the high voltage electricity;
and (3) washing the rhodamine b aqueous solution or the rhodamine b solid stain into a cuvette, detecting the ultraviolet absorbance of the rhodamine b, and comparing the ultraviolet absorbance with the rhodamine b aqueous solution which is not degraded in a control group.
And calculating the concentration of the degraded rhodamine b aqueous solution through the Lambert beer law, thereby calculating the degradation rate of the rhodamine b in the recording time.
As shown in FIG. 2, after the high-energy ion water mist is generated, the high-energy ion water mist is directly sprayed into the aqueous solution or methanol solution of rhodamine b, then the rhodamine b which is not degraded through a control experiment has very high ultraviolet absorption at 550 nm, and the degraded rhodamine b hardly absorbs.
The method specifically comprises the following steps of changing a degradation curve of rhodamine b along with time:
the above experiment was repeated as described in example 1 to obtain degradation products of rhodamine b within 0, 5, 10, 15, 20, 25, and 30 minutes, and ultraviolet absorbance of the degraded rhodamine b was measured by ultraviolet spectroscopy. According to the calculation method, the concentration of the remaining rhodamine b in each degraded solution is obtained through Lambert beer quantification, and then the degradation rate of the rhodamine b in different time periods is calculated.
As shown in fig. 3, the degradation curves of rhodamine b at 0, 5, 10, 15, 20, 25, and 30 minutes show that the degradation rate of rhodamine b is the highest at the first 15 minutes, and then the degradation rate hardly changes greatly with the time. The overall degradation rate can reach 70 percent in 30 minutes.
The mass spectrometric detection of rhodamine b degradation products comprises the following steps:
the degraded solution of rhodamine b obtained as described in example 1 above was tested for rhodamine b degradation products using electrospray mass spectrometry and compared to the original undegraded rhodamine b solution.
As shown in FIG. 4a and FIG. 4b, when rhodamine b is degraded for 30 minutes and compared with the mass spectrogram of undegraded rhodamine b, the molecular ion peak of rhodamine b with m/z 443.24 is rapidly reduced, the mass spectrum peaks of other small molecules are significantly increased in the degraded solution, and the surface rhodamine b is rapidly degraded into the small molecules.
Example 2
The degradation of multiple organic dye contaminants comprises the steps of:
500 ppm of Narlan, fluorescein and methylene blue solutions were prepared as described in example 1, respectively, and sprayed onto solid stained surfaces in three solutions or three contaminants dried. The degradation time was recorded for 30 minutes and 1 hour.
As shown in fig. 5a, 5b, 5c, 5d, other three organic contaminants are: the nailan, the fluorescein and the methylene blue have obvious degradation effect within 30 minutes of a tested experiment.
The action time of the mist high-energy ions is prolonged to 1 hour, and the degradation rate of the fluorescein and the methylene blue almost reaches 100 percent. The degradation effect of the Delrin is also 50 percent.
Example 3
The degradation of various organic pesticide contaminants comprises the following steps:
100 ppb of alachlor, demodex, tetramethrin, monocrotophos in methanol water (1; 1), solutions were prepared as described in example 1, and misty energetic ions were prepared and sprayed onto four solutions or four contaminant-dried solid stained surfaces. The degradation time is recorded for 30 minutes, and the organic phosphorus pesticide, the pyrethrin pesticide, the insecticide-mite and the like are found to have good degradation effect within 30 minutes.
Example 4
The solid surface escherichia coli sterilization method comprises the following steps:
test strains: escherichia coli BL21 (gram negative bacteria), bacillus subtilis 168 (gram positive bacteria);
culture medium: LB culture medium: 10 g/L of peptone, 5 g/L of yeast extract and 10 g/L of NaCl, adjusting the pH value to 7.0, and carrying out autoclaving at 121 ℃ for 15 min, wherein the solid culture medium contains 1.5% agar powder.
Detection of escherichia coli BL21 antagonistic activity: coli BL21 was first sparked on a solid plate and then a single colony was picked and inoculated in 3 mL of LB liquid medium overnight. Then adding the culture medium of Escherichia coli BL21 and Bacillus subtilis 168 into LB solid culture medium cooled to about 50 ℃ according to a certain ratio (1: 30), mixing uniformly to prepare a bacterium-containing plate, placing 4 filter paper sheets with the diameter of 4 mm in a cross shape at a position 2.5 cm away from the center, and preparing mist high-energy ions to be sprayed on the surface of the bacterial colony for 1 minute.
Washing the treated bacterial colony with buffer solution, centrifuging in a centrifuge tube at 3000-4000 r, removing supernatant, and washing with 1XPBS with appropriate pH of 7.2-7.4 for three times; when washing, the cells were gently suspended, centrifuged, and the supernatant removed.
E, fixing the Escherichia coli: 2.5% glutaraldehyde for about 3 h (1-12 h are all acceptable), centrifuged, and then washed three times with PBS, centrifuged, and the supernatant removed. Dehydrating the sample by using an ethanol water solution according to the concentration gradient of 30%, 50%, 70%, 80% and 90%, wherein each step is about 15 min, centrifuging, dehydrating for 15 min twice in 100% ethanol, centrifuging, removing the supernatant, placing the sample in a mixed solution of ethanol and tert-butyl alcohol at a ratio of 1:1 for 15 min, and removing the supernatant; then replacing alcohol with pure tert-butanol for 2 times, each time for 15 min, and finally sucking the mixed bacterium-tert-butanol suspension to drop on a cover glass.
Drying the sample: and (4) freezing the cover glass loaded with the sample in a refrigerator at the temperature of-80 ℃, and then putting the cover glass into a freeze dryer for freeze drying. After the sample is fully dried, the cover glass is adhered to the sample table with the conductive adhesive tape and plated with gold. And then observing under an electron microscope. As shown in FIG. 6, the colony surface without the mist-like high energy ion treatment was smooth, while as shown in FIG. 7, the surface of the E.coli treated with the mist-like high energy ion was rough and uneven, and the cell membrane had been destroyed.
The method can use a common high-voltage power supply, and the inert electrode enables the purified water in the capillary tube to generate vaporous high-energy ions, so as to generate a degradation effect on organic pollutants or solid surface pollutants in a solution contacted with the high-energy ions;
in order to improve the degradation capability of organic pollutants, the degradation effect on organic pollutants or solid surface pollutants in a solution contacted with high-energy ions can be improved by adjusting the voltage of a high-voltage power supply, the transmission distance of the high-energy ions and the yield of the high-energy ions.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method for degrading organic pollutants by high-energy liquid-phase ion clusters is characterized by comprising the following steps:
the liquid medium is energized by secondary high voltage electricity to generate high-energy atomized ion clusters, the secondary high voltage electricity is applied to a container provided with a conical small hole of a pure water belt, the liquid medium is sprayed out of the conical small hole to form micro liquid drops flying at a high speed, electric energy is firstly converted into kinetic energy and surface energy to enable the liquid to be broken into high-speed micro liquid drops, the micro liquid drops have high kinetic energy and high surface energy, the micro liquid drops with the high kinetic energy and the high surface energy are in friction collision with the air medium to enable the high kinetic energy and the high surface energy to be converted into chemical energy to generate high-chemical-energy ions, and the high-energy ion clusters exist in the micro liquid drops and act on the liquid or the solid surface, so that organic pollutants in a solution and on the solid surface are degraded.
2. The method of claim 1, wherein the high energy ionic liquid clusters are generated by sub-high voltage electrically energized liquid, the high energy ions are present in the nano micro droplets to form high energy liquid clusters, and the high energy liquid clusters comprise: hydroxyl radical, water radical cation cluster, negative oxygen ion cluster, hydronium ion.
3. The method for degrading organic pollutants by using high-energy liquid-phase ion clusters according to claim 2, wherein the degradation of the organic pollutants is carried out by spraying the high-energy ion liquid clusters into the solution of the organic pollutants or on the surface of a solid carrying the organic pollutants.
4. The method for degrading organic pollutants by using high-energy liquid-phase ion clusters according to claim 3, wherein the solvent of the organic pollutant solution comprises water and various solvents of methanol, ethanol and acetonitrile.
5. The method of claim 3, wherein the organic pollutants comprise rhodamine B, fluorescein, NalAN, methylene blue, organophosphorus pesticides, pyrethrin pesticides, and acaricide Kechung mite.
6. The method for degrading organic pollutants according to claim 3, wherein the liquid medium comprises tap water, distilled water or alcohol.
7. The method according to claim 3, wherein the solid is metal, high molecular material, fruits, vegetables or living organisms.
8. The method according to claim 3, wherein the surface of the solid body comprises a smooth surface, a rough surface and a narrow micron-scale micro-area surface, and a micron-scale narrow micro-area surface of a chip surface of an integrated circuit.
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