CN113281395B - Pollutant degradation and monitoring system and construction method and application thereof - Google Patents

Pollutant degradation and monitoring system and construction method and application thereof Download PDF

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CN113281395B
CN113281395B CN202110434303.4A CN202110434303A CN113281395B CN 113281395 B CN113281395 B CN 113281395B CN 202110434303 A CN202110434303 A CN 202110434303A CN 113281395 B CN113281395 B CN 113281395B
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monitoring system
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pollutant degradation
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CN113281395A (en
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胡良胜
赵夏
黄赞玲
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Shantou University
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Abstract

The invention belongs to the technical field of water pollution treatment, and discloses a pollutant degradation and monitoring system, and a construction method and application thereof. The pollutant degradation and monitoring system comprises a working electrode, a counter electrode, a reference electrode, an electrochemical workstation and a light source; the working electrode, the counter electrode and the reference electrode are all connected with an electrochemical workstation; the working electrode has both photocatalytic degradation and electrocatalytic detection properties. The pollutant degradation and monitoring system provided by the invention can realize degradation and real-time monitoring of pollutants at the same time, is simple to operate, does not need pretreatment, and greatly improves the treatment efficiency of the pollutants. The system has low manufacturing cost, is convenient to carry, does not need a specific working environment, can be used on site and is simple and convenient to operate; the complex pretreatment of the target pollutants is not needed, and the efficiency is higher. The system realizes the simultaneous removal of pollutants in the water body and the online monitoring of trace amount.

Description

Pollutant degradation and monitoring system and construction method and application thereof
Technical Field
The invention belongs to the technical field of water pollution treatment, and particularly relates to a pollutant degradation and monitoring system and a construction method and application thereof.
Background
With the rapid increase of the discharge amount of wastewater containing pollutants, some pollutants which have certain bioaccumulation and ecotoxicology and are difficult to self-degrade have adverse effects on human health and growth and reproduction of animals and plants. For example, the heavy metal hexavalent chromium (Cr (VI)) is easily absorbed by human body and easily causes cancer, more than 10ppm of Cr (VI) compound can cause death of aquatic life, and the Cr (VI) compound is classified as a serious carcinogen by the international cancer research organization. The common phenolic pollutants can cause skin and nerve diseases after being contacted for a long time, and the poisoning can be caused by excessive intake. Therefore, monitoring and treatment of pollutants need to be highly valued. At present, degradation and monitoring of pollutants are mostly treated separately, general operation is complex, pretreatment or special instruments are needed, the number of processes is large, the time is long, and the cost is high. The common treatment method has more defects, such as long treatment period and limited treatment capacity of the biodegradation method; the adsorption method has large consumption of regeneration energy; chemical method reagents are expensive, and secondary pollution is easy to cause. The monitoring method also has some disadvantages, such as the chromatography needs pretreatment, special personnel is needed, instruments are expensive, the sensor analysis is easy to pollute, the repeatability is poor, and the field online work can not be carried out.
Therefore, it is urgently needed to provide a method for quickly and efficiently treating pollutants, which is simple to operate and does not need pretreatment.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a pollutant degradation and monitoring system, which can simultaneously realize the degradation and real-time monitoring of pollutants, is simple to operate, does not need pretreatment, and can effectively treat the pollutants.
The invention provides a pollutant degradation and monitoring system in a first aspect.
Specifically, a pollutant degradation and monitoring system comprises a working electrode, a counter electrode, a reference electrode, an electrochemical workstation and a light source; the working electrode, the counter electrode and the reference electrode are all connected with the electrochemical workstation; the working electrode has both photocatalytic degradation and electrocatalytic detection properties.
The degradation and monitoring of the pollutants are conventionally carried out separately and independently, and sampling treatment needs to be carried out respectively.
Preferably, the working electrode comprises at least one of a noble metal-containing titanium dioxide nanomaterial, a noble metal-containing zinc oxide material, a titanium dioxide single crystal, or a phosphorus-doped carbon nitride nanomaterial. Silver-doped titanium dioxide nanoparticles (T.N. Ravishankar: electrochemical detection and photochemical detection of monovalent chromium (Cr (VI)) byAg doped TiO prepared as described by T.N. Ravishankar et al 2 Nano particles, anal. Methods,2015,7, 3493), shu Han Qing et al prepared surface-Tailored titanium dioxide single crystals (Shu Han Qing Photochemical Anti-Fouling application for Electrochemical polarization depletion on face-modified TiO) 2 Single Crystals environ, sci, technol.2017,51, 11326-11335), ag/In prepared by Wei et al 2 S 3 /ZnO(Wei Construction of Z-scheme Ag/In 2 S 3 ZnO nanoros complex photocatalysts for the classification of 4-nitrophenol Junwei Wei et al 2021 Nanotechnology 32 105706), and the like.
Further preferably, the noble metal in the noble metal-containing titanium dioxide nanomaterial is at least one of gold, silver or platinum.
Preferably, the counter electrode is a platinum counter electrode or a carbon counter electrode.
Preferably, the reference electrode is selected from an Ag/AgCl electrode, an Hg/HgO electrode, a saturated calomel electrode, or Hg/HgSO electrode 4 One of the electrodes.
Preferably, the light source is a xenon lamp light source or sunlight.
The invention provides a construction method of a pollutant degradation and monitoring system in a second aspect.
Specifically, the construction method comprises the following steps:
(1) Preparing a material with photocatalytic degradation and electrocatalytic detection performance into a working electrode;
(2) And (2) respectively connecting the counter electrode, the reference electrode and the working electrode prepared in the step (1) with an electrochemical workstation, placing the electrochemical workstation in a solution to be treated, and preparing a light source to obtain the pollutant degradation and monitoring system.
Preferably, the material having both photocatalytic degradation and electrocatalytic detection performance in the step (1) is a noble metal-containing titanium dioxide nanomaterial, and the preparation method of the noble metal-containing titanium dioxide nanomaterial comprises the following steps:
(a) Growing TiO on conductive substrate (such as carbon cloth, CC) in situ by using titanium source as raw material 2 To obtain the growth of TiO 2 The conductive substrate of (1);
(b) Growing TiO on the obtained product in the step (a) 2 The conductive substrate is soaked in a solution of a carbon source precursor for reaction to obtain a precipitate, and the precipitate is annealed to obtain carbon-coated TiO 2 ；
(c) Carbon-coated TiO prepared in step (b) by electrochemical deposition or photoreduction 2 And depositing noble metal nano particles to prepare the titanium dioxide nano material containing noble metal.
The method designs and synthesizes the titanium dioxide nano material containing noble metal by the methods of heat treatment, electrodeposition and the like. The material has good photocatalytic performance and electrocatalysis detection performance, can further promote the separation of photoproduction hole electrons in the presence of external voltage, and promotes the further improvement of optical and electrical properties under the synergistic action of photocatalytic reaction and electrode surface cleaning.
Preferably, in step (a), the titanium source is an organic or inorganic titanium salt such as tetrabutyl titanate, tetraisopropyl titanate and titanium tetrachloride.
Preferably, in the step (a), the conductive substrate is selected from at least one of conductive carbon cloth, carbon paper, titanium sheet (mesh), stainless steel mesh, copper foam or nickel foam.
Preferably, in step (b), the carbon source precursor is selected from at least one of dopamine, glucose, aniline or pyrrole.
Preferably, in the step (b), the annealing temperature is 600-1000 ℃, and the annealing time is 1-6h; further preferably, in the step (b), the annealing temperature is 700-900 ℃, and the annealing time is 2-5h.
Preferably, in step (b), the annealing process is carried out in the presence of hydrogen, CO, CH 4 、C 2 H 4 And the like in a reducing gas atmosphere.
Preferably, in the step (1), the solution to be treated contains heavy metal ions (such as hexavalent chromium (Cr (vi)), manganese, lead), phenols (such as bisphenol, phenol, chlorophenol, nitrophenol), antibiotics (such as tetracycline), and the like.
Preferably, the solution to be treated also contains an electrolyte, such as hydrochloric acid, a phosphate buffer solution and the like.
In a third aspect, the invention provides a use of a pollutant degradation, monitoring system.
The pollutant degradation and monitoring system is applied to wastewater and sewage treatment. Such as waste water or sewage containing heavy metal ions (such as hexavalent chromium (Cr (VI)), manganese and lead), phenols (such as bisphenol, phenol, chlorophenol and nitrophenol) and antibiotics (such as tetracycline).
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention uses the material with photocatalytic degradation and electrocatalysis detection performance as the working electrode, and constructs a pollutant degradation and monitoring system together with the counter electrode and the reference electrode, which can realize the degradation and real-time monitoring of pollutants simultaneously, has simple operation, does not need pretreatment, and greatly improves the treatment efficiency of pollutants.
(2) The pollutant degradation and monitoring system provided by the invention has the advantages of low manufacturing cost, convenience in carrying, no need of specific working environment, capability of being used on site and simplicity and convenience in operation; the complex pretreatment of the target pollutants is not needed, and the efficiency is higher. The system realizes the simultaneous removal of pollutants in the water body and the online monitoring of trace amount.
Drawings
FIG. 1 is a scanning electron microscope image of the gold-containing titanium dioxide nanomaterial prepared in example 1;
FIG. 2 is a time-current curve of dropping Cr (VI) of different concentrations in the absence of light in application example 1;
FIG. 3 is a graph of response current versus Cr (VI) concentration for various applications in example 1 without light;
FIG. 4 is a time-current curve of dropping Cr (VI) of different concentrations under illumination in application example 1;
FIG. 5 is a graph showing the response current versus Cr (VI) concentration in the case of application example 1 under illumination;
FIG. 6 is a time current ampere curve for application example 1;
FIG. 7 is a graph of degradation rate, photocurrent, and time for application example 1;
FIG. 8 is a graph of photodegradation, photodegradation rate, and time for application example 1;
FIG. 9 is a plot of the differential pulse voltammetry response of electrolytes of different pH in application example 2 to 2,6 dichlorophenol;
FIG. 10 is a DPV response curve for the use of various concentrations of 2,6 dichlorophenol of example 2;
FIG. 11 is a DPV response curve for various concentrations of 2,4 dichlorophenol of application example 2;
fig. 12 is a graph of DPV response of 2,6 dichlorophenol using different electrodes in example 2.
Detailed Description
In order to make the technical solutions of the present invention more clearly apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A preparation method of titanium dioxide nano material containing gold comprises the following steps:
firstly, pretreating conductive Carbon Cloth (CC), arranging conductive carbon in an ethanol solution containing 0.05mol of tetrabutyl titanate, carrying out ultrasonic treatment for 20 minutes, then placing the mixture in a muffle furnace, and annealing the mixture for 30 minutes at 400 ℃ to obtain the pretreated conductive carbon cloth;
then mixing 15mL of acetone, 15mL of HCl and 1.5mL of tetrabutyl titanate, adding pretreated conductive carbon cloth, transferring the mixture to a reaction kettle, placing the reaction kettle in an oven, reacting at 200 ℃ for 90 minutes, filtering to obtain a precipitate, cleaning the obtained precipitate by using distilled water and ethanol, then placing the precipitate into a Tris-HCl buffer solution (pH 8.5) containing dopamine (30 mu g/mL), stirring for 3 hours, filtering to obtain a precipitate, drying the precipitate, placing the dried precipitate in a crucible, placing the crucible in a tubular furnace, and treating at 800 ℃ for 3 hours in a hydrogen atmosphere. After the reaction is finished, scanning for three circles in a buffer solution (pH 7.4) containing 0.1mM tetrachloroauric acid in a range of-1.25V to-0.7V (relative to Ag/AgCl) by cyclic voltammetry, and depositing on the surface of the material to obtain the gold-containing titanium dioxide nano material. Scanning electron microscope analysis is carried out on the prepared titanium dioxide nano material containing gold, and as shown in figure 1, the composite material can be observed to be composed of nano wires, the growth is uniform, and gold particles are attached to the surface.
Example 2
A pollutant degradation and monitoring system comprises a working electrode, a platinum electrode and a silver-silver chloride electrode, wherein the working electrode, the platinum electrode and the silver-silver chloride electrode are respectively connected with an electrochemical workstation, and a light source is a xenon lamp.
A pollutant degradation, monitoring system construction comprising the steps of:
(1) Preparing a working electrode, namely cutting the gold-containing titanium dioxide nano material prepared in the embodiment 1 into 1 cm multiplied by 1.25 cm, and preparing an electrode with an exposed area of 1 square cm by combining conductive adhesive, insulating adhesive and a copper wire to obtain the working electrode;
(2) And respectively connecting the working electrode, the platinum electrode and the silver-silver chloride electrode with an electrochemical workstation.
Example 3
A pollutant degradation and monitoring system comprises a working electrode, a platinum electrode and a silver-silver chloride electrode, wherein the working electrode, the platinum electrode and the silver-silver chloride electrode are respectively connected with an electrochemical workstation, and a light source is a xenon lamp. Wherein the working electrode comprises silver-doped titanium dioxide nanoparticles prepared by T.N. Ravishankar et al (see T.N. Ravishankar: electrochemical detection and photochemical determination of monovalent chromium (Cr (VI)) by Ag nanoparticles TiO2 nanoparticles, anal. Methods,2015,7, 3493).
A pollutant degradation, monitoring system construction comprising the steps of:
(1) Preparing a working electrode, cutting a silver-doped titanium dioxide nano particle material prepared by T.N.Ravishankar and the like into 1 cm multiplied by 1.25 cm, and preparing an electrode with an exposed area of 1 square cm by combining conductive adhesive, insulating adhesive and a copper wire to obtain the working electrode;
(2) And respectively connecting the working electrode, the platinum electrode and the silver-silver chloride electrode with an electrochemical workstation.
Application example 1
The pollutant degradation and monitoring system constructed in the embodiment 2 is adopted to treat sewage containing Cr (VI), each electrode is placed in HCl electrolyte solution containing Cr (VI), a xenon lamp is turned on or off, and an electrochemical workstation is started. And the ability to treat Cr (VI) -containing wastewater was examined.
Application example 2
The phenolic pollutants were treated using the pollutant degradation, monitoring system constructed in example 2. And (3) placing each electrode in phosphate buffer solution containing phenolic pollutants, starting a xenon lamp, and starting the electrochemical workstation. And testing the ability to treat phenolic-containing contaminants.
Product effectiveness testing
(1) Treating sewage containing Cr (VI).
In the test of treating the sewage containing Cr (VI), cr (VI) with different concentrations is dripped into the electrolyte of the application example 1 under the conditions of light and no light respectively, and the detection condition is tested. FIG. 2 is a time-Current curve of Cr (VI) with different concentrations in the absence of illumination, the abscissa in FIG. 2 is time (time), the ordinate is Current density (Current density), as shown in FIG. 2,4 and 10 μ M Cr (VI) are respectively added in 50s for several times after 100s, and the Current density changes with the concentration of the added Cr (VI). Fig. 3 is a graph showing the relationship between Cr (vi) concentrations and response currents in the absence of illumination, in fig. 3, the abscissa represents Concentration (Concentration) and the ordinate represents Current density (Current density), and it can be seen from fig. 3 that the Current variation and the Cr (vi) Concentration variation exhibit a certain linear relationship. FIG. 4 is a time-current curve of Cr (VI) with different concentrations added under illumination, in FIG. 4, the abscissa is time (time) and the ordinate is Photocurrent intensity (Photocurent), and FIG. 4 is a graph showing the result of continuous multiple additions of Cr (VI) in stirred 0.1M HCl under illumination. Fig. 5 is a graph showing the relationship between Cr (vi) and response current under illumination, in fig. 5, the abscissa represents Concentration (Concentration) and the ordinate represents Photocurrent intensity (photo current), and it can be seen from fig. 5 that the current variation and the Cr (vi) Concentration variation have a certain linear relationship. As can be seen from FIGS. 2 to 5, the response current of the electrode and the Cr (VI) concentration both show good linear relationship in the presence and absence of illumination, and the electrochemical monitoring performance is excellent.
The degradation and monitoring performance of the system was further tested and fig. 6 is a Photocurrent time curve with time (time) on the abscissa and Photocurrent intensity (photo current) on the ordinate. In FIG. 6, 100s,200s, and 300s are ON moments, and 150s,250s, and 350s are OFF moments. As can be seen from FIG. 6, the overall photocurrent response was very rapid, and 120. Mu.MCr (VI) was added dropwise at 400s, the photocurrent was instantaneously decreased, and the light was applied (300W from a xenon lamp) at 500s, and the photocurrent was gradually recovered as the light application time increased. After the illumination is continued for 24 minutes, cr (VI) can be seen to be completely degraded, and the result is consistent with the test result of an ultraviolet-visible spectrophotometer. And the current and the concentration still present a linear relationship in the degradation process, which shows that the pollutant degradation and monitoring system provided by the embodiment 2 realizes the synchronous degradation and monitoring of Cr (VI).
FIGS. 7 and 8 are derived from FIG. 6, FIG. 7 is a graph of degradation rate, photocurrent versus time, along the abscissa of FIG. 7, time (time) and the left ordinate of degradation rate (C/C) along the left ordinate 0 ) The right ordinate is the Photocurrent intensity (Photocurent) and the curves represent the degradation rate and the Photocurrent intensity (Photocurent), respectively. As can be seen from FIG. 7, as the illumination time increases, the current gradually increases, i.e. Cr (VI) is gradually reduced, and 120 μ M Cr (VI) is completely reduced within 24 min. During illumination, the ultraviolet-visible spectrum test is carried out once every 4 minutes, and the electrode data are consistent with the ultraviolet-visible spectrum test result. FIG. 8 is a graph of photodegradation, photoelectric degradation rate and time, in FIG. 8, the abscissa is time (time) and the ordinate is degradation rate (C/C) 0 ) The curves represent applied light and electricity (PEC) and applied light only without applied electricity (PC), respectively. As can be seen from FIG. 8, at 1440s, the system reduced 97.9% of Cr (VI), and the reduction effect was weaker than that in the case of the applied voltage. Therefore, the reduction efficiency can be improved under the photoelectric synergistic effect, and the external voltage can accelerate the electron transfer when the electrode generates photo-generated electrons under the illumination condition.
(2) And (4) treating phenolic pollutants.
The pollutant degradation and monitoring system is constructed in example 2 to treat the phenolic pollutants (application example 2), and the performance of the pollutant degradation and monitoring system is researched under the conditions of electrolytes with different pH values and phenolic pollutants with different concentrations. FIG. 9 is a DPV response curve (differential pulse voltammetry curve) of electrolytes of varying pH to 2,6 dichlorophenol with voltage (Potential/V) on the abscissa, current on the ordinate and 50 μ A per unit length of 50 μ A in FIG. 9. As can be seen from fig. 9, pH affects the sensitivity of the electrode.
FIG. 10 is a DPV response curve with voltage (Potential/V) on the abscissa and Current (Current) on the ordinate for different concentrations of 2,6 dichlorophenol, each curve representing a different concentration of 2,6 dichlorophenol. As can be seen from fig. 10, the peak current is different depending on the concentration, and the current changes depending on the concentration of the substance, so that the substance can be quantitatively detected to some extent.
FIG. 11 is a DPV response curve for different concentrations of 2,4 dichlorophenol, with voltage (Potential/V) on the abscissa and Current (Current) on the ordinate, each curve representing a different concentration of 2,4 dichlorophenol. As can be seen from fig. 11, the peak current is different depending on the concentration, and the current is changed depending on the concentration of the substance, so that the measurement can be performed quantitatively to a certain extent.
Fig. 12 is a DPV response curve of 2,6 dichlorophenol for different electrode pairs, with voltage (Potential/V) on the abscissa and Current (Current) on the ordinate, and the three curves respectively represent the working electrode (new electrode) obtained in example 2, the contaminated electrode (contaminated electrode) obtained after the working electrode obtained in example 2 is used for a plurality of times, and the regenerated electrode (regenerated electrode) obtained by subjecting the contaminated electrode to light treatment. As can be seen from fig. 12, the peak appearance of the new electrode is significant, the peak of the contaminated electrode becomes insignificant, and the peak appearance of the regenerated electrode is significant, indicating that the electrode has good regeneration performance.
As can be seen from FIGS. 9-12, the pollutant degradation and monitoring system has good degradation and monitoring performance on phenolic pollutants.

Claims (8)

1. A pollutant degradation and monitoring system is characterized by comprising a working electrode, a counter electrode, a reference electrode, an electrochemical workstation and a light source; the working electrode, the counter electrode and the reference electrode are all connected with the electrochemical workstation; the working electrode has photocatalytic degradation and electrocatalytic detection performances at the same time;
the working electrode comprises a titanium dioxide nano material containing noble metal, and the preparation method of the titanium dioxide nano material containing noble metal comprises the following steps:
(a) Growing TiO on a conductive substrate in situ by using a titanium source as a raw material 2 To obtain a film grown with TiO 2 The conductive substrate of (1);
(b) Growing TiO on the obtained product in the step (a) 2 Soaking the conductive substrate in a solution of a carbon source precursor, reacting to obtain a precipitate, and annealing the precipitate to obtain carbon-coated TiO 2 ；
(c) By electrochemical deposition or reductionThe carbon-coated TiO produced in step (b) of the process 2 And depositing noble metal nano particles to prepare the titanium dioxide nano material containing noble metal.
2. A pollutant degradation, monitoring system according to claim 1, in which the counter electrode is a platinum or carbon counter electrode; the reference electrode is selected from Ag/AgCl electrode, hg/HgO electrode, saturated calomel electrode or Hg/HgSO electrode 4 One of the electrodes.
3. A pollutant degradation, monitoring system according to claim 1, wherein in step (a) the source of titanium is an organic or inorganic titanium salt; the conductive substrate is selected from at least one of conductive carbon cloth, carbon paper, titanium sheet, stainless steel net, copper foam or nickel foam.
4. A pollutant degradation, monitoring system according to claim 1, wherein in step (b) the carbon source precursor is selected from at least one of dopamine, glucose, aniline or pyrrole.
5. A contaminant degradation, monitoring system according to claim 1, wherein in step (b), the annealing temperature is 600-1000 ℃ and the annealing time is 1-6h.
6. The method of constructing a pollutant degradation, monitoring system according to any one of claims 1 to 5, comprising the steps of:
(1) Preparing a material with photocatalytic degradation and electrocatalytic detection performance into a working electrode;
(2) And (2) respectively connecting the counter electrode, the reference electrode and the working electrode prepared in the step (1) with an electrochemical workstation, placing the electrochemical workstation in a solution to be treated, and preparing a light source to obtain the pollutant degradation and monitoring system.
7. The constructing method according to claim 6, wherein in the step (2), the liquid to be treated further contains an electrolytic solution.
8. Use of a contaminant degradation, monitoring system according to any one of claims 1 to 5 for the treatment of wastewater.
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