CN112694198A - Method for dechlorinating trichloroacetic acid through catalytic electrolysis of vitamin B12 modified electrode - Google Patents
Method for dechlorinating trichloroacetic acid through catalytic electrolysis of vitamin B12 modified electrode Download PDFInfo
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- CN112694198A CN112694198A CN202011366800.7A CN202011366800A CN112694198A CN 112694198 A CN112694198 A CN 112694198A CN 202011366800 A CN202011366800 A CN 202011366800A CN 112694198 A CN112694198 A CN 112694198A
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
Abstract
The invention provides a method for dechlorinating trichloroacetic acid by catalyzing and electrolyzing trichloroacetic acid through a vitamin B12(VB12) modified electrode. The technical scheme is as follows: firstly, VB12 powder is dispersed in ethanol containing polymer Nafion to prepare VB12 dispersion liquid; then the VB12 dispersion liquid is dripped on the surface of the iron electrode, and the modified VB 12/iron electrode is obtained after air drying; and (3) establishing an electrolytic cell device by taking a VB 12/iron electrode as a cathode and a graphite electrode as an anode to electrolyze trichloroacetic acid. The invention aims to utilize VB12 to catalyze and electrolyze trichloroacetic acid, and the dechlorination of a target object has the advantages of targeted dechlorination, high dechlorination efficiency, no secondary pollution, low cost, simple structure, safety, stability and the like.
Description
Technical Field
The application relates to the technical field of drinking water safety guarantee, in particular to an electrolytic treatment method for dechlorinating chlorinated disinfection byproducts and reducing toxicity.
Technical Field
Chlorine is one of the high-quality and low-cost disinfectants in global drinking water treatment, is used for inactivating microorganisms and ensures that the growth of the microorganisms in a water supply network is inhibited for a long time. However, natural organic substances present in raw water are liable to react with chlorine to form various disinfection by-products, such as trihalomethane, haloacetic acid, haloacetonitrile, and the like. These disinfection by-products have a "three-fold" effect, which can have an adverse effect on human health. Haloacetic acids have been shown to be carcinogenic, teratogenic, mutagenic to rodents, embryotoxic, and to be far more carcinogenic than the sum of other disinfection byproducts. Haloacetic acid is highly harmful to the human body and even has been considered by researchers to be the leading factor contributing to the carcinogenic risk of disinfection by-products.
In order to control the amount of generated disinfection byproducts, three approaches are generally adopted, namely front-end control, namely the removal of the natural organic matter precursors is enhanced, process control, namely the use of alternative disinfectants, and post-treatment, namely the removal of generated disinfection byproducts. The front-end control mainly comprises advanced treatment technologies including an oxidation method, a reinforced flocculation method, an adsorption method and the like. The removal rate of organic matters by different technologies in the front-end control approach is different, the method is applied to the treatment of micro-polluted water sources, and the organic matters with a certain concentration still enter a disinfection stage to derive chlorinated organic matters. The process control techniques include optimizing chlorine dosing and using other disinfectants. The process control can reduce the yield of the chlorinated disinfection byproducts to a certain degree, but because the water supply of a pipe network still needs to maintain residual chlorine to inhibit the growth and the propagation of microorganisms, chlorine has enough long reaction time to react with organic matters in the water conveying process of the pipe network to generate the disinfection byproducts, and researches in recent years show that almost all the yields of the disinfection byproducts gradually increase along with the extension of the water conveying distance or the water conveying time. The post-treatment directly takes the disinfection by-product as the target object, and can effectively reduce the concentration and the toxicity of the disinfection by-product. The current commonly used post-treatment methods include an aeration method, an adsorption method, a catalytic oxidation method and the like. The aeration method can diffuse the volatile disinfection by-product components from the liquid phase to the gas phase so as to remove the volatile disinfection by-product components, but has no obvious removal effect on the difficultly volatile disinfection by-product trihaloacetic acid. The adsorption method uses activated carbon to effectively remove nonpolar or hydrophobic organic substances in water, but because the disinfection byproducts are mostly polar and weakly polar substances and are susceptible toThe interference of other substances in the matrix has limited removal effect; catalytic oxidation processes, e.g. using photocatalytic TiO2Can effectively remove disinfection by-products, but has high energy consumption and TiO2And the like, and the catalyst is not easy to recover. The invention is different from the technologies, and develops the technology for realizing the efficient dechlorination and reducing the disinfection byproducts from the angle of C-Cl bond breakage based on the theory that the toxicity of the chlorinated disinfection byproducts is mainly derived from chlorine in the molecular structure, thereby realizing the detoxification of the chlorinated disinfection byproducts and reducing the energy requirement of a reaction system. The efficient treatment technology with the target of targeted dechlorination is another idea of controlling disinfection byproducts in post-treatment and ensuring the safety of drinking water.
Disclosure of Invention
VB12, vitamin B12, contains corrin ring with Co (III) as center in chemical structure, is excellent catalyst for reduction reaction, and the action principle is that Co (III) easily captures electrons and converts the electrons into Co (II)/Co (I) with strong reduction, and then the electrons are transferred to promote the reduction reaction. Chlorine atoms in chlorinated organic matters have the tendency of getting electrons and can be effectively dechlorinated through catalytic reduction of VB 12. The technology uses VB12 loaded on the electrode as a catalyst, and the electron transfer in the electrode reaction process and VB12 form a reducing agent with targeted dechlorination, so that the trichloroacetic acid as a chlorinated disinfection by-product in water is dechlorinated step by step, the toxicity is reduced, and the influence of the chlorinated disinfection by-product on the quality of drinking water is reduced. The VB12 electrochemical catalysis chlorination by-product dechlorination has the advantages of high reaction efficiency, directional dechlorination, environmental friendliness and the like, and is an excellent method for treating various chlorinated organic compounds. The invention takes a VB12 loaded metal composite electrode as a cathode to carry out electrocatalytic reduction dechlorination on trichloroacetic acid which is a typical chlorinated disinfection by-product.
The application aims to provide a method for dechlorinating trichloroacetic acid through catalytic electrolysis under the condition of vitamin B12 modified electrodes, aims to reduce the chlorination degree of trichloroacetic acid as a disinfection by-product, and provides a new way for treating the chlorinated disinfection by-product.
In order to achieve the technical effects, the application adopts the following technical scheme that the method for dechlorinating trichloroacetic acid through catalytic electrolysis of vitamin B12 modified electrodes comprises the following steps:
s1, preparing VB12 dispersion liquid;
s2, preparing VB 12/metal electrode;
s3, building an electrolytic cell device;
s4, and catalyzing and electrolyzing trichloroacetic acid.
Preferably, the preparation of the VB12 dispersion by the S1 comprises the following steps: the desired VB12 dispersion was prepared by dispersing VB12 powder in 1.0mL of ethanol containing polymer Nafion by ultrasonic agitation.
Preferably, the solution amount of the VB12 powder is 1.0mM, and the volume amount of the polymer Nafion is 50 μ L.
Preferably, the preparation of VB 12/metal electrode by S2 comprises the following steps:
step 1: taking a metal bare electrode, grinding the metal bare electrode by abrasive paper, polishing the metal bare electrode to a bright mirror surface by using alumina slurry, and washing the metal bare electrode by using distilled water twice to obtain a metal electrode A;
step 2: sequentially placing the metal electrode A in absolute ethyl alcohol and distilled water, respectively carrying out ultrasonic treatment for 5min, washing and then airing for later use to obtain a metal electrode B;
and step 3: and (3) absorbing the ultrasonic VB12 dispersion liquid by adopting a micro liquid inlet needle, dripping the dispersion liquid on the surface of the metal electrode B for multiple times, and naturally drying at room temperature to obtain the modified VB 12/metal electrode.
Preferably, the bare metal electrode is an iron electrode.
Preferably, the step S3 of constructing the electrolytic cell device includes the steps of:
step 1: setting an electrolytic cell main body, wherein the height of the electrolytic cell main body is 158mm, the outer diameter of the electrolytic cell main body is 105mm, and a fixed clamping groove is arranged at a position 30mm away from the upper end of the bottom of the electrolytic cell main body and is used for stabilizing an electrode and controlling the polar distance of the electrode;
step 2: an anode electrode and a cathode electrode are respectively arranged in the fixing clamp grooves, the electrolytic solution in the electrolytic cell main body realizes uniform reaction through magnetic stirring, the periphery of the electrolytic cell main body is tightly wrapped by tinfoil paper, and the joint of the sampling port of the electrolytic cell main body and the electrolytic cell main body is tightly wound by a preservative film.
Preferably, the rotation speed of the magnetic stirring stirrer in the step 2 is 150 rpm.
Preferably, in the step 2, the distance between the cathode electrode and the anode electrode is 30mm, and the pH value of the electrolytic solution is 3-7.
Preferably, the catalytic electrolysis of trichloroacetic acid in S4 includes the following steps:
step 1: trichloroacetic acid solutions with different initial concentrations are prepared;
step 2: arranging a plurality of electrolytic cell devices corresponding to trichloroacetic acid solutions with different concentrations, respectively arranging an anode electrode and a cathode electrode in a fixing clamping groove of each electrolytic cell main body, wherein the anode electrode is a graphite electrode, the cathode electrode is a VB 12/metal electrode, pouring trichloroacetic acid solutions with different concentrations into each electrolytic cell main body, and sequentially carrying out current dechlorination to obtain samples with different concentrations;
and step 3: samples of different concentrations were taken to determine the concentration of trichloroacetic acid, dichloroacetic acid and monochloroacetic acid by GC/ECD and the concentration of acetic acid by ion chromatography, respectively.
Preferably, voltage regulation is needed in the current dechlorination process to enable the power supply to output constant current, and the current density is 3-11 mA/cm2。
The invention has the beneficial effects that: the application loads VB12 on the iron electrode for preparation and modification, the VB 12/iron electrode is used as a cathode, the graphite electrode is used as an anode, the electrolytic cell device is constructed, the targeted dechlorination of the trichloroacetic acid which is a chlorinated disinfection by-product can be realized, and the method has the advantages of high dechlorination efficiency, no secondary pollution, low cost, simple structure, safety, stability and the like, and is an excellent method for dechlorinating the trichloroacetic acid which is a chlorinated disinfection by-product.
Drawings
FIG. 1: a graph comparing the effect of VB12 loading dose according to the invention;
FIG. 2: the invention is a comparison graph of the influence of the electrode materials of the iron sheet, the copper sheet and the aluminum sheet;
FIG. 3: is a comparative plot of the effect of current density according to the present invention;
FIG. 4: a graph comparing the influence of the pH value of the invention;
FIG. 5: is a comparative plot of the effect of temperature according to the present invention;
FIG. 6: is a dechlorination effect graph of trichloroacetic acid with different concentrations along with time;
FIG. 7: is a product diagram of the dechlorination process of trichloroacetic acid;
FIG. 8: is a schematic flow chart of the invention.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples in conjunction with the accompanying drawings.
Embodiments of the present invention will be described in detail below with reference to examples. The following examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention. The reagents or instruments are not indicated by manufacturers, and are all conventional products which can be purchased through normal channels.
VB12 modified electrode catalyzed dechlorination of trichloroacetic acid, the initial concentration of trichloroacetic acid was 50, 100, 200 and 500 mug/L respectively.
The method specifically comprises the following steps:
s1, preparing VB12 dispersion liquid. A VB12 dispersion was prepared by dispersing 1.0mM VB12 powder in 1.0mL of ethanol containing 50. mu.L of Nafion (perfluorosulfonic acid) with ultrasonic stirring.
S2, preparing VB 12/iron electrode. Grinding an iron electrode (40 multiplied by 70 multiplied by 2mm) by abrasive paper, polishing by using alumina slurry to a bright mirror surface, washing by using distilled water twice, sequentially placing in absolute ethyl alcohol and distilled water, respectively carrying out ultrasonic treatment for 5min, and drying for later use after washing. And (3) absorbing the ultrasonic VB12 dispersion liquid by adopting a micro liquid inlet needle, dripping and coating the dispersion liquid on the surface of the metal electrode for multiple times, and naturally drying the metal electrode at room temperature to obtain the modified VB 12/iron electrode.
And S3, constructing an electrolytic cell device. The glass electrolytic cell is 158mm high, external diameter 105mm, and is set up a fixed slot for stabilizing the electrode and controlling the electrode polar distance interval to be 30mm apart from the bottom of the pool 30 mm. The anode of the electrode adopts a graphite electrode, and the cathode adopts an iron electrode. The periphery of the electrolytic cell is tightly wrapped by tinfoil paper to provide light-proof reaction conditions for VB12, and the joint of the sampling port of the reaction cell and the cell body is sealed and wound by a preservative film. The solution in the electrolytic cell realizes uniform reaction by magnetic stirring, and the rotating speed is 150 rpm. The pH was adjusted to 3.
S4, electrifying to catalyze the chlorination and disinfection by-product for dechlorination. The voltage is regulated to make the output current density of the power supply be 7mA/cm2Dechlorination is carried out by the current. Trichloroacetic acid solutions with initial concentrations of 50, 100, 200 and 500 mu g/L are prepared, dechlorination is sequentially carried out, 2 groups of parallel reaction tanks are arranged in each group, 30mL samples are taken out at 30min, 1h, 2h, 3h, 4h and 5h respectively, the concentrations of the trichloroacetic acid, the dichloroacetic acid and the monochloroacetic acid are determined through GC/ECD, and the concentration of the acetic acid is determined through ion chromatography.
The basic principle of the invention is as follows: atomic H and VB12 transfer electrons to cooperatively dechlorinate trichloroacetic acid.
In the electrochemical reduction dechlorination process, the cathode mainly generates the reduction reaction of hydrodechlorination, and the atom H (1) generated at the cathode attacks the C atom lacking electrons, so the atom H and the C atom adjacent to chlorine form a C-H bond, the formation of the C-H bond enhances the electron cloud density on the C atom, weakens the strength of the C-Cl bond, enables the C-Cl bond to be more easily attacked by nucleophilic groups, and promotes the hydrodechlorination reaction to be performed in the step (2).
H2O+e-→H·+OH- (1)
RCl+H·→RH+H++Cl- (2)
Meanwhile, VB12(Co (III)) obtains electrons to form VB12(Co (II)) in a reduced state, VB12(Co (II)) reacts with trichloroacetic acid to generate an intermediate product (VB12-R), so that the trichloroacetic acid is dechlorinated, and VB12-R can restore initial VB12(Co (III)) by self bond breaking and generate a dechlorinated product (3-4).
RCl+VB12(Co(II))→VB12-R+Cl-+X (3)
VB12-R+H+→VB12+RH (4)
A VB12 modified electrode (a modified VB 12/iron electrode) is used for catalyzing trichloroacetic acid (with the initial concentration of 50 mug/L) for dechlorination, and the trichloroacetic acid removal rate is 94% after 1h of reaction; trichloroacetic acid with the initial concentration of 100 mu g/L, and the removal rate of 95 percent after 2 h; the initial concentration is 200 mug/L trichloroacetic acid, and the removal rate is 91% in 4 h; the initial concentration is 500 mug/L trichloroacetic acid, and the 5h removal rate is 92%. The dechlorination process conforms to the first order reaction kinetics, and the dechlorination effect of trichloroacetic acid with different initial concentrations along with time is shown in figure 6.
The initial concentration of 200 ug/L of trichloroacetic acid 5h removal of 99%, 19% of the trichloroacetic acid was converted to monochloroacetic acid, 19% of the trichloroacetic acid was converted to dichloroacetic acid, 62% of the trichloroacetic acid was converted to acetic acid. The VB12 modified electrode catalyzed trichloroacetic acid dechlorination intermediate product with time change is shown in figure 7.
In conclusion, the application adopts VB12 to modify the iron electrode, effectively realizes the targeted dechlorination of trichloroacetic acid, has high dechlorination efficiency, no secondary pollution, low cost, simple structure, safety and stability, and makes up the defects of the existing method for treating the chlorination byproducts.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. A method for dechlorinating trichloroacetic acid through catalytic electrolysis of vitamin B12 modified electrodes is characterized by comprising the following steps:
s1, preparing VB12 dispersion liquid;
s2, preparing VB 12/metal electrode;
s3, building an electrolytic cell device;
s4, and catalyzing and electrolyzing trichloroacetic acid.
2. The vitamin B12 modified electrode catalyzed electrolytic trichloroacetic acid dechlorination method, according to claim 1, wherein the VB12 dispersion liquid is prepared from S1, comprising the following steps: the desired VB12 dispersion was prepared by dispersing VB12 powder in 1.0mL of ethanol containing polymer Nafion by ultrasonic agitation.
3. The method for dechlorinating trichloroacetic acid through vitamin B12 modified electrode catalysis, according to claim 2, characterized in that the mass concentration of VB12 powder is 1.0mM, and the volume of polymer Nafion is 50 μ L.
4. The vitamin B12 modified electrode catalyzed electrolytic trichloroacetic acid dechlorination method according to claim 1, wherein the VB 12/metal electrode prepared by S2 comprises the following steps:
step 1: taking a metal bare electrode, grinding the metal bare electrode by abrasive paper, polishing the metal bare electrode to a bright mirror surface by using alumina slurry, and washing the metal bare electrode by using distilled water twice to obtain a metal electrode A;
step 2: sequentially placing the metal electrode A in absolute ethyl alcohol and distilled water, respectively carrying out ultrasonic treatment for 5min, washing and then airing for later use to obtain a metal electrode B;
and step 3: and (3) absorbing the ultrasonic VB12 dispersion liquid by adopting a micro liquid inlet needle, dripping the dispersion liquid on the surface of the metal electrode B for multiple times, and naturally drying at room temperature to obtain the modified VB 12/metal electrode.
5. The method for dechlorinating trichloroacetic acid through catalysis of the vitamin B12 modified electrode according to claim 4, wherein the metal bare electrode is an iron electrode.
6. The vitamin B12 modified electrode catalyzed electrolytic trichloroacetic acid dechlorination method according to claim 1, wherein the S3 combined electrolytic cell device comprises the following steps:
step 1: setting an electrolytic cell main body, wherein the height of the electrolytic cell main body is 158mm, the outer diameter of the electrolytic cell main body is 105mm, and a fixed clamping groove is arranged at a position 30mm away from the upper end of the bottom of the electrolytic cell main body and is used for stabilizing an electrode and controlling the polar distance of the electrode;
step 2: an anode electrode and a cathode electrode are respectively arranged in the fixing clamp grooves, the electrolytic solution in the electrolytic cell main body realizes uniform reaction through magnetic stirring, the periphery of the electrolytic cell main body is tightly wrapped by tinfoil paper, and the joint of the sampling port of the electrolytic cell main body and the electrolytic cell main body is tightly wound by a preservative film.
7. The method for dechlorinating trichloroacetic acid through vitamin B12 modified electrode catalysis, according to claim 6, wherein the rotation speed of the magnetic stirring stirrer in the step 2 is 150 rpm.
8. The method for dechlorinating trichloroacetic acid through catalytic electrolysis of the vitamin B12 modified electrode according to claim 6, wherein in the step 2, the distance between the cathode electrode and the anode electrode is 30mm, and the pH value of the electrolytic solution is 3-7.
9. The method for dechlorinating trichloroacetic acid through catalysis of the vitamin B12 modified electrode according to claim 6, wherein the catalysis of the trichloroacetic acid electrolysis in S4 comprises the following steps:
step 1: trichloroacetic acid solutions with different initial concentrations are prepared;
step 2: arranging a plurality of electrolytic cell devices corresponding to trichloroacetic acid solutions with different concentrations, respectively arranging an anode electrode and a cathode electrode in a fixing clamping groove of each electrolytic cell main body, wherein the anode electrode is a graphite electrode, the cathode electrode is a VB 12/metal electrode, pouring trichloroacetic acid solutions with different concentrations into each electrolytic cell main body, and sequentially carrying out current dechlorination to obtain samples with different concentrations;
and step 3: samples of different concentrations were taken to determine the concentration of trichloroacetic acid, dichloroacetic acid and monochloroacetic acid by GC/ECD and the concentration of acetic acid by ion chromatography, respectively.
10. The method for dechlorination of trichloroacetic acid through catalytic electrolysis of the vitamin B12 modified electrode according to claim 9, wherein voltage regulation is required in the current dechlorination so that a power supply outputs constant current, and the current density is 3-11 mA/cm2。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114409025A (en) * | 2021-12-17 | 2022-04-29 | 浙江工业大学 | Method for debrominating tribromoacetic acid through catalytic electrolysis of vitamin B12 modified electrode |
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| US20040133059A1 (en) * | 2003-01-06 | 2004-07-08 | Michael Scalzi | Method for accelerated dechlorination of matter |
| JP2005288276A (en) * | 2004-03-31 | 2005-10-20 | Ecocycle Corp | Additive used in restoring contaminated soil, ground water or sedimentary soil deposit |
| CN104984994A (en) * | 2015-07-08 | 2015-10-21 | 华南理工大学 | Device and method for removing polychlorinated biphenyl in bottom mud through microorganism electrolytic tank |
| CN106876730A (en) * | 2015-12-13 | 2017-06-20 | 中国科学院大连化学物理研究所 | The porous carbon-supported base metal elctro-catalyst of N doping is prepared and electro-catalysis application |
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