CN110133071B - COD electrochemical rapid on-line monitoring method - Google Patents
COD electrochemical rapid on-line monitoring method Download PDFInfo
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- CN110133071B CN110133071B CN201910321910.2A CN201910321910A CN110133071B CN 110133071 B CN110133071 B CN 110133071B CN 201910321910 A CN201910321910 A CN 201910321910A CN 110133071 B CN110133071 B CN 110133071B
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Abstract
The invention relates to a rapid COD electrochemical on-line monitoring method, which comprises the following steps: the device comprises a sample pool, a working electrode, a reference electrode, a peristaltic pump, a magnetic stirrer, a solar cell, a solar panel, a current conversion COD chip, a wireless transmission transmitting end and a wireless transmission receiving end, wherein the working electrode adopts nano modified silicon dioxide as a carrier, and adopts waste containing carbon in petroleum processing as a raw material to prepare graphene by a thermal cracking method and modify the graphene, and then the graphene is compounded with a silicon dioxide nano modified material carrier to form the device; completely oxidizing organic matters in the sewage into H by OH hydroxyl radicals generated by the electrochemical working electrode2O and CO2The oxidation current value is converted into a COD value by a current conversion COD chip, and then the COD value is converted into a digital signal by a set circuit; the signal receiving and implementing control is carried out through a mobile phone or a network platform, and the remote control of the on-line monitor is realized.
Description
Technical Field
The invention relates to a rapid online COD electrochemical monitoring method, in particular to a rapid and accurate COD monitoring method based on an electrochemical principle and wireless transmission.
Background
COD is an important index for measuring the degree of water pollution, and the degree of water pollution is determined by the content of organic matters in the water. The content of organic matters in the sewage is detected by completely oxidizing the organic matters in the water into carbon dioxide CO by a chemical method2And water H2And O, calculating the oxygen consumption in the oxidation process to obtain the COD value of the pollution degree, namely the chemical oxygen consumption. The traditional method is that the macromolecular organic matters in the sewage are firstly degraded into micromolecules by using strong acid such as sulfuric acid and the like, and then excessive potassium permanganate or potassium dichromate is used for carrying out the degradationAnd (3) completely oxidizing the organic matters, detecting the residual potassium permanganate or potassium dichromate (also called a titration method) and calculating the oxygen consumption in a reverse mode, or measuring and calculating the oxygen consumption by a spectrophotometry method. The method has the problems of needing to adopt an organic solvent, having complex working procedures, large detection error, long detection time (6 hours), expensive equipment for realizing online monitoring and high maintenance cost.
(1) Coulomb titration method sewage COD on-line monitoring instrument
The monitoring is realized by the oxidation principle of potassium permanganate or potassium dichromate. Due to potassium permanganate MnO4The redox potential of the catalyst is only 1.33V, and the potassium dichromate K2Cr2O7The redox potential of (a) is also only 1.67V. Such oxidizing ability can oxidize only small organic molecules. Firstly, the macromolecular substance is degraded into easily-oxidized micromolecular substance by nitric acid constant-temperature closed digestion, then excessive potassium dichromate or potassium permanganate is added as oxidant, silver salt is used as catalyst, and molybdenic acid and aluminum potassium sulfate are used as cocatalyst to completely oxidize and decompose micromolecular organic matter into H2O and CO2. And titrating unreduced potassium dichromate or potassium permanganate in the water sample by using ammonium ferrous sulfate, converting the amount of consumed ammonium ferrous sulfate into the mass concentration of consumed oxygen to calculate a COD value, and transmitting the COD value to a control center through a line. However, the equipment is very complicated, the failure rate is extremely high, especially, the probe needs to be corrected regularly every day (the probe is easy to be oxidized) and different solvents need to be added quantitatively, a professional maintenance worker needs to be equipped, and meanwhile, a large amount of solvents need to be consumed and serious secondary pollution is caused. The power supply of 220V is necessary, and the detection time is 4-6 hours. Generally, the price of a terminal device without a transmission part is about 20 ten thousand yuan of renminbi (imported), the price of the terminal device is 5-8 ten thousand yuan, and the annual operating cost is 5-10 ten thousand yuan.
(2) Spectrophotometry sewage COD on-line monitor
The pretreatment of a detected sample in the method is basically the same as that of the coulometric titration method, but only potassium dichromate K2Cr2O7 is used as an oxidizing agent. The method is characterized in that hexavalent chromium in a solution is quantitatively reduced into trivalent chromium by reducing substances, the absorbance of the trivalent chromium is measured by a spectrophotometer, the COD value is quantitatively obtained through the linear relation between the absorbance and the COD of a water sample, and the COD value is transmitted to a control center through a line. The method has high accuracy of measured data. However, the equipment is very complicated, the failure rate is extremely high, especially, the probe needs to be corrected regularly every day (the probe is easy to be oxidized) and different solvents need to be added quantitatively, a professional maintenance worker needs to be equipped, and meanwhile, a large amount of solvents need to be consumed and serious secondary pollution is caused. 220v power supply must be used, and the detection and time are 4-6 hours. Generally, the price (import) of a terminal device without a transmission part is about 20 ten thousand yuan RMB, the price is domestic (5-8 ten thousand yuan), and the annual operating cost is 5-10 ten thousand yuan.
(3) Ozone oxidation COD on-line monitor
Ozone (O)3) Generated by an ozone generator specifically configured for the monitoring system. Due to ozone (O)3) The oxidation-reduction potential of the system is 2.07V, macromolecular substances in the detected solution can be completely oxidized, and the oxidizing agent (O) is measured by using a two-pair electrode system3) The amount of consumption, the electric quantity consumed by ozone, according to Faraday's law, can calculate the COD value of the water sample after being corrected. For example, the PHOENIX-1010 online COD automatic detector produced by German STIP-SICO company and the BD9372 online rapid COD analyzer produced by Beijing BeiDou star are designed according to the principle and have been widely applied in Europe and America and China. The instrument is mainly characterized by utilizing ozone (O)3) The oxidation-reduction potential of 2.07V has the characteristic of strong oxidation capacity, the pretreatment of the detected sample at high temperature of nitric acid is not carried out, the detection flow is simplified, the measurement speed is high, and the measurement time is as follows: about 30min without secondary pollution. The 220v power supply is still used, and particularly, the error between the detected accurate data and the actual value is large and can reach more than 1 or even several orders of magnitude because ozone (O)3) The oxidation-reduction potential of the organic matter is 2.07V, and the organic matter with the oxidation-reduction potential more than 2.07V can not be completely oxidized and decomposed into H2O and CO2And is only suitable for sewage systems with less macromolecular organic matters. And the instrument structure is still more complicated, and the operation maintenance volume is big, and the fault rate is high. The price (import) of a terminal device without a transmission part is 30 ten thousand RMBOn the right, the domestic production is about (8-10 ten thousand yuan), and the annual operating cost is 5-10 ten thousand yuan. The annual operating cost is about 5-10 ten thousand yuan.
(4) Lead dioxide titanium-based electrode electrochemical sewage COD on-line monitor
The titanium-based electrode of metal oxide lead dioxide with strong catalytic performance is used for electrolyzing to generate OH hydroxyl radicals with strong oxidizing capability to directly oxidize organic matters in the detected solution. Because the oxidation-reduction potential is as high as 2.8V, the organic matters in the sample can be thoroughly oxidized and completely decomposed into H2O and CO2. The COD value is obtained by the conversion relation of the electrochemical voltage and the oxidation amount. The electrochemical workstation and the transmission system are integrated to form the COD on-line monitor. Because the electricity consumption is extremely small, the 220V power supply is not used. The power supply in the field is realized by only combining a small solar panel with a solar cell. The system has the advantages of very simple equipment, high accuracy of detected data, short detection and monitoring time, only 30 minutes or so, low failure rate of the equipment and the like. However, the lead dioxide titanium-based electrode is easily oxidized by OH hydroxyl radicals to form a loose structure, so that the deviation of the detection result is large, and the accuracy of the detection result can be ensured only by regenerating the electrode every day or frequently replacing the electrode. An ELOX100ACOD on-line automatic detector from LAR company in Germany and a COD-580 on-line COD detector from Remaomagne company in Shanghai are both lead dioxide titanium-based electrode OH free radical detection modes. Generally, the price (import) of a terminal device without a transmission part is about 60 ten thousand yuan of renminbi, the price (25-30 ten thousand yuan) of a domestic terminal device is about 25-30 ten thousand yuan, and the operating cost is 20-30 ten thousand yuan per year due to frequent electrode replacement.
(5) Artificial diamond boron-based electrode electrochemical sewage COD on-line monitor
At present, the on-line COD monitor for the electrochemical sewage of the artificial diamond boron-based electrode is researched and completed by adopting a method of doping boron into the artificial diamond (diamond) with strong oxidation resistance in European and American countries. Because synthetic diamond is an insulator, it must be doped with boron, which is resistant to strong oxidation, in large amounts to achieve its electrical conductivity. The electrode shows good stability under the OH free radical oxidation condition with the oxidation-reduction potential of 2.8V. The detector detects the time of 10-30 min according to the pollution degree of the sewage, and really has the advantages of simple equipment, high accuracy of detection data, long service life of an electrode, simple operation, extremely low failure rate, stable equipment operation, low maintenance cost and the like. However, such electrodes are very complicated to manufacture and expensive. Typically one small electrode plate is around $ 5-8 million. The price of a terminal device without a transmission part is generally 100-200 ten thousand yuan RMB. There is substantially no operating cost per year.
(6) And (4) conclusion:
at present, a large number of monitoring points in rivers, lakes, water areas, industrial enterprises, urban sewage drainage and the like in China need simple, quick and low-price COD online monitoring equipment, and the COD detection in a laboratory at present adopts a digestion and spectrophotometry or titration method, so that the operation is complex, the detection time is long, and a low-price and quick detection method is also needed to replace the traditional COD detection method. The market demand is more than 1 hundred million. If a stable electrode with low price and strong resistance to OH free radical oxidation can be prepared, a COD rapid detector (on-line) with low price, stable operation, simple maintenance, high detection accuracy and convenient power supply can be developed in the true sense, and an urgent need rapid on-line monitoring system or laboratory detection device and method are provided for the market.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to prepare a COD electrochemical rapid online monitoring instrument and a method by utilizing an electrochemical principle.
In order to achieve the purpose, the invention adopts the technical scheme that:
a rapid COD electrochemical online monitoring method is characterized by comprising the following steps:
(1) a COD electrochemical rapid on-line monitor is constructed, which comprises: the device comprises a sample pool, a working electrode, a reference electrode, a peristaltic pump, a magnetic stirrer, a solar cell, a solar panel, a current conversion COD chip, a wireless transmission transmitting end and a wireless transmission receiving end, wherein the working electrode and the reference electrode are embedded in the sample pool which is made of insulating materials and has the volume of 50ml to 100ml, and a magnetic stirrer with the length of less than 2cm is placed at the bottom of the sample pool and is placed on the magnetic stirrer to complete the stirring task in the sample determination process; the working electrode is connected with a solar cell for providing current, the voltage value is 2.5v, and the daily charging of the solar cell is completed by a solar panel; the sample inlet of the sample pool is connected with a peristaltic pump through a conduit to complete sample introduction work in the online monitoring process of the sample; the output end of the working electrode is connected with a current conversion COD chip to complete the calculation and measurement of current consumption in the measuring process of the working electrode, and the current required by the operation of the current conversion COD chip is provided by the solar cell; the COD data obtained by the current conversion COD chip is subjected to 4G wireless transmission through a wireless transmission transmitting terminal and is received to a user computer through a wireless transmission receiving terminal, and the wireless transmission transmitting terminal is provided with current required by operation by a solar cell; the working electrode is formed by adopting nano modified silicon dioxide as a carrier, adopting waste containing carbon in petroleum processing as a raw material, preparing graphene by adopting a thermal cracking method, modifying the graphene, and compounding the graphene with a silicon dioxide nano modified material carrier;
(2) pumping the sewage into an oxidation tank through a peristaltic pump, wherein the flow rate of the peristaltic pump is 20 mL/min;
(3) completely oxidizing organic matters in the sewage into H by OH hydroxyl radicals generated by the electrochemical working electrode2O and CO2The oxidation time is 30 min; the voltage value of OH hydroxyl radical generated by the electrode is 2.5V, and the current value is 15 muA; OH hydroxyl radical generated by the electrode completely oxidizes organic matters in the sewage into H2O and CO2In the range of 1-50000 Mg/L;
(4) the oxidation current value is converted into a COD value by a current conversion COD chip, and the oxidation current value is converted into a COD (chemical oxygen demand) value by the current value through the established corresponding relation between the current and the oxygen consumption in the complete oxidation process; the oxidation current and the chemical oxygen consumption are in a linear relation, and an electric signal and digital signal conversion mode can be established;
(5) the COD value is converted into a digital signal through a set circuit;
(6) the COD digital signal is transmitted out by a signal transmission system by adopting a 4G signal generator;
(7) the signal receiving and implementing control is carried out through a mobile phone or a network platform, and the remote control of the on-line monitor is realized.
Further, the peristaltic pump is a bi-directional pump.
Further, in the step (2), a magnetic switch arranged at the top of the oxidation tank gives a signal of water fullness to stop the peristaltic pump.
The solar cell and the solar panel are designed to ensure that the on-line monitor can work continuously for 192 hours by monitoring for 1 time per day for 30min under the condition of no illumination.
The invention utilizes the graphene composite silicon dioxide nano material as a working electrode, and adopts an electrochemical method to realize rapid on-line monitoring of COD, and the innovation points and the advancement are as follows:
compared with the existing on-line monitor, the COD electrochemical on-line monitor has the following characteristics:
(1) the strong oxidation resistant electrode is prepared by adopting silicon dioxide nano modified material composite thermal cracking modified graphene. The electrode adopts high-inertia material silicon dioxide as a carrier and carries out nano modification as the carrier, then uses waste containing carbon in petroleum processing as a raw material, adopts a thermal cracking method to prepare graphene, and carries out modification on the graphene, and then the graphene is compounded with the silicon dioxide nano modified material carrier to form the working electrode with excellent conductivity and strong oxidation resistance.
(2) The COD electrochemical on-line monitor has short detection time. Only 5-30min is needed, and the traditional detection time is 6 hours.
(3) And the maintenance is free. The annual maintenance cost of the traditional COD detector is 10-30 ten thousand yuan per year according to different equipment.
(4) The 220V commercial power is not needed. The used solar energy can meet the requirement of power supply and is suitable for realizing on-line monitoring under all conditions.
(5) The equipment price is low. The electrode has low cost of about 3000 yuan, so that the comprehensive cost of the COD electrochemical on-line monitor is 0.5 ten thousand yuan. The market selling price is 3 ten thousand yuan, and only 1/6 which is the lowest price of the similar equipment in the current market is provided.
(6) Signal conversion and transmission are easily accomplished. The COD electrochemical on-line monitor completely oxidizes organic matters in sewage through OH free radicals, directly converts an oxidation current value into a digital signal, transmits the digital signal through 2G, and is simple to convert and easy to realize.
(7) The detection accuracy and the zero degree are high. Because OH hydroxyl radical is adopted to completely oxidize organic matters into carbon dioxide CO at one time2And water H2And O, and calculating the COD value through oxidation current. Compared with the prior art, the method has the advantages that macromolecular organic matters in the sewage are degraded into micromolecules by sulfuric acid, then chemical oxidation is carried out by excessive potassium permanganate or potassium dichromate, titration is carried out by the potassium permanganate or the potassium dichromate or detection is carried out by a spectrophotometer, the COD value is calculated, the process is complex, and the error is large. The instrument has high accuracy and sensitivity, and is even 1 order of magnitude higher than that of the existing COD detectors, such as a COD ozone detector and a COD lead dioxide electrochemical detector.
(8) The detection range is wide, and the sample does not need to be diluted. The existing COD detector is diluted and then detected only at 1000mg/L and higher than 1000mg/L, and errors are easy to occur. The detection range of the electrochemical COD detector is 1-50000 mg/L.
Drawings
FIG. 1 is a schematic diagram of a circuit topology according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples for the purpose of facilitating understanding and practice of the invention by those of ordinary skill in the art, and it is to be understood that the present invention has been described in the illustrative embodiments and is not to be construed as limited thereto.
Example 1:
the COD electrochemical rapid online monitor is started through a password arranged on a mobile phone or a network platform, a control circuit of the detector starts a peristaltic pump, the peristaltic pump pumps a water sample to be monitored into an electrolytic cell from a monitoring point, the volume of the electrolytic cell is 10 cubic millimeters, when the pumped water sample reaches 10mL, a magnetic switch arranged on an electrolytic top tank gives a signal of water fullness, a control circuit disconnects a power supply of the peristaltic pump, the peristaltic pump stops working, the control circuit supplies power to an electrode, the electrode generates OH hydroxyl radicals to oxidize the water sample in the electrolytic cell, and the electrode power supply is disconnected after the oxidation time is 30min to stop oxidation. The oxidation current value is converted into a COD value by a current conversion COD chip, and then the COD value is converted into a digital signal by a control system, and the digital signal is transmitted out by 2G or 4G arranged by the control system. And receiving by using a mobile phone or a network platform. COD electrochemical rapid on-line monitoring was completely turned off.
Example 2:
after the first completion of the procedure of example 1, the COD electrochemical rapid on-line monitoring was in a fully closed state. At the second (or nth) monitoring: the COD electrochemical rapid online monitor is started through a password set by a mobile phone or a network platform, the detector control circuit starts a peristaltic pump to run reversely, a water sample obtained by previous monitoring in an electrolytic cell is pumped out, when the water sample in the electrolytic cell is completely pumped out, a magnetic switch arranged at the bottom of the electrolytic cell gives a water empty signal, the power supply of the peristaltic pump is stopped, the control circuit starts the peristaltic pump to run forwards after inverting the power supply of the peristaltic pump, the peristaltic pump pumps the monitored water sample into the electrolytic cell from a monitoring point to clean the electrolytic cell, cleaning water flows out from a bottom water outlet, a bottom water outlet electromagnetic valve is closed after 5min of cleaning, the power supply of the peristaltic pump is disconnected, and the water sample in the electrolytic cell is 10mL at the moment. The control circuit supplies power to the electrode, OH hydroxyl radicals generated by the electrode oxidize a water sample in the electrolytic bath, and the electrode power supply is cut off after the oxidation time is 30min to stop oxidation. The oxidation current value is converted into a COD value by a current conversion COD chip, and then the COD value is converted into a digital signal by a control system, and the digital signal is transmitted out by 2G or 4G arranged by the control system. And receiving by using a mobile phone or a network platform. COD electrochemical rapid on-line monitoring was completely turned off.
It should be understood that parts of the specification not set forth in detail are well within the prior art.
It should be understood that the above description of the preferred embodiments is given for clarity and not for any purpose of limitation, and that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. A rapid COD electrochemical online monitoring method is characterized by comprising the following steps: (1) a rapid electrochemical online monitor for Chemical Oxygen Demand (COD) is constructed, and comprises: the device comprises a sample pool, a working electrode, a reference electrode, a peristaltic pump, a magnetic stirrer, a solar cell, a solar panel, a current conversion COD chip, a wireless transmission transmitting end and a wireless transmission receiving end, wherein the working electrode and the reference electrode are embedded in the sample pool which is made of insulating materials and has the volume of 50ml to 100ml, and a magnetic stirrer with the length of less than 2cm is placed at the bottom of the sample pool and is placed on the magnetic stirrer to complete the stirring task in the sample determination process; the working electrode is connected with a solar cell for providing current, the voltage value is 2.5v, and the daily charging of the solar cell is completed by a solar panel; the sample inlet of the sample pool is connected with a peristaltic pump through a conduit to complete sample introduction work in the online monitoring process of the sample; the output end of the working electrode is connected with a current conversion COD chip to complete the calculation and measurement of current consumption in the measuring process of the working electrode, and the current required by the operation of the current conversion COD chip is provided by the solar cell; the COD data obtained by the current conversion COD chip is subjected to 4G wireless transmission through a wireless transmission transmitting terminal and is received to a user computer through a wireless transmission receiving terminal, and the wireless transmission transmitting terminal is provided with current required by operation by a solar cell; the working electrode adopts nano modified silicon dioxide as a carrier, and adopts the waste containing carbon in petroleum processing as a raw material, graphene is prepared and modified by adopting a thermal cracking method, and then the graphene and the silicon dioxide nano modified material carrier are mixedCarrying out compounding to form; (2) pumping the sewage into an oxidation tank through a peristaltic pump, wherein the flow rate of the peristaltic pump is 20 mL/min; (3) ٠ OH hydroxyl free radical generated by electrochemical working electrode can completely oxidize organic matter in sewage into H2O and CO2The working voltage of the working electrode is 2.4V, and the working current is 15 muA; the oxidation time is 5-30 min; power supplies 6V, 1.6A and 10W; ٠ OH hydroxyl free radicals generated by the electrode completely oxidize organic matters in the sewage into H2O and CO2In the range of 1-50000 mg/L; (4) the oxidation current value is converted into a COD value by a current conversion COD chip, and the oxidation current value is converted into the COD value by the current value through the established corresponding relation between the current and the oxygen consumption in the complete oxidation process; the oxidation current and the chemical oxygen consumption are in a linear relation, and an electric signal and digital signal conversion mode can be established; (5) converting the COD value into a digital signal through a set circuit; (6) the COD digital signal is transmitted out by a signal transmission system by adopting a 4G signal generator; (7) the signal receiving and implementing control is carried out through a mobile phone or a network platform, and the remote control of the on-line monitor is realized.
2. The COD electrochemical rapid on-line monitoring method according to claim 1, characterized in that: the peristaltic pump is a bidirectional pump.
3. The COD electrochemical rapid on-line monitoring method according to claim 1, characterized in that: in the step (2), a magnetic switch is arranged at the top of the oxidation tank to give a signal of water fullness so that the peristaltic pump stops working.
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| CN109580744A (en) * | 2018-11-19 | 2019-04-05 | 浙江理工大学 | A kind of improved silica nano pore film modified electrode and preparation method and application |
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