CN101671085A - Microwave electrochemical method for processing waste water and devices thereof - Google Patents
Microwave electrochemical method for processing waste water and devices thereof Download PDFInfo
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- CN101671085A CN101671085A CN200910197217A CN200910197217A CN101671085A CN 101671085 A CN101671085 A CN 101671085A CN 200910197217 A CN200910197217 A CN 200910197217A CN 200910197217 A CN200910197217 A CN 200910197217A CN 101671085 A CN101671085 A CN 101671085A
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Abstract
The invention belongs to the technical field of using an electrochemical method for processing organic-polluted waste water, and in particular relates to a microwave electrochemical method for processing waste water and devices. A boron-mixed diamond membrane electrode which has stable work under microwave action is used as an anode material of electrochemical degradation processing of the invention. Devices comprise a thermostatic bath, a peristaltic pump, a flow meter, a reactor, a boron-mixed diamond membrane electrode (anode), a titanium electrode (cathode) and a microwave oven. The invention uses microwaves for promoting the mass transferring process of organic pollutants, activates the boron-mixed diamond membrane electrode, improves electrode activity and accelerates the velocity ofelectrochemical oxidizing reaction. Compared with that of the pure electrochemical oxidization, in the same time, the removal rate of 2,4-dichlorphenoxyacetic acid of the invention is increased by 152 percents. The method has simple operation, and has good processing effect on organic waste water, and wide application prospect and developing potential.
Description
Technical field
The invention belongs to electrochemical method and handle the organic polluting water technical field, be specifically related to a kind of microwave electrochemical method and device thereof of handling waste water.
Background technology
Along with social industrialization constantly develops, the global environment problem is outstanding day by day, and the discharging of especially a large amount of industrial or agricultural sewage and sanitary wastewater makes water body be subjected to organic severe contamination; Because organic pollutant presents of a great variety, a series of characteristics such as the structure of matter is complicated, poisonous and harmful is strong, concentration height, therefore how to handle difficult for biological degradation organic pollutant in the water body in the last few years and be emphasis and difficult point in the environmental protection research.
High-level oxidation technology is the popular investigative technique that a class is considered to have good development prospect at present, mainly comprises catalytic wet oxidation, photochemical catalytic oxidation, catalytic oxidation, microwave, sonochemistry oxidation, ozone oxidation, supercritical water oxidation etc.These technology have degradation effect preferably to the organic pollutant of some kind, can reach and degrade fully or be transformed into the purpose of can biodegradable product taking subsequent disposal again, but often there are the following problems: when adopting single oxidation technology, degradation efficiency is lower, defective such as effect is undesirable during the waste water complicated component.Therefore be necessary to develop the coupling or the synergy of these high-level oxidation technologies.
It is a kind of novel method that addresses the above problem that electrochemical oxidation and microwave technology organic assembling are become the microwave activation electrochemical oxidation method, and it is not the simple superposition of electrochemical oxidation and microwave oxidation.Utilize this method degradable organic pollutant, except bringing into play the effect of these two kinds of technology self, the coupling that also has both to combine is so degradation effect is very desirable.
Electrode materials is the core of electrochemical oxidation technology, the electrode of selecting for use must have oxidation capacity strong, can be in these two characteristics of continuous firing under the microwave environment.Traditional carbon dioxide process carbon electrode and metal oxide electrode very easily damage under microwave action, and working life is limited; Metal electrode is then indifferent to the oxidative degradation of pollutent.And these electrode surfaces pollute easily, the ideal electrode material that therefore not to be electrochemical oxidation make up with microwave technology.
Summary of the invention
Existing single electrochemical oxidation technology exists degradation efficiency low, shortcomings such as the easy inactivation of electrode.The purpose of this invention is to provide a kind of microwave electrochemical method and the device thereof that can efficiently handle difficult for biological degradation organic waste water.
The microwave electrochemical method of the processing waste water that the present invention proposes, concrete steps are as follows:
Open peristaltic pump and make sewage enter reactor, control its flow by under meter from storage pool; Between anode and negative electrode, apply voltage then and carry out the continuous current degraded; Start microwave oven simultaneously and apply microwave reinforced electrochemical degradation,, regulate the power that immerses electrode real work area, interpole gap, current density and microwave in the water body according to the situation of pending water sample; When pending volume of water sample during at 200-300ml, the area of anode and negative electrode is 20-30cm
2, negative electrode and anode spacing are 1-3cm, current density is 5-60mA/cm
2
Among the present invention, the described continuous current degradation treatment time is 2-5h.
Among the present invention, when pending volume of water sample was 200-300ml, the power of microwave oven was 110-200W.
Among the present invention, described pending water sample comprises: dye wastewater with high concentration, have toxic PAE pollutant, oxidizing potential is high-leveled and difficult with electrochemical degradation pollutent etc., specifically comprises 2,4 dichlorophenoxyacetic acid, tropeolin-D, phthalic acid.
The microwave electrochemical device of the processing waste water that the present invention proposes, comprise reactor 1, anode 2, negative electrode 3, direct supply 4, peristaltic pump 5, under meter 6, thermostatic bath 7 and pipeline 8, wherein: in anode 2, the negative electrode 3 difference insertion reaction devices 1, anode 2 is connected by direct supply 4 with negative electrode 3, reactor 1 is placed in the microwave oven, and in the pipeline 8 one end insertion reaction devices 1, the other end passes peristaltic pump 5, under meter 6, thermostatic bath 7 successively, insertion reaction device 1 is realized the degraded of flow circuit sample introduction.
Among the present invention, described negative electrode 3 be in titanium electrode, platinum electrode or the stainless steel electrode any, described anode 2 is a boron-doped diamond film electrode.Wherein diamond film electrode is to adopt the chemical vapor deposition (CVD) method to deposit the diamond thin of high boron-doping on silicon base.(pertinent literature: Einaga Y, Sato R, Olivia H, et al.Modified diamond electrodes forelectrolysis and electroanalysis applications.Electrochimica Acta., 2004, Vol.49 (22-23): 3989～3995.).
Use this device that organic waste waters such as 2,4 dichlorophenoxyacetic acid, tropeolin-D, phthalic acid and phenylformic acid are handled discovery, very desirable with the degradation effect of the microwave electrochemical novel method of boron-doped diamond film electrode.Compare with independent electrochemical oxidation, the clearance in the identical time has improved 119%-180% respectively.
Compared with prior art, the present invention has following advantage:
1. be anode material owing to the present invention has adopted boron-doped diamond film electrode, kind electrode has that the electromotive force window is wide, background current is low, condition of surface is stable, favorable reproducibility and the not available advantage of other electrodes such as corrosion-resistant, can reach the degradation effect that ordinary electrode hardly matches by direct oxidation and the indirect oxidation that produces hydroxyl radical free radical.
2. the present invention has adopted the combined method of microwave technology and electrochemical oxidation.The heat effect of microwave can strengthen the solid-liquid mass transfer process between the electrode and solution in the electrochemical reaction process, gives full play to the strong characteristics of diamond film electrode oxidation capacity; The passivation that simultaneously can slow down electrode makes electrode surface keep more avtive spot, thereby can the activated electrode surface, makes electrode keep active preferably; Microwave also can promote the generation of hydroxyl radical free radical in addition, accelerates degradation rate.Therefore microwave reinforced electrochemical oxidation technology has the characteristics of oxidation efficiency height, applied range.
3. boron-doped diamond film electrode is highly stable, is difficult for being damaged by microwave, be suitable in the medium-term and long-term work of microwave environment, and be the desirable anode material of electrochemical oxidation and microwave combination novel method.
Description of drawings
The scanning electron microscope (SEM) that Fig. 1 boron-doped diamond film electrode of the present invention is handled the front and rear surfaces structure at microwave electrochemical characterizes correlated photo.Wherein: (A) be photo before handling, (B) for handling the back photo.
Fig. 2 microwave reinforced boron-doped diamond film electrode device for electrochemical water preparation synoptic diagram of the present invention.
Number in the figure: 1 is reactor, and 2 is anode, and 3 is negative electrode, and 4 is direct supply, and 5 is peristaltic pump, and 6 is under meter, and 7 is thermostatic bath, and 8 is pipeline.
Embodiment
Further specify the present invention below by example.
Embodiment 1: as shown in Figure 2, this device is made up of reactor 1, anode 2, negative electrode 3, direct supply 4, peristaltic pump 5, under meter 6, thermostatic bath 7 and pipeline 8.Anode 2 adopts boron-doped diamond film electrode, negative electrode 3 adopts the titanium electrode, wherein: anode 2, negative electrode 3 are placed in respectively in the reactor 1, anode 2 and negative electrode 3 are by direct supply 4 energisings, reactor 1 is placed in the microwave oven, and in the pipeline 1 one end insertion reaction devices 1, the other end passes peristaltic pump 5, under meter 6, thermostatic bath 7 successively, insertion reaction device 1 is realized the degraded of flow circuit sample introduction.
Embodiment 2, with 2,4 dichlorophenoxyacetic acid waste water as pending water sample
The COD of water sample
CrBe 115mg/L, pH is 6, and the concentration of supporting electrolyte sodium sulfate is 0.05mol/L, and volume is 100ml.Be 5.5cm as the boron-doped diamond film electrode of anode and negative electrode and the area of titanium electrode respectively
2, interelectrode distance is 1cm, current density is 20mA/cm
2Carry out the continuous current degraded, the frequency of microwave is 2450MHz, and power is 120W.Test as a comparison with independent electrochemical degradation and to carry out effect relatively.COD when electrochemical oxidation is degraded 3h separately
CrClearance only is 54%; Clearance when adopting microwave reinforced boron-doped diamond film electrode electrochemical oxidation technology 3h significantly is increased to 88%, and clearance has improved 63%.
(model of SEM is Quanta200FEG, and producer is FEI as seen from Figure 1.), be 20mA/cm with boron-doped diamond film electrode in current density
2, microwave frequency is 2450MHz, power is microwave electrochemical degraded 30 times under the condition of 120W, (Figure 1A is for before reacting, and Figure 1B is reacted electrode surface pattern), relatively the table of discovery surface state is without any variation, kind electrode stable performance under microwave action is described, long working life.
The TOC of water sample (total organic carbon) is 101.5mg/L, and pH is 5, and the concentration of supporting electrolyte sodium sulfate is 0.05mol/L, and volume is 100ml.Be 5.5cm as the boron-doped diamond film electrode of anode and negative electrode and the area of titanium electrode respectively
2, interpole gap is 1cm, current density is 20mA/cm
2Carry out the continuous current degraded, the frequency of microwave is 2450MHz, and power is 120W.Test as a comparison with independent electrochemical degradation and to carry out effect relatively.COD when electrochemical oxidation is degraded 3h separately
CrClearance only is 49%; Clearance when adopting microwave reinforced boron-doped diamond film electrode electrochemical oxidation technology 3h significantly is increased to 96%, and clearance has improved 96%.
In the large-scale treatment facility of practical application,, can guarantee degradation effect by regulating measures such as electrode area, current density and microwave frequency, power along with increasing of wastewater treatment capacity.In the 100ml-2L scope, regulate electrode area and current density for treatment capacity, make electric current increase, in 120-200W, regulate microwave power simultaneously, can guarantee the treatment effect of organic pollutant in the waste water with the treatment capacity equal proportion.
In addition, treatment capacity is amplified little to the influence of interpole gap, and interpole gap is regulated in 1-3cm and got final product.
Above-mentioned example proves: for the waste water from dyestuff of 2,4 dichlorophenoxyacetic acid and high density, the degradation effect of the microwave reinforced boron-doped diamond film electrode electrochemical water treating method of employing microwave and electrochemistry combination is all very desirable.This method is breakthrough and the development to existing green technology, can play the effect of protection water resources, meets the environmental consciousness that present country advocates, and has very wide application prospect and industry development concurrently and is worth.
Claims (6)
1, a kind of microwave electrochemical method of handling waste water is characterized in that concrete steps are as follows:
Open peristaltic pump and make sewage enter reactor, control its flow by under meter from storage pool; Between anode and negative electrode, apply voltage then and carry out the continuous current degraded; Start microwave oven simultaneously and apply microwave reinforced electrochemical degradation,, regulate the power that immerses electrode real work area, interpole gap, current density and microwave in the water body according to the situation of pending water sample; When pending volume of water sample during at 200-300ml, the area of anode and negative electrode is 20-30cm
2, negative electrode and anode spacing are 1-3cm, current density is 5-60mA/cm
2
2, the microwave electrochemical method of processing waste water according to claim 3 is characterized in that the described continuous current degradation treatment time is 2-5h.
3, the microwave electrochemical method of processing waste water according to claim 3 is characterized in that when pending volume of water sample is 200-300ml the power of microwave oven is 110-200W.
4, the microwave electrochemical method of processing waste water according to claim 3 is characterized in that described pending water sample comprises: dye wastewater with high concentration, have toxic PAE pollutant or oxidizing potential high-leveled and difficult with in the electrochemical degradation pollutent any.
5, a kind of microwave electrochemical device of handling waste water, comprise reactor (1), anode (2), negative electrode (3), direct supply (4), peristaltic pump (5), under meter (6), thermostatic bath (7) and pipeline (8), it is characterized in that anode (2), in negative electrode (3) the difference insertion reaction device (1), anode (2) is connected by direct supply (4) with negative electrode (3), reactor (1) is placed in the microwave oven, in pipeline (8) the one end insertion reaction devices (1), the other end passes peristaltic pump (5) successively, under meter (6), thermostatic bath (7), insertion reaction device (1) is realized the degraded of flow circuit sample introduction.
6, the microwave electrochemical device of processing waste water according to claim 1, it is characterized in that described negative electrode (3) in titanium electrode, platinum electrode or the stainless steel electrode any, described anode (2) is a boron-doped diamond film electrode.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614537A (en) * | 2012-04-19 | 2012-08-01 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN102765783A (en) * | 2011-05-03 | 2012-11-07 | 同济大学 | Microwave electro-Fenton method for processing organic wastewater and device thereof |
| CN103058329A (en) * | 2012-12-04 | 2013-04-24 | 江苏丰山集团有限公司 | Method for treating trifluralin pesticide wastewater by diamond film electrode |
| CN104129835A (en) * | 2014-07-16 | 2014-11-05 | 武汉大学 | Method for treating chlorination aromatic hydrocarbon by means of molten salt electrochemistry |
| CN105819549A (en) * | 2015-01-08 | 2016-08-03 | 中国石油化工股份有限公司 | Method for processing salt-containing waste water |
| CN105819541A (en) * | 2015-01-08 | 2016-08-03 | 中国石油化工股份有限公司 | Method for processing salt-containing waste water |
| EP3067324A1 (en) | 2015-03-11 | 2016-09-14 | Politechnika Gdanska | Method for the preparation of electrodes of boron-doped nanocrystalline diamond, an electrode prepared by this method and a use thereof |
| CN107879430A (en) * | 2017-11-27 | 2018-04-06 | 浙江沁园水处理科技有限公司 | A kind of rotary BDD application of electrode is in the method for removing the pollutant in water removal |
| CN111646539A (en) * | 2020-06-04 | 2020-09-11 | 浙江大学 | UVC-LED-DSA electrode coupled photoelectrochemistry oxidized ammonia nitrogen synergistic removal system |
| CN112250277A (en) * | 2020-12-23 | 2021-01-22 | 湖南碳谷装备制造有限公司 | Sludge dewatering method and system based on microwave electrolytic catalytic oxidation |
| CN112853406A (en) * | 2021-01-04 | 2021-05-28 | 广西大学 | Device and method for dissolving out waste printed circuit board metal through microwave enhanced electrochemistry |
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- 2009-10-15 CN CN200910197217A patent/CN101671085A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765783A (en) * | 2011-05-03 | 2012-11-07 | 同济大学 | Microwave electro-Fenton method for processing organic wastewater and device thereof |
| CN102614537B (en) * | 2012-04-19 | 2014-07-23 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN102614537A (en) * | 2012-04-19 | 2012-08-01 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN103058329A (en) * | 2012-12-04 | 2013-04-24 | 江苏丰山集团有限公司 | Method for treating trifluralin pesticide wastewater by diamond film electrode |
| CN104129835A (en) * | 2014-07-16 | 2014-11-05 | 武汉大学 | Method for treating chlorination aromatic hydrocarbon by means of molten salt electrochemistry |
| CN104129835B (en) * | 2014-07-16 | 2015-11-04 | 武汉大学 | A kind of method of molten salt electrochemistry process chlorination aromatic hydrocarbon |
| CN105819541B (en) * | 2015-01-08 | 2018-12-28 | 中国石油化工股份有限公司 | A kind of processing method of brine waste |
| CN105819549A (en) * | 2015-01-08 | 2016-08-03 | 中国石油化工股份有限公司 | Method for processing salt-containing waste water |
| CN105819541A (en) * | 2015-01-08 | 2016-08-03 | 中国石油化工股份有限公司 | Method for processing salt-containing waste water |
| EP3067324A1 (en) | 2015-03-11 | 2016-09-14 | Politechnika Gdanska | Method for the preparation of electrodes of boron-doped nanocrystalline diamond, an electrode prepared by this method and a use thereof |
| CN107879430A (en) * | 2017-11-27 | 2018-04-06 | 浙江沁园水处理科技有限公司 | A kind of rotary BDD application of electrode is in the method for removing the pollutant in water removal |
| CN111646539A (en) * | 2020-06-04 | 2020-09-11 | 浙江大学 | UVC-LED-DSA electrode coupled photoelectrochemistry oxidized ammonia nitrogen synergistic removal system |
| CN112250277A (en) * | 2020-12-23 | 2021-01-22 | 湖南碳谷装备制造有限公司 | Sludge dewatering method and system based on microwave electrolytic catalytic oxidation |
| CN112250277B (en) * | 2020-12-23 | 2021-03-23 | 湖南碳谷装备制造有限公司 | Sludge dewatering method and system based on microwave electrolytic catalytic oxidation |
| CN112853406A (en) * | 2021-01-04 | 2021-05-28 | 广西大学 | Device and method for dissolving out waste printed circuit board metal through microwave enhanced electrochemistry |
| CN112853406B (en) * | 2021-01-04 | 2023-06-09 | 广西大学 | Device and method for electrochemically leaching waste printed circuit board metal by microwave enhancement |
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Open date: 20100317 |