CN101164906A - Electrooxidation degradation method for dyestuff waste water by using active carbon fibre - Google Patents
Electrooxidation degradation method for dyestuff waste water by using active carbon fibre Download PDFInfo
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- CN101164906A CN101164906A CNA2007100306318A CN200710030631A CN101164906A CN 101164906 A CN101164906 A CN 101164906A CN A2007100306318 A CNA2007100306318 A CN A2007100306318A CN 200710030631 A CN200710030631 A CN 200710030631A CN 101164906 A CN101164906 A CN 101164906A
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Abstract
This invention relates to a method for electrooxidation degradation of dye waste-water by utilizing activated carbon fiber, particularly by using the activated carbon felt as anode material. It comprises steps of: (1), feeding wastewater into the electrolytic cell, (2), the cell is equipped anode activated carbon fiber and stainless steel cathode, (3), power-in the DC power and starting the agitator, proceeding electrolysis with current density of 15-35mA/cm2, voltage of 5-12V. The absorption makes the enrichment of organic dye on the surface of the activated carbon, and oxidation and degradation of the absorbed dye occurs by electrocatalysis oxidation, after the treatment, the decolourisation is upto 99%, COD removal rate is 87.9%.
Description
Technical field
The invention belongs to application field of water treatment, be specifically related to a kind of method of utilizing activated carbon fiber to carry out the Electrooxidation degradation waste water from dyestuff as anode material.
Background technology
Dyeing waste water has characteristics such as the water yield is big, concentration is high, complicated component, colourity height, is one of unmanageable trade effluent.The traditional method that is used for dye wastewater treatment has chemical coagulation process, biological process and active carbon adsorption etc.Along with people improve constantly environmental quality requirement, traditional treatment process is difficult to satisfy wastewater discharge standard.In recent years, many high-level oxidation technologies are suggested, as O
3The coupling technique of oxidation style, wet oxidation technology, supercritical water oxidation method, photocatalytic oxidation, electrochemical oxidation process and the whole bag of tricks etc.Wherein electrochemical oxidation process is to use electronics as reactant, only needs to add need add chemical agent on a small quantity or not, can move under normal temperature, normal pressure, and the energy utilization efficiency height is a kind of cleaning, safe and effective sewage water treatment method.
Anode material is one of emphasis of electrochemical oxidation process processing waste water.At present, the anode of using morely in electrochemical oxidation process has Graphite Electrodes, the ferroelectric utmost point, PbO
2Electrode, noble metal electrode etc.Jia Jin equality people was that anode has carried out the electrochemistry decolorization experiment to dye wastewater with the compound iron of activated carbon fiber once.But owing to being anode with the compound iron of activated carbon fiber, activated carbon fiber is a negative electrode, and whole process also is attended by electric flocculation process except electrochemical redox, and the mud generation is big, has brought difficulty to aftertreatment.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing activated carbon fiber to carry out electrooxidation disaggregating treatment waste water from dyestuff.This method had both been utilized the electroconductibility and the catalytic performance of activated carbon fiber, had made full use of the absorption property of activated carbon fiber excellence again, had improved the degradation efficiency of dyestuff greatly
The method of utilizing activated carbon fiber Electrooxidation degradation waste water from dyestuff of the present invention is characterized in that with the activated carbon fiber felt as the anode material in the electrooxidation method.
In the invention described above method, the activated carbon fiber material that constitutes described activated carbon fiber felt can be viscose-based active carbon fiber, asphalt based active carbon fiber or polyacrylonitrile radical active carbon fiber, or is the composite active carbon fibre of matrix with the glass fibre.
The specific surface area of described activated carbon fiber material is generally at 300～2000m
2/ g, pore volume are generally at 0.1～1.5mL/g.Described activated carbon fiber material also contains a certain proportion of (aperture is greater than 2nm's) mesopore usually.
Among the present invention is the composite active carbon fibre of matrix with the glass fibre, can be the mixture of painting polypropylene nitrile, polyvinyl alcohol and zinc chloride etc. on glass fibre, again through carbonization, activation and make.
The inventive method generally comprises following concrete steps:
(1) waste water from dyestuff is imported in the electrolyzer continuously or off and on;
(2) in electrolyzer, be equipped with activated carbon fiber anode and stainless steel substrates negative electrode;
(3) open direct supply and agitator, connect negative electrode and anode, carry out electrolysis; Electrolytic current density is generally 15～35mA/cm
2, bath voltage is generally 5～12V.
Described activated carbon fiber anode be by the activated carbon fiber felt, fixedly the activated carbon fiber felt electrode holder and the conduction usefulness plain conductor constituted.
In the aforesaid method step (1), regulating waste water from dyestuff pH value usually is 3～11, is preferably neutrality or meta-alkalescence (pH=7～11).
When importing waste water from dyestuff in the electrolyzer off and in the aforesaid method step (1), the treatment time, generally in 1～60min scope, wastewater volume was generally 100～500mL: 1g with the ratio of activated carbon fiber weight.
When importing waste water from dyestuff in the electrolyzer continuously in the aforesaid method step (1), wastewater flow is generally 2～50mL/min: 0.1～1g with the ratio of activated carbon fiber weight.
Direct supply described in the aforesaid method step (3), its power supply mode can adopt continuous current mode or constant voltage mode.
The inventive method directly is anode with the activated carbon fiber, come dye wastewater treatment using with electrochemical oxidation process, made full use of the absorption property of activated carbon fiber excellence,, can improve dyestuff electrooxidation decomposing efficiency greatly dye adsorption being enriched on the activated carbon fiber in the waste water.This treatment process can be removed by the dyestuff decomposition that direct and indirect oxidation effect will be adsorbed on the activated carbon fiber, makes activated carbon fiber be able to real-time regeneration, uses back regenerated trouble thereby saved.This treatment process can be utilized the anodic polarized action, makes activated carbon fiber surface positively charged, move to impel electronegative dye molecule anode, thereby by oxygenolysis removal fast.This treatment process does not need to add a lot of chemical reagent, does not need the activated carbon fiber after using is regenerated yet, and is simple to operate, non-secondary pollution; Can carry out the energy efficiency height at normal temperatures and pressures; Equipment is simple, and floor space is little, convenient management.
Experiment shows that the inventive method has removal effect preferably to alizarin red S, and in the static state experiment of handling 700mg/L alizarin red S dye wastewater, rate and COD clearance are discolored in electrolysis after 60 minutes respectively can be up to 99.1% and 87.9%; In the dynamic experiment of handling 200mg/L alizarin red S dye wastewater (referring to Fig. 1), the rate of the discoloring maximum value of waste water from dyestuff is 70% and constant substantially with the increase of effluent liquid cumulative volume, the rate of discoloring height when ratio is pure sorbent material with activated carbon fiber, and long service life.
Description of drawings
Fig. 1 is respectively the rate of discoloring of anode and pure sorbent material waste water from dyestuff when handling the alizarin red S waste water from dyestuff continuously with the change curve that flows out cumulative volume with activated carbon fiber.It show with the activated carbon fiber be anode during with the electrochemical oxidation process dye wastewater treatment using in the absorption of activated carbon fiber with under the synergy of electrooxidation alizarin red S is had removal effect preferably in real time, and in the successive treating processes, dye molecule is degraded in real time, electrode is able to real-time regeneration, so the removal efficient of dyestuff can remain on high level for a long time.And when activated carbon fiber during as sorbent material, after its loading capacity reaches capacity, will constantly descend in time to the removal efficient of waste water from dyestuff.
Embodiment
Below the invention will be further described by specific embodiment.
1. treatment times of embodiment are to the influence of dyestuff removal effect
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, is that 0.251g, specific surface area are 1256m with the quality
2The viscose-based active carbon fiber felt of/g is an anode, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, timing sampling is measured the rate of discoloring and the COD clearance of different treatment waste water from dyestuff during the time in the experimentation.The rate of discoloring in the time of 20,30,40,60 minutes, and the COD clearance 60 minutes the time is as shown in table 1.The result shows that under the processing of the inventive method, the rate of discoloring of waste water from dyestuff reached waste water from dyestuff after 90.2%, 60 minute rapidly in 30 minutes the rate of discoloring and COD clearance reach 98.2% and 76.5% respectively.
In addition, also done contrast among the embodiment 1 with the inventive method under the condition and the pure adsorption treatment method of no power.With same a kind of activated carbon fiber felt with equal in quality and area is pure sorbent material, handles 60 minutes the rate of discoloring of waste water from dyestuff and COD clearance only 84.6% and 63% under cold situation.
Table 1 different treatment time electrochemical oxidation process and pure absorption method are to the contrast of dyestuff removal effect
| The rate of discoloring (%) | COD clearance (%) | ||||
| 20min | 30min | 40min | 60min | 60min | |
| Electrolysis (energising) | 76.9 | 90.2 | 95.1 | 98.2 | 76.5 |
| Pure absorption (no power) | 46.9 | 59.8 | 70.7 | 84.6 | 63 |
When embodiment 2. is anode with the different activities charcoal fibrefelt with different specific surface areas to the treatment effect of waste water from dyestuff
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, is respectively that the various activated carbon fiber felt of 0.251g is an anode with the quality, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, the rate of discoloring and the COD clearance handled after 60 minutes are as shown in table 2.
In addition, also be charcoal fiber anodic contrast experiment among the embodiment 2, be anode promptly, under identical experiment condition, waste water from dyestuff handled that the rate of discoloring of waste water from dyestuff and COD clearance only are 48.3% and 24.6% after 60 minutes with charcoal fibrefelt with equal in quality.
Table 2 different activities charcoal fibrefelt anode is to the treatment effect of waste water from dyestuff
| Viscose-based active carbon fiber | The asphalt based active carbon fiber | Polyacrylonitrile radical active carbon fiber | The fiber reinforced glass matrix composite active carbon fibre | The charcoal fiber | |
| BET specific surface area (m 2/g) | 1256 | 1980 | 756 | 350 | 4.7 |
| Total pore volume (cm 3/g) | 0.61 | 1.51 | 0.43 | 0.11 | 0.006 |
| The rate of discoloring (%) | 98.2 | 99.1 | 94.3 | 70.6 | 48.3 |
| COD clearance (%) | 76.5 | 87.9 | 73.4 | 56.7 | 24.6 |
The initial pH value of embodiment 3. waste water from dyestuff is to the influence of treatment effect
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 3～11, is that 0.251g, specific surface area are 756m with the quality
2The polyacrylonitrile radical active carbon fiber felt of/g is an anode, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, the COD clearance in the time of 60 minutes is as shown in table 3.The result shows that under neutral (pH=7) condition, the dyestuff COD removal can reach 73.1% after 60 minutes.
Table 3 initial pH value is to the influence of waste water from dyestuff COD clearance
| The pH value | 3 | 5 | 7 | 9 | 11 |
| COD clearance (%) | 67.9 | 69.7 | 73.1 | 73.9 | 73.9 |
When embodiment 4. is anode with the viscose-based active carbon fiber felt of different mass to the treatment effect of waste water from dyestuff
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, with the stainless steel substrates is negative electrode, the viscose-based active carbon fiber felt of getting different mass is an anode, the mass ratio that makes wastewater volume and anode material is between 100～500mL: between the 1g, under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, the rate of discoloring and COD clearance in the time of 60 minutes are as shown in table 4.
The viscose-based active carbon fiber felt anode of table 4 different mass is to the treatment effect of waste water from dyestuff
| Activated carbon fiber amount (g) | 0.1026 | 0.2373 | 0.3612 | 0.4857 |
| Wastewater volume and activated carbon fiber weight ratio (mL/g) | 487 | 211 | 138 | 103 |
| The rate of discoloring (%) | 82.6 | 95.7 | 99.2 | 100 |
| COD clearance (%) | 63.4 | 74.5 | 80.5 | 90.3 |
Embodiment 5. current densities are to the influence of dye wastewater treatment effect
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, is that 0.251g, specific surface area are 1256m with the quality
2The viscose-based active carbon fiber felt of/g is an anode, and stainless steel substrates is a negative electrode, under the stirring of agitator, is 15,25 and 35mA/cm in constant current density
2Condition under carry out electrolysis, the rate of discoloring and COD clearance in the time of 60 minutes are as shown in table 5.
Table 5 current density is to the influence of dye wastewater treatment effect
| Current density (mA/cm 2) | 15 | 25 | 35 |
| The rate of discoloring (%) | 90.4 | 98.0 | 98.6 |
| COD clearance (%) | 67.5 | 75.8 | 77.2 |
Embodiment 6. voltages are to the influence of dye wastewater treatment effect
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, is that 0.251g, specific surface area are 1980m with the quality
2The asphalt based active carbon fibrefelt of/g is an anode, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant bath voltage is 5V, and 8V or 12V carry out electrolysis, and the rate of discoloring and the COD clearance that record waste water from dyestuff after 60 minutes are as shown in table 6.
Table 6 voltage is to the influence of dye wastewater treatment effect
| Voltage (V) | 5 | 8 | 12 |
| The rate of discoloring (%) | 95.7 | 98.3 | 99.1 |
| COD clearance (%) | 71.2 | 78.5 | 87.9 |
Embodiment 7. activated carbon fiber felt anodic are reused the influence of number of times to the rate of discoloring
The alizarin red S dye wastewater solution of getting 50mL concentration and be 700mg/L (wherein contains Na
2SO
4Concentration 0.1mol/L) in electrolyzer, regulator solution pH is 7, is that 0.251g, specific surface area are 1256m with the quality
2The viscose-based active carbon fiber felt of/g is an anode, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, finish the rate of discoloring of experiment sampling and measuring waste water from dyestuff after 60 minutes, then remaining waste water solution in the electrolyzer is all poured out, again changing 50mL concentration is the original alizarin red S dye wastewater solution of 700mg/L, carrying out the second time handles, and the rate of discoloring of mensuration electrolysis waste water from dyestuff after 60 minutes, so circulation, same activated carbon fiber felt anode is repeated to use repeatedly to detect its work-ing life.
No power, but all the other conditions are same as described above, compared the work-ing life of activated carbon fiber felt under the pure absorption situation.
Table 7 data show that electrooxidation method dye wastewater treatment using, Activated Carbon Fiber Electrodes repeatedly use the back all can keep good performance; And simple adsorption treatment of dye waste water, the absorption property of activated carbon fiber felt sharply descends with the increase of access times, must regenerate.
The repeated use number of times of table 7 activated carbon fiber felt is to the influence of the rate of discoloring
| The rate of discoloring (%) | |||||
| For the first time | For the second time | For the third time | The 4th time | The 5th time | |
| Energising | 98.3 | 93.8 | 92.3 | 92.6 | 92.2 |
| No power | 85 | 53.3 | 41.8 | ||
The reckoning of embodiment 8. electrolytic efficiencies
In order to estimate the degradation efficiency of electrochemical oxidation to alizarin red S, we are to being adsorbed on the alizarin red S N on the activated carbon fiber after testing among the embodiment 1, dinethylformamide extracts, measure the absorbancy of extraction liquid at the 518nm place then, the electrolytic efficiency of the alizarin red S that is adsorbed in the time of can calculating energising thus is 96.4%; Nearly all alizarin red S that is adsorbed can be removed by the electrooxidation decomposition.
Electrolysis and pure absorption are to the contrast of dye wastewater treatment effect in the embodiment 9. continuous treating processess
Get the dye wastewater solution that 110mL contains the 200mg/L alizarin red S and (wherein contain Na
2SO
40.1mol/L, do not regulate the pH value, the pH value about 6.5 of original solution) and in the electrolyzer that flows, be that 0.251g, specific surface area are 1256m with the quality
2The viscose-based active carbon fiber felt of/g is an anode, and stainless steel substrates is a negative electrode, and under the stirring of agitator, constant current density is 25mA/cm
2Carry out electrolysis, continuously import original analog waste water from dyestuff solution with the speed of 2.35mL/min to electrolyzer by the constant current peristaltic pump during this time, solution after the processing is from outflow suitable for reading, and every 10min collects an effluent liquid, and the suitably rate of discoloring of dilution back mensuration effluent liquid takes a morsel.The result shows that the rate of discoloring of waste water from dyestuff increases earlier gradually with the increase of efflux volume, and to reach after 70% the increase with the effluent liquid cumulative volume constant substantially when the rate of discoloring.
In addition, also done contrast among the embodiment 9 with the inventive method under the condition and the pure adsorption treatment method of no power.With same a kind of activated carbon fiber felt with equal in quality and area is pure sorbent material, handles the dye wastewater solution that contains the 200mg/L alizarin red S under cold situation continuously.The result shows that when the effluent liquid cumulative volume was in 100mL, the rate of discoloring of waste water from dyestuff increased gradually with the increase of efflux volume, and thereafter, with the increase of effluent liquid cumulative volume, the rate of discoloring of effluent liquid constantly reduces, and its maximum rate of discoloring only is 57.3%.The mass ratio of embodiment 10. wastewater flows and activated carbon fiber is to the influence of dye wastewater treatment effect
In 2～50mL/min scope, adjust the inflow velocity of waste water from dyestuff, change viscose-based active carbon fiber felt anodic quality simultaneously, the flow that makes waste water from dyestuff and the mass ratio of activated carbon fiber between 4～50, all the other conditions and operating with embodiment 9.The result shows, although the ratio difference, the rate of discoloring all increases constant substantially then earlier with the increase of flowing out cumulative volume, and their the maximum rate value of discoloring descends (as table 8) with the ratio increase of wastewater flow and activated carbon fiber amount.
The mass ratio of table 8 wastewater flow and activated carbon fiber is to the influence of dye wastewater treatment effect
| The quality of activated carbon fiber felt (g) | 0.1032 | 0.2514 | 0.5036 | 0.7558 | 0.9897 |
| Wastewater flow (mL/min) | 2.35 | 2.35 | 2.35 | 25.85 | 49.35 |
| Ratio (the mL/min: g) of wastewater flow and activated carbon fiber amount | 22.8 | 9.3 | 4.7 | 34.2 | 50 |
| The rate of discoloring (%) | 67.7 | 70.8 | 89.6 | 65.3 | 63.7 |
Claims (10)
1. a method of utilizing activated carbon fiber Electrooxidation degradation waste water from dyestuff is characterized in that with the activated carbon fiber felt as the anode material in the electrooxidation method.
2. the method for claim 1, the activated carbon fiber material that it is characterized in that constituting described activated carbon fiber felt are viscose-based active carbon fiber, asphalt based active carbon fiber, polyacrylonitrile radical active carbon fiber or are the composite active carbon fibre of matrix with the glass fibre.
3. method as claimed in claim 2, the specific surface area that it is characterized in that described activated carbon fiber material is at 300～2000m
2/ g, pore volume is at 0.1～1.5mL/g.
4. as the described method of claim 1,2 or 3, it is characterized in that this method comprises the following steps: that (1) imports waste water from dyestuff in the electrolyzer continuously or off and on; (2) be equipped with activated carbon fiber anode and stainless steel substrates negative electrode in the electrolyzer; (3) open direct supply and agitator, connect negative electrode and anode, carry out electrolysis; Electrolytic current density is 15～35mA/cm
2, bath voltage is 5～12V.
5. method as claimed in claim 4, it is characterized in that described activated carbon fiber anode be by the activated carbon fiber felt, fixedly the activated carbon fiber felt electrode holder and the conduction usefulness plain conductor constituted.
6. method as claimed in claim 4 is characterized in that regulating waste water from dyestuff pH value in step (1) is 3～11.
7. method as claimed in claim 6 is characterized in that regulating waste water from dyestuff pH value in step (1) is 7～11.
8. method as claimed in claim 4, when it is characterized in that importing waste water from dyestuff in the electrolyzer off and in the step (1), the treatment time, wastewater volume was 100～500mL: 1g with the ratio of activated carbon fiber weight in 1～60min scope.
9. method as claimed in claim 4, when it is characterized in that importing waste water from dyestuff in the electrolyzer continuously in the step (1), wastewater flow is generally 2～50mL/min: 0.1～1g with the ratio of activated carbon fiber weight.
10. method as claimed in claim 4 is characterized in that the direct supply described in the step (3), and its power supply mode adopts continuous current mode or constant voltage mode.
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| CN101913677A (en) * | 2010-08-27 | 2010-12-15 | 上海交通大学 | Organic wastewater circular treatment method based on continuous interface adsorbing medium |
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| CN108017118A (en) * | 2017-06-15 | 2018-05-11 | 武汉科技大学 | A kind of method based on electrochemical modification method processing cationic dyes waste water |
| CN108373725A (en) * | 2018-03-19 | 2018-08-07 | 东莞市钟亿阻燃粘胶实业有限公司 | Anti- distillation bottoming slurry of one kind and its preparation method and application |
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