CN103435134B - A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton improves the method for blue charcoal wastewater biodegradability - Google Patents

A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton improves the method for blue charcoal wastewater biodegradability Download PDF

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CN103435134B
CN103435134B CN201310376171.XA CN201310376171A CN103435134B CN 103435134 B CN103435134 B CN 103435134B CN 201310376171 A CN201310376171 A CN 201310376171A CN 103435134 B CN103435134 B CN 103435134B
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waste water
fenton
blue charcoal
negative electrode
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CN103435134A (en
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申丽华
郭晓滨
魏海霞
于春侠
郑晓峰
闫蓓
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Xian University of Science and Technology
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Abstract

The invention discloses a kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, is intended to utilize CNTs/Fe 3o 4part stripping Fe ion and CNTs/Fe in weak acidic medium 3o 4adsorptivity and electroconductibility, the organic pollutant in absorption waste water, is then adsorbed near cathode electrode by magnetic field, can be reacted, repeatable operation like this under the condition of aeration by the generation Fenton of negative electrode.Meanwhile, in conjunction with the titanium base SnO that Sb mixes 2catalyzed oxidation ability.Utilize the H that negative electrode produces 2o 2, carry out the anodised method of organism, for the process of coking chemical waste water simultaneously.In this method, do not use barrier film between negative electrode and anode, organism be degraded under the effect of oxygen radical low carbon number continue after intermediate, this being swift in response is carried out, until all molecular fragments are oxidized to CO 2and H 2o, thus improve current efficiency, save power consumption.

Description

A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton improves the method for blue charcoal wastewater biodegradability
Technical field
The invention belongs to technical field of chemistry, relate to a kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water.
Background technology
Blue charcoal waste water is the trade effluent of typical high density, difficult for biological degradation, and its water quality is similar to coking chemical waste water.At present, the treatment process that coking, Lan Tan factory extensively adopt is: first carry out pre-treatment according to a conventional method, from high-concentration sewage, recycle pollutent; Then biological process is utilized to carry out secondary treatment.But adopt this technology, water outlet is difficult to the emission standard reaching national regulation, therefore, be difficult to meet the environmental requirement day by day improved.For coking chemical waste water, researcher proposes multiple method, as biological reinforcing technology, burning method, catalytic wet air oxidation and supercritical water oxidation method etc., but actual can economical, effectively Treatment of Wastewater in Coking is very few.Wherein, catalytic wet air oxidation comparatively can economically viable Treatment of Wastewater in Coking.Research for blue charcoal waste water rarely has report, and exceeds about 10 times than coking chemical waste water due to blue charcoal waste strength, belongs to the waste water of typical high density, difficult for biological degradation.Therefore, propose to adopt the blue charcoal waste water of three-dimensional electricity-Fenton oxidation method process efficiently processing high density, difficult for biological degradation herein, improve its biodegradability.
Electricity-Fenton oxidation method effectively can process poisonous and harmful waste water, and limiting one of deciding factor of its application is that current efficiency is not high, although the appearance of carbon nanotube brings hope to cathode diffusion electrode.Efficiently, stable is the key that pollutent is effectively degraded by polluting mass transfer at electrode surface, the conception of three-diemsnional electrode just in time solves this problem, three-dimensional electricity-Fenton is a kind of novel electrochemical water treatment technology, the shortcoming that it is poor for two-dimensional flat plate Electro-Fenton process mass transfer effect, current efficiency is low, energy consumption is high, granule electrode is incorporated in Fenton system, increase the surface-area of working electrode, improve mass transfer effect, improve current efficiency, avoid the secondary pollution that homogeneous phase Fenton is formed.
Summary of the invention
The object of the invention is to overcome the defect existed in prior art, provide a kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, is intended to utilize CNTs/Fe 3o 4part stripping Fe ion and CNTs/Fe in weak acidic medium 3o 4adsorptivity and electroconductibility, the organic pollutant in absorption waste water, is then adsorbed near cathode electrode by magnetic field, can be reacted, repeatable operation like this under the condition of aeration by the generation Fenton of negative electrode.Meanwhile, in conjunction with the titanium base SnO that Sb mixes 2catalyzed oxidation ability, directly produce OH, carry out the anodised method of organism, for the process of coking chemical waste water.In this method, do not use barrier film between negative electrode and anode, organism be degraded under the effect of oxygen radical low carbon number continue after intermediate, this being swift in response is carried out, until all molecular fragments are oxidized to CO 2and H 2o, thus improve current efficiency, save power consumption.That the present invention is used for the blue charcoal waste water of three-dimensional electricity-Fenton oxidation process and Primary Study processing parameter is on the impact of three-dimensional electricity-Fenton oxidation, and an economically viable approach is sought in the process for blue charcoal waste water.Its concrete technical scheme is:
A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, comprises the following steps:
(1) get the blue charcoal waste water of 200mL, passing into air, take graphite as negative electrode, Ti/SnO 2for anode, add 5V potential electrolysis, occur a large amount of black foam, produce until no longer include bubble, need 1h;
(2) the blue charcoal wastewater pH processed through (1) is 7, is 3, adds the CNTs/Fe of 1g/100mL with sulphur acid for adjusting pH 3o 4for three-diemsnional electrode particle, take graphite as negative electrode, Ti/SnO 2for anode, pass into air, electrolysis under 12V voltage, every 30min measures a BOD 5and COD crvalue;
(3) BOD is drawn 5/ COD crvalue scheme over time.
Further preferably, described CNTs/Fe 3o 4the synthesis of matrix material comprises the following steps:
A1 Purification of Carbon Nanotubes first carries out purifying pre-treatment with 65wt% nitric acid to carbon nanotube, by pretreated carbon nanotube ultrapure water cleaning to neutral, is placed in 105oC vacuum drying oven and dries, obtain the carbon nanotube after purifying;
5.9g step a1 purifying carbon nano-tube is joined 4.0gFeCl by the preparation of a2 material 36H 2o and FeCl 24H 2o, the 200mL aqueous solution is made into by the mixing of 1.75:1 amount of substance, ultrasonic 10min under nitrogen protection, is then placed in the water bath with thermostatic control of 65 DEG C, stirs and dropwise drips ammoniacal liquor simultaneously, until stop during pH=9 ~ 10 adding ammoniacal liquor, temperature is adjusted to 70 DEG C and continues stirring reaction 30min, stopped reaction, uses magnet quiescent setting, with deionized water and dehydrated alcohol repetitive scrubbing to neutral solution, be placed in the dry 6h of 85 DEG C of vacuum drying ovens;
A3 nanometer Fe 3o 4preparation nanometer Fe 3o 4preparation method and step a2 nanometer CNTs/Fe 3o 4the preparation method of material is all identical except not adding CNTs.
Further preferably, described Ti/SnO 2the preparation of electrode comprises the following steps:
B1 fine sandpaper beats the zone of oxidation on surface;
B2 alkali cleaning, uses alkali cleaning 30min in ultrasonic instrument, is cleaned by the titanium plate after alkali cleaning in ultrasonic instrument with distilled water;
The passivation of b3 acid etching technique strong acid, the corrodibility of the oxalic acid solution of 10wt% is very strong, titanium plate after oil removing is etched 2h in the oxalic acid of 10%, clean with distilled water in ultrasonic apparatus again, be kept in dehydrated alcohol for subsequent use after drying up, titanium-based surface after acid etching forms rough grey pitted skin, without metalluster;
The preparation of b4 electroplate liquid takes 4g SnCl 45H 2o is dissolved in the dehydrated alcohol of 50mL, takes the SbCl of 0.26g simultaneously 3be dissolved in the dehydrated alcohol of 20mL, two kinds of mixtures are put into closed container respectively;
B5 is using the titanium plate processed as negative electrode, and graphite is anode, 0.25mol/L SnCl 4ethanolic soln is the direct current of electrolytic solution, 3-4V, and plating 10min, then leaves standstill 5min, repeatedly electroplating process 5-6 time;
The titanium plate electroplated is dried by b6 in an oven, then puts into retort furnace 550 DEG C of roastings, 2h.
Compared with prior art, beneficial effect of the present invention is:
(1) take Fenton reagent as purport, select iron to be main active ingredient; CNTs/Fe has been prepared by coprecipitation method 3o 4composite catalyst, carries out specific surface area analysis by BET, CNTs/Fe 3o 4matrix material compares Fe 3o 4catalyzer has higher specific surface area; XRD and the display of tem analysis result, CNTs/Fe 3o 4fe in matrix material 3o 4have and be well scattered on the outside surface of CNTs, improve the activity of catalyzer simultaneously.
(2) CNTs/Fe is used 3o 4matrix material Modified graphite electrode, for simulation phenolic waste water of degrading, the cyclic voltammetry curve of modified electrode shows nanometer CNTs/Fe 3o 4modified electrode Degradation of Phenol has katalysis, to O 2reduction generates H 2o 2there is promoter action.Stripping Fe n+with H 2o 2reaction generates OH, and methylenum coeruleum have detected the existence of OH.Optimize the impact of pH and voltage Degradation of Phenol, result is 5 at pH, and voltage is 5V, and after electrolysis 120min, the clearance of phenol can reach 92%.
(3) in order to improve current efficiency, design with CNTs/Fe 3o 4matrix material is the electricity-Fenton system of three-diemsnional electrode particle, and with the Toxic pyridine in blue charcoal waste water for degraded object, investigates the oxidation capacity of this system.Laboratory top condition is: voltage 12V, pH=3-5, CNTs/Fe 3o 4matrix material addition 1.5g/mL.
(4) composition of blue charcoal quenching waste water is analyzed, its COD crcan up to 28000mg/L, BOD 5be only 656mg/L, pH=9, electrode process has a large amount of bubble formation, not easily Electrocatalytic Oxidation process, after electrooxidation stripping, CODcr and BOD 5be down to 3260mg/L, 298mg/L respectively.BOD 5/ CODcr is elevated to 10.5% from 2.3%, and biodegradability increases.
(5) by the blue charcoal waste water after electric stripping, with the process of three-dimensional electricity-Fenton system, after the 4h that degrades under optimum experimental condition, CODcr and BOD 5be down to 286mg/L, 248mg/L respectively, BOD 5/ CODcr is close to 86%.Again measure CODcr to the waste water through culture method process in five days, its value is only 30mg/L, reaches sewage discharge national standard completely.
Accompanying drawing explanation
Fig. 1 is the change of wastewater biodegradability with electrolysis time;
Fig. 2 the present invention is based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the process flow sheet of method of blue charcoal waste water;
Fig. 3 the present invention is based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the experimental installation structure iron of method of blue charcoal waste water.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in more detail.
Analyze its feasibility with reference to Fig. 1, determine blue charcoal wastewater treatment process figure, as shown in Figure 2, the present invention is based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the schema of method of blue charcoal waste water.
A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, and experimental installation as shown in Figure 3, comprises the following steps:
(1) blue charcoal waste water itself has good electroconductibility, and pH value is 9, containing a large amount of deliquescent particulate matters.Get the blue charcoal waste water of 200mL, passing into air, take graphite as negative electrode, Ti/SnO 2for anode, add 5V potential electrolysis, occur a large amount of black foam, produce until no longer include bubble, about need 1h.
(2) the blue charcoal wastewater pH processed through (1) is about 7, is 3, adds the CNTs/Fe of 1g/100mL with sulphur acid for adjusting pH 3o 4for three-diemsnional electrode particle, take graphite as negative electrode, Ti/SnO 2for anode, pass into air, electrolysis under 12V voltage, every 30min measures a BOD 5and COD crvalue.
(3) BOD is drawn 5/ COD crvalue over time as Fig. 1
Further preferably, described CNTs/Fe 3o 4the synthesis of matrix material comprises the following steps:
A1 Purification of Carbon Nanotubes first carries out purifying pre-treatment with 65wt% nitric acid to carbon nanotube, strengthen the wetting ability of carbon nanotube, make carbon nanotube degree of graphitization high, chemically reactive is low, remove the metal in carbon nano tube surface or Compound deposition thing, in order to modify and activated carbon nano-tube carbon nanotube further, pre-treatment must be carried out to carbon nanotube.Carbon nanotube dispersed after pretreatment is good, the oxygenizement of concentrated nitric acid, can in many very stable functional groups such as the hydroxyl of carbon nano tube surface generating high density, carboxyls, the functional group of these enrichments can make carbon nanotube better mix with solution, improves dispersiveness.By pretreated carbon nanotube ultrapure water cleaning to neutral, be placed in 105oC vacuum drying oven and dry, obtain the carbon nanotube after purifying;
5.9g step a1 purifying carbon nano-tube is joined 4.0g FeCl by the preparation of a2 material 36H 2o and FeCl 24H 2o, the 200mL aqueous solution is made into by the mixing of 1.75:1 amount of substance, ultrasonic 10min under nitrogen protection, is then placed in the water bath with thermostatic control of 65 DEG C, stirs and dropwise drips ammoniacal liquor simultaneously, until stop during pH=9 ~ 10 adding ammoniacal liquor, temperature is adjusted to 70 DEG C and continues stirring reaction 30min, stopped reaction, uses magnet quiescent setting, with deionized water and dehydrated alcohol repetitive scrubbing to neutral solution, be placed in the dry 6h of 85 DEG C of vacuum drying ovens;
A3 nanometer Fe 3o 4preparation nanometer Fe 3o 4preparation method and step a2 nanometer CNTs/Fe 3o 4the preparation method of material is all identical except not adding CNTs;
Further preferably, described Ti/SnO 2the preparation of electrode comprises the following steps:
B1 fine sandpaper beats the zone of oxidation on surface;
B2 alkali cleaning, uses alkali cleaning 30min in ultrasonic instrument, is cleaned by the titanium plate after alkali cleaning in ultrasonic instrument with distilled water;
The passivation of b3 acid etching technique strong acid, the corrodibility of the oxalic acid solution of proper concn is very strong, meanwhile, considers that the titanium base after oxalic acid treatment can form hydrogen bond and be not easy by secondary oxidation, therefore, selects oxalic acid to carry out pickling.Titanium plate after oil removing is etched 2h in the oxalic acid of 10%, then cleans with distilled water in ultrasonic apparatus, be kept in dehydrated alcohol for subsequent use after drying up.Titanium-based surface after acid etching forms rough grey pitted skin, without metalluster;
The preparation of b4 electroplate liquid takes 4g SnCl 45H 2o is dissolved in the dehydrated alcohol of 50mL, takes the SbCl of 0.26g simultaneously 3be dissolved in the dehydrated alcohol of 20mL, two kinds of mixtures are put into closed container respectively;
B5 is using the titanium plate processed as negative electrode, and graphite is anode, 0.25mol/L SnCl 4ethanolic soln is the direct current of electrolytic solution, 3-4V, and plating 10min, then leaves standstill 5min.Electroplating process 5-6 time repeatedly.
The titanium plate electroplated is dried by b6 in an oven, then puts into retort furnace 550 DEG C of roastings, 2h.
The above; be only the present invention's preferably embodiment; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the simple change of the technical scheme that can obtain apparently or equivalence are replaced and are all fallen within the scope of protection of the present invention.

Claims (2)

1. one kind based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, it is characterized in that, comprises the following steps:
(1) get the blue charcoal waste water of 200mL, passing into air, take graphite as negative electrode, Ti/SnO 2for anode, add 5V potential electrolysis, occur a large amount of black foam, produce until no longer include bubble, need 1h;
(2) the blue charcoal wastewater pH processed through (1) is 7, is 3, adds the CNTs/Fe of 1g/100mL with sulphur acid for adjusting pH 3o 4for three-diemsnional electrode particle, take graphite as negative electrode, Ti/SnO 2for anode, pass into air, electrolysis under 12V voltage, every 30min measures a BOD 5and COD crvalue; Draw BOD 5/ COD crvalue scheme over time;
Wherein, described CNTs/Fe 3o 4the synthesis of matrix material comprises the following steps:
A1, Purification of Carbon Nanotubes: first carry out purifying pre-treatment with 65wt% nitric acid to carbon nanotube, by pretreated carbon nanotube ultrapure water cleaning to neutral, be placed in 105 DEG C of vacuum drying ovens and dry, obtain the carbon nanotube after purifying;
A2, CNTs/Fe 3o 4the preparation of matrix material: 5.9g step a1 purifying carbon nano-tube is joined 4.0gFeCl 36H 2o and FeCl 24H 2o; the 200mL aqueous solution is made into by 1.75: 1 amount of substance mixing; ultrasonic 10min under nitrogen protection, is then placed in the water bath with thermostatic control of 65 DEG C, stirs and dropwise drips ammoniacal liquor simultaneously; until stop during pH=9 ~ 10 adding ammoniacal liquor; temperature is adjusted to 70 DEG C and continues stirring reaction 30min, stopped reaction, uses magnet quiescent setting; with deionized water and dehydrated alcohol repetitive scrubbing to neutral solution, be placed in the dry 6h of 85 DEG C of vacuum drying ovens.
2. according to claim 1 based on CNTs/Fe 3o 4three-dimensional electricity-Fenton degrades the method for blue charcoal waste water, it is characterized in that, described Ti/SnO 2the preparation of electrode comprises the following steps:
B1, beat the zone of oxidation on titanium plate surface with fine sandpaper;
B2, alkali cleaning, use alkali cleaning 30min in ultrasonic instrument, cleaned by the titanium plate after alkali cleaning in ultrasonic instrument with distilled water;
B3, the passivation of acid etching technique strong acid, the corrodibility of the oxalic acid solution of 10wt% is very strong, titanium plate after oil removing is etched 2h in the oxalic acid of 10%, clean with distilled water in ultrasonic apparatus again, be kept in dehydrated alcohol for subsequent use after drying up, titanium-based surface after acid etching forms rough grey pitted skin, without metalluster;
B4, electroplate liquid are prepared: take 4g SnCl 45H 2o is dissolved in the dehydrated alcohol of 50mL, takes the SbCl of 0.26g simultaneously 3be dissolved in the dehydrated alcohol of 20mL, two kinds of mixtures are put into closed container respectively;
B5, using the titanium plate processed as negative electrode, graphite is anode, and with the electroplate liquid prepared in step b4, the direct current of 3-4V, plating 10min, then leaves standstill 5min, repeatedly electroplating process 5-6 time;
B6, the titanium plate electroplated to be dried in an oven, then put into retort furnace 550 DEG C of roastings, 2h.
CN201310376171.XA 2013-08-23 2013-08-23 A kind of based on CNTs/Fe 3o 4three-dimensional electricity-Fenton improves the method for blue charcoal wastewater biodegradability Expired - Fee Related CN103435134B (en)

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