CN105731606A - Method for treating organic wastewater through synergistic activation of persulfate using electrochemistry and Ni-Fe-LDH/rGO catalyst - Google Patents
Method for treating organic wastewater through synergistic activation of persulfate using electrochemistry and Ni-Fe-LDH/rGO catalyst Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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Abstract
The invention provides a method for treating organic wastewater through synergistic activation of persulfate using electrochemistry and a Ni-Fe-LDH/rGO catalyst. The method comprises the specific steps: adding persulfate and the Ni-Fe-LDH/rGO catalyst in an electrolysis device containing organic wastewater, degrading the organic wastewater under the effect of external electric field, providing a constant current for the electrolysis process by using a constant potential rectifier, using 0.1M of Na2SO4 as a support electrolyte in the electrolysis process, and continuously performing magnetic stirring in the test process so as to guarantee the sufficient contact of the catalyst and solution. The method not only can activate the persulfate through the electrochemical manner, but also can enhance the capability of the original catalyst to activate the persulfate, and multiple paths are used for synergistically degrading the organic pollutants. The method is simple in operation, flexible in reaction, high in catalysis efficiency, and good in degradation effect; the catalyst has good magnetism and stability, and has wide application prospect in the environment pollution governance field.
Description
Technical field
The invention belongs to technical field of water pollution control, be specifically related to a kind of electrochemistry and work in coordination with Ni-Fe-LDH/rGO
The method of activation of catalyst organic wastewater treatment through persulfate.
Background technology
High-level oxidation technology, as a kind of environmentally-friendly technique, is widely used in field of waste water treatment.Although with
H2O2High-level oxidation technology for oxidant can realize the degraded of most organic pollutants, but due to H2O2
Have that self is unstable, store transport difficult, severe reaction conditions and can not to Organic substances such as perfluorocarboxylic acids
The shortcomings such as effective degraded, limit its application.Therefore, high-level oxidation technology based on potentiometric titrations should
Fortune and give birth to, this technology it is crucial that can activate efficiently and stably persulfate generation potentiometric titrations.Cross
Cross the homogeneous reaction system that metal ion is formed with persulfate (PDS), such as Co2+/PDS、Fe2+/ PDS etc.
There is catalytic efficiency high, the advantages such as oxidability is strong, there is also certain limitation, such as Co simultaneously2+To environment
Unfriendly, Fe2+System can be made to produce iron cement etc..If able to metal ion is fixed, the most do not lose simultaneously and urge
Change activity, then just can overcome disadvantage mentioned above.Therefore people develop the heterogeneous of cobalt/cobalt oxide and Supported Co
Catalyst, although can realize various organic efficient degradation, but, the dissolution problem of cobalt can not be kept away
Exempt from, remain to cause potential secondary pollution and bio-toxicity.Therefore, find a kind of new catalyst to replace
Co catalysts realizes being particularly important the efficiently activation of persulfate.Dan Chen etc. have studied
Fe3O4/ Cu (Ni) Cr-LDH complex activating peroxy-monosulfate degraded AO7 dyestuff, independent Fe3O4Activated one
Sulfate degradation rate is 31%, and Fe3O4/ Cu (Ni) Cr-LDH complex degradation rate reaches 95%, shows LDH
Play an important role (Journal of Hazardous Materials, 2014,279:476-in the composite
484).Nano-carbon material has that specific surface area is big, nontoxic, high activity, high selectivity and good stability
Etc. advantage, show superior performance as catalyst or catalyst carrier.Therefore, prepared by the present invention
A kind of Ni-Fe-LDH/rGO catalyst, it has huge specific surface area, good pore structure, is inhaling
Attached, ion exchanges and catalytic field has wide practical use.But have not yet to see about Ni-Fe-LDH/
The document of rGO catalytic activation persulfate and patent report.
Electrochemical process (EC) because of low cost, good environment compatibility and become at a kind of emerging waste water
Reason technology, but individually electrochemical process is inefficient, typically by improving electric current density or extending reaction
Time improves degradation effect.Therefore, electrochemical process and sulfate radical high-level oxidation technology being combined can
Reach the degradation effect strengthened.Patent of invention CN102249378B is disclosed, and " a kind of electrochemistry works in coordination with persulfuric acid
The method of salt treatment organic wastewater " in be by Fe under cathode electric field effect3+It is reduced into Fe2+, continuous activation over cure
Hydrochlorate, but due to add iron salt make in system produce iron cement, ferrous ion residual, and this system need exist
Carry out under bigger electric current, consume energy bigger；Disclosed " a kind of electrochemistry association of patent of invention CN104787853A
Method with activated carbon organic wastewater treatment through persulfate activation " in be to be activated by electric field-enhanced activated carbon
The degradation effect of sulfate, but this system degradation effect when pH is more than 5 is decreased obviously, and activated carbon repeats to make
Also it is decreased obviously by four postactivated abilities.
For above present situation, the present invention proposes the electrochemically strengthening of a kind of Ni-Fe-LDH/rGO activation persulfate
Method, i.e. under electric field action, can realize the collaborative activation of various ways, and system produces strong oxygen continuously
The living radical of the property changed, thus strengthen degradation effect.
Summary of the invention
It is an object of the invention to provide a kind of electrochemistry and work in coordination with Ni-Fe-LDH/rGO activation of catalyst persulfuric acid
The method of salt treatment organic wastewater；This method is simple to operate, and flexibly, the response time is short in reaction, and response speed is fast,
Show good degradation effect.
In order to achieve the above object, the technical scheme is that
A kind of electrochemistry works in coordination with the side of Ni-Fe-LDH/rGO activation of catalyst organic wastewater treatment through persulfate
Method, comprises the following steps: add oxidant and Ni-Fe-LDH/rGO magnetic catalyst containing organic wastewater
In electrolysis unit, the initial pH of reactant liquor is 3.1～10, degrades in reactant liquor under DC Electric Field
Organic wastewater, persistently carries out magnetic agitation to ensure that catalyst fully contacts with solution in experimentation.Described
Oxidant be persulfate, including sodium peroxydisulfate, potassium peroxydisulfate, Ammonium persulfate., oxidant is in organic waste
Dosage in water is 0.5g/L～2.0g/L；Described Ni-Fe-LDH/rGO magnetic catalyst is in organic waste
Dosage in water is 0.5g/L～2.0g/L；Described electric current density is 4.88～39.06mA/cm2.Described
Electrolysis unit: anode uses 2cm × 2cm Pt plate electrode, negative electrode uses the thick rustless steel of 1.6cm × 1.6cm
Net, electrode spacing 2.5cm.A constant electric current is provided for electrolytic process with potentiostat.Use 0.1M
Na2SO4As the supporting electrolyte in electrolytic process.
The preparation method of above-mentioned Ni-Fe-LDH/rGO magnetic catalyst, specifically includes following steps:
The first step, prepares graphene oxide GO
Use the Hummers method improved, take a certain amount of graphite oxide ultrasonic disperse in aqueous,
To graphene oxide suspension.
Second step, prepares Ni-Fe-LDH/rGO magnetic catalyst
By the Ni (NO that mol ratio is 2～4:13)2·6H2O and Fe (NO3)3·9H2O joins containing carbamide
In graphene oxide suspension, under room temperature, stirring forms uniform solution；Uniform solution is put into autoclave
In, 100 DEG C～180 DEG C of reacting by heating 6h～24h, react and after terminating, naturally cool to room temperature, product washing,
Obtain chemical machining nano Ni-Fe-LDH/rGO magnetic catalyst after drying.Described Ni (NO3)2·6H2O and oxidation stone
The mass ratio of ink alkene is 5.2～-26.1.Described carbamide is 2～4:1 with the mol ratio of total metal ion.
By Ni (NO3)2·6H2O、Fe(NO3)3·9H2O and carbamide join in graphene oxide suspension,
Under room temperature, stirring forms uniform solution；Uniform solution is proceeded in autoclave, 100 DEG C～180 DEG C heating
Reaction 6h～24h, reaction naturally cools to room temperature after terminating, product washs, obtains nanometer after drying
Ni-Fe-LDH/rGO magnetic catalyst.Described Ni (NO3)2·6H2O Yu Fe (NO3)3·9H2O mole
Ratio is 2～4:1.Described Ni (NO3)2·6H2O is 5.2～26.1 with the mass ratio of graphene oxide.Described
The mol ratio of carbamide and total metal ion be 2～4:1.
The dominant response principle processing waster water process is: first Ni-Fe-LDH/rGO composite catalyst is huge because of it
Big specific surface area and good pore structure, by Adsorption of Organic on its surface, for follow-up oxidative degradation
Provide favourable condition.Under the effect of electric field, the oxidation of anode generation water produces the hydroxyl of strong oxidizing property certainly
By base, the most also both potentiometric titrations Synergistic degradation Organic substance can be produced by electro-active persulfate.Heavier
, under the effect of cathode electric field, by there is own electronic in catalyst active center's metal ion
Gain and loss circulation continuous collaborative activation persulfate, produces the potentiometric titrations of strong oxidizing property, and in neutrality
Under the conditions of alkalescence, potentiometric titrations can be converted into hydroxyl radical free radical, by the Synergistic degradation of the two,
It is carbon dioxide and water by thorough for organic pollution mineralising.
Beneficial effects of the present invention: 1) Ni-Fe-LDH/rGO composite catalyst has superior absorption and catalysis
Performance, the addition of rGO increases the specific surface area of composite, can be that organic attachment provides more
Active site position, beneficially subsequent degradation；RGO is not only catalyst carrier simultaneously, is also the work of catalyst
Property position, enhance original catalyst catalysis activity；2) electricity of Ni-Fe-LDH/rGO activation persulfate
Chemical enhanced method can realize the collaborative activation of various ways, and system produces the activity of strong oxidizing property continuously
Free radical, thus strengthen degradation effect；3) this catalyst has good magnetic and stability, facilitates follow-up
Separation and recycle, reduce cost of sewage disposal；4) having widened pH value in reaction scope, reaction is in acid
Property, neutrality and alkalescence all show good degradation effect, decreases subsequent treatment process；5) operation
Method is simple, and reaction condition is gentle, and catalytic efficiency is high, and good degrading effect has broad application prospects.
Accompanying drawing explanation
Fig. 1 is that catalyst amounts affects figure to RhB removal effect；
Fig. 2 is that oxidant dosage affects figure to RhB removal effect；
Fig. 3 is that electric current density affects figure to RhB removal effect；
Fig. 4 is that original ph affects figure to RhB removal effect；
Fig. 5 is that 3 kinds of different catalysts affect figure to RhB removal effect；
Fig. 6 is that 8 kinds of different degraded systems affect figure to RhB removal effect；
Fig. 7 is the stability diagram of catalyst.
Detailed description of the invention
Below in conjunction with embodiment, outstanding feature and the marked improvement of the present invention are further elucidated with, are only that
The bright present invention and be in no way limited to following instance.Rhodamine B (RhB) dyestuff is given up by the method using the present invention
Water processes.
Embodiment 1
The impact on RhB removal effect of the Ni-Fe-LDH/rGO catalyst amounts
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；The dosage of oxidant is 1.0
g/L；Electric current density is 19.53mA/cm2；The dosage of Ni-Fe-LDH/rGO catalyst be respectively 0.5g/L,
1.0g/L, 1.5g/L and 2.0g/L.
Experimental result is as shown in Figure 1.Result shows, degradation effect presents elder generation with the increase of catalyst amounts
Trend constant after increase, the optimum dosage of Ni-Fe-LDH/rGO catalyst is 1.0g/L.
The impact on RhB removal effect of the embodiment 2 oxidant dosage
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；Ni-Fe-LDH/rGO is catalyzed
The dosage of agent is 1.0g/L；Electric current density is 19.53mA/cm2；The dosage of oxidant is respectively 0.5
G/L, 1.0g/L, 1.5g/L and 2.0g/L.
Experimental result is as shown in Figure 2.Result shows, degradation effect presents elder generation with the increase of oxidant dosage
The trend reduced after increase, because the oxidant of excess can consume the potentiometric titrations of generation so that degrading
Effect reduces, and therefore, the optimum dosage of oxidant is 1.0g/L.
The impact on RhB removal effect of embodiment 3 electric current density
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；Ni-Fe-LDH/rGO is catalyzed
The dosage of agent is 1.0g/L；The dosage of oxidant is 1.0g/L；Electric current density is 4.88mA/cm2、
9.76mA/cm2、19.53mA/cm2、29.29mA/cm2And 39.06mA/cm2。
Experimental result is as shown in Figure 3.Result shows, degradation effect presents with the increase of electric current density first to be increased
The trend of rear reduction, too high electric current density can cause side reaction, causes separating out hydrogen at negative electrode.Therefore,
Optimum current density is 19.53mA/cm2。
The impact on RhB removal effect of embodiment 4 original ph
The concentration of experimental condition: RhB is 20mg/L；The dosage of Ni-Fe-LDH/rGO catalyst is 1.0
g/L；The dosage of oxidant is 1.0g/L；Electric current density is 19.53mA/cm2；Original ph is 3.1,
6.8 and 10.
Experimental result is as shown in Figure 4.Result shows, initial pH is at bar acid, neutral, even alkalescence
Under part, all having higher degradation effect, in 25 minutes, degradation rate respectively reaches 98.73%, 100%, 97.58%.
Embodiment 5 experiment compares independent Ni-Fe-LDH catalyst, independent rGO catalyst and
The impact on RhB removal effect of the Ni-Fe-LDH/rGO composite catalyst
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；The dosage of three kinds of catalyst
It is 1.0g/L；The dosage of oxidant is 1.0g/L；Electric current density is 19.53mA/cm2。
Experimental result is as shown in Figure 5.Result shows, in 25 minutes, the degradation efficiency of three kinds of catalyst divides
Do not reach 56.33%, 82.42%, 100%.This shows compared with independent catalyst, composite catalyst table
Reveal more preferable catalysis activity, specify that Ni-Fe-LDH and rGO institute during catalytic degradation further
Role.
Embodiment 6 experiment compares the impact on RhB removal effect of 8 kinds of different degraded systems
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；Ni-Fe-LDH/rGO is catalyzed
The dosage of agent is 1.0g/L；The dosage of oxidant is 1.0g/L；Electric current density is 19.53mA/cm2。
Experimental result is as shown in Figure 6.Result shows, single PDS oxidability is limited, for RhB's
Degradation effect is faint；Individually Ni-Fe-LDH catalyst is the most very poor to the adsorption effect of RhB, this be because of
It is anion adsorbent for LDH, and RhB is the dye of positive ion；But Ni-Fe-LDH/rGO adsorbs effect
Fruit significantly improves, and this rGO being primarily due to be combined has superior absorption property；Individually EC,
In 25 minutes, degradation efficiency is 43.78%, this is because anode water oxidation produces OH；EC/PDS system,
RhB reaches 54.8% at 25 minutes interior degradation efficiencies, and this is owing to producing except the oxidation of system Anodic water
OH outside, create part SO still through electro-active PDS4 ·-；EC/Ni-Fe-LDH/rGO system,
In 25 minutes, the degradation efficiency of RhB is 81.5%, this is because the absorption of Ni-Fe-LDH/rGO and body
It it is the common effect of the OH that anode water oxidation produces；PDS/Ni-Fe-LDH/rGO system, in 25 minutes
Degradation efficiency reached 94.4%, high degradation efficiency mainly due to Ni-Fe-LDH/rGO absorption make
With the SO producing strong oxidizing property with follow-up catalytic activation PDS4 ·-；EC/PDS/Ni-Fe-LDH/rGO system,
In 25 minutes, the degradation efficiency of RhB reaches 100%.
The stability of embodiment 7 catalyst
The concentration of experimental condition: RhB is 20mg/L；Initial pH is 6.8；Ni-Fe-LDH/rGO is catalyzed
The dosage of agent is 1.0g/L；The dosage of oxidant is 1.0g/L；Electric current density is 19.53mA/cm2.
Experimental result is as shown in Figure 7.Result shows, under electrochemical action, catalyst recycles three times
Remain to reach 97.2% at 25 minutes interior decolorizing efficiencies, illustrate that catalyst has good cyclical stability.
Claims (5)
1. an electrochemistry works in coordination with the side of Ni-Fe-LDH/rGO activation of catalyst organic wastewater treatment through persulfate
Method, it is characterised in that the method is particularly as follows: add oxidant and Ni-Fe-LDH/rGO catalyst
In electrolysis unit containing organic wastewater, the organic wastewater in reactant liquor of degrading under DC Electric Field,
Continuing magnetic force stirring in degradation process；Described oxidant is persulfate, including sodium peroxydisulfate, mistake
Potassium sulfate, Ammonium persulfate., oxidant dosage in organic wastewater is 0.5g/L～2.0g/L；Institute
The Ni-Fe-LDH/rGO catalyst stated dosage in organic wastewater is 0.5g/L～2.0g/L.
Method the most according to claim 1, it is characterised in that the initial pH of described reactant liquor be 3.1～
10。
Method the most according to claim 1 and 2, it is characterised in that the described electric current in electrolysis unit
Density is 4.88～39.06mA/cm2。
Method the most according to claim 1 and 2, it is characterised in that use in described electrolysis unit
The Na of 0.1M2SO4As supporting electrolyte.
Method the most according to claim 3, it is characterised in that use 0.1M in described electrolysis unit
Na2SO4As supporting electrolyte.
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| CN108033522A (en) * | 2017-12-21 | 2018-05-15 | 南昌航空大学 | A kind of electro-catalysis couples advanced oxidation system |
| CN108107101A (en) * | 2017-12-12 | 2018-06-01 | 中国科学院合肥物质科学研究院 | A kind of three-dimensional carbon cloth/ferronickel stratiform hydroxide nano piece composite material and its application |
| CN108314172A (en) * | 2018-03-13 | 2018-07-24 | 上海交通大学 | A kind of biodegrading process of organic pollution |
| CN110015746A (en) * | 2019-05-13 | 2019-07-16 | 上海大学 | A kind of preparation method and application of graphene multi-element metal composite material |
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| CN108033522B (en) * | 2017-12-21 | 2020-08-04 | 南昌航空大学 | Electrocatalysis coupling advanced oxidation system |
| CN108033522A (en) * | 2017-12-21 | 2018-05-15 | 南昌航空大学 | A kind of electro-catalysis couples advanced oxidation system |
| CN108314172A (en) * | 2018-03-13 | 2018-07-24 | 上海交通大学 | A kind of biodegrading process of organic pollution |
| CN110230072A (en) * | 2019-05-06 | 2019-09-13 | 湖北大学 | A kind of preparation method and application of the N-NiZnCu LDH/rGO nano-chip arrays material in nickel foam |
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