CN102500376B - Activated carbon loaded iron-cobalt oxide catalyst and application thereof in degrading organic pollutants - Google Patents
Activated carbon loaded iron-cobalt oxide catalyst and application thereof in degrading organic pollutants Download PDFInfo
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- CN102500376B CN102500376B CN 201110324834 CN201110324834A CN102500376B CN 102500376 B CN102500376 B CN 102500376B CN 201110324834 CN201110324834 CN 201110324834 CN 201110324834 A CN201110324834 A CN 201110324834A CN 102500376 B CN102500376 B CN 102500376B
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Abstract
The invention relates to an activated carbon loaded iron-cobalt oxide catalyst of which the components and content in weight percentage are that: 80.0 percent to 99.0 percent of activated carbon and 1.0 percent to 20.0 percent of iron-cobalt bi-metal oxide, wherein the cobalt and iron mole ratio is 1:1 to 1:19. The catalyst is integrated with ultrasonic wave and persulfate, and is used for treating organic wastewater. The catalyst and the persulfate are used for treating the organic wastewater with azo dye orange II as a target pollutant, and the decolorization rate reaches 74.5 percent within 30min; after the ultrasonic wave is added, the decolorization rate can be improved to 81.2 percent within 30min, and the total organic carbon (TOC) removal rate can reach 43.4 percent. The catalyst has the advantages of high catalytic efficiency and low metal ion dissolution rate. The catalyst is integrated with the ultrasonic wave and the activated persulfate to treat the organic pollutants in the wastewater, the treatment is carried out under milder conditions, the method is simple, the cost is low and the treatment effect is good.
Description
Technical field
The present invention relates to a kind of activated carbon supported iron cobalt dual-metal oxide catalyst, and this catalyst combines with persulfate and ultrasonic wave, handle the organic pollution in the waste water, belong to field of waste water treatment.
Background technology
Organic wastewater is the waste water of a class difficult degradation.Be example with the dyeing waste water, its discharge capacity is big, organic pollution content height, kind complexity.Because organic chemical contaminant Stability Analysis of Structures, toxicity are big, the intractability height, traditional treatment technology has been subjected to serious challenge.It is used the conventional treatment technology, as the method for physico-chemical process, chemical method and bioanalysis and combination thereof, be difficult to the treatment effect that reaches satisfied.
High-level oxidation technology, its characteristics are to produce to have strong oxidability in a large number
OH is oxidant, and under reaction conditions such as HTHP, electricity, sound, light irradiation, catalyst, coming macromolecular organic pollutant degradation is little molecule.The method of using high-level oxidation technology processing organic pollution at present mainly contains heterogeneous Fenton method and Fenton-like method, catalytic wet air oxidation, photocatalytic oxidation etc.Reclaim difficulty because homogeneous catalyst exists, weakness such as environmental pollution are so heterogeneous catalysis is to become the research focus of high-level oxidation technology in recent years.
Based on sulfate radical free radical (SO
4) high-level oxidation technology be the toxic organic pollutant oxidative degradation new technology that development in recent years is got up.The general activation persulfate that adopts produces highly active sulfate radical free radical (SO
4), the toxic organic pollutant matter in the oxidation Decomposition water body is impelled most of hardly degraded organic substance oxidative degradations.
Utilize the pollutant in the ultrasonic degradation water, the organic pollution of difficult degradation especially is a kind of novelty, clean and have the novel water technology of industrial prospect.
Summary of the invention
Problem to be solved by this invention provides a kind of cheap, callable catalyst, and the utilization on degradable organic pollutant.
Activated carbon supported iron cobalt/cobalt oxide catalyst of the present invention, its component and content are: the active carbon weight percent content is 80.0 ~ 99.0%, and iron cobalt dual-metal oxide weight degree is 1.0 ~ 20.0 %, and wherein the ferro-cobalt mol ratio is 1:1 ~ 1:19.
Described active carbon diameter is preferably 300 orders.
Above-mentioned activated carbon supported iron cobalt/cobalt oxide Preparation of catalysts method may further comprise the steps:
(1), with active carbon with 10wt% inorganic acid solution dipping 24h after, filter, deionized water is washed till neutrality;
(2), with step (1) processed active carbon, behind 10wt% inorganic alkali solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven and dry, stand-by;
(3), preparation contains the salting liquid of iron and cobalt ions, wherein the ferro-cobalt mol ratio is 1:1 ~ 1:19, the pH of regulator solution is 2～7;
(4), active carbon is added in the solution of step (3) preparation, at 20～60 ℃ of dipping 24h;
(5), filter, sub-argument has gone out to flood the active carbon of iron cobalt, oven dry;
(6), the active carbon of load iron cobalt is moved in the tube furnace, be warming up to 300 ~ 800 ℃ under noble gas atmosphere, calcining 4 ~ 6 h obtain the catalyst of activated carbon supported iron cobalt/cobalt oxide.
The method that activated carbon supported iron cobalt/cobalt oxide catalyst of the present invention is handled organic wastewater in conjunction with persulfate is as follows:
Organic wastewater is placed heterogeneous activated reactor, add persulfate and activated carbon supported iron cobalt/cobalt oxide catalyst, under room temperature, react.
With activated carbon supported iron cobalt/cobalt oxide catalyst of the present invention, the method for handling organic wastewater of being combined with ultrasonic wave, persulfate is as follows:
Organic wastewater is placed heterogeneous activated reactor, add persulfate, activated carbon supported iron cobalt/cobalt oxide catalyst under the ultrasonic wave effect, reacts under room temperature.
Because the main deficiency of heterogeneous catalysis is activity of such catalysts surface meeting passivation gradually, finally causes catalysqt deactivation.When ultrasonic wave when heterogeneous high-level oxidation technology is combined, near the high-speed jet that avalanche causes solid catalyst surface or particle of the cavitation bubble of ultrasonic generation, micro slipstream, shock wave etc. can be strengthened the solid-liquid mass transfer between pollutant and the catalyst, acoustic streaming in the ultrasonic field and little acoustic streaming can continue the cleaning catalyst surface in addition, keep catalyst activity, stability and the life-span of having improved catalyst.Ultrasonic and heterogeneous high-level oxidation technology coupling also can overcome the deficiency that free radical isoreactivity species in the independent power ultrasonic field only are distributed in the cavitation bubble surface in addition, improving the solution main body concentration of interior free radical isoreactivity species mutually, is a kind of method of very effective reinforcement pollutant decomposability.
The present invention utilizes prepared activated carbon supported iron cobalt dual-metal oxide catalyst and persulfate and ultrasonic combining, constitute novel high-level oxidation technology system respectively, the orange beta-naphthol simulated wastewater has been reached good effect of removing, and the stripping of solid-phase catalyst metal ion is low, is easy to separate; Technological process is simple, and cost is low, has the prospect of good practice.
The present invention compares the beneficial effect that has with prior art:
Catalyst of the present invention is to be raw material with molysite and cobalt salt, active carbon is carrier, molysite, cobalt salt are loaded on the active carbon, through handling the oxide catalyst that obtains activated carbon supported iron and cobalt, this method for preparing catalyst is easy, and is cheap, the catalytic activity height, the metal ion stripping is low, good stability.Be applied to heterogeneous activation persulfate, ultrasonic/heterogeneous activation persulfate processing orange beta-naphthol simulated wastewater with this catalyst, can carry out reaction condition gentleness, good decolorizing effect at ambient temperature.
Description of drawings
The comparison of the different system oxidative degradation of Fig. 1 orange beta-naphthol, orange beta-naphthol initial concentration: 50mg/L, ultrasonic power: 60W, persulfate consumption: 0.5g/L, catalyst amount: 0.8g/L.
Fig. 2 is ultrasonic/heterogeneous activation persulfate system under the uv-vis spectra of orange II with the variation in reaction time, orange beta-naphthol initial concentration: 50mg/L, ultrasonic power: 60W, persulfate consumption: 0.5g/L, catalyst amount: 1.0g/L.
Fig. 3 is ultrasonic/heterogeneous activation persulfate system under the result of orange beta-naphthol and TOC, orange beta-naphthol initial concentration: 50mg/L, ultrasonic power: 60W, persulfate consumption: 0.5g/L, catalyst amount: 1.0g/L, time: 30min.
Fig. 4 catalyst is reused result, orange beta-naphthol initial concentration: 50mg/L, ultrasonic power: 60W, persulfate consumption: 0.5g/L, catalyst amount: 2.5g/L, time: 60min.
The specific embodiment
Further specify the present invention below in conjunction with drawings and Examples, wherein preparation condition is not limitation of the present invention only as the explanation of typical case.
Embodiment one:Preparation contains the activated carbon supported iron cobalt/cobalt oxide catalyst of ferro-cobalt mol ratio 1:1, and activated carbon supported cobalt iron oxide catalyst activation persulfate is handled organic wastewater.
The preparation method comprises following step:
(1) with behind the active carbon usefulness 10wt% hydrochloric acid solution dipping 24h, filter, deionized water is washed till neutrality;
(2) with step (1) processed active carbon, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, stand-by.
(3) 1 gram active carbon is added 50ml and contain 1.25*10
-3Mol iron ion and 1.25*10
-3In the salting liquid of mol cobalt ions, the pH that adds hydrochloric acid conditioning solution is 2～7;
(4) at 40 ℃ of dipping gained solution 24h;
(5) filter maceration extract, and in 120 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, is warming up to 400 ℃ under nitrogen atmosphere, calcining 4 ~ 6 h, and products therefrom is down to room temperature in nitrogen, obtain the catalyst of activated carbon supported iron, cobalt/cobalt oxide.
(7) simulated wastewater (initial concentration the is 50mg/L) 200ml that will contain orange beta-naphthol places heterogeneous activated reactor, adds persulfate (0.5g/L), activated carbon supported iron cobalt/cobalt oxide catalyst 0.16g, and reaction is 60 minutes under room temperature.
As seen from Figure 1 heterogeneous activation persulfate system (among the figure with " persulfate+catalyst " expression) to the orange beta-naphthol degradation efficiency apparently higher than independent persulfate oxidation (among the figure with " persulfate " expression).Separately behind the persulfate oxidation reaction 60min, the percent of decolourization of orange beta-naphthol is had only 10%, and heterogeneous activation persulfate oxidation has reached more than 80% at the percent of decolourization to orange beta-naphthol behind the 60min.
Embodiment two:Preparation contains the activated carbon supported iron cobalt/cobalt oxide catalyst of ferro-cobalt mol ratio 1:1, with ultrasonic wave, persulfate Combined Treatment organic wastewater.
The preparation method comprises following step:
(1) with behind the active carbon usefulness 10wt% salpeter solution dipping 24h, filter, deionized water is washed till neutrality;
(2) with step (1) processed active carbon, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, stand-by.
(3) 1 gram active carbon is added 50ml and contain 1.25*10
-3Mol iron ion and 1.25*10
-3In the salting liquid of mol cobalt ions, the pH that adds hydrochloric acid conditioning solution is 2～7;
(4) at 40 ℃ of dipping gained solution 24h;
(5) filter maceration extract, and in 120 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, is warming up to 400 ℃ under nitrogen atmosphere, calcining 4 ~ 6 h, and products therefrom is down to room temperature in nitrogen, obtain the catalyst of activated carbon supported iron, cobalt/cobalt oxide.
(7) simulated wastewater (initial concentration the is 50mg/L) 200ml that will contain orange beta-naphthol places heterogeneous activated reactor, add persulfate (0.5g/L), active carbon supported ferriferous oxide catalyst 0.16g, under ultrasonication (ultrasonic power 60W), reaction is 60 minutes under room temperature.
As shown in Figure 1, heterogeneous activation persulfate system percent of decolourization to orange beta-naphthol behind 60min has reached 80%; And heterogeneous activation persulfate/ultrasonic system has reached more than 90% at the percent of decolourization to orange beta-naphthol behind the 60min.Illustrate that ultrasonic energy strengthens the treatment effect of heterogeneous activation persulfate system.
As shown in Figure 2, in the molecular structure of orange beta-naphthol, it has very strong absworption peak about 485nm, corresponding to the absworption peak of orange II molecule azo structure; At ultra-violet (UV) band 229nm and 310nm, corresponding to the absworption peak of phenyl ring and naphthalene ring in the orange II structure.When reaction proceeded to 30 minutes, solution reduced rapidly at the absworption peak of 485nm, illustrated that chromophoric group can rupture rapidly at short notice, and orange II azo structure is destroyed.Along with proceeding of reaction, solution is at 485nm, and 229nm and 310nm have had significantly reduction, illustrate that azo structure (chromophore), phenyl ring and naphthalene ring are almost destroyed fully.As from the foregoing, the heterogeneous activation persulfate of the activated carbon supported iron cobalt/cobalt oxide system orange beta-naphthol of having degraded has effectively reached the purpose of deep oxidation.
Under ultrasonic/heterogeneous activation persulfate system, after 30min was carried out in reaction, the percent of decolourization of orange beta-naphthol had reached 81.2% as seen from Figure 3, and the clearance of TOC has reached 43.4%; Illustrate that this system can reach the purpose of deep oxidation to orange beta-naphthol.
As seen from Figure 4, along with catalyst is reused the number of times increase, the orange beta-naphthol percent of decolourization changes little, and after catalyst used 3 times, percent of decolourization descended not obvious, illustrates that catalyst life is higher.
Embodiment three:Preparation contains the activated carbon supported iron cobalt/cobalt oxide catalyst of ferro-cobalt mol ratio 1:2, with ultrasonic wave, persulfate Combined Treatment organic wastewater.
The preparation method comprises following step:
(1) with behind the active carbon usefulness 10wt% hydrochloric acid solution dipping 24h, filter, deionized water is washed till neutrality;
(2) with step (1) processed active carbon, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, stand-by.
(3) 1 gram active carbon is added 50ml and contain 1.25*10
-3Mol iron and 6.3*10
-4In the salting liquid of mol cobalt ions, the pH that adds hydrochloric acid conditioning solution is 2～7;
(4) at 60 ℃ of dipping gained solution 24h;
(5) filter maceration extract, and in 120 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, is warming up to 800 ℃ under nitrogen atmosphere, calcining 4 ~ 6 h, and products therefrom is down to room temperature in nitrogen, obtain the catalyst of activated carbon supported iron, cobalt/cobalt oxide.
(7) simulated wastewater (initial concentration the is 50mg/L) 200ml that will contain orange beta-naphthol places heterogeneous activated reactor, add persulfate (0.5g/L), active carbon supported ferriferous oxide catalyst 0.16g, under ultrasonication (ultrasonic power 60W), reaction is 60 minutes under room temperature.
According to the method for testing in the embodiment 2, more than Zhi Bei catalyst and combination of ultrasound activate persulfate, and the effect of oxidation orange beta-naphthol is remarkable.
Embodiment four:Preparation contains the activated carbon supported iron cobalt/cobalt oxide catalyst of ferro-cobalt mol ratio 1:19, with ultrasonic wave, persulfate Combined Treatment organic wastewater.
The preparation method comprises following step:
(1) with behind the active carbon usefulness 10wt% hydrochloric acid solution dipping 24h, filter, deionized water is washed till neutrality;
(2) with step (1) processed active carbon, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, stand-by.
(3) 1 gram active carbon is added 50ml and contain 1.25*10
-3Mol iron and 6.58*10
-5In the salting liquid of mol cobalt ions, the pH that adds hydrochloric acid conditioning solution is 2～7;
(4) at 30 ℃ of dipping gained solution 24h;
(5) filter maceration extract, and in 120 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, is warming up to 300 ℃ under nitrogen atmosphere, calcining 4 ~ 6 h, and products therefrom is down to room temperature in nitrogen, obtain the catalyst of activated carbon supported iron, cobalt/cobalt oxide.
(7) simulated wastewater (initial concentration the is 50mg/L) 200ml that will contain orange beta-naphthol places heterogeneous activated reactor, add persulfate (0.5g/L), active carbon supported ferriferous oxide catalyst 0.16g, under ultrasonication (ultrasonic power 60W), reaction is 60 minutes under room temperature.
According to the method for testing in the embodiment 2, more than Zhi Bei catalyst and combination of ultrasound activate persulfate, and the effect of oxidation orange beta-naphthol is remarkable.
This shows, activated carbon supported iron cobalt double oxide catalyst and combination of ultrasound activation persulfate, the effect of oxidation orange beta-naphthol is remarkable.The catalyst that the present invention is prepared, but a series of radical chain reactions take place in synergistic oxidation agent (as persulfate and ultrasonic) and pollutant, reduce the activation energy of contaminant degradation reaction or change the reaction mechanism mechanism of reaction, thereby reach deep oxidation, remove the purpose of organic pollution to greatest extent.The catalyst of the present invention's preparation, method is simple, the catalytic activity height, the metal ion stripping is low, good stability; To organic pollutant removal efficient height in the waste water, reaction condition gentleness, good decolorizing effect.
The present invention not only is confined to foregoing description, in the scope that it is illustrated in not breaking away from claim of the present invention, can be changed by multiple mode or improve.For example adopt cobalt oxalate, ferric oxalate, cobalt acetate, ferric acetate, cobalt nitrate, ferric nitrate are iron, cobalt source raw material, and the catalyst for preparing by the inventive method all can obtain identical result.
Claims (2)
1. activated carbon supported iron cobalt/cobalt oxide is characterized in that in the purposes of handling on the organic wastewater: organic wastewater is placed heterogeneous activated reactor, add persulfate and activated carbon supported iron cobalt/cobalt oxide catalyst, react under room temperature;
Described activated carbon supported iron cobalt/cobalt oxide catalyst, its component and content are: the active carbon weight percent content is 80.0 ~ 99.0%, and iron cobalt dual-metal oxide weight degree is 1.0 ~ 20.0 %, and wherein the ferro-cobalt mol ratio is 1:1 ~ 1:19.
2. activated carbon supported iron cobalt/cobalt oxide catalyst is in the purposes of handling on the organic wastewater, it is characterized in that: organic wastewater is placed heterogeneous activated reactor, add persulfate, activated carbon supported iron cobalt/cobalt oxide catalyst, under the ultrasonic wave effect, under room temperature, react;
Described activated carbon supported iron cobalt/cobalt oxide catalyst, its component and content are: the active carbon weight percent content is 80.0 ~ 99.0%, and iron cobalt dual-metal oxide weight degree is 1.0 ~ 20.0 %, and wherein the ferro-cobalt mol ratio is 1:1 ~ 1:19.
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| CN1431048A (en) * | 2001-11-23 | 2003-07-23 | 中国科学院山西煤炭化学研究所 | Load typed iron catalyst and its preparing method and application |
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