CN102580746A - Activated carbon supported cobalt oxide catalyst and application of same in organic pollutant degradation - Google Patents
Activated carbon supported cobalt oxide catalyst and application of same in organic pollutant degradation Download PDFInfo
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- CN102580746A CN102580746A CN2012100135796A CN201210013579A CN102580746A CN 102580746 A CN102580746 A CN 102580746A CN 2012100135796 A CN2012100135796 A CN 2012100135796A CN 201210013579 A CN201210013579 A CN 201210013579A CN 102580746 A CN102580746 A CN 102580746A
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Abstract
The invention discloses an activated carbon supported cobalt oxide catalyst and application of the same in organic pollutant degradation. The weight ratio of cobalt element to activated carbon is 0.5-10%. When the activated carbon supported cobalt oxide catalyst and persulfate are used for treating organic wastewater containing azo dyestuffs orange II taken as a target pollutant, under the radiation of ultraviolet light, the decolorization rate reaches 86.0% within 30 minutes and 95.8% within 60 minutes, and the COD (chemical oxygen demand) removal rate reaches 38.5%, the cost is low and the treating effect is good. The activated carbon supported cobalt oxide catalyst disclosed by the invention has the advantages of high catalysis efficiency and low metal ion dissolution.
Description
Technical field
The present invention relates to a kind of activated carbon supported cobalt/cobalt oxide Preparation of catalysts, this catalyst is applicable to persulfate and ultra-violet radiation and combines, and handles the organic pollution in the waste water.
Background technology
Dyeing waste water is the organic wastewater of the difficult degradation of a quasi-representative.This type chroma in waste water is big, complicated component, and chemical oxygen consumption (COC) is high, and general microorganism is difficult to degraded to it, and traditional processing method can not reach satisfied effect, is the difficult point of present wastewater treatment.
Traditional high-level oxidation technology is to utilize
OH is main active material degradation of contaminant.Advanced oxidization method commonly used has: Fenton method, Fenton-like method, electrochemical oxidation process, catalytic wet air oxidation, photocatalytic oxidation etc.The persulfate high-level oxidation technology is the technology of the new degradable organic pollutant that grew up in recent years.Persulfate is activated the persulfate free radical that produces strong oxidizing property, the organic pollution materials of the difficult degradation in the oxidative degradation water in water.At present, in water treatment system commonly used, homogeneous reaction has accounted for very big ratio.But because shortcoming such as this type of reaction exists catalyst to be difficult to reclaim, and environmental pollution is serious makes heterogeneous reaction slowly become the focus of research.
The method that the activation persulfate produces the sulfate radical free radical has a lot, and that uses always has thermal activation, photoactivation, transition metal activation, anion activation, microwave activation and a ultrasonic activation etc.The uv-activated persulfate can be rapidly and efficiently degradation of organic substances, and, shown wide application prospect having studied the degradation efficiency of various persistent organic pollutants under uv-activated persulfate condition.
The present invention utilizes prepared activated carbon supported cobalt metal oxide catalyst to combine with persulfate and ultra-violet radiation; Constitute novel high-level oxidation technology system respectively; Orange beta-naphthol simulation dyeing waste water 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.
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 cobalt/cobalt oxide catalyst of the present invention is made up of active carbon and cobalt/cobalt oxide, and cobalt element weight is 0.5 ~ 10% with the ratio of active carbon weight.
Described active carbon is preferably 300 orders.
Above-mentioned 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, again with behind the 10wt% inorganic alkali solution dipping 24h, filtration, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry;
(2), the active carbon processed adding is contained in the salting liquid of cobalt ions, 30～50 ℃ of dipping 24h, oven dry then;
(3), the active carbon of load cobalt salt is moved in the tube furnace, under nitrogen atmosphere, be warming up to 300 ~ 500 ℃, calcining 4 ~ 6 h reduce to room temperature in the nitrogen then, obtain the catalyst of activated carbon supported cobalt/cobalt oxide.
Combine the method for persulfate processing organic wastewater following activated carbon supported cobalt/cobalt oxide catalyst of the present invention:
Organic wastewater is placed heterogeneous activated reactor, add persulfate and activated carbon supported cobalt/cobalt oxide catalyst, under room temperature, react.
With activated carbon supported iron cobalt/cobalt oxide catalyst of the present invention, the method that combines to handle organic wastewater with ultra-violet radiation, persulfate is following:
Organic wastewater is placed heterogeneous activated reactor, add persulfate, activated carbon supported cobalt/cobalt oxide catalyst is opened ultra-violet radiation, under room temperature, reacts.
The present invention compares the beneficial effect that is had with prior art:
Catalyst of the present invention is to be raw material with the cobalt salt, and active carbon is a carrier, and cobalt salt is loaded on the active carbon; Obtain activated carbon supported cobalt/cobalt oxide catalyst through handling, this method for preparing catalyst is easy, and is cheap; Catalytic activity is high, and the metal ion stripping is low, good stability.Handle the orange beta-naphthol simulated wastewater with this catalyst applications in heterogeneous persulfate/ultra-violet radiation oxidation technology, can carry out at ambient temperature, reaction condition is gentle, good decolorizing effect.
Description of drawings
Fig. 1 different content catalyst oxidation degraded orange beta-naphthol.
Fig. 2 catalyst is the oxidative degradation orange beta-naphthol under different systems.
Orange beta-naphthol and COD contrast before and after the heterogeneous persulfate of Fig. 3/ultra-violet radiation system is handled.
The heterogeneous persulfate of Fig. 4/ultra-violet radiation system oxidative degradation orange beta-naphthol ultraviolet-visible light spectrogram.
The specific embodiment:
Further specify the present invention below in conjunction with accompanying drawing and instance, wherein the part preparation condition is not a limitation of the present invention only as the explanation of typical case.
Embodiment one:Cobalt content is Preparation of catalysts and the activation persulfate of 10wt% (cobalt/active carbon), handles organic wastewater.
This method comprises following step:
(1) with active carbon with 10wt% salpeter solution dipping 24h after, filter, deionized water is washed till neutrality;
(2) with step (1) active carbon processed, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, for use.
(3) 1 gram active carbon is added 50 milliliters and contain 1.697
10
-3In the solution of mol cobalt ions;
(4) at 30～50 ℃ of dipping gained solution 24h;
(5) the gained solid is in 100 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ~ 500 ℃, calcining 4 ~ 6 h, and products therefrom is reduced to room temperature in nitrogen, obtain the catalyst of activated carbon supported cobalt/cobalt oxide.
Simulated wastewater (initial concentration the is 50mg/L) 200ml that (7) will contain orange beta-naphthol places heterogeneous persulfate oxidation reaction unit; Add activated carbon supported cobalt/cobalt oxide catalyst (cobalt content is 10%) 0.16g; Persulfate 1.0g/L); Under room temperature, react, through the filter membrane filtration of 0.22 μ m, filtrating is the waste water of handling.
Embodiment two:Cobalt content is Preparation of catalysts and ultraviolet light, the persulfate Combined Treatment organic wastewater of 1w% (cobalt/active carbon).
This method comprises following step:
(1) with 300 purpose active carbons with 10wt% salpeter solution dipping 24h after, filter, deionized water is washed till neutrality;
(2) with step (1) active carbon processed, behind 10wt% sodium hydroxide solution dipping 24h, filter, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry, for use.
(3) 1 gram active carbon is added 50 milliliters and contain 1.697
10
-4In the solution of mol cobalt ions;
(4) at 30～50 ℃ of dipping gained solution 24h;
(5) the gained solid is in 120 ℃ of oven dry 12h;
(6) sample of gained loading metal-salt moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ~ 500 ℃, calcining 4 ~ 6h, and products therefrom is reduced to room temperature in nitrogen, obtain the catalyst of activated carbon supported cobalt/cobalt oxide.
Simulated wastewater (initial concentration the is 50mg/L) 200ml that (7) will contain orange beta-naphthol places heterogeneous persulfate oxidation reaction unit; Add activated carbon supported cobalt/cobalt oxide catalyst (cobalt content is 1%) 0.16g; Persulfate 1.0g/L), opens ultra-violet radiation, under room temperature, react; Filter membrane through 0.22 μ m filters, and filtrating is the waste water of handling.
Fig. 1 is the catalyst of carried by active carbon different cobalt content in the heterogeneous system, the curve map of activation persulfate degraded orange beta-naphthol.Orange beta-naphthol initial concentration: 50mg/L, persulfate consumption: 0.5g/L, catalyst amount: 0.2g/L, temperature: 22 ± 2 ℃.We can obviously find out from figure, and degradation efficiency is the highest when catalyst cobalt content is 1%.Under the reaction condition of 3h, the percent of decolourization of orange beta-naphthol has reached more than 40%.
In order to investigate the strengthening effect of ultra-violet radiation to carried by active carbon Co catalysts activation persulfate, we have done the experiment of catalyst and ultra-violet radiation associating activation persulfate under Fig. 1 condition.Orange beta-naphthol initial concentration: 50mg/L, persulfate consumption: 0.5g/L, catalyst amount: 0.2g/L, uviol lamp: 5W, temperature: 22 ± 2 ℃.As shown in Figure 2, when cobalt content is 1% catalyst, during activation persulfate degraded orange beta-naphthol, reaction later stage percent of decolourization is significantly improved under ultra-violet radiation.The percent of decolourization of orange beta-naphthol has reached more than 50% in the time of 180 minutes, apparently higher than the heterogeneous system that does not add ultra-violet radiation.
When catalyst persulfate dosage is respectively 1.0 and 0.8 g/L, react through 3h, the percent of decolourization of orange beta-naphthol reaches 98.1%.The COD clearance is 38.5%, and is as shown in Figure 3.Orange beta-naphthol initial concentration: 50mg/L, persulfate consumption: 0.8g/L, catalyst amount: 1.0 g/L, uviol lamp: 5W, temperature: 22 ± 2 ℃, times 180 min.
Fig. 4 is heterogeneous persulfate/ultra-violet radiation system oxidative degradation orange beta-naphthol ultraviolet-visible light spectrogram orange.Yellow II initial concentration: 50mg/L, persulfate consumption: 0.8g/L, catalyst amount: 1.0 g/L, uviol lamp: 5W, temperature: 22 ± 2 ℃.Fig. 4 shows that 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; 229nm and 310nm in the ultra-violet (UV) band are corresponding to the absworption peak of phenyl ring and naphthalene ring in the orange II structure.When reaction proceeded to 30min, solution reduced rapidly at the absworption peak of 485nm, explained 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, explains that azo structure (chromophore), phenyl ring and naphthalene ring are almost destroyed fully.By on can know that the heterogeneous activation persulfate of the activated carbon supported cobalt/cobalt oxide system orange beta-naphthol of having degraded has effectively reached the purpose of deep oxidation.
This shows that activated carbon supported cobalt/cobalt oxide catalyst combines the activation persulfate with ultra-violet radiation, the effect of oxidation orange beta-naphthol is remarkable.The catalyst that the present invention is prepared; Can work in coordination with persulfate, ultra-violet radiation and pollutant a series of radical chain reactions take place; 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, and catalytic activity is high, and is high to organic pollutant removal efficient in the waste water, and reaction condition is gentle, 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 changed or improves by multiple mode.For example the cobalt/cobalt oxide of preparation comprises cobaltosic oxide, cobalt sesquioxide, and cobalt oxides etc. or their mixture are by all obtaining result preferably with method of the present invention.
Claims (5)
1. an activated carbon supported cobalt/cobalt oxide catalyst is characterized in that, is made up of active carbon and cobalt/cobalt oxide, and cobalt element weight is 0.5 ~ 10% with the ratio of active carbon weight.
2. catalyst according to claim 1 is characterized in that, described active carbon is 300 orders.
3. claim 1 is stated the Preparation of catalysts method, it is characterized in that, may further comprise the steps:
(1), with active carbon with 10wt% inorganic acid solution dipping 24h after, filter, deionized water is washed till neutrality, again with behind the 10wt% inorganic alkali solution dipping 24h, filtration, deionized water is washed till neutrality; Put into baking oven, 90 ~ 100 ℃ of oven dry;
(2), the active carbon processed adding is contained in the salting liquid of cobalt ions, 30～50 ℃ of dipping 24h, oven dry then;
(3), the active carbon of load cobalt salt is moved in the tube furnace, under nitrogen atmosphere, be warming up to 300 ~ 500 ℃, calcining 4 ~ 6 h reduce to room temperature in the nitrogen then, obtain the catalyst of activated carbon supported cobalt/cobalt oxide.
4. the described activated carbon supported cobalt/cobalt oxide catalyst of claim 1 combines persulfate; Be used to handle organic wastewater; It is characterized in that: organic wastewater is placed heterogeneous activated reactor, add persulfate and activated carbon supported cobalt/cobalt oxide catalyst, under room temperature, react.
5. the described activated carbon supported iron cobalt/cobalt oxide catalyst of claim 1 combines with ultra-violet radiation, persulfate; Be used to handle organic wastewater; It is characterized in that: organic wastewater is placed heterogeneous activated reactor, add persulfate, activated carbon supported cobalt/cobalt oxide catalyst; Open ultra-violet radiation, under room temperature, react.
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| CN102744055A (en) * | 2012-07-20 | 2012-10-24 | 武汉大学 | Active carbon loaded zinc oxide catalyst and application thereof in degradation of organic pollutant |
| CN102963950A (en) * | 2012-10-31 | 2013-03-13 | 华中科技大学 | Method for treating printing and dyeing wastewater by steel slag |
| CN104496092A (en) * | 2014-12-30 | 2015-04-08 | 武汉大学 | Organic wastewater treatment method by recycling saturated activated carbon of adsorbing heavy metals |
| CN104624191A (en) * | 2013-11-11 | 2015-05-20 | 中国科学院大连化学物理研究所 | CoO/C catalyst and preparation method thereof |
| CN104667930A (en) * | 2015-02-28 | 2015-06-03 | 长沙学院 | Magnetic mesoporous carbon-supported cobalt catalyst and preparation method and application of catalyst |
| CN104801272A (en) * | 2015-04-15 | 2015-07-29 | 南通职业大学 | Preparation method of cobalt-supported activated carbon as well as condition and device for adsorbing methylbenzene with cobalt-supported activated carbon |
| CN107243346A (en) * | 2017-05-05 | 2017-10-13 | 上海电力学院 | A kind of catalyst of the cobalt containing extra granular and its preparation method and application |
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| CN108006666A (en) * | 2017-10-26 | 2018-05-08 | 昆明理工大学 | A kind of processing method of organic exhaust gas |
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Application publication date: 20120718 |