CN102744055A - Active carbon loaded zinc oxide catalyst and application thereof in degradation of organic pollutant - Google Patents
Active carbon loaded zinc oxide catalyst and application thereof in degradation of organic pollutant Download PDFInfo
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- CN102744055A CN102744055A CN2012102520425A CN201210252042A CN102744055A CN 102744055 A CN102744055 A CN 102744055A CN 2012102520425 A CN2012102520425 A CN 2012102520425A CN 201210252042 A CN201210252042 A CN 201210252042A CN 102744055 A CN102744055 A CN 102744055A
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Abstract
The invention relates to active carbon loaded zinc oxide catalyst and application thereof for treating organic wastewater after being combined with ultrasonic wave or ultraviolet light and persulfate. The catalyst can be combined with disulfate to treat the organic wastewater taking azo dye orange II as target pollutant, and decolorization rate can reach 68% in 60 minutes; and after the ultrasonic wave is jointly used, the decolorization rate can be increased to 92% in 60 minutes; meanwhile, the catalyst can be combined with peroxy-monosulfate to treat the organic wastewater taking azo dye reactive black 5 as target pollutant, and decolorization rate can reach 36% in 60 minutes; and after the ultraviolet light is jointly used, the decolorization rate can be increased to 91% in 60 minutes. The active carbon loaded zinc oxide catalyst is high in catalyzing efficiency and low in metal ion digestion. The active carbon loaded zinc oxide catalyst is combined with the ultrasonic wave or the ultraviolet light and the persulfate to treat organic pollutant in the wastewater, the treatment can be performed in a mild condition, and the treatment is simple to process, low in cost and good in treatment efficiency.
Description
Technical field
The present invention relates to a kind of activated carbon supported Zinc oxide catalytic and the utilization on degradable organic pollutant thereof, belong to water-treatment technology field.
Background technology
Organic wastewater is the waste water of one type of difficult degradation.With the dyeing waste water is example, and its discharge capacity is big, and organic pollution content is high, and kind is complicated.Because organic chemical contaminant Stability Analysis of Structures, toxicity are big, intractability is high, and traditional treatment technology has received serious challenge.It is used the conventional treatment technology,, be difficult to the treatment effect that reaches satisfied like the method for physico-chemical process, chemical method and bioanalysis and combination thereof.
High-level oxidation technology, its characteristics are to produce to have strong oxidability in a large number
OH is an 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 has 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 organic pollution of pollutant, especially difficult degradation in ultrasonic wave or the ultraviolet degradation water, be 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.
Zinc oxide has catalytic efficiency preferably, simultaneously because active carbon has bigger specific area, and contains loose structure, zinc oxide is loaded on can make catalyst component be dispersed in carrier surface on the active carbon, improves its catalytic performance.Yet this catalyst is not applied in the persulfate high-level oxidation technology.Among the present invention, load there be the catalysis material of the active carbon of zinc oxide, studied its preparation method and method for using, obtained good effect as the persulfate high-level oxidation technology.
Activated carbon supported Zinc oxide catalytic of the present invention is a carrier with the active carbon, and zinc oxide is active component, and wherein the content of zinc element is 1～10wt%.
The preparation method of above-mentioned activated carbon supported Zinc oxide catalytic may further comprise the steps:
(1), with active carbon with 10wt% inorganic acid solution dipping 24h after, filter, deionized water is washed till neutrality, with 10wt% inorganic alkali solution dipping 24h, filtration is washed till neutrality with deionized water, 90～100 ℃ of oven dry again;
(2), the active carbon processed adding is contained in the salting liquid of zinc ion 20～60 ℃ of dipping 24h, oven dry then;
(3), the active carbon of zinc supported ion is moved in the tube furnace, under inert atmosphere, be warming up to 300～600 ℃, calcining 4～6 h reduce to room temperature then in inert atmosphere, obtain the catalyst of activated carbon supported zinc oxide.
Combine the method for persulfate processing organic wastewater following activated carbon supported Zinc oxide catalytic of the present invention:
Organic wastewater is placed heterogeneous activated reactor, add persulfate and activated carbon supported Zinc oxide catalytic, in 30 ℃ of reactions down.
The method that activated carbon supported Zinc oxide catalytic of the present invention is combined to handle organic wastewater with ultrasonic wave, peroxydisulfate is following: organic wastewater is placed heterogeneous activated reactor; When adding peroxydisulfate (PDS); Add activated carbon supported Zinc oxide catalytic; Under ultrasonic wave (US) effect, in 30 ℃ of reactions down.
The method that activated carbon supported Zinc oxide catalytic of the present invention is combined to handle organic wastewater with ultraviolet light, peroxy-monosulfate is following: organic wastewater is placed heterogeneous activated reactor; When adding peroxy-monosulfate (PMS); Add activated carbon supported Zinc oxide catalytic; Under ultraviolet light (UV) effect, in room temperature (25 ℃) reaction down.
Because the main deficiency of heterogeneous catalysis is activity of such catalysts surface meeting passivation gradually, finally causes catalysqt deactivation.When ultrasonic wave combines with heterogeneous high-level oxidation technology; 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, the stability and the life-span of having improved catalyst.Ultrasonic in addition 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; Improving the solution main body concentration of interior free radical isoreactivity species mutually, is a kind of method of very effective reinforcement pollutant decomposability.When ultraviolet light combined with heterogeneous high-level oxidation technology, ultraviolet light can produce synergy with catalyst, and common catalysis persulfate improves the productive rate of free radical, thereby reaches treatment effect preferably.
The present invention utilizes prepared activated carbon supported zinc metal oxide catalyst and peroxydisulfate and combination of ultrasound; And with peroxy-monosulfate and uv light combined; Constitute novel high-level oxidation technology system respectively; Orange beta-naphthol and reactive black 5 simulated wastewater have 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.
Before this, the someone has prepared active carbon supported ferriferous oxide catalyst, and is applied to heterogeneous Fenton wastewater treatment system and heterogeneous ozonisation wastewater treatment system.And the present invention utilizes prepared activated carbon supported zinc metal oxide catalyst and peroxydisulfate and combination of ultrasound, and with peroxy-monosulfate and uv light combined, constituted the novel high-level oxidation technology system that is different from above system respectively.
The present invention compares the beneficial effect that is had with prior art:
Catalyst of the present invention is to be active component with zinc oxide, and active carbon is a carrier, and zinc oxide is loaded on the active carbon, prepares activated carbon supported Zinc oxide catalytic.This method for preparing catalyst is easy, and is cheap, and catalytic activity is high, and the metal ion stripping is low, good stability.This catalyst applications is handled the orange beta-naphthol simulated wastewater in heterogeneous activation peroxydisulfate, ultrasonic/heterogeneous activation peroxydisulfate; And heterogeneous activation peroxy-monosulfate, ultraviolet light/heterogeneous activation peroxy-monosulfate is handled the reactive black 5 simulated wastewater; Can carry out at ambient temperature; Reaction condition is gentle, good decolorizing effect.
Description of drawings
The comparison of the different peroxy-disulfuric acid salt system of Fig. 1 oxidative degradation orange beta-naphthol.
The comparison of the different permonosulphuric acid salt system of Fig. 2 oxidative degradation activity black 5.
The specific embodiment
Further specify the present invention below in conjunction with accompanying drawing and embodiment, wherein the part preparation condition is not a limitation of the present invention only as the explanation of typical case.
Embodiment one:Prepare activated carbon supported Zinc oxide catalytic, activated carbon supported Zinc oxide catalytic activation peroxydisulfate is handled organic wastewater.
This method comprises following step:
(1) with active carbon (PAC) 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) 1 gram active carbon is added 50ml and contain 4.58 * 10
-4In the salting liquid of mol zinc ion;
(3) at 25 ℃ of above-mentioned solution 24h of dipping;
(4) filter maceration extract, and in 120 ℃ of oven dry 12h;
(5) the gained solid sample moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ℃, calcining 4～6 h, and products therefrom is reduced to room temperature in nitrogen, obtain the catalyst (load capacity is 3%) of activated carbon supported zinc oxide.
Simulated wastewater (initial concentration the is 50mg/L) 200ml that (6) will contain orange beta-naphthol places heterogeneous activated reactor, adds peroxydisulfate (0.5g/L), activated carbon supported Zinc oxide catalytic 0.1g, and reaction is 60 minutes under 30 ℃ of conditions.
The materiality research of porous material is the mensuration of specific area and pore structure through analytical method commonly used.Assay method commonly used has gas adsorption method, mercury injection method, gas osmosis, bubble point method etc.The distribution in the specific area of the catalyst in this experiment, pore volume and aperture is to adopt ASAP 2020 type gas absorption appearance to measure, and utilizes highly purified nitrogen adsorption-analytic properties assay determination.Wherein, the specific area S of catalyst
BETAnalysis be to test through BET method specific area (single-point and multiple spot); Pore-size distribution is through Barrett-Joyner-Halenda (BJH) formula highly purified nitrogen adsorption-desorption isotherm to be obtained, at certain relative pressure P/P
0Down, calculate the pore volume of the catalyst of preparation, the result lists in table 1.
The specific area of table 1 catalyst, pore volume and aperture
| Sample | Specific area (m 2/g） | Pore volume (cm 2/g） | Average pore size (nm) |
| PAC | 165.4492 | 0.109018 | 2.63568 |
| ZnO-PAC | 228.2031 | 0.172177 | 3.01797 |
Can find out that from table 1 specific surface of activated carbon supported Zinc oxide catalytic, pore volume and aperture are all big than the carrier active carbon catalyst.The specific surface of catalyst increases, and orange beta-naphthol Molecular Adsorption amount increases; It is big that pore volume and aperture become, and causes reactant orange beta-naphthol molecule and oxidizer molecule to reduce at the micropore inside diffusional resistance, thereby the reaction rate of orange beta-naphthol degradation reaction is increased, and catalyst performance improves.
By Fig. 1 can find out heterogeneous activation peroxy-disulfuric acid salt system (among the figure with " PDS+ZnO/PAC " expression) to the orange beta-naphthol degradation efficiency apparently higher than independent peroxydisulfate (among the figure with " PDS " expression) oxidation.Separately behind the peroxydisulfate oxidation reaction 60min, the percent of decolourization of orange beta-naphthol is had only 10%, and the oxidation of heterogeneous activation peroxydisulfate has reached about 70% at the percent of decolourization to orange beta-naphthol behind the 60min.
Embodiment two:Prepare activated carbon supported Zinc oxide catalytic, activated carbon supported Zinc oxide catalytic activation peroxydisulfate is handled organic wastewater.
This method comprises following step:
(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) 1 gram active carbon is added 50ml and contain 4.58*10
-4In the salting liquid of mol zinc ion,
(3) at 25 ℃ of above-mentioned solution 24h of dipping;
(4) filter maceration extract, and in 120 ℃ of oven dry 12h;
(5) the gained solid sample moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ℃, calcining 4～6 h, and products therefrom is reduced to room temperature in nitrogen, obtain the catalyst (load capacity is 3%) of activated carbon supported zinc oxide.
Simulated wastewater (initial concentration the is 50mg/L) 200ml that (6) will contain orange beta-naphthol places heterogeneous activated reactor; Add peroxydisulfate (0.5g/L); Activated carbon supported Zinc oxide catalytic 0.1g, under ultrasonication (ultrasonic power 60W), reaction is 60 minutes under room temperature.
Visible like Fig. 1, heterogeneous activation peroxy-disulfuric acid salt system has reached about 70% at the percent of decolourization to orange beta-naphthol behind the 60min; And heterogeneous activation peroxydisulfate/ultrasonic system has reached more than 90% at the percent of decolourization to orange beta-naphthol behind the 60min.Explain that ultrasonic energy strengthens the treatment effect of heterogeneous activation peroxy-disulfuric acid salt system.
Embodiment three:Prepare activated carbon supported Zinc oxide catalytic, activated carbon supported Zinc oxide catalytic activation peroxy-monosulfate is handled organic wastewater.
This method comprises following step:
(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) 1 gram active carbon is added 50ml and contain 1.53*10
-4In the salting liquid of mol zinc ion,
(3) at 25 ℃ of above-mentioned solution 24h of dipping;
(4) filter maceration extract, and in 120 ℃ of oven dry 12h;
(5) the gained solid sample moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ℃, calcining 4 ~ 6 h, and products therefrom is reduced to room temperature in nitrogen, obtain activated carbon supported Zinc oxide catalytic (load capacity is 1%).
Simulated wastewater (initial concentration the is 100mg/L) 200ml that (6) will contain reactive black 5 places heterogeneous activated reactor; Add peroxy-monosulfate (0.119g/L); Activated carbon supported Zinc oxide catalytic 0.075g; Under action of ultraviolet light (uviol lamp power is 5w), reaction is 60 minutes under room temperature.
Visible like Fig. 2, heterogeneous activation permonosulphuric acid salt system (among the figure with " PMS+ZnO/PAC " expression) to the reactive black 5 degradation efficiency apparently higher than independent peroxy-monosulfate (among the figure with " PMS " expression) oxidation.Separately behind the peroxy-monosulfate oxidation reaction 60min, the percent of decolourization of reactive black 5 is had only about 3%, and the oxidation of heterogeneous activation peroxy-monosulfate behind the 60min to the percent of decolourization about 36% of reactive black 5.
Embodiment four:Prepare activated carbon supported Zinc oxide catalytic, activated carbon supported Zinc oxide catalytic activation peroxy-monosulfate is handled organic wastewater.
This method comprises following step:
(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) 1 gram active carbon is added 50ml and contain 1.53*10
-4In the salting liquid of mol zinc ion;
(3) at 25 ℃ of above-mentioned solution 24h of dipping;
(4) filter maceration extract, and in 120 ℃ of oven dry 12h;
(5) the gained solid sample moves in the tube furnace, under nitrogen atmosphere, is warming up to 300 ℃, calcining 4 ~ 6 h, and products therefrom is reduced to room temperature in nitrogen, obtain activated carbon supported Zinc oxide catalytic (load capacity is 1%).
Simulated wastewater (initial concentration the is 100mg/L) 200ml that (6) will contain reactive black 5 places heterogeneous activated reactor; Add peroxy-monosulfate (0.119g/L); Activated carbon supported Zinc oxide catalytic 0.075g; Under the uviol lamp effect (uviol lamp power is 5w), reaction is 60 minutes under room temperature.
Visible like Fig. 2, heterogeneous activation permonosulphuric acid salt system behind the 60min to the percent of decolourization position about 36% of reactive black 5; And heterogeneous activation peroxy-monosulfate/ultraviolet system has reached more than 90% at the percent of decolourization to reactive black 5 behind the 60min.Explain that ultraviolet can strengthen the treatment effect of heterogeneous activation permonosulphuric acid salt system.
Claims (5)
1. an activated carbon supported Zinc oxide catalytic is characterized in that, is carrier with the active carbon, and zinc oxide is active component, and wherein the content of zinc element is 1～10wt%.
2. the preparation method of the described activated carbon supported Zinc oxide catalytic of claim 1 may further comprise the steps:
(1), with active carbon with 10wt% inorganic acid solution dipping 24h after, filter, deionized water is washed till neutrality, with 10wt% inorganic alkali solution dipping 24h, filtration is washed till neutrality with deionized water, 90～100 ℃ of oven dry again;
(2), the active carbon processed adding is contained in the salting liquid of zinc ion 20～60 ℃ of dipping 24h, oven dry then;
(3), the active carbon of zinc supported ion is moved in the tube furnace, under inert atmosphere, be warming up to 300～600 ℃, calcining 4～6 h reduce to room temperature then in inert atmosphere, obtain the catalyst of activated carbon supported zinc oxide.
3. the described activated carbon supported Zinc oxide catalytic of claim 1 combines persulfate to be used to handle organic wastewater; It is characterized in that: organic wastewater is placed heterogeneous activated reactor; Add persulfate and activated carbon supported Zinc oxide catalytic, in 30 ℃ of reactions down.
4. the described activated carbon supported Zinc oxide catalytic of claim 1 combines with ultrasonic wave, peroxydisulfate; Be used to handle organic wastewater; It is characterized in that: organic wastewater is placed heterogeneous activated reactor, when adding peroxydisulfate, add activated carbon supported Zinc oxide catalytic; Under the ultrasonic wave effect, in 30 ℃ of reactions down.
5. the described activated carbon supported Zinc oxide catalytic of claim 1; Combine with ultraviolet light, peroxy-monosulfate, be used to handle organic wastewater, it is characterized in that: organic wastewater is placed heterogeneous activated reactor; When adding peroxy-monosulfate; Add activated carbon supported Zinc oxide catalytic, under action of ultraviolet light, under room temperature, react.
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