CN102909073A - Preparation method and application of heterogeneous Fenton-like catalyst - Google Patents
Preparation method and application of heterogeneous Fenton-like catalyst Download PDFInfo
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- CN102909073A CN102909073A CN2012103881721A CN201210388172A CN102909073A CN 102909073 A CN102909073 A CN 102909073A CN 2012103881721 A CN2012103881721 A CN 2012103881721A CN 201210388172 A CN201210388172 A CN 201210388172A CN 102909073 A CN102909073 A CN 102909073A
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Abstract
Disclosed are a preparation method and application of heterogeneous Fenton-like catalyst. The preparation method includes the steps of firstly, dissolving complexing agent and metal salt in distilled water to respectively prepare complexing agent and metal salt solutions; secondly dropwise adding the metal salt solution into the complexing agent solution under the action of a magnetic mixer, and mixing for 20-60 after dropwise addition to obtain metal complex solution; and thirdly, impregnating activated carbon fiber in the metal complex solution for 1-24h, and subjecting taken-out activated carbon fiber to distilled water washing and drying to obtain the heterogeneous Fenton-like catalyst. The preparation method is simple, and conditions are mild. Environment-friendly hydrogen peroxide is used as oxidant, no extra ultraviolet light or even visible light is needed, and the heterogeneous Fenton-like catalyst is capable of efficiently degrading organic pollutants such as dye within a wide pH range of 2-10. The heterogeneous Fenton-like catalyst is well repeatable, and secondary pollution of the homogeneous Fenton reagent caused by iron ions is avoided.
Description
Technical field
The present invention relates to a kind of preparation method and application of the heterogeneous class Fenton catalyst for treatment of dyeing wastewater, belong to the dyeing wastewater through organic matter treatment technology.
Background technology
By Fe
2+And H
2O
2The Fenton reagent that forms can produce hydroxyl radical free radical (the oxidizing potential 2.8V with strong oxidizing property, the oxidizing potential 2.87V that is only second to fluorine), can remove poisonous persistent organic pollutants in the waste water, so the Fenton technology is a kind of high-level oxidation technology that is widely used in wastewater treatment.But there is in actual applications following problem: the residual Fe of having in the solution after (1) reaction
2+, cause easily secondary pollution; (2) Fenton's reaction generally carries out in the strong acid medium of pH2-3.5, and actual dying is neutral even alkaline mostly, and therefore stronger acid condition has increased the cost of wastewater treatment greatly, has limited the further application of Fenton reagent.
Class Fenton technology is a kind of high-level oxidation technology that grows up on traditional Fenton reagent basis, in broad terms, except Fenton reagent, other adopts hydrogen peroxide to produce hydroxyl radical free radical isoreactivity base and processes the technology of organic pollution and all be called class Fenton technology, such as the fragrant class of electric class pause technology, light class Fenton technology, heterogeneous class Fenton technology etc.In recent years, heterogeneous class Fenton technology is because having the degradation efficiency height, reduce secondary pollution, can widening the advantages such as pH value of solution reaction by extensive concern.In the known technology, application number: 201110116847.2 " a kind of preparation methods of the heterogeneous Fenton catalyst of processing for Methyl Orange in Wastewater " are disclosed to be the heterogeneous Fenton catalyst of processing for Methyl Orange in Wastewater, then metal oxide supported to biomass carrier with iron, copper, nickel etc. can get the heterogeneous Fenton catalyst through calcining.Application number: 201210081648.7 " a kind of preparation methods of heterogeneous Fenton reagent oxidation catalyst of activated carbon supported ferrous iron " disclose Fe
2+Load to and make heterogeneous Fenton catalyst on the active carbon.Application number: 201010531848.9 " preparation methods of a kind Fenton catalytic membrane " disclose PVDF powder and Fenton system compound, make a kind Fenton catalytic membrane by film technique, this film has good catalytic oxidation performance to organic pollutants in pH is the scope of 3-11.The people such as Kasiri make the iron modified catalyst with the modification with Fe zeolite, under the irradiation of ultraviolet light, in conjunction with hydrogen peroxide degradable acid blue dye (Appl.Catal.B:Environ., 2008,84 (1-2): 9-15).
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of method is simple, cost is low, reaction condition is gentle and provide, easily preparation method and the application thereof of the heterogeneous class Fenton catalyst of suitability for industrialized production.
The preparation method of heterogeneous class Fenton catalyst of the present invention, this preparation method may further comprise the steps: (1) is dissolved in complexing agent and slaine in the distilled water, is mixed with respectively complexing agent and metal salt solution; (2) then under the magnetic stirring apparatus effect, metal salt solution is dropwise joined in the enveloping agent solution, drip rear stirring 20-60min and can get metal complex solution; (3) activated carbon fiber is immersed in 1-24h in the metal complex solution, takes out activated carbon fiber and wash through distilled water, oven dry namely gets described heterogeneous class Fenton catalyst.
Aforesaid complexing agent can be citric acid, citrate, oxalic acid, oxalates etc., and they can be used alone, but also also mix together.
Aforesaid slaine refers to the mixture of mantoquita or molysite or two kinds of salt, and wherein said molysite can be FeCl
2, FeCl
3, Fe (NO
3)
3, FeSO
4, Fe
2(SO
4)
3Deng, they can be used alone, but also also mix together; Described mantoquita can be CuSO
4, CuCl
2, Cu (NO
3)
2Deng, they can be used alone, but also also mix together.
Activated carbon fiber refers to viscose base activated carbon fiber, polyacrylonitrile based activated carbon fiber, asphalt activity carbon fiber and phenolic resin based activated carbon fiber as mentioned above.
Said method loads to iron ion or the copper ion form with complex compound on the activated carbon fiber, can be in wider pH scope stable existence, activated carbon fiber has good adsorption capacity simultaneously, can be with complex compound absorption in its surface stably.Iron ion or copper ion complex on the activated carbon fiber surface effectively the catalytic decomposition hydrogen peroxide produce hydroxyl radical free radical, thereby make the quick oxidized degraded of dye molecule, for heterogeneous class Fenton technology opens up a new way.The heterogeneous class Fenton catalyst of preparation to waste water from dyestuff pH equal effective catalysis hydrogen peroxide in the scope of 2-10, has improved traditional Fenton technology pH narrow range, has easily produced the shortcoming of secondary pollution, has good economy, environmental and social benefits.
Application of the present invention is as follows:
Be used for the degraded of the organic pollutions such as dyestuff, it is: to containing Reactive Red K-2BP, X-3B or azogeramine, the Acid Orange II etc. that concentration is 0.01-0.5g/L, pH adds heterogeneous class Fenton catalyst and hydrogen peroxide in the waste water from dyestuff of 2-10, under being 20-90 ℃, temperature stirs 5-40min, wherein the addition of heterogeneous class Fenton catalyst is 0.5-10g/L, and the addition of hydrogen peroxide is 5-50mmol/L.
The present invention compares with above-mentioned prior art, and the novelty of its technology is that the good catalytic performance of the adsorption capacity that NACF is superpower and iron complex organically combines, and prepares a kind of novel heterogeneous class Fenton catalyst.The inventive method is simple, cost is low, reaction condition is gentle, and suitability for industrialized production is the processing method of a kind of economy, green easily.The heterogeneous class Fenton catalyst of the present invention preparation utilizes the efficiently organic wastewater such as fast degradation dyestuff of hydrogen peroxide under the condition of not regulating wastewater pH, do not need the irradiation of ultraviolet light even visible light, and catalyst can be repeatedly used.Therefore, the prepared class Fenton catalyst of the present invention not only can be applicable to serious treatment of dyeing wastewater, but also can be applicable to the wastewater treatment of the industries such as papermaking, chemical industry, pharmacy.
Preparation method of the present invention is simple, mild condition, take the environment-friendly type hydrogen peroxide as oxidant, need not extra ultraviolet light even visible light, the heterogeneous class Fenton catalyst of preparation can efficient degradation in the 2-10 wider pH range organic pollution such as dyestuff, and such Fenton catalyst has good reusability, the secondary pollution of having avoided the homogeneous phase Fenton reagent to bring because of iron ion.This invention can be applicable to the advanced treating of dyeing waste water, pollutes significant to solving day by day serious water.
Description of drawings
Fig. 1 is that the heterogeneous class Fenton catalyst of embodiment 1 preparation is to Reactive Red K-2BP removal effect figure.
Fig. 2 is the heterogeneous class Fenton catalyst of the embodiment 1 preparation removal effect figure to Reactive Red K-2BP under different pH values.
The specific embodiment
The preparation method of a kind of heterogeneous class Fenton catalyst of the present invention, this preparation method may further comprise the steps: (1) is dissolved in complexing agent and slaine in the distilled water, is mixed with respectively complexing agent and metal salt solution; (2) then under the magnetic stirring apparatus effect, metal salt solution is dropwise joined in the enveloping agent solution, drip rear stirring 20-60min and can get metal complex solution; (3) activated carbon fiber is immersed in 1-24h in the metal complex solution, takes out activated carbon fiber and wash through distilled water, oven dry namely gets described heterogeneous class Fenton catalyst.
Described complexing agent refers to citric acid, citrate, oxalic acid, oxalates; Described slaine refers to the mixture of mantoquita or molysite or two kinds of salt, and wherein said mantoquita comprises CuSO
4, CuCl
2, Cu (NO
3)
2, described molysite comprises FeCl
2, FeCl
3, Fe (NO
3)
3, FeSO
4, Fe
2(SO
4)
3
Described activated carbon fiber refers to viscose base activated carbon fiber, polyacrylonitrile based activated carbon fiber, asphalt activity carbon fiber and phenolic resin based activated carbon fiber.
A kind of as mentioned above application of heterogeneous class Fenton catalyst, be mainly used in the degraded of the organic pollutions such as dyestuff, it is to containing Reactive Red K-2BP, X-3B or the azogeramine that concentration is 0.01-0.5g/L, Acid Orange II etc., pH adds heterogeneous class Fenton catalyst and hydrogen peroxide in the waste water from dyestuff of 2-10, stir 5-40min under temperature is 20-90 ℃, wherein the addition of heterogeneous class Fenton catalyst is 0.5-10g/L, and the addition of hydrogen peroxide is 2-50mmol/L.
Below in conjunction with several implementation cases; the present invention is further understood in exemplary explanation and help; but the case study on implementation detail only is for the present invention is described; do not represent the present invention and conceive lower whole technical scheme; therefore should not be construed as limited overall technical solution; some are In the view of the technical staff; the unsubstantiality that does not depart from the present invention's design increases and change; for example simple the change or replacement of technical characterictic to have same or similar technique effect all belongs to protection domain of the present invention.
With natrium citricum and FeCl
3Be dissolved in the distilled water, be mixed with respectively natrium citricum and FeCl
3Solution is then under the magnetic stirring apparatus effect, with FeCl
3Solution dropwise joins in the sodium citrate solution, drips rear stirring 20min and can get ironic citrate solution, and activated carbon fiber is immersed in 12h in the ironic citrate solution, takes out activated carbon fiber and washs through distilled water, and oven dry namely gets novel heterogeneous class Fenton catalyst.
Experiment shows, is that Reactive Red K-2BP, the pH of 0.05g/L adds 0.5g heterogeneous class Fenton catalyst and 0.3ml hydrogen peroxide in 7 the waste water from dyestuff in 100ml concentration, is under 50 ℃ in temperature, stirring reaction 9min, and degradation rate can reach 99.1%
Fig. 1 has provided the heterogeneous class Fenton catalyst of present embodiment preparation to the removal effect figure of Reactive Red K-2BP, can find out, this heterogeneous class Fenton catalyst can the catalysis hydrogen peroxide, effectively removes Reactive Red K-2BP.
The heterogeneous class Fenton catalyst that Fig. 2 has provided the present embodiment preparation to the removal effect figure of Reactive Red K-2BP, can find out that heterogeneous class Fenton catalyst has obvious removal effect to Reactive Red K-2BP in the pH value is 2-10 under different pH values.
With natrium citricum and Fe
2(SO
4)
3Be dissolved in the distilled water, be mixed with respectively natrium citricum and Fe
2(SO
4)
3Solution is then under the magnetic stirring apparatus effect, with Fe
2(SO
4)
3Solution dropwise joins in the sodium citrate solution, drips rear stirring 20min and can get ironic citrate solution, and activated carbon fiber is immersed in 12h in the ironic citrate solution, takes out activated carbon fiber and washs through distilled water, and oven dry namely gets novel heterogeneous class Fenton catalyst.
Experiment shows, is that activated red X-3B, the pH of 0.05g/L adds 0.5g heterogeneous class Fenton catalyst and 0.3ml hydrogen peroxide in 9 the waste water in 100ml concentration, is under 50 ℃ in temperature, stirring reaction 9min, and degradation rate can reach 99.3%
With sodium oxalate and Fe
2(SO
4)
3Be dissolved in the distilled water, be mixed with respectively sodium oxalate and Fe
2(SO
4)
3Solution is then under the magnetic stirring apparatus effect, with Fe
2(SO
4)
3Solution dropwise joins in the sodium oxalate solution, drips rear stirring 20min and can get ironic citrate solution, and activated carbon fiber is immersed in 12h in the ferric oxalate solution, takes out activated carbon fiber and washs through distilled water, and oven dry namely gets novel heterogeneous class Fenton catalyst.
Experiment shows, is that azogeramine, the pH of 0.05g/L adds 0.5g heterogeneous class Fenton catalyst and 0.3ml hydrogen peroxide in 4 the waste water in 100ml concentration, is under 50 ℃ in temperature, stirring reaction 9min, and degradation rate can reach 98.8%
With citric acid and Fe (NO
3)
2Be dissolved in the distilled water, be mixed with respectively citric acid and Fe (NO
3)
2Solution is then under the magnetic stirring apparatus effect, with Fe (NO
3)
2Solution dropwise joins in the citric acid solution, drip rear stirring 20min and can get ironic citrate solution, activated carbon fiber is immersed in 12h in the edta solution, take out activated carbon fiber and wash through distilled water, oven dry namely gets novel heterogeneous class Fenton catalyst.
Experiment shows, is that Acid Orange II, the pH of 0.05g/L adds 0.5g heterogeneous class Fenton catalyst and 0.3ml hydrogen peroxide in 3 the waste water in 100ml concentration, is under 50 ℃ in temperature, stirring reaction 9min, and degradation rate can reach 98.2%
With natrium citricum and CuSO
4Be dissolved in the distilled water, be mixed with respectively natrium citricum and CuSO
4Solution is then under the magnetic stirring apparatus effect, with CuSO
4Solution dropwise joins in the sodium citrate solution, drips rear stirring 20min and can get copper citrate solution, and activated carbon fiber is immersed in 12h in the copper citrate solution, takes out activated carbon fiber and washs through distilled water, and oven dry namely gets novel heterogeneous class Fenton catalyst.
Experiment shows, is that azogeramine, the pH of 0.05g/L adds 0.5g heterogeneous class Fenton catalyst and 0.3ml hydrogen peroxide in 3 the waste water in 100ml concentration, is under 50 ℃ in temperature, stirring reaction 15min, and degradation rate can reach 78.8%.
To those skilled in the art; under this patent design and specific embodiment enlightenment; the distortion that can directly derive or associate from this patent disclosure and general knowledge; or the substituting of known technology commonly used in the prior art; and the mutual various combination between feature; for example according to different waste water and pollutant levels; determine different amounts; and different molysite, mantoquita; the unsubstantiality of carboxylate etc. is changed, and can be employed equally, can both realize and the essentially identical function of above-described embodiment and effect; give an example no longer one by one, all belong to the protection domain of this patent.
Claims (4)
1. the preparation method of a heterogeneous class Fenton catalyst, it is characterized in that this preparation method may further comprise the steps: (1) is dissolved in complexing agent and slaine in the distilled water, is mixed with respectively complexing agent and metal salt solution; (2) then under the magnetic stirring apparatus effect, metal salt solution is dropwise joined in the enveloping agent solution, drip rear stirring 20-60min and can get metal complex solution; (3) activated carbon fiber is immersed in 1-24h in the metal complex solution, takes out activated carbon fiber and wash through distilled water, oven dry namely gets described heterogeneous class Fenton catalyst.
2. the preparation method of heterogeneous class Fenton catalyst according to claim 1 is characterized in that described complexing agent refers to citric acid, citrate, oxalic acid, oxalates; Described slaine refers to the mixture of mantoquita or molysite or two kinds of salt, and wherein said mantoquita comprises CuSO
4, CuCl
2, Cu (NO
3)
2, described molysite comprises FeCl
2, FeCl
3, Fe (NO
3)
3, FeSO
4, Fe
2(SO
4)
3
3. according to the preparation method of claims 1 described heterogeneous class Fenton catalyst, it is characterized in that described activated carbon fiber refers to viscose base activated carbon fiber, polyacrylonitrile based activated carbon fiber, asphalt activity carbon fiber and phenolic resin based activated carbon fiber.
4. application such as heterogeneous class Fenton catalyst as described in claim 1 or 2 or 3 is characterized in that described heterogeneous class Fenton catalyst is used and is:
Be used for the degraded of the organic pollutions such as dyestuff, to containing Reactive Red K-2BP, X-3B or the azogeramine that concentration is 0.01-0.5g/L, Acid Orange II etc., pH adds heterogeneous class Fenton catalyst and hydrogen peroxide in the waste water from dyestuff of 2-10, under being 20-90 ℃, temperature stirs 5-40min, wherein the addition of heterogeneous class Fenton catalyst is 0.5-10g/L, and the addition of hydrogen peroxide is 2-50mmol/L.
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