CN103831108A - Copper ferrite-loaded activated carbon fiber, preparation method and application of fiber, and method for degrading activated azo dye wastewater - Google Patents
Copper ferrite-loaded activated carbon fiber, preparation method and application of fiber, and method for degrading activated azo dye wastewater Download PDFInfo
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Abstract
The invention discloses a copper ferrite-loaded activated carbon fiber, a preparation method and an application of the fiber, and a method for degrading activated azo dye wastewater, belongs to the field of wastewater treatment, and discloses a method for preparing a microwave catalyst for the copper ferrite-loaded activated carbon fiber. The method comprises the following steps: adding copper nitrate and ferric nitrate into water; adding citric acid, and heating to form sol; adding a pretreated activated carbon fiber felt; heating for evaporating a solvent; and roasting under the protection of nitrogen. The method for degrading the activated azo dye wastewater through microwave catalytic oxidation by using the copper ferrite-loaded activated carbon fiber which is prepared by adopting the method comprises the following steps: decontaminating the wastewater through a grid, standing, precipitating, adding supernatant liquid into a reactor, adding the catalyst and a small amount of H2O2, and performing radiation in a microwave oven, so that the dye wastewater is degraded. According to the adopted catalyst, the situation of easiness in loss of a conventional powder catalyst in the treatment process is avoided, and the catalyst can be used repeatedly and continuously, has the cost-saving effect, and is short in treatment time and high in degradation efficiency.
Description
Technical field
The invention belongs to field of waste water treatment, more particularly, relate to the method for NACF of a kind of load coppe ferrite and preparation method thereof, application and degrading activity azo dye wastewater.
Background technology
Along with dyestuff chemistry industrial expansion, synthetic dyestuffs are widely used in the industries such as weaving, leather, food, daily-use chemical industry.China is DYE PRODUCTION big country at present, and within 2010, dyestuff output has reached 75.6 ten thousand
t, account for 60% of world's dyestuff.In artificial synthetic dyestuff, more than approximately 50% be azo dyes, in addition azo dyes is fabric clothing most widely used class synthetic dyestuffs in dyeing and printing process, for dyeing and the stamp of multiple natural and synthetic fibers, also for painting, plastics, rubber etc. painted.Due under aerobic conditions, azo dyes be difficult for decomposing and long-term existence in environment, the aromatic amine under anaerobic easily being decomposed by micro-reduction Cheng Gengnan, thus cause that this type of COD value of waste water is very high, colourity is large, stable and difficult degradation.Therefore, azo dye wastewater must effectively be processed.
At present, the processing method of azo dye wastewater mainly contains bioanalysis, Physical and chemical method.And bioanalysis comprises that the anaerobic technique processing time is long, and be difficult to reduce its toxicity, cause the product that much toxicity is larger.Physical method comprises electrocoagulation, absorption method, membrane separation process and flocculence, often bad adaptability of these physical methods, in addition the pollutant that is adsorbed or is retained down, also have other additives because not only comprising dyestuff, dyestuff is difficult to recycle, solid after treatment is also needed to after-treatment, increased processing procedure and expense.Chemical method is as photocatalytic degradation, Ozonation, although do not bring secondary pollution, the processing time is long, and cost is higher.Microwave irradiation technology has become one of focus that numerous environmentalists pay close attention in recent years, due to its fast, advantage efficient and non-secondary pollution enjoys researchers' favor.Under microwave, microwave energy is acted on catalyst or its carrier Induced catalytic reaction occurs, add a small amount of H
2o
2as oxidant, degrading waste water quickly, but also do not have theory to show that it can apply at reactive azo dyes waste water.
NACF is the new and effective sorbing material that development in recent years is got up; and because it is compared grain active carbon and has larger specific area and have a large amount of micropores; and there is acid and alkali-resistance, corrosion resistant characteristic; therefore the carrier of a lot of catalyst of conduct; add that it can be made into the different shapes such as felt, cloth, paper, has become the environment-friendly engineering material of extensive use.In addition, NACF belongs to carbonaceous material, therefore has very strong microwave absorbing property, has been used as in the Study on degradation of microwave inducing catalyst for water waste water from dyestuff.Once but adsorb saturatedly, after desorption, easily produce secondary pollution, and can not reuse.
As the one of Ferrite Material, coppe ferrite has good microwave absorbing property and magnetic performance.At H
2o
2there is the lower Fenton-like reagent that forms, through the irradiation of microwave, can produce the hydroxyl radical free radical of strong oxidability, can accelerate the azo bond fracture in azo dye wastewater, thus fast degradation waste water.This laboratory is using coppe ferrite as catalyst, study its catalytic oxidation waste water from dyestuff (Hongzhe Chen under microwave condition, Shaogui Yang, Jiao Chang, Kai Yu, Dongfang Li, Cheng Sun, Aimin Li, Efficient degradation of crystal violet in magnetic CuFe2O4aqueous solution coupled with microwave radiation, Chemosphere, 89(2), 185 – 189), but the coppe ferrite powder of nanometer particle size easily runs off in processing engineering, also cause the obstruction of reactor, little easily recovery, therefore be difficult in actual applications promote.
Summary of the invention
1. the technical problem that will solve
The catalyst used for existing processing reactive azo dyes waste water easily runs off in course of reaction, the slow-footed problem of degradation of dye waste water, the invention provides the method for NACF of a kind of load coppe ferrite and preparation method thereof, application and degrading activity azo dye wastewater, and efficient fast degradation waste water from dyestuff.
2. technical scheme
In order to overcome the above problems, the concrete technical scheme that the present invention adopts is as follows:
A preparation method for the NACF of load coppe ferrite, the steps include:
(1) copper nitrate and the ferric nitrate that are 3:10 by mass ratio are dissolved in the water, and under 50-70 ℃ of water bath condition, stir;
(2) in the solution of step (1), add citric acid as complexing agent, be warming up to 70-90 ℃, continue to stir to form colloidal sol;
(3) active carbon fiber felt is cut into small pieces, in deionized water, boils 1-2 hour, to remove volatile materials wherein, then in baking oven, dry;
(4) charcoal fibrofelt after treatment in step (3) be impregnated in the colloidal sol obtaining in step (2), be then warming up to 90-100 ℃; With evaporating solvent;
(5) charcoal fibrofelt after treatment step (4) is placed in constant temperature blast drying oven and is dried, obtain the charcoal fiber of load coppe ferrite;
(6) the charcoal fiber of step (5) load coppe ferrite after treatment is calcined to 2-3 hour under tube furnace in nitrogen atmosphere, can obtain the NACF of load coppe ferrite.
Preferably, mixing time in described step (1) is 2h, citric acid and the ferric nitrate mol ratio of in step (2), adding are that 1:3.5 is to 1:5.5, mixing time in step (2) is 2h, to guarantee that copper nitrate solution and iron nitrate solution are uniformly dispersed, and form stable vitreosol system in solution.
Preferably, in described step (3), NACF is viscose-based active carbon fiber felt, and it has certain toughness, Heat stability is good; The square that is shaped as 100mm*100mm of described fritter, makes it fully contact with the colloidal sol forming, and the temperature of baking oven is 120 ℃, and drying time is fully to dry with assurance gel for 24 hours.
Preferably, in described step (4), the mass ratio of the metal ion in charcoal fibrofelt and colloidal sol is 5:1.
Preferably, the oven dry of described step (5) is to process and within 12 hours, make pretreated charcoal fibrofelt keep dry in temperature is the constant temperature blast drying oven of 120 ℃.
Preferably, in described step (6), the nitrogen flow of calcining is 100mL/min, the heating rate of calcining is 3 ℃/min, not oxidized to guarantee NACF, temperature is raised to after 500 ℃ of target temperatures, calcining at constant temperature is able to the content that coppe ferrite has good crystal formation and can reduce the copper that coppe ferrite reduced by NACF, makes coppe ferrite purity higher.
The NACF of load coppe ferrite prepared by the preparation method of the NACF of above load coppe ferrite.
The application of the NACF of load coppe ferrite in degrading activity azo dye wastewater.
A method that adopts the NACF microwave catalysis oxidation degrading activity azo dye wastewater of load coppe ferrite, the steps include:
(a) reactive azo dyes waste water is passed through, after grid removal of impurities natural subsidence, get its supernatant liquor;
(b) step (a) gained supernatant liquor is introduced in reactor, added activated carbon fiber-loaded coppe ferrite, be placed in microwave reaction cavity and carry out irradiation, and to add mass fraction be 30% H
2o
2, there is catalytic oxidation.
Preferably, in step (b), the power of microwave is 400-800W.
3. beneficial effect
Than prior art, beneficial effect of the present invention is:
(1) the fiber-loaded coppe ferrite cost of material activity charcoal of the present invention is low, can repeatedly use, and has avoided its loss in use and the obstruction to reactor than fine catalyst, is easy to industrialization and uses.
(2) material feedstock of the present invention is easy to get, and owing to being block, after reaction, easily reclaims.
(3) the present invention is because active carbon fibre peacekeeping coppe ferrite is all absorbing material, therefore can be to waste water fast degradation, non-secondary pollution in the short time in Microwave system.
(4) material applied range of the present invention, except waste water from dyestuff being had obvious decolorizing effect, also has very large removal effect to the COD of waste water from dyestuff.
(5) power of microwave of the present invention is 400-800W, and microwave is domestic microwave, and practical and workable, energy consumption is lower.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of the activated carbon fiber-loaded coppe ferrite composite of the embodiment of the present invention 1 gained.
Fig. 2 is the scanning electron microscope (SEM) photograph of the activated carbon fiber-loaded coppe ferrite composite of the embodiment of the present invention 1 gained.
Fig. 3 is the absorbance curve over time of the active yellow K-RN simulation reactive azo dyes waste water of preparation in embodiment 1.
Fig. 4 is the concentration curve over time of the active yellow K-RN simulation reactive azo dyes waste water of preparation in embodiment 1.
Fig. 5 is the concentration curve over time of the reactive brilliant red x-3b simulation reactive azo dyes waste water of preparation in embodiment 2.
Fig. 6 is the concentration curve over time of the activity palm fibre 2 simulation reactive azo dyes waste water of preparation in embodiment 6.
Fig. 7 is the high concentration reactive azo dyes waste water COD curve over time of Jiangsu Jihua Chemical Co., Ltd. in embodiment 8.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A preparation method for the NACF of load coppe ferrite, the steps include:
(1) by 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, obtain green solution stir 2 hours under 55 ℃ of water bath condition after;
(2) in the solution of step (1), add citric acid as complexing agent, the citric acid of interpolation and ferric nitrate mol ratio are 1:4.5, are warming up to 75 ℃, continue to stir 2 hours to form colloidal sol;
(3) active carbon fiber felt is cut into the square tiles of 100mm*100mm, boils 1 hour in deionized water, to remove volatile materials wherein, then in baking oven, dry, the temperature of baking oven is 120 ℃, and drying time is 24 hours;
(4) charcoal fibrofelt after treatment in 4.4g step (3) be impregnated in the colloidal sol obtaining in step (2), be then warming up to 90 ℃; With evaporating solvent;
(5) charcoal fibrofelt after treatment step (4) being placed on to temperature is to process 12 hours in the constant temperature blast drying oven of 120 ℃, obtains the charcoal fiber of load coppe ferrite;
(6) the charcoal fiber of step (5) load coppe ferrite after treatment is calcined under tube furnace 2 hours in nitrogen atmosphere, the nitrogen flow of calcining is 100mL/min, the heating rate of calcining is 3 ℃/min, temperature is raised to after 500 ℃ of target temperatures, calcining at constant temperature, can obtain the NACF of load coppe ferrite, its XRD collection of illustrative plates and scanning electron microscope (SEM) photograph are as depicted in figs. 1 and 2.
Take the NACF of the load coppe ferrite that 0.1g prepared in round-bottomed flask, the H that the active yellow K-RN simulation reactive azo dyes waste water that to join concentration that 100mL prepares be in advance 100mg/L and 0.1mL mass fraction are 30%
2o
2, under the microwave power of 800W, react after 7min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 90.5%, specifically referring to Fig. 3 and Fig. 4.In the 7min of reaction, the absorbance of strong absworption peak declines rapidly as shown in the figure, and percent of decolourization also improves constantly.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir 2 hours under 60 ℃ of water-baths after, obtain green solution, in the solution of step (1), add citric acid as complexing agent, citric acid and the ferric nitrate mol ratio of adding are 1:3.5, be warming up to 80 ℃, continue to stir 2 hours formation colloidal sol, add that after pretreatment, (pretreatment of the present embodiment and below embodiment is all identical with embodiment 1, repeat no more) felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 95 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 3 hours, obtain catalyst.Take catalyst that 0.2g prepared in round-bottomed flask, the reactive brilliant red x-3b simulation reactive azo dyes waste water that the 100mL concentration that joins preparation is 100mg/L and the H of 0.3mL
2o
2, under the microwave power of 800W, react after 9min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 84.6%, specifically referring to Fig. 5.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 200ml water, stir 2 hours under 65 ℃ of water-baths after, obtain green solution, add citric acid, citric acid and the ferric nitrate mol ratio of adding are 1:4, be warming up to 85 ℃, continue to stir and form colloidal sol in 2 hours, add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 100 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 3 hours, obtain catalyst.Take catalyst that 0.1g prepared in round-bottomed flask, in the activity palm fibre 2 simulation reactive azo dyes waste water that the 100mL concentration that joins preparation is 50mg/L, and add the H that 0.1mL mass fraction is 30%
2o
2, under the microwave power of 600W, react after 7min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 88.6%.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir two hours under 60 ℃ of water-baths after, obtain green solution, citric acid and the ferric nitrate mol ratio of adding are 1:5, be warming up to 80 ℃, continue to stir 2 hours formation colloidal sol, add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 95 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 2 hours, obtain catalyst.Take catalyst that 0.1g prepared in round-bottomed flask, in the active yellow K-RN simulation reactive azo dyes waste water that the 100mL concentration that joins preparation is 20mg/L, and add the H that 0.1mL mass fraction is 30%
2o
2, under the microwave power of 400W, react after 7min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 86.4%.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir two hours under 50 ℃ of water-baths after, obtain green solution, citric acid and the ferric nitrate mol ratio of adding are 1:5.5, be warming up to 70 ℃, continue to stir 2 hours formation colloidal sol, add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 90 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 2 hours, obtain catalyst.Take catalyst that 0.2g prepared in round-bottomed flask, in the activity palm fibre 2 simulation reactive azo dyes waste water that the 100mL concentration that joins preparation is 100mg/L, and add the H that 0.4mL mass fraction is 30%
2o
2, under the microwave power of 800W, react after 10min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 85.5%.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir two hours under 60 ℃ of water-baths after, obtain green solution, citric acid and the ferric nitrate mol ratio of adding are 1:5.3, are warming up to 90 ℃, continue to stir 2 hours formation colloidal sol, viscose based active carbon fiber felt is cut into 100mm*100mm fritter, in deionized water, boil 1 hour, to remove volatile materials wherein, then in baking oven, dry, the temperature of baking oven is 120 ℃, and drying time is 24 hours.Add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 90 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 2 hours, obtain catalyst, the nitrogen flow of calcining is 100mL/min, and the heating rate of calcining is 3 ℃/min, and temperature is raised to after 500 ℃ of target temperatures, calcining at constant temperature.Take catalyst that 0.1g prepared in round-bottomed flask, in the activity palm fibre 2 simulation reactive azo dyes waste water that the 100mL concentration that joins preparation is 20mg/L, and add the H that 0.1mL mass fraction is 30%
2o
2, under the microwave power of 800W, react after 5min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 90.9%, specifically referring to Fig. 6.
In embodiment 2-6, the pretreatment of felt shape NACF is all that viscose based active carbon fiber felt is cut into 100mm*100mm fritter, in deionized water, boil 2 hours, to remove volatile materials wherein, then in baking oven, dry, the temperature of baking oven is 120 ℃, and drying time is 24 hours.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir two hours under 60 ℃ of water-baths after, obtain green solution, citric acid and the ferric nitrate mol ratio of adding are 1:5.2, are warming up to 80 ℃, continue to stir 2 hours formation colloidal sol, viscose based active carbon fiber felt is cut into 100mm*100mm fritter, in deionized water, boil 1.5 hours, to remove volatile materials wherein, then in baking oven, dry, the temperature of baking oven is 120 ℃, and drying time is 24 hours.Add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 90 ℃ of evaporating solvents.In tube furnace, under nitrogen protection, calcine and within 3 hours, obtain catalyst, the nitrogen flow of calcining is 100mL/min, and the heating rate of calcining is 3 ℃/min, and temperature is raised to after 500 ℃ of target temperatures, calcining at constant temperature.Take catalyst that 0.1g prepared in round-bottomed flask, in the reactive brilliant red x-3b simulation reactive azo dyes waste water that the 100mL concentration that adds preparation is 50mg/L, and add the H that 0.1mL mass fraction is 30%
2o
2, under the microwave power of 600W, react after 7min, by its absorbance of ultraviolet-visible luminosity instrumentation, calculating its degradation rate is 83.2%.
Take 2.42g copper nitrate and 8.07g ferric nitrate in 100ml water, stir two hours under 60 ℃ of water-baths after, obtain green solution, citric acid and the ferric nitrate mol ratio of adding are 1:5.5, are warming up to 80 ℃, continue to stir 2 hours formation colloidal sol, viscose based active carbon fiber felt is cut into 100mm*100mm fritter, in deionized water, boil 1.5 hours, to remove volatile materials wherein, then in baking oven, dry, the temperature of baking oven is 120 ℃, and drying time is 24 hours.Add pretreated felt shape NACF 7.04g, in 120 ℃ of baking ovens, dry 12 hours after being warming up to 90 ℃ of evaporating solvents.In tube furnace, calcine and within 2.5 hours, obtain catalyst under nitrogen protection, calcination condition is with embodiment 1.Take catalyst that 0.1g prepared in round-bottomed flask, join in the high concentration reactive azo dyes waste water of 100mL Jiangsu Jihua Chemical Co., Ltd., and add the H that 0.1mL mass fraction is 30%
2o
2, under the microwave power of 800W, react after 15min, calculate COD by National Standard Method and be reduced to 910mg/L from initial 1800mg/L, as shown in Figure 7.
Claims (10)
1. a preparation method for the NACF of load coppe ferrite, the steps include:
(1) copper nitrate and the ferric nitrate that are 3:10 by mass ratio are dissolved in the water, and under 50-70 ℃ of water bath condition, stir;
(2) in the solution of step (1), add citric acid as complexing agent, be warming up to 70-90 ℃, continue to stir to form colloidal sol;
(3) active carbon fiber felt is cut into small pieces, in deionized water, boils 1-2 hour, then in baking oven, dry;
(4) charcoal fibrofelt after treatment in step (3) be impregnated in the colloidal sol obtaining in step (2), be then warming up to 90-100 ℃;
(5) charcoal fibrofelt after treatment step (4) is placed in constant temperature blast drying oven and is dried, obtain the charcoal fiber of load coppe ferrite;
(6) the charcoal fiber of step (5) load coppe ferrite after treatment is calcined to 2-3 hour under tube furnace in nitrogen atmosphere, can obtain the NACF of load coppe ferrite.
2. the preparation method of the NACF of a kind of load coppe ferrite according to claim 1, it is characterized in that: the mixing time in described step (1) is 2h, the citric acid adding in step (2) and ferric nitrate mol ratio be 1:3.5 to 1:5.5, the mixing time in step (2) is 2h.
3. the preparation method of the NACF of a kind of load coppe ferrite according to claim 1, is characterized in that: in described step (3), NACF is viscose-based active carbon fiber felt; The square that is shaped as 100mm*100mm of described fritter, the temperature of baking oven is 120 ℃, drying time is 24 hours.
4. the preparation method of the NACF of a kind of load coppe ferrite according to claim 1, is characterized in that: the mass ratio of the metal ion in described step (4) in charcoal fibrofelt and colloidal sol is 5:1.
5. the preparation method of the NACF of a kind of load coppe ferrite according to claim 1, is characterized in that: the oven dry of described step (5) is to process 12 hours in temperature is the constant temperature blast drying oven of 120 ℃.
6. according to the preparation method of the NACF of a kind of load coppe ferrite described in any one in claim 1-5, it is characterized in that: in described step (6), the nitrogen flow of calcining is 100mL/min, the heating rate of calcining is 3 ℃/min, temperature is raised to after 500 ℃ of target temperatures, calcining at constant temperature.
7. the NACF of the load coppe ferrite of preparing in the method for claim 1-6.
8. the application of the NACF of load coppe ferrite claimed in claim 7 in degrading activity azo dye wastewater.
9. a method that adopts the NACF microwave catalysis oxidation degrading activity azo dye wastewater of load coppe ferrite, the steps include:
(a) reactive azo dyes waste water is passed through, after grid removal of impurities natural subsidence, get its supernatant liquor;
(b) step (a) gained supernatant liquor is introduced in reactor, added the NACF of load coppe ferrite, be placed in microwave reaction cavity and carry out irradiation, and add H
2o
2, there is catalytic oxidation.
10. the method for a kind of NACF microwave catalysis oxidation degrading activity azo dye wastewater that adopts load coppe ferrite according to claim 9, is characterized in that: in described step (b), the power of microwave is 400-800W.
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