CN103861629A - Catalyst for degrading organic waste water in microwave-assisted way as well as preparation method and application of catalyst - Google Patents
Catalyst for degrading organic waste water in microwave-assisted way as well as preparation method and application of catalyst Download PDFInfo
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Abstract
The invention discloses a catalyst for degrading organic waste water in a microwave-assisted way as well as a preparation method and the application of the catalyst. The catalyst is silicon carbide section loaded with a metal compound, the metal compound is compound of Cu, Fe, Mn, Ni or Co, the silicon carbide section is a carbon-silicon rod, a carbon-silicon tube or a carbon-silicon plate. The preparation method of the catalyst comprises the following steps of (1) pretreatment: putting the silicon carbide section into a nitric acid solution with the mass fraction of 1-5%, and carrying out ultrasonic treatment for 30-60 minutes; taking out the silicon carbide section, washing by deionized water and drying; (2) putting the pretreated silicon carbide section into a metal salt solution with the concentration of 0.1-1mol/ L, taking out the silicon carbide section after 10-24 hours, washing by the deionized water, and heating and drying for 8-12 hours at the temperature of 80-300 DEG C to obtain the catalyst which is the silicon carbide section loaded with the metal compound. The catalyst can be used for rapidly and effectively degrading organic pollutant in the waste water, and is low in cost, stable in performance, convenient to recover and reusable; the method is simple and easy to operate; therefore, the catalyst is wide in application scope, suitable for various degradation-resistant organic waste water and free from secondary pollution.
Description
Technical field
The invention belongs to technical field of waste water processing, more specifically, relate to a kind of microwave assistant degradation organic wastewater Catalysts and its preparation method and application.
Background technology
The industries such as papermaking, dyestuff, organic synthesis, plating all can produce a large amount of organic wastewater with difficult degradation thereby, the features such as they have that complicated component, stability are strong, hard degradation, biodegradability are poor, certainly will cause serious harm to the ecosystem and human health in entered environment.Therefore, very necessity of new method of this class waste water can be efficiently processed in research.At present, process organic wastewater and mainly adopt the GC-MS between Physical, chemical method, bioanalysis and three, although these methods can make COD (the Chemical Oxygen Demand of waste water, COD) significantly reduce, but cannot thoroughly process the organic matter of hard degradation in waste water, be necessary so find a kind of new technology efficiently.
Micro ware auxiliary catalysis oxidation technology is a kind of novel wastewater processing technology.Heating using microwave have speed fast, without after reaction, without advantages such as thermogrades.The treatment effeciency that microwave and other oxidation technology couplings can be improved to organic wastewater with difficult degradation thereby adds some Microwave Senstizer and more can accelerate the processing speed of waste water in processing.The employing MW-Cu/GAC combined degradation organic matters such as L.L.Bo are obtained good effect (Journal of Hazardous Materials.153 (2008) 1201 – 1206).Publication number is a kind of method that the Chinese invention patent application of CN102923811B discloses microwave cooperating perovskite catalytic degradation high concentrated organic wastewater, utilizes citric acid complex method to prepare the La of cerium doping
1-xce
xbO
3perovskite, as catalyst, is realized organic degraded under the synergy of microwave.The Microwave Senstizer material adopting in these methods is mostly powder or graininess, is difficult to reclaim, and can not recycle.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of microwave assistant degradation organic wastewater Catalysts and its preparation method and application, on carborundum section bar carried metal compound as catalyst, the fast and effeciently organic pollution in degrading waste water, catalyst cost is low, stable performance, is convenient to reclaim, and can recycle, method is simple to operation, applied range, is applicable to various organic wastewater with difficult degradation thereby, non-secondary pollution.
For achieving the above object, according to one aspect of the present invention, a kind of microwave assistant degradation organic wastewater catalyst is provided, it is characterized in that, described catalyst is the carborundum section bar of carried metal compound, wherein, described metallic compound is the compound of Cu, Fe, Mn, Ni or Co, and described carborundum section bar is globar, carbon silicone tube or carbon silicon plate.
Preferably, described metallic compound is basic copper nitrate, and in every kilogram of described catalyst, the content of copper is 8000mg.
According to another aspect of the present invention, the preparation method of a kind of microwave assistant degradation organic wastewater catalyst is provided, it is characterized in that, comprise the steps: (1) pretreatment: it is 1%～5% the ultrasonic 30～60min of salpeter solution that carborundum section bar is put into mass fraction, take out carborundum section bar, with dry after washed with de-ionized water; (2) pretreated carborundum section bar is put into the metal salt solution that concentration is 0.1～1mol/L, after 10～24h, takes out, with after washed with de-ionized water at 80～300 ℃ heat dry 8～12h, obtain carborundum section bar carried metal compound catalyst.
Preferably, described carborundum section bar is globar, carbon silicone tube or carbon silicon plate.
Preferably, described metal salt solution is the salting liquid of Cu, Fe, Mn, Ni or Co.
According to another aspect of the present invention, a kind of method of microwave assistant degradation organic wastewater is provided, it is characterized in that, in organic wastewater, add the catalyst of preparing with said method, be 1～4:1 by the mol ratio of oxidant and waste water COD, in organic wastewater, add oxidant, regulate pH value of waste water to 6～8, with the microwave irradiation processing of 300～700W, realize the degraded of organic wastewater.
Preferably, the mass volume ratio of described catalyst and organic wastewater is 50～140:1g/L.
Preferably, described oxidant is hydrogen peroxide, persulfate or oxygen.
In general, the above technical scheme of conceiving by the present invention compared with prior art, has following beneficial effect:
1, carried metal compound on carborundum section bar, has good microwave absorbing property and catalytic activity, in microwave assisted oxidation degradation of organic waste water system, can catalysis produce active oxidation species (as OH and SO
4 2-), the fast and effeciently organic pollution in degrading waste water.
2, catalyst cost is low, and stable performance is convenient to reclaim, and can recycle.
3, method is simple to operation, and reaction speed is fast, and applied range is applicable to various organic wastewater with difficult degradation thereby, non-secondary pollution.
Accompanying drawing explanation
Fig. 1 is the XRF characterization result of the catalyst of the embodiment of the present invention 1;
Fig. 2 is the XRD characterization result of the catalyst of the embodiment of the present invention 1;
Fig. 3 is that the wastewater through organic matter content of the embodiment of the present invention 1 is with the change curve of exposure time;
Fig. 4 is that the wastewater through organic matter clearance of the embodiment of the present invention 4 is with the change curve of exposure time;
Fig. 5 is that the waste water COD degradation rate of the embodiment of the present invention 5 is with the change curve of exposure time.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
Carbofrax material, comprise the difform moulding carbofrax materials such as globar, carbon silicone tube, carbon silicon plate, it is a kind of non-oxide ceramic material of function admirable, there is the advantages such as density is low, hardness is high, wear-resisting, heat-resisting, corrosion-resistant, with low cost, and have good heat conduction, conductive capability and good microwave absorbing property.The present invention, using carbofrax material as catalyst carrier, has the metallic compound of catalytic performance at its area load, form the composite catalyzing agent material with high catalytic activity, heat endurance and microwave sensitization.Under microwave irradiation, can there is electronics and shift in this catalyst, make metal obtain electronics between metal and carborundum, catalytic oxidant produces active specy, oxidation of organic compounds, and also oxidation reaction mainly occurs in solution, the reaction of catalyst surface free-radical oxidation, has important booster action.This composite catalyzing agent material for micro ware auxiliary catalysis degradation of organic waste water, can be significantly improved to the degradation effect to waste water, and catalyst is easy to reclaim, reusable, can greatly promote the engineering application of micro ware auxiliary catalysis oxidized organic wastewater.
The method of the microwave assistant degradation organic wastewater of the embodiment of the present invention comprises the steps:
(1) prepare carborundum section bar carried metal compound catalyst, further comprise the steps:
(1-1) pretreatment: it is 1%～5% the ultrasonic 30～60min of salpeter solution that carborundum section bar is put into mass fraction, removes surface impurity, takes out carborundum section bar, with dry after washed with de-ionized water.Carborundum section bar is difform moulding carborundum, is specially globar, carbon silicone tube or carbon silicon plate.
(1-2) pretreated carborundum section bar is put into the metal salt solution that concentration is 0.1～1mol/L, after 10～24h, takes out, with after washed with de-ionized water at 80～300 ℃ heat dry 8～12h, obtain carborundum section bar carried metal compound catalyst.Wherein, metal salt solution is specially the salting liquid of Cu, Fe, Mn, Ni or Co etc.
(2) press the mass volume ratio 50～140:1g/L of catalyst and organic wastewater, in organic wastewater, add catalyst, be 1～4:1 by the mol ratio of oxidant and waste water COD, in organic wastewater, add oxidant, regulate pH value of waste water to 6～8, with the microwave irradiation processing of 300～700W, realize the degraded of organic wastewater.Wherein, oxidant is hydrogen peroxide, persulfate or oxygen.
For making those skilled in the art understand better the present invention, below in conjunction with specific embodiment, the method for microwave assistant degradation organic wastewater of the present invention is elaborated.
The method of microwave assistant degradation organic wastewater comprises the steps:
(1) carbon silicone tube supported copper compound catalyst, further comprises the steps:
(1-1) pretreatment: it is 1% the ultrasonic 30min of salpeter solution that carbon silicone tube is put into mass fraction, takes out carbon silicone tube, with dry after washed with de-ionized water.
(1-2) pretreated carbon silicone tube is put into the copper nitrate solution that concentration is 0.5mol/L, after 12h, takes out, with after washed with de-ionized water at 80 ℃ heat dry 8h, obtain carbon silicone tube supported copper compound catalyst.
The XRF of this catalyst and XRD characterization result are respectively as depicted in figs. 1 and 2.Known by the XRF analysis to copper, before and after load, the content of copper has significant difference, copper content 30mg/kg left and right before load, copper content 8000mg/kg left and right after load, can find out that carborundum tube is very large to the load capacity of copper before and after contrast load; Can be found out by XRD figure, roasting at 80 ℃, copper mainly exists with basic copper nitrate.
(2) (mass volume ratio of catalyst and organic wastewater is 50:1g/L in the phenolsulfonic acid simulated wastewater that is 50mg/L to 100mL concentration, to add the hydrogenperoxide steam generator that 5g catalyst and 0.04mL mass fraction are 30%, the mol ratio of hydrogen peroxide and waste water COD is 1:1), regulate pH value of waste water to 6, with the microwave irradiation processing of 700W, realize the degraded of organic wastewater.
As shown in Figure 3, after irradiation 4min, the clearance of phenolsulfonic acid reaches more than 90%, and after 6min, clearance can reach more than 95%, after 8min, can reach 100%.
The method of microwave assistant degradation organic wastewater comprises the steps:
(1) prepare globar supported copper compound catalyst, further comprise the steps:
(1-1) pretreatment: it is 5% the ultrasonic 40min of salpeter solution that globar is put into mass fraction, takes out globar, with dry after washed with de-ionized water.
(1-2) pretreated globar is put into the copper nitrate solution that concentration is 0.1mol/L, after 10h, is taken out, with after washed with de-ionized water at 100 ℃ heat dry 10h, obtain globar supported copper compound catalyst.
(2) (mass volume ratio of catalyst and organic wastewater is 70:1g/L in the phenol synthetic water that is 50mg/L to 100mL concentration, to add 7g catalyst and 0.05g persulfate, the mol ratio of persulfate and waste water COD is 1:1), regulate pH value of waste water to 7, with the microwave irradiation processing of 300W, realize the degraded of organic wastewater.
Result shows, after irradiation 10min, the clearance of phenol can reach 99.97%.
The method of microwave assistant degradation organic wastewater comprises the steps:
(1) prepare carbon silicone tube supported copper compound catalyst, further comprise the steps:
(1-1) pretreatment: it is 3% the ultrasonic 60min of salpeter solution that carbon silicone tube is put into mass fraction, takes out carbon silicone tube, with dry after washed with de-ionized water.
(1-2) pretreated carbon silicone tube is put into the copper nitrate solution that concentration is 1mol/L, after 24h, takes out, with after washed with de-ionized water at 300 ℃ heat dry 12h, obtain carbon silicone tube supported copper compound catalyst.
(2) (mass volume ratio of catalyst and organic wastewater is 70:1g/L in the phenolsulfonic acid simulated wastewater that is 50mg/L to 100mL concentration, to add the hydrogenperoxide steam generator that 7g catalyst and 0.08mL mass fraction are 30%, the mol ratio of hydrogen peroxide and waste water COD is 2:1), regulate pH value of waste water to 7, with the microwave irradiation processing of 700W, realize the degraded of organic wastewater.
Result shows, after irradiation 6min, the clearance of phenolsulfonic acid can reach more than 95%.
The method of microwave assistant degradation organic wastewater comprises the steps:
(1) prepare carbon silicone tube supported copper compound catalyst, further comprise the steps:
(1-1) pretreatment: it is 5% the ultrasonic 40min of salpeter solution that carbon silicone tube is put into mass fraction, takes out carbon silicone tube, with dry after washed with de-ionized water.
(1-2) pretreated carbon silicone tube is put into the copper nitrate solution that concentration is 1mol/L, after 24h, takes out, with after washed with de-ionized water at 300 ℃ heat dry 12h, obtain carbon silicone tube supported copper compound catalyst.
(2) (mass volume ratio of catalyst and organic wastewater is 70:1g/L in the phenol synthetic water that is 50mg/L to 100mL concentration, to add the hydrogenperoxide steam generator that 7g catalyst and 0.08mL mass fraction are 30%, the mol ratio of hydrogen peroxide and waste water COD is 2:1), regulate pH value of waste water to 8, with the microwave irradiation processing of 700W, realize the degraded of organic wastewater.
As shown in Figure 4, after irradiation 2min, the clearance of phenol can reach more than 90%, and after 2.5min, clearance can reach more than 95%.
Embodiment 5
The method of microwave assistant degradation organic wastewater comprises the steps:
(1) prepare carbon silicone tube supported copper compound catalyst, further comprise the steps:
(1-1) pretreatment: it is 5% the ultrasonic 30min of salpeter solution that carbon silicone tube is put into mass fraction, takes out carbon silicone tube, with dry after washed with de-ionized water.
(1-2) pretreated carbon silicone tube is put into the copper nitrate solution that concentration is 0.5mol/L, after 12h, takes out, with after washed with de-ionized water at 80 ℃ heat dry 12h, obtain carbon silicone tube supported copper compound catalyst.
(2) (mass volume ratio of catalyst and organic wastewater is 140:1g/L in the simulated wastewater containing phenol and phenolsulfonic acid (concentration is respectively 1500mg/L and 3000mg/L), to add the hydrogenperoxide steam generator that 14g catalyst and 4.8mL mass fraction are 30% to 100mL, the mol ratio of hydrogen peroxide and waste water COD is 4:1), regulate pH value of waste water to 7, with the microwave irradiation processing of 700W, realize the degraded of organic wastewater.
As shown in Figure 5, after irradiation 20min, COD degradation rate reaches more than 96%, and COD reduces to 223mg/L, and total organic carbon (Total Organic Carbon, TOC) is surplus 27.67mg/L only.
The time that organic wastewater that existing method of wastewater treatment is degraded identical needs will be considerably beyond 4min, and clearance is difficult to reach more than 95.Testing result in conjunction with above-described embodiment is known, and the method for microwave assistant degradation organic wastewater of the present invention all has overwhelming superiority on processing time and treatment effect, fast and effeciently the organic pollution in degrading waste water.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a microwave assistant degradation organic wastewater catalyst, it is characterized in that, described catalyst is the carborundum section bar of carried metal compound, wherein, described metallic compound is the compound of Cu, Fe, Mn, Ni or Co, and described carborundum section bar is globar, carbon silicone tube or carbon silicon plate.
2. microwave assistant degradation organic wastewater catalyst as claimed in claim 1, is characterized in that, described metallic compound is basic copper nitrate, and in every kilogram of described catalyst, the content of copper is 8000mg.
3. a preparation method for catalyst for microwave assistant degradation organic wastewater, is characterized in that, comprises the steps:
(1) pretreatment: it is 1%～5% the ultrasonic 30～60min of salpeter solution that carborundum section bar is put into mass fraction, takes out carborundum section bar, with dry after washed with de-ionized water;
(2) pretreated carborundum section bar is put into the metal salt solution that concentration is 0.1～1mol/L, after 10～24h, takes out, with after washed with de-ionized water at 80～300 ℃ heat dry 8～12h, obtain carborundum section bar carried metal compound catalyst.
4. the preparation method of catalyst for microwave assistant degradation organic wastewater as claimed in claim 3, is characterized in that, described carborundum section bar is globar, carbon silicone tube or carbon silicon plate.
5. the preparation method of catalyst for the microwave assistant degradation organic wastewater as described in claim 3 or 4, is characterized in that, described metal salt solution is the salting liquid of Cu, Fe, Mn, Ni or Co.
6. the method for a microwave assistant degradation organic wastewater, it is characterized in that, in organic wastewater, add the catalyst of preparing by the method described in any one in claim 3 to 5, be 1～4:1 by the mol ratio of oxidant and waste water COD, in organic wastewater, add oxidant, regulate pH value of waste water to 6～8, with the microwave irradiation processing of 300～700W, realize the degraded of organic wastewater.
7. the method for microwave assistant degradation organic wastewater as claimed in claim 6, is characterized in that, the mass volume ratio of described catalyst and organic wastewater is 50～140:1g/L.
8. the method for the microwave assistant degradation organic wastewater as described in claim 6 or 7, is characterized in that, described oxidant is hydrogen peroxide, persulfate or oxygen.
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