CN101372368A - Method for microwave induced catalytic degradation of triphenyl methane dye waste water - Google Patents
Method for microwave induced catalytic degradation of triphenyl methane dye waste water Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 26
- 230000003197 catalytic effect Effects 0.000 title claims description 22
- 230000015556 catabolic process Effects 0.000 title claims description 18
- 238000006731 degradation reaction Methods 0.000 title claims description 18
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 57
- 239000003054 catalyst Substances 0.000 claims abstract description 10
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- 238000005273 aeration Methods 0.000 claims description 12
- 230000006698 induction Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims 2
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- 239000002351 wastewater Substances 0.000 abstract description 15
- 238000006555 catalytic reaction Methods 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 5
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- 239000000243 solution Substances 0.000 description 37
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 10
- 229940107698 malachite green Drugs 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- JFTBTTPUYRGXDG-UHFFFAOYSA-N methyl violet Chemical compound Cl.C1=CC(=NC)C=CC1=C(C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 JFTBTTPUYRGXDG-UHFFFAOYSA-N 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 230000035484 reaction time Effects 0.000 description 8
- 238000009833 condensation Methods 0.000 description 7
- 230000005494 condensation Effects 0.000 description 7
- MECHNRXZTMCUDQ-RKHKHRCZSA-N vitamin D2 Chemical compound C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)/C=C/[C@H](C)C(C)C)=C\C=C1\C[C@@H](O)CCC1=C MECHNRXZTMCUDQ-RKHKHRCZSA-N 0.000 description 7
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000004847 absorption spectroscopy Methods 0.000 description 4
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- 238000010521 absorption reaction Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000004961 triphenylmethanes Chemical class 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000001000 anthraquinone dye Substances 0.000 description 1
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Abstract
The invention discloses a method for degrading triphenylmethane dye wastewater by the method of microwave induced catalysis. The microwave induced catalysis method is adopted, and nano NiO is taken as a catalyst to degrade triphenylmethane dyes in a microwave device. The dosage of the nano NiO is 0.4-1.0g/L, and the initial concentration of the triphenylmethane dyes is 30-100mg/L. A reaction solution is aerated for 30 minutes at first, put into the microwave device for reaction, and kept aerated in the course of the reaction. The method adopts a microwave induced catalysis system, and catalytic reaction is carried out without any light source, which overcomes the defects of low light utilization rate and low light quantum efficiency of the photocatalysis technology. The experimental device adopted by the method is simple and convenient to be operated, and the reaction can be carried out at normal temperature and normal pressure, thus achieving the effects of saving energy and lowering energy consumption. By adopting the method, typical triphenylmethane dyes which are difficult to be biodegraded can be effectively degraded, which causes no secondary pollution, and has high TOC removing efficiency, and the method is characterized by high speed and high efficiency.
Description
Technical field
The present invention relates to the treatment process of triphenylmethane dye waste water, the method for the microwave induced catalytic degradation of triphenyl methane dye waste water of saying so more specifically.
Background technology
Along with the development of dyestuff and printing and dyeing industry, its factory effluent has become one of current topmost pollution source of water body, to environment structure serious day by day threat.According to related data, the dyestuff that accounts for world dyestuff ultimate production 1-10% loses in dyeing and printing process and as discharge of wastewater, is that the water body color and luster pollutes and the main source of eutrophication.
Triphenylmethane dye is a kind of many benzene ring compounds, and the principal character of its structure is to be connected with three phenyl ring around central carbon atom, and one of them phenyl ring links to each other with two keys with carbon atom.Such dyestuff is the third-largest dyestuff of usage quantity after azoic dyestuff, anthraquinone dye, produces a large amount of waste water in its production, use.Wherein the middle degraded product of some dye well is in the news and has " three cause " effect, and these pollutents enter environment from links such as production, transportation, uses, pollute, for ecotope brings impact.This class waste water from dyestuff has characteristics such as concentration height, colourity are dark, strong toxicity, difficult for biological degradation, is the difficult point of Industrial Wastewater Treatment.Therefore, the triphenylmethane dye of how removing in the waste water is the hot issue that researcher is paid close attention to always.
To the removal of dye class pollutent, traditional method comprises physical method and bioremediation and chemical treatment methods such as charcoal absorption, chemical flocculation and ion-exchange.Yet traditional physical method can not destroy the organic structure of dyestuff, just with organic pollutant from water transfer to other mutually, thereby will cause secondary pollution.Simultaneously, owing to the reasons such as high stability that contain a large amount of aromatics and modern dyestuff in the waste water from dyestuff, bioremediation also is difficult to it is decoloured and degrades.
In more than ten years in the past, along with increasingly sharpening that the poisonous and harmful organic pollutant of the difficult degradation in the water surrounding pollutes, high-level oxidation technology in the chemical treatment method has developed into the effective means of removing organic dye waste water, has all obtained significant progress such as wet oxidation, catalytic wet oxidation, supercritical water oxidation, photochemical catalytic oxidation, microwave-assisted photochemical catalysis and microwave induction catalytic etc.These methods all have characteristics and deficiency separately.Wet oxidation, catalytic wet oxidation, supercritical water oxidation technology all need be carried out under high temperature, high pressure, conversion unit had relatively high expectations, and high temperature resistant, the high pressure of palpus, and corrosion-resistant.Photochemical catalytic oxidation and microwave-assisted photocatalysis technology are a kind of water treatment new techniques that development in recent years is got up.But photocatalysis technology ubiquity light utilization efficiency is low and the low problem of photo-quantum efficiency: at first, photochemical catalysis to be adopted by high voltage mercury lamp or electrodeless lamp and is stimulated the UV-light that produces and simulating nature light as light source.This class lamp (particularly electrodeless lamp) influences degradation effect because all there is self factors of instability in the problem of manufacturing technology, thereby causes the instability of light source, and the utilization ratio of natural light is then lower.Secondly, for the processing dye wastewater with high concentration, thereby the light of use is difficult to penetrate the difficult removal effect that reaches expection of waste water, and this has also restricted this The Application of Technology.Therefore, the research and development high-level oxidation technology that need not illumination comes that organic dye pollutant is of great practical significance in the catalyzed degradation waste water from dyestuff.The present invention adopts the carry out Study on degradation of microwave induction catalytic system to typical triphenylmethane class dyestuff.
Microwave induction catalytic is to introduce the strong ripple material (as activated carbon, transition metal and oxide compound etc.) of inhaling pollutent is degraded in microwave field, can overcome the shortcoming that to use light source in the photochemical catalysis, and reaction can be carried out at normal temperatures and pressures, reach energy-conservation, consumption reduction, efficient, quick simultaneously, the target of non-secondary pollution.Studies have shown that under microwave radiation, many catalyzer can make methane decompose fast, suitably control condition then can obtain lower or higher (fragrance) hydro carbons selectively.S.L.Suib (Suib S L, Zerger R P.A directcontinuous, low power catalytic conversion of methane to higherhydrocarbons via microwave plasmas.J Catal.1993.139:383-391) etc. low pressure microwave plasma technology is applied to methane and directly transforms the C2 hydrocarbon (mainly being ethene and ethane) that obtains high yield, it for example is catalyzer with Ni, pressure 1.3MPa, microwave power 60W, methane conversion reaches 52%, and ethane and selectivity of ethylene reach 50% and 25%.Wang Jincheng (Wang Jincheng, Xue Daming, mediate entirely, Xiong Li, Yang Fenglin, Zhao Yazhi. the research of microwave radiation processing Reactive Brilliant Blue KN-R dye solution. ACTA Scientiae Circumstantiae, 2001,21 (5): 628-630) wait studies show that of people: microwave irradiation can make Reactive Brilliant Blue KN-R solution decolour rapidly in the presence of gac, the Reactive Brilliant Blue KN-R solution 50mL that every g activated carbon treatment concentration is 300mg/L, and microwave radiation 4min percent of decolourization reaches 97.1%.
Summary of the invention
1. goal of the invention:
Characteristics such as, strong toxicity dark, difficult for biological degradation at triphenylmethane dye waste water concentration height, colourity, the invention provides a kind of method of microwave induced catalytic degradation of triphenyl methane dye waste water, promptly adopt the microwave induction catalytic system to make the method for triphenylmethane dye waste water degraded, can be easy to operate, need not can carry out catalysis process under illumination, non-secondary pollution, the normal temperature target that can reach decolouring at short notice, degrade, remove dyestuff.
2. technical scheme:
Ultimate principle of the present invention:
Many organic compound directly do not absorb microwave significantly, but can utilize " sensitizing agent " of certain strong absorption microwave micro-wave energy to be passed to these materials and the induced chemical reaction generation.If select this " sensitizing agent " carrier for use, just can under microwave exposure, realize some catalyzed reaction, so-called microwave induction catalytic reaction that Here it is as catalyzer or catalyzer.Its ultimate principle is as follows: high strength short pulse microwave radiation is focused on the solid catalyst surface that contains certain energy strong absorption microwave, owing to of the strong interaction of surface metal point position with micro-wave energy, micro-wave energy will be transformed into heat, thereby make some surface point position optionally be heated to very high-temperature very soon.Organic reagent in the reactor can be by the microwave direct heating, but can react when contacting with the surface point position that is stimulated.These " sensitizing agents " mostly are that some absorb the very capable material of microwave, as gac, semiconductor catalyst, ferromagnetic metal and compound thereof etc.Because the ununiformity of this class material surface, its surface can produce many " focuses " during microwave radiation; The temperature of these " focuses " is more much higher than other positions, causes chemical reaction to take place easily, and Chang Zuowei induces the catalyzer of chemical reaction.The present invention adopts NiO as " sensitizing agent ", and promptly catalyzer carries out the research of microwave induction catalytic degraded typical triphenylmethane class dyestuff.
The technical scheme that realizes goal of the invention is as follows:
A kind of method of microwave induced catalytic degradation of triphenyl methane dye waste water, it adopts the method for microwave induction catalytic, is catalyzer with the nano NiO, carries out degradation of triphenylmethane dye in microwave device.
The consumption of above-mentioned catalyst nano NiO is 0.4～1.0g/L.The triphenylmethane dye starting point concentration is 30～100mg/L, and the aeration 30min of reaction solution elder generation places microwave device to react, and keep aeration always in reaction process.
Nano NiO Preparation of catalysts wherein is with Ni (NO
3)
26H
2O, NaOH and NaClO are raw material, adopt ultrasonic radiation precipitation-oxidation style to be prepared, and products therefrom in 110 ℃ of dry 20h down, and is calcined 2h down at 300 ℃ in retort furnace, promptly obtain black solid NiO catalyzer, is stored in the moisture eliminator.
As long as the microwave device that the present invention uses can produce microwave and have protection function.Can be that the 600w household microwave oven is reequiped voluntarily with microwave power.The operating method of triphenylmethane dye degradation method is in the reaction flask that aqueous dye solutions is packed into, the NiO catalyzer that adds the present invention's preparation subsequently, place the microwave oven cavity after the repacking to react, reaction times can be controlled voluntarily, insert recirculated water in the reaction process and carry out condensation, simultaneously in reaction process, constantly reaction solution is carried out aeration, finish, measure dye strength and change and mineralization degree until reaction.
3. beneficial effect:
Compared with the prior art, beneficial effect of the present invention is embodied in: one, the present invention adopts the microwave induction catalytic system, need not adopt any light source can carry out catalyzed reaction, has overcome the low and low problem of photo-quantum efficiency of the light utilization efficiency that exists in the photocatalysis technology.Two, simple, easy to operate, the reaction of the experimental installation that adopts of the present invention can be carried out at normal temperatures and pressures, reaches energy-saving and cost-reducing effect.Three, treatment process of the present invention can be degraded effectively to being difficult to biodegradable typical triphenylmethane class dyestuff, non-secondary pollution, and TOC removes the efficient height, has characteristics fast and efficiently.
Four, description of drawings
Fig. 1 microwave induction catalytic reaction unit synoptic diagram;
The uv-visible absorption spectroscopy figure of malachite green under Fig. 2 microwave, the microwave-NiO catalyst system;
The uv-visible absorption spectroscopy figure of differential responses time malachite green under Fig. 3 embodiment 1 microwave-NiO catalyst system;
The uv-visible absorption spectroscopy figure of differential responses time methyl violet under Fig. 4 embodiment 4 microwaves-NiO catalyst system;
The uv-visible absorption spectroscopy figure of differential responses time Viola crystallina under Fig. 5 embodiment 5 microwaves-NiO catalyst system.
Five, embodiment
Further specify the present invention by the following examples.
Embodiment 1:
Preparation 0.8M Ni (NO
3)
26H
2O solution, 1.6M NaOH solution and 12wt%NaClO solution for standby.At first get 50mL Ni (NO
3)
26H
2O solution dropwise drops to and obtains Ni (OH) in the 50mL NaOH solution (mol ratio 1:2)
2Subsequently, 100mL NaClO solution is dropwise dropped in the solution of above-mentioned preparation under agitation condition, solution gradually becomes black precipitate by green again.Above-mentioned being reflected in the water-bath carried out, and temperature is 70 ℃, subsequently above-mentioned reaction solution is positioned over ultrasonic 15min in the ultrasonic device.Gained precipitation is carried out suction filtration, and after repeatedly washing with deionized water, collecting precipitation is transferred in the retort furnace in 110 ℃ of dry 20h down, at last at 300 ℃ of calcining 2h down.The gained black solid is the NiO catalyzer, is stored in the moisture eliminator.Catalyzer is characterized.Reaction finishes the back collection catalyst, and catalyzer and the 12wt% NaClO that collection obtains reacted again, the reaction after drying, and calcining can reuse.
Embodiment 2:
Preparation 100mg/L malachite green aqueous solution dye wastewater is measured the 50mL aqueous solution and is packed in the reaction flask.React with being placed in the microwave oven.Wherein 1 is prolong, 2
With microwave power is that the 600w household microwave oven is reequiped voluntarily, and as shown in Figure 1, wherein aeration tube 1, prolong 2, aluminum sleeve pipe 3, Florence flask 4, microwave generator 5, pipe connecting 6, microwave cavity 7.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment, and the reaction times is to get final product about 5min.It is centrifugal that reaction finishes postcooling, collects reaction solution.Following two kinds of reaction systems are set, measure the changing conditions of malachite green concentration with the reaction times.
1) reaction is only carried out under microwave action, does not add catalyzer;
2) take by weighing 40mg NiO (0.8mg/L) catalyzer and add the microwave reaction system.
The result as shown in Figure 2, reaction solution only in microwave action following time, do not degrade substantially by malachite green, and after adding catalyzer, malachite green is degraded rapidly.Concentration reduced by 99.8% in Fig. 3 result showed among the malachite green 2min, and the TOC clearance reaches 81.8%.
Embodiment 3:
Preparation 10mg/L malachite green aqueous solution dye wastewater is measured the 50mL dye solution and is packed in the reaction flask.Take by weighing 20mg NiO (0.4mg/L) catalyzer and add above-mentioned reaction solution, react with being placed in the microwave oven.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment.It is centrifugal that reaction finishes postcooling, collects reaction solution.Mensuration malachite green concentration is with the changing conditions in reaction times, and experimental result shows that interior concentration reduces by 99.7% among the malachite green 2min, and the TOC clearance reaches 82.4%.
Embodiment 4:
Preparation 30mg/L methyl violet aqueous solution dye wastewater is measured 50mL methyl violet solution and is packed in the reaction flask.Take by weighing 60mg NiO (1.2mg/L) catalyzer and add above-mentioned reaction solution, react with being placed in the microwave oven.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment.It is centrifugal that reaction finishes postcooling, collects reaction solution.Mensuration methyl violet concentration is with the changing conditions in reaction times, and experimental result shows that interior concentration reduces by 99.4% among the methyl violet 3min, and the TOC clearance reaches 63.2%.
Embodiment 5:
Preparation 100mg/L methyl violet aqueous solution dye wastewater is measured 50mL methyl violet solution and is packed in the reaction flask.Take by weighing 40mg (0.8mg/L) NiO catalyzer and add above-mentioned reaction solution, react with being placed in the microwave oven.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment.It is centrifugal that reaction finishes postcooling, collects reaction solution.Mensuration methyl violet concentration is with the changing conditions in reaction times, and experimental result shows that interior concentration reduces by 98.7% among the methyl violet 3min, and the TOC clearance reaches 53.1%.
Embodiment 6:
Preparation 100mg/L Viola crystallina aqueous solution dye wastewater is measured the 50mL crystal violet solution and is packed in the reaction flask.Take by weighing 40mg NiO (0.8mg/L) catalyzer and add above-mentioned reaction solution, react with being placed in the microwave oven.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment.It is centrifugal that reaction finishes postcooling, collects reaction solution.Measure the changing conditions of Viola crystallina concentration with the reaction times: concentration reduces by 98.5% among the Viola crystallina 2min, and the TOC clearance reaches 90.4%.
Embodiment 7:
Preparation 100mg/L Viola crystallina aqueous solution dye wastewater is measured the 50mL aqueous solution and is packed in the reaction flask.Take by weighing 80mg NiO (1.6mg/L) catalyzer and add above-mentioned reaction solution, react with being placed in the microwave oven.Regulate microwave power, connect water of condensation, and reaction solution is continued to carry out aeration, bay during the rotation microwave, microwave oven is started working, and pick up counting this moment.It is centrifugal that reaction finishes postcooling, collects reaction solution.Measure the changing conditions of Viola crystallina concentration with the reaction times: concentration reduces by 99.5% among the Viola crystallina 2min, and the TOC clearance reaches 93.8%.
Claims (4)
1. the method for a microwave induced catalytic degradation of triphenyl methane dye waste water is characterized in that adopting the method for microwave induction catalytic, is catalyzer with the nano NiO, carries out degradation of triphenylmethane dye in microwave device.
2. the method for microwave induced catalytic degradation of triphenyl methane dye waste water according to claim 1, the consumption that it is characterized in that catalyst nano NiO is 0.4～1.0g/L.
3. the method for microwave induced catalytic degradation of triphenyl methane dye waste water according to claim 2, it is characterized in that the triphenylmethane dye starting point concentration is 30～100mg/L, the aeration 30min of reaction solution elder generation places microwave device to react, and keep aeration always in reaction process.
4. according to the method for each described microwave induced catalytic degradation of triphenyl methane dye waste water in the claim 1～3, it is characterized in that nano NiO catalyzer wherein is a raw material with nickelous nitrate, sodium hydroxide and clorox, adopt precipitation～oxidation style to make.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885530A (en) * | 2010-07-20 | 2010-11-17 | 环境保护部华南环境科学研究所 | Method for efficiently removing typical triphenylmethane dye from water |
| CN103739035A (en) * | 2014-01-06 | 2014-04-23 | 山东大学 | Rapid microwave treatment method of dye wastewater |
-
2008
- 2008-09-03 CN CNA2008101247862A patent/CN101372368A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885530A (en) * | 2010-07-20 | 2010-11-17 | 环境保护部华南环境科学研究所 | Method for efficiently removing typical triphenylmethane dye from water |
| CN103739035A (en) * | 2014-01-06 | 2014-04-23 | 山东大学 | Rapid microwave treatment method of dye wastewater |
| CN103739035B (en) * | 2014-01-06 | 2016-01-20 | 山东大学 | A kind of Rapid microwave treatment method of waste water from dyestuff |
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