CN100391863C - Process for treating waste water of methylene blue dye and process for preparing catalyst - Google Patents

Process for treating waste water of methylene blue dye and process for preparing catalyst Download PDF

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CN100391863C
CN100391863C CNB2005101227827A CN200510122782A CN100391863C CN 100391863 C CN100391863 C CN 100391863C CN B2005101227827 A CNB2005101227827 A CN B2005101227827A CN 200510122782 A CN200510122782 A CN 200510122782A CN 100391863 C CN100391863 C CN 100391863C
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nanometer rods
methylene blue
preparation
catalyst
blue dye
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CN1792866A (en
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张卫新
杨则恒
张愿成
王雪
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Hefei University of Technology
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Hefei University of Technology
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Abstract

The present invention relates to a process for treating waste water of methylene blue dye and a process for preparing a catalyst. The process for treating waste water of methylene blue dye is characterized in that a heterogeneous catalytic oxidation method is adopted, and a nano-structure oxide of manganese is used as a catalyst to catalyze H2O2 at normal temperature in order to oxidize and decompose methylene blue dye. The process for treating waste water of methylene blue dye of the present invention is a process which has the advantages of no requirement of illumination, no secondary pollution, oxidative decomposition of dye waste water by catalyzing hydrogen peroxide at normal temperature, cheap raw materials, low operating cost and high catalytic efficiency.

Description

Methylene blue dye method of wastewater treatment and method for preparing catalyst
Technical field:
The present invention relates to water treatment method, the method for more specifically saying so the waste water from dyestuff that contains methylene blue being handled, with and involved Preparation of catalysts method.
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.Because this class waste water complicated component, often contain multiple organic dye and intermediate thereof, colourity is dark, strong toxicity, difficult degradation, the fluctuation of pH value greatly, and concentration height, the water yield are big, are the difficult points of Industrial Wastewater Treatment always.They to environment structure day by day serious threat.It is reported, the dyestuff that accounts for world dyestuff ultimate production 1-20% loses in dyeing and printing process and as discharge of wastewater, be that the water body color and luster pollutes and the main source of eutrophication, and by oxidation, hydrolysis or other chemical reactions take place may cause the by product generation that endangers.Therefore, the decolored degradation of waste water from dyestuff comes into one's own day by day.
For the removal of dyestuff contaminant, adopt traditional physical method usually, as charcoal absorption, ultrafiltration, reverse osmosis, chemical flocculation, ion-exchange or the like.Yet these methods are not all destroyed the organic molecule of dyestuff, they just organic pollution is transferred to from water other mutually in, therefore, can cause secondary pollution.The result also needs to expend the further reproducing adsorbent of substantial contribution and solid waste is carried out subsequent treatment.
Owing to contain the high stability of a large amount of aromatic compound and modern dyestuff in the dyestuff, also be difficult to they are carried out decolorization and degradation with traditional bioremediation.In addition, in order to satisfy the painted requirement of the degree of depth, many dyestuffs all are high water solubles.Therefore traditional method of wastewater treatment all day by day loses effectiveness as flocculence, active carbon adsorption and biological treatment.
These reasons are impelled and have been developed " high-level oxidation technology " (Advanced Oxidation Processes) in the past in 10 years, because they can solve dye molecule degradation problem in the aqueous systems, and become the research focus.The advanced oxidation process is to utilize hydroxy radical (OH) oxidation Decomposition organic matter, and general using oxidant, ray and catalyst produce hydroxy radical, as: O 2/ catalyst, UV/O 3, UV/H 2O 2, ultrasonic US, US/H 2O 2, O 3, H 2O 2, H 2O 2/ Fe 2+(Fenton reagent), light-Fenton catalysis, TiO 2Photocatalysis etc.In a series of assembly of the oxygenant/catalyzer of advanced oxidation, hydrogen peroxide/catalyzer has best oxidation capacity.Chinese scholars is consistent in recent years thinks that hydrogen peroxide oxidation is the comparatively cost-effective method of dye wastewater treatment using.Yet these methods still are difficult to apply at present, as the pH value narrow range that the Fenton oxidation style is suitable for, only are 2-4; TiO 2Photochemical catalysis is because of relating to intensity of illumination, pH value, temperature, concentration of reactants and structure, TiO 2Experiment parameters such as concentration DeR and processing cost are had complicated influence.For this reason, the research and development effective catalyst that need not illumination comes that dye molecule has crucial meaning in the catalyzed degradation waste water from dyestuff system.
Waste water from dyestuff contains multiple dyestuff contaminant, and methylene blue is difficult to biodegradable typical dyestuff contaminant as a kind of, and the treatment process of bibliographical information is to utilize TiO usually 2Photocatalyst carries out photocatalytic degradation, but this needs light source.
In recent years, along with nano material synthetic with the going deep into of applied basic research, the research of nanocatalyst is paid close attention to widely.Nano material is little because of particle diameter, specific surface area is big, surface atom is many, has very high chemically reactive.In the world nanocatalyst as the 4th generation catalyst research and develop.
About the preparation of the nanostructured oxide of manganese, according to " Chemistry-A European Journal " (2003, the 9th volume, 1645-1651 page or leaf) report, with [{ Mn (SO 4) (4,4/-bpy) (H 2O) 2N] polymkeric substance and NaOH solution is raw material, can be by the synthetic γ-MnO of hydrothermal chemical reaction 2Nano wire, but this method cost height, poor repeatability, reliability are low.U.S.'s " Solid-state Chemistry magazine " (Journal of Solid State Chemistry) (2004, the 177th volume, 2628-2631 page or leaf) has reported use electrospinning yarn technology and has prepared Mn 2O 3And Mn 3O 4Nanofiber, but this method need to all multi-steps such as sol-gel technology, electrospinning yarn process and calcining, and complicated operation, experiment condition harshness, be difficult for a large amount of production.
Summary of the invention:
The present invention is for avoiding above-mentioned existing in prior technology weak point, a kind of methylene blue dye method of wastewater treatment is provided, need not to implement under illumination, non-secondary pollution, the normal temperature so that handle, reach decolouring, degraded, remove the purpose of depolluting for methylene blue dye waste water.
The present invention provides the Preparation of catalysts that is applied in this treatment process method simultaneously, that this preparation method should possess is simple to operate, need not complex steps, easily mass production, products therefrom purity height, good dispersity, thereby is suitable for methylene blue dye waste water is handled industrial applications.
The technical scheme that technical solution problem of the present invention is adopted is:
Methylene blue dye method of wastewater treatment of the present invention is characterized in that adopting the method for heterogeneous catalytic oxidation, take the nanostructured oxide of manganese as catalyst, and catalysis H at normal temperatures 2O 2The oxidation Decomposition methylene blue dye.
The characteristics of methylene blue dye method of wastewater treatment of the present invention also are take catalyst amount to 0.25-0.75g/L, methylene blue initial mass concentration is 15.15-62.5mg/L, H 2O 2Mass percent is that 1.5-4.5% is reaction condition, fully stirs and evenly mixs, in normal-temperature reaction 0.5-3.5 hour.
The characteristics of methylene blue dye method of wastewater treatment of the present invention are that also the nanostructured oxide of described manganese is Mn 3O 4Nano particle, or β-MnO 2Nanometer rods, or Mn 2O 3Nanometer rods, or Mn 3O 4Nanometer rods.
The characteristics that the present invention is applied in the preparation method of the catalyst in the wastewater treatment are take ethanolic solution and potassium permanganate as raw material, adopt solvent heat synthetic method single step reaction to make Mn 3O 4Nano particle.
This wherein, the percent by volume of feed ethanol is greater than 70%, synthesis temperature is that 100-200 ℃, pressure are 1.0-2.0Mpa.
The preparation method that the present invention is applied in the catalyst in the wastewater treatment can also be: earlier take ethanolic solution and potassium permanganate as raw material, adopt the solvent heat synthetic method to prepare γ-MnOOH nanometer rods; Then under different temperatures and different atmosphere, calcine γ-MnOOH nanometer rods and make respectively β-MnO 2Nanometer rods, Mn 2O 3Nanometer rods and Mn 3O 4Nanometer rods.
This wherein, the percent by volume of feed ethanol is 0.5-10%, synthesis temperature is that 100-200 ℃, pressure are 0.5-1.0Mpa.
This wherein, described β-MnO 2The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 250 ℃-400 ℃ in air in temperature lower calcination 4-16 hour; Described Mn 2O 3The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 600 ℃-800 ℃ in air in temperature lower calcination 8-16 hour; Described Mn 3O 4The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 500 ℃-800 ℃ in nitrogen atmosphere in temperature lower calcination 4-16 hour.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, to be used for the adaptability of dye wastewater treatment using strong for method of wastewater treatment of the present invention, can carry out under the normal temperature.The hydroxy radical qiao that utilizes hydrogen peroxide decomposition to produce has very strong oxidation capacity, and standard potential 2.180V can the most organism of oxidation and be swift in response.
2, method of wastewater treatment of the present invention need not to adopt any light source can carry out catalyzed reaction, not influenced by illumination condition.
3, the methylene blue visible light spectrogram from changing with the reaction times, method of wastewater treatment of the present invention have reached the treatment effect of decolouring, degraded to methylene blue dye.Oxidant H 2O 2Participating in reacted residue can decompose voluntarily, does not stay remnants, no longer forms secondary pollution.
4, the nanostructured oxide catalyzer of manganese is repeatedly reusable among the present invention, need not regeneration, and it is promptly recyclable to carry out filtration drying after using.Catalyzer is reused back methylene blue decolorizing efficiency and is had only a little decline, and good economy performance is the nano-structured calalyst of a kind of high reactivity, stable performance.
5, the nanostructured oxide Preparation of catalysts method of manganese has that cost of material is cheap, preparation simply, reliably, easily realizes characteristics such as scale operation, gained catalyzer purity height, good dispersity among the present invention.
Description of drawings
Fig. 1 for the nanostructured oxide of the manganese that makes with the inventive method be catalyzer, methylene blue percent of decolourization over time.
Wherein:
A:H 2O 2+ methylene blue; B:Mn 2O 3Nanometer rods+methylene blue;
C:Mn 3O 4Nanometer rods+methylene blue; D:Mn 3O 4Nano particle+methylene blue;
E: β-MnO 2Nanometer rods+methylene blue; F:Mn 2O 3Nanometer rods+H 2O 2+ methylene blue;
G:Mn 3O 4Nanometer rods+H 2O 2+ methylene blue; H:Mn 3O 4Nano particle+H 2O 2+ methylene blue;
I: β-MnO 2Nanometer rods+H 2O 2+ methylene blue.
Fig. 2 is with Mn in the inventive method 3O 4Nano particle as catalyst be example, the methylene blue visible light spectrogram that changes with the reaction time.Wherein:
A：0min；?B：5min；?C：10min；D：20min；?E：40min；
F：50min；G：60min；H：75min；I：120min；J：150min。
Referring to Fig. 1, the serial oxide of the manganese that will make by the inventive method records the methylene blue percent of decolourization over time respectively as catalyst, wherein be take catalyst amount as 0.5g/L, methylene blue initial mass concentration is 31.25mg/L, H2O 2Mass fraction is 4.5% for reaction condition. As can be seen from Figure in reaction system the oxide of no manganese, only have H2O 2Under the condition of individualism (curve A), the methylene blue percent of decolourization almost takes place significantly to change in time, and methylene blue and H be describeds under the condition of the oxide existence of no manganese2O 2Between oxidation reaction takes place hardly.
In reaction system, there is not H2O 2, only have under the condition that the oxide of manganese exists, the methylene blue percent of decolourization is tending towards saturated within a short period of time very soon, is up to 16% (Mn2O 3Nanometer rods) (curve B), 20% (Mn3O 4Nanometer rods) (curve C), 27% (Mn3O 4Nano particle) (curve D), 35% (β-MnO2Nanometer rods) (curve E).
The oxide and the H that in reaction system, have simultaneously manganese2O 2The time, the percent of decolourization of methylene blue after 150 minutes, the minimum 73% (Mn that reaches2O 3Nanometer rods) (curve F), 85% (Mn3O 4Nanometer rods) (curve G), 93% (Mn3O 4Nano particle) (curve H), 98% (β-MnO2Nanometer rods) (curve I).
To Fig. 1 analysis, curve B-E has represented the nanostructured oxide of different manganese to the suction-operated of methylene blue, and curve F-I has illustrated that the nanostructured oxide of manganese has accelerated H2O 2To the decomposition of methylene blue, in reaction system, really played the effect of catalyst, wherein β-MnO2Nanometer rods and Mn3O 4Nano particle has better catalytic effect as catalyst.
Fig. 2 is with Mn in the inventive method3O 4Nano particle is catalyst, with the methylene blue visible light of reaction time variation Spectrogram. Experimental procedure is as follows:
Under the differential responses time, take out the 1mL reaction solution with pipette, with 25mL volumetric flask dilution constant volume, dilution warp Pipette supernatant liquor after the centrifugation, in wavelength 400-800nm scope, survey its visible light spectrogram, relatively change with the reaction time Methylene blue visible light spectrogram. As can be seen from Figure, the molecular structure of methylene blue is substantially destroyed after 1 hour.
Embodiment:
Embodiment 1: the preparation of γ-MnOOH nanometer rod
After 4g potassium permanganate, 400mL distilled water, 4mL dehydrated alcohol mixed, reaction was 24 hours under 150 ℃, 0.5-1.0Mpa.Then take out product, with distilled water washing 3-5 time, use again absolute ethanol washing 1 time earlier.70 ℃ of following vacuum-dryings 4 hours, promptly obtain pale brown toner end.
Through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) analysis revealed products therefrom is monoclinic γ-MnOOH nanometer rod, and diameter is between 30-500nm, and length is at several microns to tens microns.
Embodiment 2: β-MnO 2The preparation of nanometer rod
In air,, obtain the black product in 250 ℃ of calcining γ-MnOOH nanometer rod 8 hours.
Through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) analysis revealed products therefrom is the β-MnO of tetragonal system 2Nanometer rod, diameter are between 40-300nm, and length is at several microns to tens microns.
Embodiment 3:Mn 2O 3The preparation of nanometer rods
In air,, obtain the black product in 700 ℃ of calcining γ-MnOOH nanometer rod 8 hours.
The analysis showed that through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) products therefrom is the Mn of rhombic system 2O 3Nanometer rods, diameter are between 50-300nm, and length is about several microns.
Embodiment 4:Mn 3O 4The preparation of nanometer rods
In nitrogen atmosphere,, obtain the khaki color product in 600 ℃ of calcining γ-MnOOH nanometer rod 8 hours.
The analysis showed that through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) products therefrom is the Mn of tetragonal crystal system 3O 4Nanometer rods, diameter are between 50-400nm, and length is about several microns.
Embodiment 5:Mn 3O 4The preparation of nano particle
After 4g potassium permanganate, 20mL distilled water, 400mL dehydrated alcohol mixed, reaction was 24 hours under 150 ℃, 1.0-2.0Mpa.Then take out product, with distilled water washing 3-5 time, use again absolute ethanol washing 1 time earlier.70 ℃ of lower vacuum drying 4 hours, namely obtain khaki Mn 3O 4Nano particle.
The analysis showed that through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) products therefrom is the Mn of tetragonal crystal system 3O 4, particle size is more even, and average grain diameter is about 50-100nm.
Embodiment 6: β-MnO 2Nanometer rods catalysis H 2O 2Decompose methylene blue dye
With β-MnO 2The nanometer rods consumption is that 0.5g/L, methylene blue initial mass concentration are 31.25mg/L, H 2O 2Mass fraction is 4.5% the reaction condition that is, fully reacts 0.5-3.5 hour in room temperature under stirring action.
Embodiment 7:Mn 2O 3Nanometer rods catalysis H 2O 2Decompose methylene blue dye
With Mn 2O 3The nanometer rods consumption is that 0.5g/L, methylene blue initial mass concentration are 31.25mg/L, H 2O 2Mass fraction is 4.5% for reaction condition, fully reacts 0.5-3.5 hour in room temperature under stirring action.
Embodiment 8:Mn 3O 4Nanometer rods catalysis H 2O 2Decompose methylene blue dye
With Mn 3O 4The nanometer rods consumption is that 0.5g/L, methylene blue initial mass concentration are 31.25mg/L, H 2O 2Mass fraction is 4.5% for reaction condition, fully reacts 0.5-3.5 hour in room temperature under stirring action.
Embodiment 9:Mn 3O 4Nano particle catalysis H 2O 2Decompose methylene blue dye
With Mn 3O 4The nano particle consumption is that 0.5g/L, methylene blue initial mass concentration are 31.25mg/L, H 2O 2Mass fraction is 4.5% for reaction condition, fully reaction 0.5-3.5 hour in room temperature under stirring action.

Claims (4)

1. methylene blue dye method of wastewater treatment is characterized in that adopting the method for heterogeneous catalytic oxidation, take the nanostructured oxide of manganese as catalyst, and catalysis H at normal temperatures 2O 2The oxidation Decomposition methylene blue dye;
In the method for described heterogeneous catalytic oxidation, take catalyst amount as 0.25-0.75g/L, methylene blue initial mass concentration is 15.15-62.5mg/L, H 2O 2Mass percent is that 1.5-4.5% is reaction condition, fully stirs and evenly mixs, in normal-temperature reaction 0.5-3.5 hour;
The nanostructured oxide of described manganese is Mn 3O 4Nano particle, or β-MnO 2Nanometer rods, or Mn 2O 3Nanometer rods, or Mn 3O 4Nanometer rods.
2. the preparation method of the catalyst in the described method of claim 1 is characterized in that adopting solvent heat synthetic method single step reaction to make Mn take ethanolic solution and potassium permanganate as raw material 3O 4Nano particle; The percentage by volume of described feed ethanol is greater than 70%, and synthesis temperature is that 100-200 ℃, pressure are 1.0-2.0Mpa.
3. the preparation method of the catalyst in the described method of claim 1 is characterized in that earlier adopting the solvent heat synthetic method to prepare γ-MnOOH nanometer rods take ethanolic solution and potassium permanganate as raw material; Then under different temperatures and different atmosphere, calcine γ-MnOOH nanometer rods and make respectively β-MnO 2Nanometer rods, Mn 2O 3Nanometer rods and Mn 3O 4Nanometer rods; The percentage by volume of described feed ethanol is 0.5-10%, and synthesis temperature is that 100-200 ℃, pressure are 0.5-1.0Mpa.
4. according to the described preparation method of claim 3, it is characterized in that described β-MnO 2The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 250 ℃-400 ℃ in air in temperature lower calcination 4-16 hour; Described Mn 2O 3The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 600 ℃-800 ℃ in air in temperature lower calcination 8-16 hour; Described Mn 3O 4The preparation of nanometer rods is that γ-MnOOH nanometer rods was obtained in 500 ℃-800 ℃ in nitrogen atmosphere in temperature lower calcination 4-16 hour.
CNB2005101227827A 2005-11-29 2005-11-29 Process for treating waste water of methylene blue dye and process for preparing catalyst Expired - Fee Related CN100391863C (en)

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CN100569673C (en) * 2006-10-25 2009-12-16 中国科学院大连化学物理研究所 A kind of method of catalysis wet-type oxidation degradation dyestuff contaminant
CN101411981B (en) * 2007-10-17 2011-04-13 中国科学院沈阳应用生态研究所 Method for preparing combined modified catalyst for processing coloring agent waste water
MD4008C1 (en) * 2009-07-01 2010-09-30 Институт Химии Академии Наук Молдовы Process for sewage water purification from methylene blue
CN102557143B (en) * 2010-12-07 2015-03-18 海洋王照明科技股份有限公司 Preparation method of Mn2O3 and catalyst
CN103464218B (en) * 2013-06-25 2015-04-15 新疆大学 Method used for direct synthesis of nano particle in waste water, and for water treatment by nano particle
CN104276650B (en) * 2014-10-30 2019-03-26 湖北科技学院 A kind of method of degradation of methylene blue
CN105032498B (en) * 2015-07-24 2018-10-30 浙江工业大学 Loaded catalyst and preparation method with natural biological skeleton structure and application
CN105461044A (en) * 2015-12-29 2016-04-06 泉州师范学院 Method for degrading methylene blue solution
CN108640197A (en) * 2018-04-25 2018-10-12 阜南县大喜柳编工艺品有限公司 The treatment and purification method of waste water from dyestuff in a kind of processing of timber
CN108686649B (en) * 2018-05-09 2020-09-29 济南大学 Mn based on absorbent cotton biological form3O4/ZnO/ACFs micromotor photocatalyst and application thereof
CN108816179B (en) * 2018-06-22 2021-07-13 中国科学院上海硅酸盐研究所 Porous high-specific-surface-area amorphous MnPO material and preparation method and application thereof
CN109264786A (en) * 2018-10-17 2019-01-25 国电环境保护研究院有限公司 A kind of γ-MnOOH, preparation method and its application
CN115106079A (en) * 2021-03-18 2022-09-27 中国科学院上海硅酸盐研究所苏州研究院 Catalyst capable of promoting generation of singlet oxygen and preparation method and application thereof
CN114349149A (en) * 2022-01-12 2022-04-15 攀枝花学院 Method for degrading methylene blue dye wastewater by using blast furnace slag

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