CN101125683A - Preparation method for photocatalysis water-purifying material MoO3 and application thereof - Google Patents

Preparation method for photocatalysis water-purifying material MoO3 and application thereof Download PDF

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Publication number
CN101125683A
CN101125683A CNA2007100240382A CN200710024038A CN101125683A CN 101125683 A CN101125683 A CN 101125683A CN A2007100240382 A CNA2007100240382 A CN A2007100240382A CN 200710024038 A CN200710024038 A CN 200710024038A CN 101125683 A CN101125683 A CN 101125683A
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moo
purifying material
photocatalysis
preparation
photocatalysis water
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宋继梅
胡媛
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Anhui University
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Anhui University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a preparation method and application of MoO3, a photocatalysis purified water material. Under room temperature, ammonium molybdate aqueous solution is first prepared and surfactant hexadecyl trimethyl ammonium bromide is added to be evenly mixed; thin hydrochloric acid solution is dripped during stirring until a large amount of precipitate appears, the precipitate is collected, repeatedly washed, dried to obtain precursor; the precursor is roasted to get MoO3, a photocatalysis purified water material. The invention can be applied to the treatment of waste liquid of organic dye with decolorization ratio towards various organic dyes reaching up to 80 percent, removal rate of CODCr of simulating dye waste water reaching to 94.7 percent and removal rate of BOD5 reaching to 97.2 percent. The catalyst of the invention has simple preparation method, high photocatalysis purified water efficiency and very good industrial application future.

Description

Photocatalysis water-purifying material MoO 3Preparation method and application thereof
Technical field
The invention belongs to field of nanometer material technology, specifically is a kind of photocatalysis water-purifying material MoO 3Preparation of nanomaterials and application thereof.
Background technology
In recent years, the control of water pollution has become the human major issue of being badly in need of solution with improvement.Waste water from dyestuff is one of more unmanageable trade effluent of generally acknowledging, the waste water from dyestuff of cation type bio-refractory particularly, itself is to the microorganisms toxic action, and adopt the coagulating treatment effect also undesirable, so senior oxidation technologies such as the Fenton of employing oxidation are handled or pre-treatment more, but these degradation techniques react complicated and need to consume other chemical substance.Photochemical catalytic oxidation-the reduction reaction of carrying out as photocatalyst with semiconductor material becomes a kind of have broad prospect of application and one of effective environmental Pollution abatement new technology the most with its particular performances.
Photochemical catalytic oxidation-reduction technique is to utilize sunlight or other light as the energy, at normal temperatures and pressures with the organic pollutant complete oxidation to CO 2, H 2O and non-toxic products, and the technology that catalyzer self can reuse are one of active research fields the most in the world in recent years.This method can be handled multiple pollutent, and is applied widely, and particularly the organic dye to difficult degradation has good oxygenolysis.Photocatalysis technology has simple to operate, and outstanding advantage such as non-secondary pollution has quite tempting application prospect aspect environmental protection.The research in this field is in the ascendant, and wherein the efficient catalytic material is one of present research forward position.MoO 3Itself have stronger surface adsorption performance, have broad application prospects in photocatalysis field.Except that being used for photocatalysis degradation organic contaminant, MoO 3As a kind of n type semiconductor oxide, also can be used as photocatalysis antibacterial material.
The domestic and international at present research to photocatalyst mainly concentrates on the nano material aspect, as nano-TiO 2, ZnO, CdS etc.Adopt nano material to have many advantages such as particle diameter is little, density is little, specific surface area is big, reactive behavior is high, selectivity is strong as catalyzer.Its particle is little but nano material is made catalyzer, easily suspends in water and very difficult the separation.The catalyzer that particle diameter is bigger, though be easy to separate, catalytic activity is lower again.The method that solves this contradiction is general to adopt the way that nanocatalyst is carried out load, but often catalytic activity can be subjected to a certain degree influence.
Summary of the invention
The purpose of this invention is to provide photocatalysis water-purifying material MoO 3Preparation method and application thereof.Adopt the surfactant templates method to realize the self-assembly of nano particle; Utilize MoO 3The photocatalysis performance of nano material self, the organic effect that purifies water that reaches simultaneously in degrading waste water.Resulting MoO 3Nanocatalyst can be recycled, and it is good to have a treatment effect, and stability is high, and use cost is low, advantages such as non-secondary pollution.
Technical scheme of the present invention is as follows:
Photocatalysis water-purifying material MoO 3The preparation method, it is characterized in that: under the room temperature, the preparation ammonium molybdate aqueous solution, to wherein adding the tensio-active agent cetyl trimethylammonium bromide, mix; Stir and drip dilute hydrochloric acid solution down, to a large amount of precipitations of appearance, the collecting precipitation thing, repetitive scrubbing, drying make precursor; The roasting precursor obtains photocatalysis water-purifying material MoO 3
Washing with acetone is adopted in described washing, and described drying is meant under 50 ℃ dry, and described roasting is meant 400 ℃ of roasting precursors.
Photocatalysis water-purifying material MoO 3The preparation method, it is characterized in that: under the room temperature, the preparation ammonium molybdate aqueous solution, to wherein adding the tensio-active agent cetyl trimethylammonium bromide, mix; Stir and drip dilute hydrochloric acid solution down, to a large amount of precipitations of appearance, the collecting precipitation thing, repetitive scrubbing, drying make precursor; The roasting precursor obtains photocatalysis water-purifying material MoO 3
Washing with acetone is adopted in described washing, and described drying is meant under 50 ℃ dry, and described roasting is meant 400 ℃ of roasting precursors.
Photocatalysis water-purifying material MoO 3Application, it is characterized in that being used to containing the processing of the waste liquid of organic dye.
With photocatalysis water-purifying material MoO 3Put into the waste liquid that contains organic dye, only need solar light irradiation, photocatalysis water-purifying material MoO 3Can make the organic dye catalyzed degradation.
Catalysis degradation modulus to organic dye under the logical atmospheric condition is higher.
MoO with the present invention's preparation 3Nano material is carried out percent of decolourization and is measured: with the MoO of the present invention's preparation of 5mg 3The nano material and the MoO of self-assembly not 3Nano material is added into organic dye solution respectively, and the organic dye original solution of 20mg/L and the solution after the decolouring have been carried out ultraviolet-visible (UV-vis) spectroscopic analysis.Observation has or not dyestuff adding MoO under the illumination condition 3Colour-change behind the sample is measured illumination front and back solution absorbency, and then is calculated MoO 3Percent of decolourization:
D = A 0 - A A 0 × 100 %
(A is the absorbancy after decolouring, A 0Absorbancy for original solution)
The UV-vis spectral measurement shows: MoO 3The MoO of nano particle and the present invention's preparation 3The light decoloration performance of micron bar close (table); MoO with self-assembly 3Micron bar recycles 5 times repeatedly, and its percent of decolourization does not become substantially.This shows the MoO of this self-assembly 3Micron bar is as the photocatalyst stable performance of organic dye decolouring, and is reusable.
In the experiment, the micron bar of the present invention preparation promptly began sedimentation in about 3 hours after light-catalyzed reaction, and unassembled MoO 3Nano particle needs 3 talent's beginning sedimentations, and MoO 3Nano particle is difficult for separating from solution, needs centrifugation.The MoO obvious, that nano particle is assembled into 3Micron bar is settlement separate easily, is convenient to recycle, and is the dye decolored catalyzer of ideal.
Mass color takes quadrature picture MoO down 3Catalysis percent of decolourization (D%) to various dyestuffs
Viola crystallina Hydrochloric acid Nai Er indigo plant Rhodamine B Sarranine premium T
Self-assembly MoO 3Micron bar MoO 3Nano particle 94.0 89.6 95.1 97.2 97.3 80.0 97.7 96.0
MoO among the present invention 3Method for preparing catalyst is simple, and photocatalysis water-purifying efficient height has better industrial application prospect.
Description of drawings
Accompanying drawing is the self-assembly MoO of the present invention's preparation 3The stereoscan photograph of micron bar.
Embodiment
Nanometer MoO 3Synthesizing of material: under the room temperature, the ammonium molybdate that takes by weighing 4.023g is dissolved in the 40mL distilled water, mixes, and drips the hydrochloric acid of the 6mol/L about 2.0mL, is stirred to while dripping a large amount of precipitations to occur.Suction filtration, gained precipitation are with dehydrated alcohol or washing with acetone 2-3 time, and 50 ℃ of dryings make precursor.Under 400 ℃, precursor is heat-treated, obtain product.It is quadrature phase MoO as can be known by the XRD detection 3
Photocatalysis water-purifying material MoO 3The preparation method: reaction conditions and above-mentioned experiment basically identical, just earlier the tensio-active agent cetyl trimethylammonium bromide (CTAB) that adds 0.004-0.006g drips dilute hydrochloric acid again and carries out the solution acidifying in reaction solution.Precipitation acetone repetitive scrubbing, dried precursor is at 400 ℃ of following roasting 3h, obtains the self-assembly product.XRD detects proof, and it is quadrature phase MoO 3
The photocatalysis water-purifying experiment
The multiphase photocatalysis process mainly is divided into two classes: gas-solid phase photochemical catalysis and liquid-solid phase photochemical catalysis, the species that the former is used for oxidation are O 2, the main species that the latter is used for oxidation are H 2O.
The photocatalytic degradation experiment of the Viola crystallina dye solution of 1. couples of 20mg/L of example: with the MoO of 5mg 3Catalyzer adds in this dye solution of 10mL, carries out solar light irradiation in uncovered test tube.With MoO 3Nano particle be catalyzer behind illumination 1h, COD CrClearance is 77.3%, under the same terms with the MoO of self-assembly 3Micron bar is a catalyzer, COD CrClearance is 91.9%.Obviously, the back MoO of self-assembly 3Material is significantly improved to the light degradation property of organic dye.MoO with self-assembly 3Micron bar recycles its COD 5 times after reclaiming repeatedly CrClearance does not become substantially, and this MoO is described 3Micron bar is as the photocatalyst stable performance of organic dye degraded, and is reusable.
The photocatalytic degradation of the Congo red dye solution of 2. couples of 20mg/L of example experiment: with the MoO of the self-assembly of 5mg 3Catalyzer adds in this dye solution of 10mL, carries out solar light irradiation 1 hour in uncovered test tube, and the percent of decolourization of Congo red solution reaches 91.5%, corresponding C OD CrClearance is 80%.When in the catalytic process only during the obstructed atmosphere of illumination, the percent of decolourization of Congo red solution only is 23%, corresponding C OD CrClearance reduces to 12%.Confirm O in Congo red catalysis decolorization thus 2Help its photocatalytic degradation.
Example 3. utilizes the mixing solutions dye wastewater (its concentration is 20mg/L) of Viola crystallina, hydrochloric acid Nai Er indigo plant, rhodamine B, sarranine premium T, Congo red dyestuff to carry out photocatalytic degradation experiment: with the MoO of the self-assembly of 5mg 3Catalyzer adds in this dye solution of 10mL, carries out solar light irradiation 1 hour in uncovered test tube.The result shows that this catalyzer all reaches more than 80% the percent of decolourization of each organic dye, to the COD of dye wastewater CrClearance can reach 94.7%, and BOD 5Clearance also reaches 97.2%.

Claims (5)

1. photocatalysis water-purifying material MoO 3The preparation method, it is characterized in that: under the room temperature, the preparation ammonium molybdate aqueous solution, to wherein adding the tensio-active agent cetyl trimethylammonium bromide, mix; Stir and drip dilute hydrochloric acid solution down, to a large amount of precipitations of appearance, the collecting precipitation thing, repetitive scrubbing, drying make precursor; The roasting precursor obtains photocatalysis water-purifying material MoO 3
2. photocatalysis water-purifying material MoO according to claim 1 3The preparation method, it is characterized in that: washing with acetone is adopted in described washing, described drying be meant 50 ℃ dry down, described roasting is meant 400 ℃ of roasting precursors.
3. according to the prepared photocatalysis water-purifying material MoO of the described method of claim 1 3Application, it is characterized in that being used to containing the processing of the waste liquid of organic dye.
4. photocatalysis water-purifying material MoO according to claim 3 3Application, to need only to it is characterized in that solar light irradiation, photocatalysis water-purifying material MoO 3Can make the organic dye catalyzed degradation.
5. according to claim 3 or 4 described photocatalysis water-purifying material MoO 3Application, it is characterized in that the catalysis degradation modulus to organic dye is higher under the logical atmospheric condition.
CNA2007100240382A 2007-07-14 2007-07-14 Preparation method for photocatalysis water-purifying material MoO3 and application thereof Pending CN101125683A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663561A (en) * 2012-09-10 2014-03-26 中国石油化工股份有限公司 Recycling method of molybdenum in filament-melting waste acid
CN104190402A (en) * 2014-08-13 2014-12-10 南京信息工程大学 Cerium-doped catalyst material as well as preparation method and application thereof
CN105836802A (en) * 2016-03-29 2016-08-10 河南师范大学 MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof
CN110252282A (en) * 2019-07-19 2019-09-20 广东工业大学 A kind of composite photo-catalyst and its preparation method and application
CN112195483A (en) * 2020-09-22 2021-01-08 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
CN112374538A (en) * 2019-09-27 2021-02-19 德州学院 Molybdenum trioxide micron rod with adjustable size and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663561A (en) * 2012-09-10 2014-03-26 中国石油化工股份有限公司 Recycling method of molybdenum in filament-melting waste acid
CN104190402A (en) * 2014-08-13 2014-12-10 南京信息工程大学 Cerium-doped catalyst material as well as preparation method and application thereof
CN105836802A (en) * 2016-03-29 2016-08-10 河南师范大学 MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof
CN110252282A (en) * 2019-07-19 2019-09-20 广东工业大学 A kind of composite photo-catalyst and its preparation method and application
CN110252282B (en) * 2019-07-19 2022-07-29 广东工业大学 Composite photocatalyst and preparation method and application thereof
CN112374538A (en) * 2019-09-27 2021-02-19 德州学院 Molybdenum trioxide micron rod with adjustable size and preparation method thereof
CN112195483A (en) * 2020-09-22 2021-01-08 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode
CN112195483B (en) * 2020-09-22 2021-11-16 深圳先进技术研究院 Method for constructing Z-type heterojunction photo-anode and Z-type heterojunction photo-anode

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