CN106944038A - A kind of Sb2MoO6The preparation method and application of catalysis material - Google Patents

A kind of Sb2MoO6The preparation method and application of catalysis material Download PDF

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Publication number
CN106944038A
CN106944038A CN201710129958.4A CN201710129958A CN106944038A CN 106944038 A CN106944038 A CN 106944038A CN 201710129958 A CN201710129958 A CN 201710129958A CN 106944038 A CN106944038 A CN 106944038A
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moo
catalysis material
methyl orange
preparation
application
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CN106944038B (en
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孔泳
陈中平
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Changzhou University
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Changzhou University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/28Molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/03Precipitation; Co-precipitation
    • B01J37/031Precipitation
    • B01J37/033Using Hydrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • C02F1/32Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/40Organic compounds containing sulfur
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • 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 present invention relates to a kind of Sb2MoO6The preparation and application of catalysis material.Comprise the following steps:Prepare Sb2MoO6Catalysis material, by Sb2MoO6Materials application is in the degraded of water body common contaminant methyl orange.The beneficial effects of the invention are as follows:Sb2MoO6The preparation method of catalysis material is simple and very fast to the degradation rate of the organic molecules such as methyl orange.

Description

A kind of Sb2MoO6The preparation method and application of catalysis material
Technical field
The present invention relates to a kind of Sb2MoO6The preparation method and application of catalysis material, belongs to wastewater treatment and materials synthesis Field.
Technical background
With developing rapidly for China's economy, living standards of the people are stepped up, agricultural effluent, industrial wastewater and life Quantity of wastewater effluent increases severely, and water pollution problems is on the rise.In numerous pollutants, persistence organic pollutant is used as a kind of allusion quotation The environmental contaminants of type, it is maximum to environmental hazard.This pollutant has the feature of high toxicity, fat-solubility, extended residual, And it is difficult to be removed that water process means conventional at present, which such as filter, adsorb method,.Due to biography can be enriched with food chain Pass, persistence organic pollutant has serious harm to health and ecological environment.Methyl orange is that typical persistence has Organic pollutants, and widely used in industries such as printing and dyeing, textiles.The present invention chooses methyl orange as application, with one Fixed representativeness.
Methyl orange is a kind of azo dyes, and the aqueous solution is in orange, if untreated in industrial production be just discharged into water body, Coloured water body is not only set to hinder aquatic plant to absorb sunlight, and methyl orange is poisonous in itself, and this is to being contaminated water body periphery The existence of animals and plants causes serious threat.
Photocatalytic method is a kind of Novel sewage treatment method.Its principle is:Under the conditions of certain wavelength light photograph, semiconductor light Electron transition in catalysis material valence band leaves in valence band hole to conduction band.Subsequent light induced electron and hole and ion or Molecule is combined, living radical of the generation with oxidisability or reproducibility.This living radical can will be organic in water body Macromolecular mineralising is water and carbon dioxide, so as to reach the purpose of degradable organic pollutant.Photocatalytic method is compared to traditional dirt Method for treating water has many advantages.First, when carrying out photocatalysis in water body, hole is easily acted on hydrone, forms oxidisability Extremely strong hydroxyl radical free radical.The free radical can be extremely adapted in processing sewage with all organic substances of the mineralising of non-selectivity Organic principle.Secondly, photocatalytic method is originated using luminous energy as energy, by seeking the catalysis material of visible light absorbing, can be with Solar energy is effectively utilized, it is economic and environment-friendly.Finally, in catalytic reaction process, photochemical catalyst does not change in itself, therefore can To recycle, with practicality.
Sb2MoO6The features such as with stable chemical nature, cheap and easy production, be light-catalysed ideal material.But It is that the material is not applied to photocatalysis field also so far.It is an object of the invention to probe into Sb2MoO6Photocatalytic activity, And a kind of Sb is provided2MoO6The preparation method of catalysis material.
The content of the invention
It is an object of the invention to provide a kind of Sb2MoO6The preparation method and application of catalysis material.
A kind of Sb of the present invention2MoO6The preparation and application of catalysis material, comprise the following steps:
A, preparation Sb2MoO6Catalysis material:Trichloride antimony is added in hydrochloric acid solution, continues to add molybdenum after stirring Sour sodium dihydrate.Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.By obtained dark green solid Precipitation and centrifugal separation is simultaneously alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, is put into oven for drying, is obtained Sb2MoO6Photocatalysis material Material.
b、Sb2MoO6Catalysis material is applied to the methyl orange in degradation water:Certain density methyl orange solution is prepared, is used Sb made from step a2MoO6Methyl orange in catalysis material degradation water, while detecting first using ultraviolet-uisible spectrophotometer The characteristic absorption peak intensity of base orange solution.When characteristic absorption peak disappears, that is, illustrate that the methyl orange degradation in solution is complete, record The degraded time used.
Further, concentration of hydrochloric acid solution is 0.1~2mol/L in step a, and consumption is 30~80mL.
Further, trichloride antimony consumption is 0.1~10g in step a.
Further, sodium molybdate dihydrate consumption is 0.05~5g in step a.
Further, the concentration of methyl orange solution is 1~100mg/L in step b.
Further, Sb in step b2MoO6The concentration of catalysis material is 0.01~1g/L.
Further, in step b the characteristic absorption peak of methyl orange at 465nm.
The beneficial effects of the invention are as follows:Sb2MoO6The preparation method of catalysis material is simple and to organic molecules such as methyl oranges Degradation rate it is very fast.
Brief description of the drawings
This experiment is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is Sb in embodiment one2MoO6The X-ray diffractogram of catalysis material.
Fig. 2 is Sb in embodiment one2MoO6The uv drses figure of catalysis material.
Fig. 3 is Sb in embodiment one2MoO6The field emission scanning electron microscope figure of catalysis material.
Fig. 4 is Sb in embodiment two2MoO6Catalysis material is applied to the design sketch of methyl orange degradation.
Fig. 5 is initial influence of the concentration of hydrochloric acid to catalyst photocatalysis effect in embodiment three.
Embodiment
Presently in connection with specific embodiment, the present invention will be further described, following examples be intended to illustrate invention rather than Limitation of the invention further.
The percent of decolourization of methyl orange solution shown in narration in detail of the invention and examples of implementation is to calculate as follows 's:Certain density methyl orange solution is prepared, the absorbance at 465nm is measured using ultraviolet-visible spectrophotometer, is designated as a0.Sampled during UV degradation, measure the absorbance at 465nm using ultraviolet-visible spectrophotometer, be designated as an(n For sampling number of times).Percent of decolourization bnCalculated by below equation:
bn=1-an/a0(n=0,1,2 ...)
Embodiment one:
The hydrochloric acid solution that 70mL concentration is 0.5mol/L is measured, 4.56g trichloride antimonies are added, in its solution after stirring Middle addition 2.42g sodium molybdate dihydrates.Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.It will separate out Dark green solid precipitation and centrifugal separation and alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into oven for drying, be made Sb2MoO6Catalysis material.As shown in Figure 1, it is Sb to show made sample of the invention to X ray diffracting spectrum2MoO6.Solid violet Outer diffusing reflection collection of illustrative plates as shown in Figure 2, shows Sb2MoO6Catalysis material has good absorbability to light.Scanning electron shows Micro mirror image as shown in Figure 3, shows Sb2MoO6Catalysis material is sheet or club shaped structure.
Embodiment two:
Compound concentration is 6mg/L methyl orange solution 500mL, weighs the Sb of the preparation of embodiment one2MoO6Catalysis material 0.05g, the methyl orange under 11W ultra violet lamps in degradation water, sampling in each hour once, uses UV, visible light spectrophotometric The characteristic absorption peak intensity of meter detection methyl orange solution, calculates solution percent of decolourization.As a result as shown in Figure 4, after ultraviolet irradiation 5h Percent of decolourization is 36.5%.
Embodiment three:
Initial concentration of hydrochloric acid solution is investigated to Sb2MoO6The influence of photocatalysis effect.Compound concentration is 0mol/L, 0.5mol/ L, 1mol/L and 2mol/L hydrochloric acid solution, measure 70mL respectively, 4.56g trichloride antimonies are added, in its solution after stirring Middle addition 2.42g sodium molybdate dihydrates.Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.It will separate out Dark green solid precipitation and centrifugal separation and alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into oven for drying, obtain not Same Sb2MoO6Sample, is respectively labeled as Sb2MoO6-0、Sb2MoO6-0.5、Sb2MoO6-1、Sb2MoO6-2.Compound concentration is 6mg/ L methyl orange solution 500mL, weigh the above-mentioned Sb of 0.05g respectively2MoO6Sample, the methyl under 11W ultra violet lamps in degradation water Orange, sampling in each hour once, the characteristic absorption peak intensity of methyl orange solution is detected using ultraviolet-uisible spectrophotometer, is calculated Solution percent of decolourization.As a result as shown in Figure 5, photocatalysis effect is optimal when initial concentration of hydrochloric acid solution is 0.5mol/L.

Claims (3)

1. a kind of Sb2MoO6The preparation and application of catalysis material, step are as follows:
A, preparation Sb2MoO6Catalysis material:Trichloride antimony is added in hydrochloric acid solution, continues to add sodium molybdate after stirring Dihydrate.Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.The dark green solid of precipitation is precipitated Centrifuge and alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into oven for drying, obtain Sb2MoO6Catalysis material.
b、Sb2MoO6Methyl orange of the catalysis material materials application in degradation water:Certain density methyl orange solution is prepared, is used Sb made from step a2MoO6Methyl orange in catalysis material degradation water, while detecting first using ultraviolet-uisible spectrophotometer The characteristic absorption peak intensity of base orange solution.When characteristic absorption peak disappears, that is, illustrate that the methyl orange degradation in solution is complete, record Time used by lower degraded.
2. a kind of Sb according to claim 12MoO6The preparation and application of catalysis material, it is characterized in that:In the step a Concentration of hydrochloric acid solution be 0.1~2mol/L, trichloride antimony consumption be 0.1~10g, sodium molybdate dihydrate consumption be 0.05~ 5g, hydrochloric acid solution consumption is 30~80mL.
3. a kind of Sb according to claim 12MoO6The preparation and application of catalysis material, it is characterized in that:In the step b The concentration of methyl orange solution is 1~100mg/L, Sb2MoO6The concentration of catalysis material is 0.01~1g/L.The feature of methyl orange Absworption peak is at 465nm.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108636457A (en) * 2018-05-25 2018-10-12 常州大学 A kind of APTES-Sb can be used for photochemical catalyst2WO6The preparation method of-GQDs composite materials
CN113385168A (en) * 2021-06-10 2021-09-14 宁波大学 Sb in hexagonal pyramid form2MoO6Method for preparing material and catalytic use thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU833540A1 (en) * 1979-09-21 1981-05-30 Институт Естественных Наукбурятского Филиала Co Ah Cccp Method of producing antimony molybdate
CN104843661A (en) * 2015-04-29 2015-08-19 岭南师范学院 Preparation method for template-free synthesis of phosphoric acid microspheres
CN105633390A (en) * 2016-01-07 2016-06-01 西安交通大学 Novel lithium/sodium ion battery negative electrode material Sb2MoO6 and preparation method therefor
CN106268768A (en) * 2016-08-04 2017-01-04 苏州德捷膜材料科技有限公司 A kind of preparation with visible light-responded antimony yttrium molybdate nano-photocatalyst and light degradation application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU833540A1 (en) * 1979-09-21 1981-05-30 Институт Естественных Наукбурятского Филиала Co Ah Cccp Method of producing antimony molybdate
CN104843661A (en) * 2015-04-29 2015-08-19 岭南师范学院 Preparation method for template-free synthesis of phosphoric acid microspheres
CN105633390A (en) * 2016-01-07 2016-06-01 西安交通大学 Novel lithium/sodium ion battery negative electrode material Sb2MoO6 and preparation method therefor
CN106268768A (en) * 2016-08-04 2017-01-04 苏州德捷膜材料科技有限公司 A kind of preparation with visible light-responded antimony yttrium molybdate nano-photocatalyst and light degradation application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108636457A (en) * 2018-05-25 2018-10-12 常州大学 A kind of APTES-Sb can be used for photochemical catalyst2WO6The preparation method of-GQDs composite materials
CN113385168A (en) * 2021-06-10 2021-09-14 宁波大学 Sb in hexagonal pyramid form2MoO6Method for preparing material and catalytic use thereof

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