CN106944038B - 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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CN106944038B
CN106944038B CN201710129958.4A CN201710129958A CN106944038B CN 106944038 B CN106944038 B CN 106944038B CN 201710129958 A CN201710129958 A CN 201710129958A CN 106944038 B CN106944038 B CN 106944038B
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moo
catalysis material
methyl orange
degradation
solution
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CN106944038A (en
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孔泳
陈中平
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Changzhou Chengrui Energy Co ltd
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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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)
  • Physical Water Treatments (AREA)

Abstract

The present invention relates to a kind of Sb2MoO6The preparation and application of catalysis material.The following steps are included: preparation Sb2MoO6Catalysis material, by Sb2MoO6Material is applied to the degradation of water body common contaminant methyl orange.The beneficial effects of the present invention are: 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 the rapid economic development in our country, living standards of the people step 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 as a kind of allusion quotation The environmental contaminants of type, to environmental hazard maximum.This pollutant has high toxicity, fat-solubility, the feature of extended residual, And the methods of currently used water process means such as filtering, absorption are difficult to be removed.Since biography can be enriched in food chain It passs, persistence organic pollutant has serious harm to human health and ecological environment.Methyl orange is that typical persistence has Machine pollutant, and be widely used in industries such as printing and dyeing, textiles.The present invention chooses methyl orange as application, has one Fixed representativeness.
Methyl orange is a kind of azo dyes, and 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 that sunlight is absorbed and utilized, but also methyl orange itself is toxic, this is to 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 is shone, semiconductor light Electron transition in catalysis material valence band leaves hole to conduction band in valence band.Subsequent light induced electron and hole and ion or Molecule combines, and generates the living radical with oxidisability or reproducibility.This living radical can will be organic in water body Macromolecular mineralising is water and carbon dioxide, to achieve the purpose that degradable organic pollutant.Photocatalytic method is compared to traditional dirt Method for treating water has many advantages.Firstly, hole is easily acted on hydrone when carrying out photocatalysis in water body, oxidisability is formed Extremely strong hydroxyl radical free radical.The free radical can be extremely suitble in processing sewage with all organic substances of the mineralising of non-selectivity Organic principle.It, can be with by seeking the catalysis material of visible light absorbing secondly, photocatalytic method is using luminous energy as energy source Solar energy is effectively utilized, it is economic and environment-friendly.Finally, photochemical catalyst itself does not change in catalytic reaction process, therefore can To recycle, there is practicability.
Sb2MoO6Have the characteristics that chemical property is stable, cheap and production is easy, is 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 provide a kind of Sb2MoO6The preparation method of catalysis material.
Summary of the invention
The purpose of the present invention is 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, comprising the following steps:
A, Sb is prepared2MoO6Catalysis material: being added antimony trichloride in hydrochloric acid solution, continues to add molybdenum after mixing evenly Sour sodium dihydrate.Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h.The dark green solid that will be obtained Precipitation and centrifugal separation is simultaneously alternately washed each 3 times with dehydrated alcohol and ultrapure water, is put into baking oven drying, is obtained Sb2MoO6Photocatalysis material Material.
b、Sb2MoO6Catalysis material is applied to the methyl orange in degradation water: preparing certain density methyl orange solution, uses Sb made from step a2MoO6Methyl orange in catalysis material degradation water, while first is detected 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, records It degrades the time used.
Further, concentration of hydrochloric acid solution is 0.1~2mol/L in step a, and dosage is 30~80mL.
Further, antimony trichloride dosage is 0.1~10g in step a.
Further, sodium molybdate dihydrate dosage 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 present invention are: Sb2MoO6The preparation method of catalysis material is simple and to organic molecules such as methyl oranges Degradation rate it is very fast.
Detailed description of the invention
This experiment is further illustrated with reference to the accompanying drawing.
Fig. 1 is Sb in embodiment one2MoO6The X-ray diffractogram of catalysis material.
Fig. 2 is Sb in embodiment one2MoO6The uv drs 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 effect picture of methyl orange degradation.
Fig. 5 is initial influence of the concentration of hydrochloric acid to catalyst photocatalysis effect in embodiment three.
Specific embodiment
Presently in connection with specific embodiment, the present invention will be further described, following embodiment be intended to illustrate invention rather than Limitation of the invention further.
The percent of decolourization of the methyl orange solution shown in narration in detail of the invention and examples of implementation is to calculate as follows : certain density methyl orange solution is prepared, using the absorbance at ultraviolet-visible spectrophotometer measurement 465nm, is denoted as a0.It is sampled during UV degradation, using the absorbance at ultraviolet-visible spectrophotometer measurement 465nm, is denoted as an(n To sample number).Percent of decolourization bnIt is calculated by following formula:
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 antimony trichloride is added, after mixing evenly in its solution Middle addition 2.42g sodium molybdate dihydrate.Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h.It will be precipitated Dark green solid precipitation and centrifugal separation and alternately washed each 3 times with dehydrated alcohol and ultrapure water, be put into baking oven drying, be made Sb2MoO6Catalysis material.X ray diffracting spectrum is as shown in Fig. 1, shows that the made sample of the present invention is Sb2MoO6.Solid violet Outer diffusing reflection map is as shown in Fig. 2, shows Sb2MoO6Catalysis material has good absorbability to light.Scanning electron is aobvious Micro mirror image is as shown in Fig. 3, shows Sb2MoO6Catalysis material is sheet or club shaped structure.
Embodiment two:
Compound concentration is the methyl orange solution 500mL of 6mg/L, weighs the Sb of the preparation of embodiment one2MoO6Catalysis material 0.05g, in the methyl orange of the ultraviolet light irradiation decline Xie Shuizhong of 11W, sampling in each hour is primary, 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 Fig. 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, the hydrochloric acid solution of 1mol/L and 2mol/L measures 70mL respectively, 4.56g antimony trichloride is added, after mixing evenly in its solution Middle addition 2.42g sodium molybdate dihydrate.Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h.It will be precipitated Dark green solid precipitation and centrifugal separation and alternately washed each 3 times with dehydrated alcohol and ultrapure water, be put into baking oven 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 weighs the above-mentioned Sb of 0.05g respectively2MoO6Sample, in the methyl of the ultraviolet light irradiation decline Xie Shuizhong of 11W Orange, sampling in each hour is primary, using the characteristic absorption peak intensity of ultraviolet-uisible spectrophotometer detection methyl orange solution, calculates Solution percent of decolourization.As a result as shown in Fig. 5, photocatalysis effect is best when initial concentration of hydrochloric acid solution is 0.5mol/L.

Claims (3)

1. a kind of Sb2MoO6Catalysis material is applied to the methyl orange in degradation water, and steps are as follows:
A, Sb is prepared2MoO6Catalysis material: being added antimony trichloride in hydrochloric acid solution, continues to add sodium molybdate after mixing evenly Dihydrate;Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h;The dark green solid of precipitation is precipitated It is centrifugated and is alternately washed each 3 times with dehydrated alcohol and ultrapure water, be put into baking oven drying, obtain Sb2MoO6Catalysis material;
b、Sb2MoO6Catalysis material is applied to the methyl orange in degradation water: certain density methyl orange solution is prepared, with step a Sb obtained2MoO6Methyl orange in catalysis material degradation water, at the same it is molten using ultraviolet-uisible spectrophotometer detection methyl orange The characteristic absorption peak intensity of liquid;When characteristic absorption peak disappears, that is, illustrates that the methyl orange degradation in solution is complete, record degradation Time used.
2. a kind of Sb according to claim 12MoO6Catalysis material is applied to the methyl orange in degradation water, it is characterized in that: institute Stating concentration of hydrochloric acid solution in step a is 0.1~2mol/L, and antimony trichloride dosage is 0.1~10g, sodium molybdate dihydrate dosage For 0.05~5g, hydrochloric acid solution dosage is 30~80mL.
3. a kind of Sb according to claim 12MoO6Catalysis material is applied to the methyl orange in degradation water, it is characterized in that: institute The concentration for stating methyl orange solution in step b is 1~100mg/L, Sb2MoO6The concentration of catalysis material is 0.01~1g/L;Methyl The characteristic absorption peak of orange is at 465nm.
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CN108636457B (en) * 2018-05-25 2019-10-11 常州大学 A kind of APTES-Sb can be used for photochemical catalyst2WO6The preparation method of-GQDs composite material
CN113385168B (en) * 2021-06-10 2023-04-11 宁波大学 Sb in hexagonal pyramid shape 2 MoO 6 Method for preparing material and catalytic use thereof

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SU833540A1 (en) * 1979-09-21 1981-05-30 Институт Естественных Наукбурятского Филиала Co Ah Cccp Method of producing antimony molybdate
CN104843661B (en) * 2015-04-29 2017-06-16 岭南师范学院 A kind of preparation method without templated synthesis phosphoric acid antimony microballoon
CN105633390B (en) * 2016-01-07 2020-09-29 西安交通大学 Lithium/sodium ion battery negative electrode material Sb2MoO6And method for preparing the same
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

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