CN105498770A - Catalyst composition for degrading methylene blue dye in waste water as well as preparation method and application thereof - Google Patents

Catalyst composition for degrading methylene blue dye in waste water as well as preparation method and application thereof Download PDF

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CN105498770A
CN105498770A CN201510861372.8A CN201510861372A CN105498770A CN 105498770 A CN105498770 A CN 105498770A CN 201510861372 A CN201510861372 A CN 201510861372A CN 105498770 A CN105498770 A CN 105498770A
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methylene blue
preparation
catalyst
carbon monoxide
olefin polymeric
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CN105498770B (en
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周国华
汪彬
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Hubei University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
    • B01J23/686—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with molybdenum
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a ternary composite oxide Ag2Sb2MoO7 catalyst for degrading a methylene blue dye in waste water as well as a preparation method and an application thereof, and belongs to the field of inorganic functional material preparation technology. Silver salt, molybdenum salt, an antimony compound and citric acid are added into water in order, stirring is carried out for dissolving, glycol is added, temperature is raised to 100-130 DEG C, preferably 120 DEG C, and stirring is continuously carried out for forming gel; the gel is calcined at 500-1000 DEG C for 4-15 hours, preferably at 600-900 DEG C for 7 hours, and the Ag2Sb2MoO7 catalyst is prepared. The catalyst is used for effectively treating the methylene blue dye in waste water at normal temperature and normal pressure without oxidizing agents and light irradiation, and degradation rate of methylene blue exceeds 90%; the catalyst has the advantages of simple and rapid preparation, fast degradation speed of organic pollutants and substantial effects, low treatment cost without secondary pollution, etc. The catalyst can be recycled, and degradation rates of the catalyst in a second and a third cycle for the methylene blue dye both exceed 90.0%.

Description

A kind of carbon monoxide-olefin polymeric for methylene blue in waste dye degrades and its preparation method and application
Technical field
The invention belongs to inorganic functional material preparing technical field, relate to a kind of carbon monoxide-olefin polymeric of methylene blue in waste dye degrades, particularly relate to a kind of ternary compound oxides Ag for methylene blue in waste dye degrades 2sb 2moO 7catalysts and its preparation method and application.
Background technology
Current organic dye waste water has become one of main pollution source of water body.This waste water has that the water yield is large, concentration is high, complicated component, colourity are dark and the feature such as difficult degradation.Most of dyestuff also has toxicity, carcinogenicity, teratogenesis and mutagenic effect.Methylene blue is a kind of important organic chemical synthesis dye of positive ion, and commercial Application widely.Such as, can be applicable to fiber crops, silk fabric, the dyeing of paper and the painted of bamboo and wood, be applied to biology, bacterial organisms dyeing and be applied to manufacture ink and color lake etc.Methylene blue extensive use industrially also will cause containing methylene blue dye wastewater the severe contamination of water body.The processing method of current organic dye waste water mainly contains bioanalysis, Coagulation Method, high-level oxidation technology, photocatalytic method, absorption method and membrane separation process etc.Bioanalysis, by the impact of the factors such as pH value, temperature, salt and kind of dyes, makes the effect of Biochemical method not ideal enough.The operating cost of Coagulation Method is higher, and body refuse amount is large and dehydration is difficult, and the pH value range be suitable for is narrow.High-level oxidation technology cost is high, conventional oxidant also can show oxidability strong, there is the shortcomings such as selective oxidation, and easily introduce impurity in processing procedure and cause secondary pollution.Photocatalytic method needs light source irradiation system, large by weather effect in actual applications.Absorption method is subject to the impacts such as suspension in water and grease, and adsorbent amount is large and costly.Membrane separation process is divided into electroosmose process, hyperfiltration, nano filtering process and ultrafiltration etc., wherein the advantage of electroosmose process, hyperfiltration, nano filtering process is that dyestuff clearance is high, the dyestuff in waste water can be reclaimed, technique is simple, but the cost of film used is higher, operating pressure is comparatively large, causes the energy consumption of embrane method higher, have impact on its industrial applications.Traditional ultrafiltration is comparatively large due to membrane aperture, is difficult to remove low-molecular-weight organic pollution.Therefore, the catalyst developing a kind of simple and efficient process methylene blue dye wastewater has great importance.
Prior art discloses an application number is that the patent application " double-layer catalyst and preparation thereof and the application of this catalyst in the equal acid anhydride of preparation " of 201210145478.4 is containing effective dose active constituent V 2o 5, TiO 2, P 2o 5, Na 2o, MoO 3, Sb 2o 3, other metal compound and must crystalline substance respectively through weighings, dosing, join spray slurries, be sprayed on carrier, roasting, the processing step such as cooling make catalyst E, G, catalyst G, E are placed in respectively material mixed gas arrival end and the reaction gas port of export, equal acid anhydride is prepared under the condition such as low-speed, lower temperature, but this catalytic component is various, complicated process of preparation, and obtained catalyst need use under temperature is 400 ~ 430 DEG C of conditions, energy consumption is high.Present patent application inventor discloses several the prior aries relevant to present patent application before this, such as, application number be 201310014950.5 patent application " a kind of preparation method processing the carbon monoxide-olefin polymeric of methylene blue dye wastewater " and application number be 201210474494.8 patent " a kind of carbon monoxide-olefin polymeric for the treatment of methylene blue dye wastewater and its preparation method and application ", these two application respectively adopt general formula be K 2oCr 2o 3xMoO 3(x=1 ~ 8) and Na 2oCr 2o 3xMoO 3the ternary compound oxides of (x=1 ~ 8) is as catalyst degradation methylene blue dye wastewater, but the two degradation time is all longer, need more than 60min, therefore, still have to be developed go out a kind of NEW TYPE OF COMPOSITE oxide, while the above-mentioned dye degrades rate of guarantee, significantly shorten degradation time, improve degradation efficiency.And patent application of the present invention also inventor's achievement of making based on research institute further on the basis of aforementioned operation just, have developed the another kind of new and effective ternary compound oxides catalyst A g for methylene blue in waste dye degrades 2sb 2moO 7.
Summary of the invention
In view of the deficiencies in the prior art, the object of the invention is to solve the above-mentioned technical problem existed in prior art,
A kind of simple and effective carbon monoxide-olefin polymeric for methylene blue in waste dye degrades and its preparation method and application is provided.
To achieve these goals, the present invention obtains following technical scheme after being studied by lot of experiments:
A kind of carbon monoxide-olefin polymeric for methylene blue in waste dye degrades of the present invention is a kind of composite oxides, and the general formula of described composite oxides is Ag 2sb 2moO 7.
The preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades described above, described method comprises the steps:
(1) silver salt, antimonial, molybdenum salt and citric acid are added to the water successively, stirring and dissolving, the molybdenum in the silver in described silver salt, the antimony in antimonial, molybdenum salt and the mol ratio of citric acid are 2:2:1:5 ~ 20.
(2) add ethylene glycol, ethylene glycol addition is 3 times of citric acid molal quantity, after stirring 10min, is heated to 100 DEG C ~ 130 DEG C, continues to stir to form gel;
(3) gel is calcined 4 ~ 15 hours at 500 DEG C ~ 1000 DEG C, obtain ternary compound oxides Ag 2sb 2moO 7.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades described in technique scheme, wherein the calcining heat described in step (3) is 600 DEG C ~ 900 DEG C, and calcination time is 7 hours.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades described in technique scheme, the mol ratio of the silver wherein in silver salt described in step (1), the antimony in antimonial, the molybdenum in molybdenum salt and citric acid is 2:2:1: 11.0.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades described in technique scheme, wherein the silver salt described in step (1) is selected from silver nitrate.
Further, the preparation method of the carbon monoxide-olefin polymeric for described methylene blue in waste dye degrades described in technique scheme, the molybdenum salt described in step (1) is ammonium molybdate.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades described in technique scheme, the antimonial described in step (1) is antimony oxide and/or antimony chloride.
According to the method for above-mentioned carbon monoxide-olefin polymeric degrading waste water Methylene Blue dyestuff, comprise described carbon monoxide-olefin polymeric to be suspended in methylene blue dye wastewater and process.
The method of described methylene blue in waste dye degrades, preferably adds described composite oxides Ag in the ratio of 0.5 ~ 4.0g/L waste water 2sb 2moO 7, under agitation process 5 ~ 30 minutes.
Ternary compound oxides Ag of the present invention 2sb 2moO 7catalyst application in the processing method of methylene blue waste water is: with ternary compound oxides Ag 2sb 2moO 7for catalyst, degradation conditions is: methylene blue concentration is in 1mg/L ~ 90mg/L scope, and the catalyst amount processing often liter of methylene blue waste water is 0.5 ~ 4g, and solution system is in normal temperature and pressure.When methylene blue solution volume is 40mL, when concentration is 10mg/L, under agitation add catalyst 0.10g, catalytic degradation 10 minutes, the degradation rate of methylene blue reaches more than 90%.Residual solution color is colourless.Catalyst recycle use is carried out again after residual solution being replaced with new methylene blue solution.Result shows, the degradation rate of the methylene blue dye of catalyst in second time circulation, third time recycle all reaches more than 90.0%.
The present invention at normal temperatures and pressures, without the need to oxidant, effectively can process methylene blue dye wastewater under also penetrating without the need to illumination.Have catalytic degradation efficiency high, technological process is simple, and non-secondary pollution produces, and the feature such as operating cost is low, there is very high actual application value.
Compared with prior art, the method that the present invention relates to methylene blue in waste dye degrades has following significant advantage and significant progress:
(1) method for preparing catalyst of the present invention is simple.
(2) catalyst activity of the present invention is high, can in the short period of time fast and efficient degradation pollutant.
(3) method of wastewater treatment of the present invention can carry out at normal temperatures and pressures, and technological process is simple and cost is low.
(4) method of wastewater treatment of the present invention is without the need to using oxidant, does not also need to adopt any light source irradiation degraded system.
(5) catalyst of the present invention is repeatedly reusable.
Detailed description of the invention
Form is described in further detail foregoing of the present invention again by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
By 2.02g silver nitrate (1.19 × 10 -2mol), 1.06g Ammonium Molybdate Tetrahydrate (8.58 × 10 -4mol), 1.74g antimony oxide (5.95 × 10 -3and 12.61g citric acid (6.44 × 10 mol) -2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then adds 12.10g ethylene glycol (1.93 × 10 -1mol) stir 10min afterwards, be warmed up to 120 DEG C and continue to stir, until form gel, then gel is heated 7 hours at 600 DEG C, obtain ternary compound oxides Ag 2sb 2moO 7catalyst.
Get 0.10 gram of ternary compound oxides Ag prepared as stated above 2sb 2moO 7catalyst degradation methylene blue waste water, methylene blue concentration is 10mg/L, and volume is 40mL, under stirring in normal temperature and pressure catalysis degradation of methylene blue certain hour, then centrifugal on centrifuge, gets supernatant.Adopt spectrophotometer, measure absorbance in methylene blue maximum absorption wave strong point (660nm), be converted into the concentration of aqueous solution of methylene blue by absorbance-concentration working curve, result is as shown in table 1, when degradation time is 10 minutes, methylene blue degradation rate is 90.0%.
Table 1 degradation time and methylene blue dye degradation rate
Catalyst degradation time/min 3 6 10 14
Degradation rate/% 82.5 85.9 90.0 92.5
Embodiment 2
By 2.02g silver nitrate (1.19 × 10 -2mol), 1.06g Ammonium Molybdate Tetrahydrate (8.58 × 10 -4mol), 1.74g antimony oxide (5.95 × 10 -3and 12.61g citric acid (6.44 × 10 mol) -2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then adds 12.10g ethylene glycol (1.93 × 10 -1mol) stir 10min afterwards, be warmed up to 120 DEG C and continue to stir, until form gel, then gel is heated 7 hours at 700 DEG C, obtain ternary compound oxides Ag 2sb 2moO 7catalyst.
Get 0.10 gram of ternary compound oxides Ag prepared as stated above 2sb 2moO 7catalyst degradation methylene blue waste water, methylene blue concentration is 10mg/L, volume is 40mL, under stirring in normal temperature and pressure catalysis degradation of methylene blue 10 minutes, then, within centrifugal 10 minutes on centrifuge, get supernatant, adopt spectrophotometer, measure absorbance in methylene blue maximum absorption wave strong point (660nm), be converted into the concentration of aqueous solution of methylene blue by absorbance-concentration working curve, when degradation time is 10 minutes, methylene blue degradation rate is 91.8%.
Embodiment 3
By 2.02g silver nitrate (1.19 × 10 -2mol), 1.06g Ammonium Molybdate Tetrahydrate (8.58 × 10 -4mol), 1.74g antimony oxide (5.95 × 10 -3and 12.61g citric acid (6.44 × 10 mol) -2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, adds 12.10g ethylene glycol (1.93 × 10 -1mol) stir 10min afterwards, be warmed up to 120 DEG C and continue to stir, until form gel, gel is heated 7 hours at 900 DEG C, obtains ternary compound oxides Ag 2sb 2moO 7catalyst.
Get 0.10 gram of Ag prepared as stated above 2sb 2moO 7catalyst degradation methylene blue waste water, methylene blue concentration is 10mg/L, volume is 40mL, under stirring in normal temperature and pressure catalysis degradation of methylene blue 10 minutes, then, within centrifugal 10 minutes on centrifuge, get supernatant, adopt spectrophotometer, measure absorbance in methylene blue maximum absorption wave strong point (660nm), be converted into the concentration of aqueous solution of methylene blue by absorbance-concentration working curve, when degradation time is 10 minutes, methylene blue degradation rate is 92.3%.
Embodiment 4
Situation is recycled, the ternary compound oxides Ag that the preparation method of catalyst described in Example 3 obtains in order to what investigate catalyst 2sb 2moO 7carry out continuous three degradation of methylene blue dye tests.Each degradation time is 10 minutes.
Fill 40mL 10mg/L methylene blue solution beaker in add the ternary compound oxides Ag of 0.10g 2sb 2moO 7under magnetic agitation effect, after normal temperature and pressure catalysis is degraded 10 minutes, within centrifugal 10 minutes on centrifuge, get supernatant, adopt spectrophotometer, absorbance is measured in methylene blue maximum absorption wave strong point (660nm), the concentration of aqueous solution of methylene blue is converted into by absorbance-concentration working curve, by the supernatant dropper sucking-off after centrifugal, only leave catalyst solid part, add the 10mg/L methylene blue solution that 40mL is new, repeat above-mentioned degradation of methylene blue process, so recycle ternary compound oxides Ag 2sb 2moO 7catalyst carries out second time circulation, recycles degradation of methylene blue dye test for the third time, and result is as shown in table 2.
Table 2 catalyst circulation degradation of methylene blue dyestuff
Catalyst access times 1 2 3
Degradation rate/% 92.5 91.3 90.1
As can be seen from Table 2, the degradation rate of catalyst degradation of methylene blue dyestuff in three circulations is all more than 90.0%.This shows ternary compound oxides Ag 2sb 2moO 7catalyst can recycle.

Claims (10)

1. for a carbon monoxide-olefin polymeric for methylene blue in waste dye degrades, be a kind of composite oxides, it is characterized in that: the general formula of described composite oxides is Ag 2sb 2moO 7.
2. a preparation method for the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 1, is characterized in that: described method comprises the steps:
(1) silver salt, antimonial, molybdenum salt and citric acid are added to the water successively, stirring and dissolving, the molybdenum in the silver in described silver salt, the antimony in antimonial, molybdenum salt and the mol ratio of citric acid are 2:2:1:5 ~ 20.
(2) add ethylene glycol, ethylene glycol addition is 3 times of citric acid molal quantity, after stirring 10min, is heated to 100 DEG C ~ 130 DEG C, continues to stir to form gel;
(3) gel is calcined 4 ~ 15 hours at 500 DEG C ~ 1000 DEG C, obtain ternary compound oxides Ag 2sb 2moO 7.
3. the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 2, is characterized in that: the calcining heat described in step (3) is 600 DEG C ~ 900 DEG C.
4. the preparation method of the carbon monoxide-olefin polymeric of methylene blue in waste dye degrades according to Claims 2 or 3, is characterized in that: the calcination time described in step (3) is 7 hours.
5. the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 4, is characterized in that: the molybdenum in the silver in silver salt described in step (1), the antimony in antimonial, molybdenum salt and the mol ratio of citric acid are 2:2:1: 11.0.
6. the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 2, is characterized in that: the silver salt described in step (1) is selected from silver nitrate.
7. the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 2, is characterized in that: the molybdenum salt described in step (1) is ammonium molybdate.
8. the preparation method of the carbon monoxide-olefin polymeric for methylene blue in waste dye degrades according to claim 2, is characterized in that: the antimonial described in step (1) is antimony oxide and/or antimony chloride.
9. the method for carbon monoxide-olefin polymeric degrading waste water Methylene Blue dyestuff according to claim 1, is characterized in that: comprise described carbon monoxide-olefin polymeric to be suspended in methylene blue dye wastewater and process.
10. the method for methylene blue in waste dye degrades according to claim 9, is characterized in that: add described composite oxides Ag in the ratio of 0.5 ~ 4.0g/L waste water 2sb 2moO 7, under agitation process 5 ~ 30 minutes.
CN201510861372.8A 2015-11-30 2015-11-30 A kind of carbon monoxide-olefin polymeric and its preparation method and application for the degradation of methylene blue in waste dyestuff Expired - Fee Related CN105498770B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107055731A (en) * 2017-05-19 2017-08-18 宝鸡市金得利新材料有限公司 A kind of ternary compound oxides of efficient process Methyl Orange in Wastewater and its preparation method and application

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Publication number Priority date Publication date Assignee Title
CN1799691A (en) * 2006-01-13 2006-07-12 南京大学 Visible light responsible photocatalytic material of Ag2ZO4 type composite oxide, its preparation and application
CN104815654A (en) * 2015-04-09 2015-08-05 湖北文理学院 Visible light nano composite photocatalysis material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1799691A (en) * 2006-01-13 2006-07-12 南京大学 Visible light responsible photocatalytic material of Ag2ZO4 type composite oxide, its preparation and application
CN104815654A (en) * 2015-04-09 2015-08-05 湖北文理学院 Visible light nano composite photocatalysis material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107055731A (en) * 2017-05-19 2017-08-18 宝鸡市金得利新材料有限公司 A kind of ternary compound oxides of efficient process Methyl Orange in Wastewater and its preparation method and application
CN107055731B (en) * 2017-05-19 2019-04-30 宝鸡文理学院 A kind of ternary compound oxides and its preparation method and application of efficient process Methyl Orange in Wastewater

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