CN105836802A - MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof - Google Patents
MoO3 wet catalyst for degradation of dye wastewater and preparation method thereof Download PDFInfo
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- CN105836802A CN105836802A CN201610184807.4A CN201610184807A CN105836802A CN 105836802 A CN105836802 A CN 105836802A CN 201610184807 A CN201610184807 A CN 201610184807A CN 105836802 A CN105836802 A CN 105836802A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J23/16—Catalysts 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a MoO3 wet catalyst for degradation of dye wastewater and a preparation method thereof. The method is as below: adding (NH4)6MoO7O24.4H2O to water to obtain a clarified solution, dropwise adding nitric acid into the clarified solution, stirring to obtain a suspension liquid, then transferring the suspension liquid to a high pressure hydrothermal reaction kettle for hydrothermal reaction, naturally cooling, filtering, washing by water and ethanol three times each, drying to obtain a light blue pure MoO3 catalyst; and calcining the pure MoO3 catalyst at 200-500 DEG C to obtain a target product of light green MoO3 wet catalyst. The MoO3 catalyst prepared by the invention has good catalytic performance, and can effectively degrade high concentration dye wastewater under the condition of normal temperature, normal pressure and no illumination.
Description
Technical field
The invention belongs to wet oxidizing catalyst and dye wastewater degradation technical field, be specifically related to a kind of MoO for degradation of dye waste water3Catalytic wet agent and preparation method thereof.
Background technology
Waste water from dyestuff is one of typical difficult for biological degradation organic wastewater.Colourity is deep, COD concentration is high, alkalescence is big, organic principle is complicated, salinity is high, biodegradability is poor, discharge capacity is big, intractability height dyestuff enters environment in producing and using, wherein have possibly together with carcinogen such as phenyl ring, amido, azo groups, serious environment pollution, the especially chroma pollution of waste water from dyestuff is particularly acute, and uses conventional biological treatment removal effect not ideal enough.And colored water is known from experience and affect the transmission of sunlight, being unfavorable for hydrobiological growth and breeding, and then affect the self purification of water body, additionally, waste water from dyestuff major part meta-alkalescence, entrance farmland can make saline Land.At present, it has been recognized that, wet oxidation process is to process high concentration, and toxicity is big, the effective ways of the organic wastewater of biological degradability difference, and its advantage such as also to have floor space little, non-secondary pollution；But its actual popularization also suffers from limiting, the reaction temperature being primarily due to wet oxidation process requirement is higher, generally 220-320 DEG C, thus there is the defect high to equipment requirements, energy consumption is big, additionally reaction needs to maintain High Temperature High Pressure just can carry out, so the waste water being only applicable to the high concentration of low discharge processes；For the waste water of low concentration, it not the most very economical, be the most just that this limits the further genralrlization of wet air oxidation technology.CWO technology is the new technique with certain competitiveness grown up on the basis of traditional wet oxidation process the seventies.It is primarily referred to as adding suitable catalyst in original technology, thus reduces the temperature and pressure of reaction, improves oxidative decomposition capacity, shortens the response time, prevents and reduce cost, and then overcome the reaction condition of the High Temperature High Pressure of wet oxidation process.Molybdenum and molybdenum alloy material not only have good high temperature strength and hardness, but also have good conduction, heat conduction, the performance such as anticorrosive.MoO3It is not only the primary raw material preparing molybdenum and molybdenum alloy, and itself also there is the characteristics such as electrochromism, photochromic, photocatalytic degradation and air-sensitive, therefore in terms of many functional materials such as synthesizing sensitive element, catalyst, fast-ionic conductor, there is specific use.
Summary of the invention
Present invention solves the technical problem that and there is provided a kind of simple to operate and eco-friendly MoO for degradation of dye waste water3Catalytic wet agent and preparation method thereof.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, for the MoO of degradation of dye waste water3Catalytic wet agent, it is characterised in that prepared by following methods: by (NH4)6MoO7O24·4H2O is added to the water and obtains settled solution, salpeter solution is dripped in above-mentioned settled solution, continue stirring after being added dropwise to complete and obtain suspension, it is transferred in high-pressure hydrothermal reaction kettle carry out hydro-thermal reaction by above-mentioned suspension again, then natural cooling, filtering, water and ethanol are respectively washed three times, are dried to obtain nattier blue pure MoO3Catalyst, finally by pure MoO3Catalyst obtains the absinthe-green MoO of target product in 200-500 DEG C of calcining3Catalytic wet agent.
MoO for degradation of dye waste water of the present invention3The preparation method of catalytic wet agent, it is characterised in that concretely comprise the following steps:
(1) by 1.86g (NH4)6MoO7O24·4H2O joins in 15mL deionized water, and stirring and dissolving obtains settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in above-mentioned settled solution, continues stirring 10min after being added dropwise to complete and obtain milk-white coloured suspension；
(3) being transferred to by suspension in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, naturally cool to room temperature and filter, water and ethanol are respectively washed three times, are then dried to obtain nattier blue pure MoO in 80 DEG C in thermostatic drying chamber3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace and obtains the absinthe-green MoO of target product in 200-500 DEG C of calcining3Catalytic wet agent.
Further preferably, the calcining heat in step (4) is preferably 400 DEG C.
MoO prepared by the present invention3Catalyst has good catalytic performance, at normal temperature and pressure and under conditions of not having illumination, it is possible to the waste water from dyestuff of efficient degradation high concentration, has potential using value in the treatment technology of degradable organic pollutant.
Accompanying drawing explanation
Fig. 1 is the MoO that embodiment of the present invention 1-7 prepares3The degradation property curve of catalytic wet agent；
Fig. 2 is the MoO that embodiment of the present invention 1-7 prepares3The XRD figure spectrum of catalytic wet agent；
Fig. 3 is the MoO that the embodiment of the present invention 1 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 4 is the MoO that the embodiment of the present invention 2 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 5 is the MoO that the embodiment of the present invention 3 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 6 is the MoO that the embodiment of the present invention 4 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 7 is the MoO that the embodiment of the present invention 5 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 8 is the MoO that the embodiment of the present invention 6 prepares3The SEM collection of illustrative plates of catalytic wet agent；
Fig. 9 is the MoO that the embodiment of the present invention 7 prepares3The SEM collection of illustrative plates of catalytic wet agent.
Calcining heat is to MoO as shown in Figure 13The catalytic performance of catalyst has important impact, and when calcining heat is 400 DEG C at normal temperatures and pressures, degradation effect is best.
Sample being carried out X-ray diffraction analysis, is shown by XRD result, this catalyst has crystal conversion, MoO when 300 DEG C3-MoO3The principal crystalline phase of-3 samples is all h-MoO3, and MoO3-4-MoO3The principal crystalline phase of-7 samples is all r-MoO3。
Fig. 3-9 explanation calcining heat affects MoO3The pattern of catalyst, when not calcining, catalyst surface is smooth and is hexa-prism, and along with the increase of calcining heat, six prismatic surface gradually ftracture, column structure is also destroyed, split into laminated structure, when calcining heat is 700 DEG C, being completely dispersed and come, catalytic degradation performance also drastically reduces.
Detailed description of the invention
Being described in further details the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all technology realized based on foregoing of the present invention belong to the scope of the present invention.
Embodiment 1
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst, is labeled as MoO3；
MoO3Catalyst is degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 69.67%.
Embodiment 2
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 200 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-2；
MoO3-2 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 80.06%.
Embodiment 3
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 300 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-3；
MoO3-3 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 73.01%.
Embodiment 4
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 400 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-4；
MoO3-4 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 85.86%.
Embodiment 5
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 500 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-5；
MoO3-5 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 74.31%.
Embodiment 6
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 600 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-6；
MoO3-6 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 68.96%.
Embodiment 7
(1) by 1.86g
(NH4)6MoO7O24·4H2O solid particle joins in 15mL deionized water, and magnetic agitation dissolves to obtain settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in settled solution, continues stirring 10min after being added dropwise to complete and obtain milky suspension；
(3) suspension is transferred in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, then room temperature is naturally cooled to through filtering, after water and ethanol respectively wash three times, it is placed in thermostatic drying chamber and obtains nattier blue pure MoO in 80 DEG C of dry 3h3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace to be calcined in 700 DEG C, finally gives the absinthe-green MoO of target product3Catalytic wet agent, is labeled as MoO3-7；
MoO3-7 catalyst are degraded the rhdamine B waste water of 5mg/L at normal temperatures and pressures, and the degradation rate of 3h is 8.26%.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; under the scope without departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements each fall within the scope of protection of the invention.
Claims (3)
1. for the MoO of degradation of dye waste water3Catalytic wet agent, it is characterised in that prepared by following methods: by (NH4)6MoO7O24·4H2O is added to the water and obtains settled solution, salpeter solution is dripped in above-mentioned settled solution, continue stirring after being added dropwise to complete and obtain suspension, it is transferred in high-pressure hydrothermal reaction kettle carry out hydro-thermal reaction by above-mentioned suspension again, then natural cooling, filtering, water and ethanol are respectively washed three times, are dried to obtain nattier blue pure MoO3Catalyst, finally by pure MoO3Catalyst obtains the absinthe-green MoO of target product in 200-500 DEG C of calcining3Catalytic wet agent.
2. the MoO for degradation of dye waste water described in a claim 13The preparation method of catalytic wet agent, it is characterised in that concretely comprise the following steps:
(1) by 1.86g (NH4)6MoO7O24·4H2O joins in 15mL deionized water, and stirring and dissolving obtains settled solution；
(2) under conditions of magnetic agitation, the salpeter solution that 4.77mL molar concentration is 2.2mol/L is added drop-wise in above-mentioned settled solution, continues stirring 10min after being added dropwise to complete and obtain milk-white coloured suspension；
(3) being transferred to by suspension in the high-pressure hydrothermal reaction kettle of teflon gasket in 170 DEG C of hydro-thermal reactions 24h, naturally cool to room temperature and filter, water and ethanol are respectively washed three times, are then dried to obtain nattier blue pure MoO in 80 DEG C in thermostatic drying chamber3Catalyst；
(4) the pure MoO that will obtain3Catalyst is placed in Muffle furnace and obtains the absinthe-green MoO of target product in 200-500 DEG C of calcining3Catalytic wet agent.
MoO for degradation of dye waste water the most according to claim 23The preparation method of catalytic wet agent, it is characterised in that: the calcining heat in step (4) is preferably 400 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107706407A (en) * | 2017-10-23 | 2018-02-16 | 陕西科技大学 | A kind of pure phase lithium ion battery negative material Mo4O11Synthetic method |
| CN113181898A (en) * | 2021-03-31 | 2021-07-30 | 南京信息工程大学 | Catalyst for low-temperature degradation of low-density polyethylene and application thereof |
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| CN113181898A (en) * | 2021-03-31 | 2021-07-30 | 南京信息工程大学 | Catalyst for low-temperature degradation of low-density polyethylene and application thereof |
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Application publication date: 20160810 |