CN107055731A - A kind of ternary compound oxides of efficient process Methyl Orange in Wastewater and its preparation method and application - Google Patents
A kind of ternary compound oxides of efficient process Methyl Orange in Wastewater and its preparation method and application Download PDFInfo
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- CN107055731A CN107055731A CN201710356033.3A CN201710356033A CN107055731A CN 107055731 A CN107055731 A CN 107055731A CN 201710356033 A CN201710356033 A CN 201710356033A CN 107055731 A CN107055731 A CN 107055731A
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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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
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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
- B01J23/16—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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- 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
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a kind of ternary compound oxides of efficient process Methyl Orange in Wastewater and its preparation method and application, belong to field of waste water treatment.The preparation method includes：Lanthanum salt, molybdenum salt, cerium salt and citric acid are added to the water, sequentially add to be formed under DTAC and ethylene glycol, condition of water bath heating and be calcined 1 2h after gel, gel drying at 280 400 DEG C, 7 15h are calcined at 600 800 DEG C again, ternary compound oxides are obtained.The ternary compound oxides activity that the present invention is obtained is high, at normal temperatures and pressures, without can effectively handle Methyl Orange in Wastewater under illumination condition, has very high clearance to the Methyl Orange in Wastewater of various concentrations, and the ternary compound oxides can be reused.
Description
Technical field
The invention belongs to field of waste water treatment, and in particular to a kind of composite oxides of processing Methyl Orange in Wastewater and its preparation
Method.
Background technology
With the rapid development of economy, the rapid growth of modern industry, the development of industry, it is toxic be difficult to explain it is organic
The discharge capacity of waste water also rolls up, the development of the industry such as medicine, chemical industry and dyestuff, more causes the used water difficult to degradate of high content to increase
Many, the COD of this kind of waste water is generally very high, and most representational in organic wastewater is exactly Methyl Orange in Wastewater, the row of methyl orange
Put and come from the industries such as weaving, plastics, papermaking, leather, what methyl orange was brought to fresh water is not singly color stain, a small amount of methyl
Orange can also hinder sunlight in the permeability of water, so that the serious existence that have impact on organism in water, destruction organism in water ecology
How balance, along with hypertoxicity and carcinogenicity that methyl orange has, therefore effectively handle organic wastewater and receive extensive concern,
Although existing patent discloses the material of a variety of catalytic degradation methyl oranges, there is various limitations or deficiency.
Patent 201410146893.0《A kind of method of perovskite/polysaccharide composite photocatalyst for degrading methyl orange》Disclose
Perovskite oxide is prepared using agglutinating nature yeast, then perovskite is combined with chitosan, the composite photo-catalyst prepares numerous
It is trivial, and degraded methyl orange is to need the 470-490min under ultraviolet light, and the degradation efficiency of first time is no more than 70%.
Patent 201410526490.9《A kind of synthesis of AgI bases inorganic-organic hybridization semi-conducting material and photocatalytic degradation
The application of dyestuff》Disclose and the organic component containing N, S atom is introduced in inorganic AgI semiconductor systems, but need also exist for
75min is radiated under ultraviolet light.
Patent 201510373800.2《A kind of Microbe synthesis method of iron content active matter and its methyl orange degradation be catalyzed lead
The application in domain》, the catalyst includes iron content active matter 73%, citric acid 20% and titanium dioxide 7%, wherein utilizing ferrous oxide
Bacillus reacts obtained iron content active matter with ferrous sulfate, and it is higher that the catalyst produces activity using iron content active matter in water
Fe(OH)2+、Fe2(OH)2 4+, these materials organic acid, oxygen effect under cooperate with titanium dioxide generation strong oxidizing property it is oxygen-containing
Free radical, the catalyst needs biological culture 1-3 days, and ferrous oxide bacillus activity there are certain requirements, and existing biological culture
Yield to be far below chemical synthesis process.
Patent 201410579948.7《A kind of modified graphene of efficient absorption methyl orange dye and preparation method thereof》It is public
Open Effect of Water Soluble Quaternary Ammonium Salt of Chitosan by chemical action, graphene has been modified, improved graphene to methyl orange dye
Absorption property, but when methyl orange concentration be higher than 50mg/L when adsorption rate reduce, only less than 87%.
The content of the invention
Additional light source is not needed to handle the three of a large amount of Methyl Orange in Wastewater under the conditions of irradiating it is an object of the invention to provide a kind of
First composite oxides and its preparation method and application.
In order to realize the purpose of the present invention, by lot of experiments research and unremitting effort, following technical scheme is finally obtained：
A kind of ternary compound oxides preparation method of efficient process Methyl Orange in Wastewater, comprises the following steps：
(1) lanthanum salt, molybdenum salt, cerium salt and citric acid are taken, is sequentially added in water, stirring and dissolving obtains mixed solution, wherein lanthanum
Lanthanum in salt, the molybdenum in molybdenum salt, the cerium in cerium salt, the mol ratio of citric acid and water are (0.07-0.12)：1：(4-8)：(10-
15)：(80-200)；
(2) it is slowly added dropwise while stirring in mixed solution after DTAC, completion of dropping and is further continued for stirring
10-15min is mixed, DTAC addition is lanthanum, molybdenum, the 5-8% of three kinds of element mole total amounts of cerium；
(3) mixed solution for obtaining step (2) heating water bath at 70-90 DEG C, while adding ethylene glycol, ethylene glycol adds
It is 1-1.8 times of citric acid mole to enter amount, continues to stir until forming gel；
(4) particle will be ground to form after gel drying, obtained dry gel particle is calcined 1-2h at 280-400 DEG C, then
7-15h is calcined at 600-800 DEG C, ternary compound oxides are obtained.
Preferably, the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein step (1) lanthanum salt
In lanthanum, the molybdenum in molybdenum salt, the mol ratio of the cerium in cerium salt and citric acid be 0.1：1：6：13.
Preferably, done in the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein step (4)
Gel particle is calcined at 300-350 DEG C, then calcines 9-11h at 680-750 DEG C.
Preferably, the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein the lanthanum salt is
Lanthanum nitrate or lanthanum chloride.
Preferably, the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein the molybdenum salt is
Ammonium Molybdate Tetrahydrate or nitric acid molybdenum.
Preferably, the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein the cerium salt is
Any one in cerous nitrate, cerous sulfate or cerium chloride.
Preferably, the ternary compound oxides preparation method of above-mentioned efficient process Methyl Orange in Wastewater, wherein the water is steaming
Distilled water or deionized water.
In addition, the present invention also provides the ternary compound oxides that above-mentioned ternary compound oxides preparation method is obtained.
Further, the present invention also provides and handles the method containing Methyl Orange in Wastewater using above-mentioned ternary compound oxides, will
The ternary compound oxides are suspended in containing being handled in Methyl Orange in Wastewater.
It is further preferred that method of the above-mentioned processing containing Methyl Orange in Wastewater, in 0.4-4g/L ratio to Methyl Orange in Wastewater
In add the ternary compound oxides, then stirring at normal temperature processing 0.5-2h.
The present invention has the following technical effect that relative to prior art：
Ternary compound oxides preparation method of the present invention is simple, and obtained ternary compound oxides activity is high, can compared with
Quickly and efficiently degraded in short time methyl orange pollutant, methyl orange clearance can reach more than 93%；The tri compound oxygen
Compound can carry out catalytic degradation to Methyl Orange in Wastewater at normal temperatures and pressures, be not required to additional any light source and be irradiated；It can use
Carry out Methyl Orange in Wastewater of the concentration for the treatment of in below 100mg/L any concentration；Obtained ternary compound oxides can be repeated several times
Utilize, methyl orange clearance still reaches more than 89.7% after three circulations.
Embodiment
The embodiment to the present invention is described further below.
Embodiment 1
Weigh 0.65g lanthanum nitrates (1.50 × 10-3Mol), 3.53g Ammonium Molybdate Tetrahydrates (2.86 × 10-3mol)、34.97g
Cerous nitrate (9 × 10-2Mol) and 38.47g citric acids (0.2mol), (1.61mol), magnetic agitation are added sequentially in 28.9g water
To being completely dissolved, then 1.62g DTACs (6.14 × 10 are slowly added dropwise-3Mol), continue to stir 10min；
Above-mentioned mixed solution is stirred while addition 12.42g ethylene glycol (0.2mol), continues to stir under 75 DEG C of water bath conditions
Mix, until forming gel；
Obtained gel is dried in baking oven, xerogel particle is ground to form into agate mortar, obtained particle exists
1h is first calcined at 280 DEG C in Muffle furnace, then is warming up at 620 DEG C and calcines 8h, ternary compound oxides are obtained.
Embodiment 2
Weigh 1.04g lanthanum nitrates (2.4 × 10-3Mol), 3.53g Ammonium Molybdate Tetrahydrates (2.86 × 10-3mol)、58.28g
Cerous nitrate (0.15mol) and 53.85g citric acids (0.28mol), are added sequentially in 70g water (3.89mol), magnetic agitation is extremely
It is completely dissolved, then 3.59g DTACs (1.36 × 10 is slowly added dropwise-2Mol), continue to stir 15min；
Above-mentioned mixed solution is stirred while addition 41g ethylene glycol (0.66mol), continues to stir under 90 DEG C of water bath conditions
Mix, until forming gel；
Obtained gel is dried in baking oven, xerogel particle is ground to form into agate mortar, obtained particle exists
2h is first calcined at 380 DEG C in Muffle furnace, then is warming up at 790 DEG C and calcines 11h, ternary compound oxides are obtained.
Embodiment 3
Weigh 0.87g lanthanum nitrates (2 × 10-3Mol), 3.53g Ammonium Molybdate Tetrahydrates (2.86 × 10-3Mol), 46.62g nitre
Sour cerium (0.12mol) and 50g citric acids (0.26mol), are added sequentially in 40g water (2.23mol), magnetic agitation to completely it is molten
Solution, then 2.62g DTACs (9.9 × 10 are slowly added dropwise-3Mol), continue to stir 15min；
Above-mentioned mixed solution is stirred while addition 41g ethylene glycol (0.66mol), continues to stir under 80 DEG C of water bath conditions
Mix, until forming gel；
Obtained gel is dried in baking oven, xerogel particle is ground to form into agate mortar, obtained particle exists
2h is first calcined at 340 DEG C in Muffle furnace, then is warming up at 700 DEG C and calcines 13h, ternary compound oxides are obtained.
Embodiment 4
Weigh 2.22g lanthanum chlorides (9 × 10-3Mol), the water nitric acid molybdenums (1.13 × 10 of 5g five-2Mol), 19.5g cerium chlorides
(7.9×10-2Mol) and 28.23g citric acids (0.15mol), it is added sequentially in 30.5g water (1.69mol), magnetic agitation is extremely
It is completely dissolved, then 1.83g DTACs (6.9 × 10 is slowly added dropwise-3Mol), continue to stir 12min；
Above-mentioned mixed solution is stirred while addition 14g ethylene glycol (0.23mol), continues to stir under 850 DEG C of water bath conditions
Mix, until forming gel；
Obtained gel is dried in baking oven, xerogel particle is ground to form into agate mortar, obtained particle exists
1.5h is first calcined at 340 DEG C in Muffle furnace, then is warming up at 750 DEG C and calcines 10h, composite oxides are obtained.
Embodiment 5：Adsorption of Methyl Orange effect detection
Each 0.05g of composite oxide catalysts that embodiment 1-4 is obtained is weighed, 100ml conical flasks are put into, added
50ml50mg/L methyl orange solution, is placed on magnetic stirring apparatus, and normal temperature is slowly stirred 1h, and (flowing water is fast in simulation sewage treatment plant
Degree), solution is filtered after the completion of absorption, filtrate is then surveyed into its extinction with ultraviolet-uisible spectrophotometer at wavelength 463nm
Degree, methyl orange solution concentration during adsorption equilibrium is converted into according to absorbance-concentration working curve, and then calculate methyl orange
Clearance R%.
Methyl orange after R%={ (Co-Ct)/Co } × 100, wherein Co-methyl orange initial concentration (mg/L), Ct -1h
Concentration (mg/L).
The different composite oxide adsorbent methyl orange of table 1
As known from Table 1, the composite oxides that the present invention is prepared have significant adsoption catalysis effect to methyl orange, and
More than 93.4 % are up to the clearance of methyl orange, highest can reach 98.1%.
Embodiment 6
The composite oxides that Example 1-4 is prepared, the addition of composite oxides is in the same manner as in Example 5, changes
It is respectively 30min, 1h, 1.5h to become mixing time, investigates methyl orange clearance, obtains result as shown in table 2.
The different mixing time Methyl Orange clearances of table 2
As known from Table 2, upon agitation between from 30min to 1h when, the increase of Adsorption of Methyl Orange rate is notable, when from 1h to 1.5h
When, Adsorption of Methyl Orange rate improves unobvious, therefore in actual treatment, selection composite oxides add mixing time after methyl orange
Higher than 30min, mixing time is in 1h or so, no more than 1.5h.
Embodiment 7
The composite oxides that embodiment 2 is obtained are weighed, are added into methyl orange solution, other steps and embodiment 5
Identical, it is 25mg/L, 50mg/L, 75mg/L, 100mg/L to change methyl orange solution concentration, investigates its clearance, obtains such as table 3
Shown result.
The various concentrations methyl orange solution clearance of table 3
It was found from the data of table 3, the ternary compound oxides that the present invention is obtained are less than 100mg/L Methyl Orange in Wastewater to concentration
Treatment effect is notable, and clearance can reach more than 96.58%.
Embodiment 7
Embodiment 5 is adsorbed for the first time terminate after, remaining methyl orange solution is replaced with the methyl orange solution of same initial concentration
Change, then be slowly stirred at normal temperatures after 1h, filtering solution surveys the absorbance of filtrate at wavelength 463nm
The circulation of the ternary compound oxides of table 4 removes methyl orange solution data
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Second of clearance (%) | 91.8 | 97.5 | 93.1 | 94.8 |
| Third time clearance (%) | 89.7 | 95.3 | 91.8 | 92.7 |
From table 4, it can be seen that can repeatedly to circulate removal methyl orange molten for the ternary compound oxides that prepare of the present invention
Liquid, after three circulations, methyl orange clearance still can reach more than 89.7%.
Embodiment 8
Weigh 0.44g lanthanum nitrates (3.0 × 10-3Mol), 3.53g Ammonium Molybdate Tetrahydrates (2.86 × 10-3Mol), 15.54g
Cerous nitrate (0.04mol), remaining material dosage and process as described in Example 1, obtain composite oxides, weigh 0.05g and obtain
Composite oxides, the processing procedure as described in embodiment 5 is added in 50mg/L methyl orange solutions, and measuring methyl orange clearance is
71.9%.
Weigh 1.30g lanthanum nitrates (1.0 × 10-3Mol), 3.53g Ammonium Molybdate Tetrahydrates (2.86 × 10-3Mol), 77.70g
Cerous nitrate (0.2mol), remaining material dosage and process as described in Example 1, obtain composite oxides, weigh what 0.05g was obtained
Composite oxides, the processing procedure as described in embodiment 5 is added in 50mg/L methyl orange solutions, is measured methyl orange clearance and is
82.4%.
Therefore when lanthanum element, molybdenum element and Ce elements ratio are outside 1-4 of embodiment of the present invention scopes of disclosure, to methyl
The clearance of orange solution is far below clearance of the ternary compound oxides of the invention prepared to methyl orange solution.
Claims (9)
1. a kind of ternary compound oxides preparation method of efficient process Methyl Orange in Wastewater, it is characterised in that this method includes as follows
Step：
(1) lanthanum salt, molybdenum salt, cerium salt and citric acid are taken, is sequentially added in water, stirring and dissolving obtains mixed solution, wherein in lanthanum salt
Lanthanum, the molybdenum in molybdenum salt, the cerium in cerium salt, the mol ratio of citric acid and water be (0.07-0.12)：1：(4-8)：(10-15)：
(80-200)；
(2) it is slowly added dropwise while stirring in mixed solution after DTAC, completion of dropping and is further continued for stirring 10-
15min, DTAC addition is lanthanum, molybdenum, the 5-8% of three kinds of element mole total amounts of cerium；
(3) mixed solution for obtaining step (2) heating water bath at 70-90 DEG C, while adding ethylene glycol, ethylene glycol addition
For 1-1.8 times of citric acid mole, continue to stir until forming gel；
(4) particle will be ground to form after gel drying, obtained dry gel particle is calcined 1-2h at 280-400 DEG C, then in 600-
7-15h is calcined at 800 DEG C, ternary compound oxides are obtained.
2. ternary compound oxides preparation method according to claim 1, it is characterised in that：Lanthanum in step (1) lanthanum salt,
The mol ratio of molybdenum in molybdenum salt, the cerium in cerium salt and citric acid is 0.1：1：6：13.
3. ternary compound oxides preparation method according to claim 1, it is characterised in that：Xerogel in step (4)
Grain is calcined at 300-350 DEG C, then calcines 9-11h at 680-750 DEG C.
4. ternary compound oxides preparation method according to claim 1, it is characterised in that：The lanthanum salt be lanthanum nitrate or
Person's lanthanum chloride.
5. ternary compound oxides preparation method according to claim 1, it is characterised in that：The molybdenum salt is four hydration molybdenums
Sour ammonium or nitric acid molybdenum.
6. ternary compound oxides preparation method according to claim 1, it is characterised in that：The cerium salt is cerous nitrate, sulphur
Any one in sour cerium or cerium chloride.
7. ternary compound oxides preparation method according to claim 1, it is characterised in that：The water is distilled water or gone
Ionized water.
8. the method that the ternary compound oxides described in a kind of utilization claim any one of 1-7 handle Methyl Orange in Wastewater, it is special
Levy and be：The ternary compound oxides are suspended in Methyl Orange in Wastewater and handled.
9. the method containing Methyl Orange in Wastewater is handled according to claim 8, it is characterised in that：In 0.4-4g/L ratio to first
The ternary compound oxides are added in base orange waste water, then stirring at normal temperature processing 0.5-2h.
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| CN109987622A (en) * | 2019-04-10 | 2019-07-09 | 宁波大学 | A kind of cobalt doped lanthanum molybdate micro Nano material and preparation method thereof |
| CN110759457A (en) * | 2019-10-30 | 2020-02-07 | 武汉大学 | Method for removing organic pollutants in water based on perovskite oxide |
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| CN104307538A (en) * | 2014-10-13 | 2015-01-28 | 东南大学 | Preparation and application methods of high-efficiency composite photocatalytic material |
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| US20170001186A1 (en) * | 2015-07-01 | 2017-01-05 | Umm Al-Qura University | Zinc-based nanohybrids, devices and methods thereof |
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| CN109987622A (en) * | 2019-04-10 | 2019-07-09 | 宁波大学 | A kind of cobalt doped lanthanum molybdate micro Nano material and preparation method thereof |
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| CN110759457A (en) * | 2019-10-30 | 2020-02-07 | 武汉大学 | Method for removing organic pollutants in water based on perovskite oxide |
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