CN105498753A - Catalyst composition for methylene blue dye wastewater treatment as well as preparation method and application thereof - Google Patents
Catalyst composition for methylene blue dye wastewater treatment as well as preparation method and application thereof Download PDFInfo
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- CN105498753A CN105498753A CN201510863375.5A CN201510863375A CN105498753A CN 105498753 A CN105498753 A CN 105498753A CN 201510863375 A CN201510863375 A CN 201510863375A CN 105498753 A CN105498753 A CN 105498753A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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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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- 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
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention relates to catalyst composition for methylene blue dye wastewater treatment as well as a preparation method and an application thereof and belongs to the technical field of preparation of inorganic functional materials. A potassium compound, a manganese salt, molybdate and citric acid are sequentially added to water and stirred to be dissolved, then glycol is added, and the mixture is heated to 100-130 DEG C and continuously stirred to form gel; the gel is calcined at the temperature of 500-900 DEG C for 4-15 h, preferably, at the temperature of 550-700 DEG C for 7 h, and a ternary composite oxide K2Mn(MoO4)2 catalyst is prepared. Methylene blue dye wastewater can be effectively treated by the aid of the catalyst at the normal temperature and under the normal pressure without an oxidizing agent and light irradiation, the methylene blue degradation rate is higher than 95%, and the catalyst has the advantages of simplicity and rapidness in preparation, high organic pollutant degradation speed, significant organic pollutant degradation effect, low treatment cost, avoidance of secondary pollution and the like. The catalyst can be recycled and has methylene blue dye degradation rates higher than 95.0% when recycled for second and third times.
Description
Technical field
The invention belongs to inorganic functional material preparing technical field, relate to a kind of carbon monoxide-olefin polymeric for methylene blue dye wastewater process, particularly relate to a kind of ternary compound oxides K for methylene blue dye wastewater process
2mn (MoO
4)
2catalysts 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.
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.In addition, application number is 201510425576.7 application discloses and a kind ofly process carbon monoxide-olefin polymeric of methylene blue waste water and its preparation method and application, and this carbon monoxide-olefin polymeric is ternary compound oxides K
2cuMo
2o
8, the ternary compound oxides K of this application
2cuMo
2o
8catalyst is by potassium compound, mantoquita, molybdate and citric acid, is added to the water successively, stirring and dissolving, then add a certain amount of ethylene glycol, be heated to 100 ~ 130 DEG C, continue to stir formation gel, then gel is calcined at 300 ~ 1000 DEG C 4 ~ 15 hours obtained, obtained K
2cuMo
2o
8catalyst application is in the catalytic degradation of methylene blue waste water, catalytic degradation 10 minutes, the degradation rate of methylene blue reaches more than 90%, and present patent application is also just based on inventor's scientific achievement that further research institute makes on the basis of previous work, the application utilizes the raw material different from previous work, and optimize preparation technology, have developed another kind of new and effective ternary compound oxides catalyst K
2mn (MoO
4)
2.
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 dye wastewater process 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 dye wastewater process of the present invention is a kind of composite oxides, and the general formula of described composite oxides is K
2mn (MoO
4)
2.
The preparation method of the composite oxides for methylene blue dye wastewater process described above, described method comprises the steps:
(1) potassium compound, manganese salt, molybdate and citric acid are added to the water successively, stirring and dissolving, the mol ratio of the manganese in the potassium in described potassium compound, manganese salt, the molybdenum in molybdate and citric acid is 1:0.5:1:4 ~ 10;
(2) add ethylene glycol, ethylene glycol addition is 4 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 ~ 900 DEG C, obtain ternary compound oxides K
2mn (MoO
4)
2.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process described in technique scheme, wherein the calcining heat described in step (3) is 550 DEG C ~ 700 DEG C, and calcination time is 7 hours.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process described in technique scheme, the mol ratio of the potassium wherein in potassium compound described in step (1), the manganese in manganese salt, the molybdenum in molybdate and citric acid is 1: 0.5: 1: 5.5.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process described in technique scheme, wherein the potassium compound described in step (1) is selected from following one or more: potassium hydroxide, potassium chloride, potash, saleratus, potassium sulfate, potassium acid sulfate, potassium nitrate, potassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, potassium formate, potassium acetate, potassium citrate.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process described in technique scheme, wherein the manganese salt described in step (1) is one or more in manganese nitrate, manganese sulfate, manganese acetate, manganese chloride.
Further, the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process described in technique scheme, wherein the molybdate described in step (1) is that ammonium molybdate is or/and potassium molybdate.
According to the method for above-mentioned carbon monoxide-olefin polymeric process methylene blue waste water, comprise described carbon monoxide-olefin polymeric to be suspended in methylene blue waste water and process.
The method of described methylene blue dye wastewater process, preferably adds described composite oxides K in the ratio of 0.5 ~ 4.0g/L waste water
2mn (MoO
4)
2, under agitation process 5 ~ 30 minutes.
Ternary compound oxides K of the present invention
2mn (MoO
4)
2catalyst application in the processing method of methylene blue dye wastewater is: with ternary compound oxides K
2mn (MoO
4)
2for catalyst, degradation conditions is: methylene blue concentration is in 1mg/L ~ 90mg/L scope, the catalyst amount processing often liter of methylene blue dye wastewater is 0.5 ~ 4g, 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 95%, residual solution color is colourless, carries out catalyst recycle use 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 95.0%.
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, it is high that catalyst of the present invention has catalytic degradation efficiency, and preparation technology's flow process is simple, and non-secondary pollution produces, and the features such as operating cost is low, have very high actual application value.
Compared with prior art, the method that the present invention relates to methylene blue dye wastewater process 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, the K that the present invention obtains
2mn (MoO
4)
2catalyst can reach 98% to the degradation efficiency of methylene blue dye in 3min.
(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 1.78g potassium nitrate (1.76 × 10
-2mol), 1.56g manganese nitrate (8.77 × 10
-3mol), 3.10g tetra-water ammonium molybdate (2.51 × 10
-3and 18.30g citric acid (9.34 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then add 22.97g ethylene glycol (0.37mol) and stir 10min afterwards, be warmed up to 120 DEG C to continue to stir, until formation gel, again gel is heated 7 hours at 550 DEG C, obtain ternary compound oxides K
2mn (MoO
4)
2catalyst.
Get 0.10 gram of ternary compound oxides K prepared as stated above
2mn (MoO
4)
2catalyst 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 certain hour, then, centrifugal 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, result is as shown in table 1, when degradation time is 3 minutes, methylene blue degradation rate is 98.5%.
Table 1 degradation time and methylene blue dye degradation rate
| Catalyst degradation time/min | 3 | 6 | 10 | 14 |
| Degradation rate/% | 98.5 | 98.7 | 99.0 | 99.5 |
Embodiment 2
By 1.78g potassium nitrate (1.76 × 10
-2mol), 1.56g manganese nitrate (8.77 × 10
-3mol), 3.10g tetra-water ammonium molybdate (2.51 × 10
-3and 18.30g citric acid (9.34 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving.Add 22.97g ethylene glycol (0.37mol) and stir 10min afterwards, be warmed up to 120 DEG C and continue to stir, until form gel.Gel is heated 7 hours at 700 DEG C, obtains ternary compound oxides K
2mn (MoO
4)
2catalyst.
Get 0.10 gram of ternary compound oxides K prepared as stated above
2mn (MoO
4)
2catalyst 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 98.3%.
Embodiment 3
By 1.78g potassium nitrate (1.76 × 10
-2mol), 1.56g manganese nitrate (8.77 × 10
-3mol), 3.10g tetra-water ammonium molybdate (2.51 × 10
-3and 18.30g citric acid (9.34 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving.Add 22.97g ethylene glycol (0.37mol) and 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 K
2mn (MoO
4)
2catalyst.
Get 0.10 gram of K prepared as stated above
2mn (MoO
4)
2catalyst 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 96.9%.
Embodiment 4
Situation is recycled, the ternary compound oxides K that the preparation method of catalyst described in Example 1 obtains in order to what investigate catalyst
2mn (MoO
4)
2carry 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 K of 0.10g
2mn (MoO
4)
2under 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 K
2mn (MoO
4)
2catalyst 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/% | 98.5 | 96.9 | 95.4 |
As can be seen from Table 2, the degradation rate of catalyst degradation of methylene blue dyestuff in three circulations is all more than 95.0%.This shows ternary compound oxides K
2mn (MoO
4)
2catalyst can recycle.
Claims (9)
1. for a carbon monoxide-olefin polymeric for methylene blue dye wastewater process, be a kind of composite oxides, it is characterized in that: the general formula of described composite oxides is K
2mn (MoO
4)
2.
2. a preparation method for the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to claim 1, is characterized in that: described method comprises the steps:
(1) potassium compound, manganese salt, molybdate and citric acid are added to the water successively, stirring and dissolving, the mol ratio of the manganese in the potassium in described potassium compound, manganese salt, the molybdenum in molybdate and citric acid is 1:0.5:1:4 ~ 10;
(2) add ethylene glycol, ethylene glycol addition is 4 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 ~ 900 DEG C, obtain ternary compound oxides K
2mn (MoO
4)
2.
3. the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to claim 2, is characterized in that: the calcining heat described in step (3) is 550 DEG C ~ 700 DEG C, and calcination time is 7 hours.
4. the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to Claims 2 or 3, is characterized in that: the mol ratio of the potassium in potassium compound described in step (1), the manganese in manganese salt, molybdenum in molybdate and citric acid is 1: 0.5: 1: 5.5.
5. the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to Claims 2 or 3, is characterized in that: the potassium compound described in step (1) is selected from following one or more: potassium hydroxide, potassium chloride, potash, saleratus, potassium sulfate, potassium acid sulfate, potassium nitrate, potassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, potassium formate, potassium acetate, potassium citrate.
6. the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to Claims 2 or 3, is characterized in that: the manganese salt described in step (1) is one or more in manganese nitrate, manganese sulfate, manganese acetate, manganese chloride.
7. the preparation method of the carbon monoxide-olefin polymeric for methylene blue dye wastewater process according to Claims 2 or 3, is characterized in that: the molybdate described in step (1) is ammonium molybdate and/or potassium molybdate.
8. the method for carbon monoxide-olefin polymeric process methylene blue dye wastewater according to claim 1, is characterized in that: described method comprises described carbon monoxide-olefin polymeric to be suspended in methylene blue waste water and processes.
9. process the method for methylene blue waste water according to claim 8, it is characterized in that: add described composite oxides K in the ratio of 0.5 ~ 4.0g/L waste water
2mn (MoO
4)
2, under agitation process 5 ~ 30 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658357A (en) * | 2017-04-01 | 2018-10-16 | 深圳华联世纪生物工程股份有限公司 | A kind of extension reverse osmosis membrane service life technical solution |
| 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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| CN104971734A (en) * | 2015-07-20 | 2015-10-14 | 湖北工业大学 | Catalyst composition capable of treating methylene blue waste water as well as preparation method and application of catalyst composition |
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2015
- 2015-11-30 CN CN201510863375.5A patent/CN105498753A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104971734A (en) * | 2015-07-20 | 2015-10-14 | 湖北工业大学 | Catalyst composition capable of treating methylene blue waste water as well as preparation method and application of catalyst composition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658357A (en) * | 2017-04-01 | 2018-10-16 | 深圳华联世纪生物工程股份有限公司 | A kind of extension reverse osmosis membrane service life technical solution |
| 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 |
| CN109987622B (en) * | 2019-04-10 | 2021-07-30 | 宁波大学 | Cobalt-doped lanthanum molybdate micro-nano material and preparation method thereof |
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Application publication date: 20160420 |