CN105457650A - Catalyst composition and preparation method and application thereof in aspect of treating methylene blue industrial wastewater - Google Patents
Catalyst composition and preparation method and application thereof in aspect of treating methylene blue industrial wastewater Download PDFInfo
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- CN105457650A CN105457650A CN201510929085.6A CN201510929085A CN105457650A CN 105457650 A CN105457650 A CN 105457650A CN 201510929085 A CN201510929085 A CN 201510929085A CN 105457650 A CN105457650 A CN 105457650A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8872—Alkali or alkaline earth metals
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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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
-
- 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
Abstract
The invention relates to a Li2Ni2Mo3O12 catalyst composition and a preparation method and application thereof in the aspect of treating methylene blue industrial wastewater, and belongs to the technical field of inorganic functional material preparation. According to the Li2Ni2Mo3O12 catalyst composition, a lithium compound, nickel salt, molybdate and citric acid are sequentially added to water according to the molar ratio of 1 to 1 to 1.5 to 7-20, stirring is conducted for dissolving, ethylene glycol is added, the temperature rises to range from 100 DEG C to 130 DEG C, continuous stirring is conducted to form gel, the gel is calcined for 4-15 h at the temperature ranging from 400 DEG C to 900 DEG C finally, and the Li2Ni2Mo3O12 catalyst composition is prepared. The catalyst can efficiently catalyze hydrogen peroxide to conduct oxygenolysis on methylene blue dye in industrial wastewater at normal temperature and normal pressure without light irradiation, and the Li2Ni2Mo3O12 catalyst composition and the preparation method and application thereof in the aspect of treating the methylene blue industrial wastewater have the advantages that preparation is easy and rapid, the speed of degrading organic pollutants is high, the effect is significant, the treatment cost is low, and secondary pollution is not produced. In addition, the catalyst can be reused repeatedly, the degradation rates of the Li2Ni2Mo3O12 catalyst to the methylene blue industrial wastewater in second reuse and third reuse both exceed 90.0 percent.
Description
Technical field
The invention belongs to inorganic functional material preparing technical field, relate to a kind of carbon monoxide-olefin polymeric, particularly relate to a kind of Li
2ni
2mo
3o
12carbon monoxide-olefin polymeric and preparation method thereof and the application in process methylene blue industrial wastewater.
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, photocatalytic method, absorption method, membrane separation process and high-level oxidation technology 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.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.
In oxidation technology method, normally adopt the Fenton reagent degradating organic dye be made up of ferrous ion and hydrogen peroxide, principle is ferrous ion catalysis decomposing hydrogen dioxide solution organic matter, but the method exist ferrous ion be difficult to reclaim and easily cause the shortcomings such as secondary pollution.Application number is the Cu that application discloses a kind of degrading MB industrial waste water of 201110058905.0
2the preparation method and application of S catalyst, this patent application is that cupric and organic matter 4-chloro-3-amino phenyl sulfonyl acid reaction are prepared copper organic coordination compound, then with ethylene glycol and ethylenediamine for solvent, add copper organic coordination compound and dissolvable sulfide, in hydrothermal reaction kettle, reaction prepares Cu in 6 ~ 48 hours
2s catalyst, Cu
2the time of S catalysis hydrogen peroxide degradation of methylene blue dyestuff is 100 minutes, and therefore the method exists complicated process of preparation, and Cu
2the defects such as S is long to methylene blue degradation time, and degradation efficiency is low.Application number be 200510122782.7 application discloses a kind of methylene blue dye wastewater processing method and method for preparing catalyst, the method prepares the nanostructured oxide of manganese with solvent-thermal method, and catalysis decomposing hydrogen dioxide solution methylene blue dye, there is catalyst preparation process complexity equally, the deficiencies such as degradation of methylene blue dyestuff time required time is long.Authorization Notice No. be CN102760876B patent discloses a kind of niobates and composite and its thereof application in serondary lithium battery, niobates has following general formula: LaMbNbcOd, L are selected from one or more of Li, Na or K; M is selected from one or more in B, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Ce, Y, Zr, Mo, La, Ta, but niobates obtained in this invention and composite thereof use mainly as the negative pole of secondary lithium battery.
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 carbon monoxide-olefin polymeric and preparation method thereof and the application in process methylene blue industrial wastewater are 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 of the present invention is a kind of ternary compound oxides, and the general formula of described composite oxides is Li
2ni
2mo
3o
12, described composite oxides can be used as the methylene blue dye in catalyst hydrogen peroxide oxidation degraded industrial wastewater.
The preparation method of carbon monoxide-olefin polymeric described above, described method comprises the steps:
(1) lithium compound, nickel salt, molybdate and citric acid are added to the water successively, stirring and dissolving, the molybdenum in the lithium in described lithium compound, the nickel in nickel salt, molybdate and the mol ratio of citric acid are 1:1:1.5:7 ~ 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 400 DEG C ~ 900 DEG C, obtain ternary compound oxides Li
2ni
2mo
3o
12.
Further, the preparation method of the carbon monoxide-olefin polymeric 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 described in technique scheme, the mol ratio of lithium, the nickel in nickel salt, the molybdenum in molybdate and citric acid wherein in lithium compound described in step (1) is 1: 1: 1.5: 7.
Further, the preparation method of the carbon monoxide-olefin polymeric described in technique scheme, wherein the lithium compound described in step (1) is selected from following one or more: lithium hydroxide, lithium chloride, lithium carbonate, lithium sulfate, lithium nitrate, lithium phosphate, lithium hydrogen phosphate, lithium dihydrogen phosphate, lithium formate, lithium acetate, lithium citrate.
Further, the preparation method of the carbon monoxide-olefin polymeric described in technique scheme, wherein the nickel salt described in step (1) is one or more in nickel nitrate, nickelous sulfate, nickel acetate, nickel chloride.
Further, the preparation method of the carbon monoxide-olefin polymeric described in technique scheme, wherein the molybdate described in step (1) is any one or two kinds of in ammonium molybdate, lithium molybdate.
The application of carbon monoxide-olefin polymeric described above in process methylene blue industrial wastewater, is be suspended in methylene blue waste water by described carbon monoxide-olefin polymeric, then adds hydrogen peroxide oxidant and carry out oxidation Decomposition process.
Further, the application of carbon monoxide-olefin polymeric described in technique scheme in process methylene blue industrial wastewater, preferably adds described composite oxides Li in the ratio of 0.5 ~ 4.0g/L waste water
2ni
2mo
3o
12, process 5 ~ 30 minutes under agitation.
Ternary compound oxides Li of the present invention
2ni
2mo
3o
12catalyst application in the concrete processing method of methylene blue industrial wastewater is: with ternary compound oxides Li
2ni
2mo
3o
12for 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, hydrogen peroxide addition is 2.0 ~ 23.0g/L, 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, hydrogen peroxide 0.3g, 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, catalyst is in second time circulation, the degradation rate of the methylene blue dye during third time recycles all reaches more than 90%.
The present invention at normal temperatures and pressures, can effectively process methylene blue dye wastewater under penetrating without the need to illumination, and it is high that catalyst of the present invention has catalytic degradation efficiency, preparation technology's flow process is simple, 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 dye wastewater process has following significant outstanding substantive distinguishing features with significant progressive:
(1) catalyst Li of the present invention
2ni
2mo
3o
12preparation method is simple;
(2) the catalyst Li that obtains of the present invention
2ni
2mo
3o
12active 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 need not adopt any light source irradiation degraded system;
(5) catalyst Li of the present invention
2ni
2mo
3o
12repeatedly 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 0.89g lithium nitrate (1.29 × 10
-2mol), 3.70g nickel nitrate (1.28 × 10
-2mol), 3.42g Ammonium Molybdate Tetrahydrate (2.77 × 10
-3and 19.10g citric acid (9.10 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then add 16.65g ethylene glycol (0.27mol) 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 400 DEG C, obtain ternary compound oxides Li
2ni
2mo
3o
12catalyst.
Get 0.10 gram of ternary compound oxides Li prepared as stated above
2ni
2mo
3o
12catalyst and 0.3g hydrogen peroxide degradation of 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, 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, result is as shown in table 1, and when degradation time is 10 minutes, methylene blue degradation rate is 94.4%.
Table 1 degradation time and methylene blue dye degradation rate
| Catalyst degradation time/min | 3 | 6 | 10 | 14 |
| Degradation rate/% | 90.1 | 92.7 | 94.4 | 96.0 |
Embodiment 2
By 0.89g lithium nitrate (1.29 × 10
-2mol), 3.70g nickel nitrate (1.28 × 10
-2mol), 3.42g Ammonium Molybdate Tetrahydrate (2.77 × 10
-3and 19.10g citric acid (9.10 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then add 16.65g ethylene glycol (0.27mol) 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 Li
2ni
2mo
3o
12catalyst.
Get 0.10 gram of ternary compound oxides Li prepared as stated above
2ni
2mo
3o
12catalyst and 0.3g hydrogen peroxide degradation of 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, supernatant is got, 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, when degradation time is 10 minutes, methylene blue degradation rate is 95.35%.
Embodiment 3
By 0.89g lithium nitrate (1.29 × 10
-2mol), 3.70g nickel nitrate (1.28 × 10
-2mol), 3.42g Ammonium Molybdate Tetrahydrate (2.77 × 10
-3and 19.10g citric acid (9.10 × 10 mol)
-2mol) add in 60mL (3.33mol) distilled water successively, stirring and dissolving, then add 16.65g ethylene glycol (0.27mol) 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 900 DEG C, obtain ternary compound oxides Li
2ni
2mo
3o
12catalyst.
Get 0.10 gram of Li prepared as stated above
2ni
2mo
3o
12catalyst and 0.3g hydrogen peroxide degradation of 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, supernatant is got, 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, when degradation time is 10 minutes, methylene blue degradation rate is 95.90%.
Embodiment 4
Situation is recycled, the ternary compound oxides Li that the preparation method of catalyst described in Example 1 obtains in order to what investigate catalyst
2ni
2mo
3o
12carry out continuous three catalysis hydrogen peroxide 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 Li of 0.10g
2ni
2mo
3o
12and 0.3g hydrogen peroxide, under 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, supplement hydrogen peroxide, repeat above-mentioned degradation of methylene blue process, so recycle ternary compound oxides Li
2ni
2mo
3o
12catalyst 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/% | 94.1 | 92.9 | 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 Li
2ni
2mo
3o
12catalyst can recycle.
Claims (9)
1. a carbon monoxide-olefin polymeric, is a kind of ternary compound oxides, it is characterized in that: the general formula of described composite oxides is Li
2ni
2mo
3o
12.
2. a preparation method for carbon monoxide-olefin polymeric according to claim 1, is characterized in that: described method comprises the steps:
(1) lithium compound, nickel salt, molybdate and citric acid are added to the water successively, stirring and dissolving, the molybdenum in the lithium in described lithium compound, the nickel in nickel salt, molybdate and the mol ratio of citric acid are 1:1:1.5:7 ~ 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 400 DEG C ~ 900 DEG C, obtain ternary compound oxides Li
2ni
2mo
3o
12.
3. the preparation method of carbon monoxide-olefin polymeric 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 according to Claims 2 or 3, is characterized in that: the mol ratio of the lithium in lithium compound described in step (1), the nickel in nickel salt, the molybdenum in molybdate and citric acid is 1: 1: 1.5: 7.
5. the preparation method of the carbon monoxide-olefin polymeric according to Claims 2 or 3, is characterized in that: the lithium compound described in step (1) is selected from following one or more: lithium hydroxide, lithium chloride, lithium carbonate, lithium sulfate, lithium nitrate, lithium phosphate, lithium hydrogen phosphate, lithium dihydrogen phosphate, lithium formate, lithium acetate, lithium citrate.
6. the preparation method of the carbon monoxide-olefin polymeric according to Claims 2 or 3, is characterized in that: the nickel salt described in step (1) is one or more in nickel nitrate, nickelous sulfate, nickel acetate, nickel chloride.
7. the preparation method of the carbon monoxide-olefin polymeric according to Claims 2 or 3, is characterized in that: the molybdate described in step (1) is any one or two kinds of in ammonium molybdate or lithium molybdate.
8. the application of carbon monoxide-olefin polymeric according to claim 1 in process methylene blue industrial wastewater, is characterized in that: be suspended in methylene blue waste water by described carbon monoxide-olefin polymeric, then add hydrogen peroxide oxidant and carry out oxidation Decomposition process.
9. the application of carbon monoxide-olefin polymeric according to claim 8 in process methylene blue industrial wastewater, is characterized in that: add described composite oxides Li in the ratio of 0.5 ~ 4.0g/L waste water
2ni
2mo
3o
12, process 5 ~ 30 minutes under agitation.
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| CN110252355A (en) * | 2018-11-21 | 2019-09-20 | 湖北工业大学 | A kind of photochemical catalyst and preparation method thereof handling organic wastewater |
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| CN106423038A (en) * | 2016-09-20 | 2017-02-22 | 东北大学秦皇岛分校 | Citric-acid-assisted Mn-dope yttrium molybdate selective-adsorption nano material and preparation method thereof |
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| CN106345484B (en) * | 2016-11-10 | 2018-09-18 | 东北大学秦皇岛分校 | A kind of selectivity composite photo-catalyst powder and its preparation method and application |
| CN111171082A (en) * | 2018-11-09 | 2020-05-19 | 盐城师范学院 | Nickel complex with properties of catalyzing photodegradation and adsorbing dye and preparation method thereof |
| CN111171082B (en) * | 2018-11-09 | 2024-05-03 | 盐城师范学院 | Nickel complex with properties of catalyzing photodegradation and adsorbing dye and preparation method thereof |
| CN110252312A (en) * | 2018-11-21 | 2019-09-20 | 湖北工业大学 | A kind of catalyst and preparation method thereof for degradation of dye waste water |
| CN110252355A (en) * | 2018-11-21 | 2019-09-20 | 湖北工业大学 | A kind of photochemical catalyst and preparation method thereof handling organic wastewater |
| CN110252355B (en) * | 2018-11-21 | 2023-05-16 | 湖北工业大学 | Photocatalyst for treating organic wastewater and preparation method thereof |
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| CN105457650B (en) | 2018-09-25 |
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