CN102806082A - Method for preparing visible light catalyst for degrading sulphide ore dressing organic wastewater - Google Patents
Method for preparing visible light catalyst for degrading sulphide ore dressing organic wastewater Download PDFInfo
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- CN102806082A CN102806082A CN2012102438774A CN201210243877A CN102806082A CN 102806082 A CN102806082 A CN 102806082A CN 2012102438774 A CN2012102438774 A CN 2012102438774A CN 201210243877 A CN201210243877 A CN 201210243877A CN 102806082 A CN102806082 A CN 102806082A
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- visible light
- water
- sulphide ore
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- light catalyst
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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
Abstract
The invention discloses a method for preparing a visible light catalyst for degrading sulphide ore dressing organic wastewater. The method takes ferric nitrate, malonic acid and water as raw materials which are uniformly mixed, the mixture is vaporized in a water bath of 80 DEG C to be pasty, is dried at the condition of 105 DEG C-120 DEG C, and is calcinated at 200 DEG C-500 DEG C, and nanocrystalline iron oxide powder is obtained. An iron oxide photocatalyst can effectively degrade the organic ingredients of the sulphide ore dressing organic wastewater under the irradiation of visible lights. The method has the advantages of simple and quick catalyst preparation, quick organic pollutant degradation, obvious pollutant removing effect and low cost, and does not cause secondary pollution.
Description
Technical field
The present invention relates to a kind of method of Beneficiation Wastewater, particularly to a kind of visible light catalyst preparation method of the sulphide ore ore dressing organic wastewater of degrading.
Background technology
Along with the development of mining industry, the consumption of the floating agent that uses in the ore dressing process is increasing, and the environmental pollution that the while floating agent brings is also more and more serious.Because the floating agent consumption is big, efficient is low, high poison and high pollution; Medicament residual volume in the beneficiation wastewater is bigger; Cause many mining area ecological environments constantly to worsen, water body and soil receive severe contamination, and health of human body, agricultural production and fishery have all been caused very big harm.The technology of therefore, how to seek a kind of improvement beneficiation wastewater effectively and reasonably is the great difficult problem that people need to be resolved hurrily.
At present, the method for organic principle has bioanalysis, chemical method, physisorphtion and mine tailing storehouse self-purification method etc. in the processing beneficiation wastewater of sulphide ore.Bioanalysis is poor to the organic principle degradation property in some sulfide flotation waste water.Chinese patent CN101875960A tests the biological degradability of the organic principle hydrocarbyl xanthate in the sulfide flotation waste water; The result shows that ethyl xanthate is biodegradable, but isopropyl xanthate, normal-butyl xanthate, Isobutylxanthic acid and n-pentyl xanthate all belong to difficult for biological degradation.Chinese patent CN101279804A discloses the method with ozone method degraded sulphide ore ore dressing organic wastewater.This method reaction speed is fast, and it is remarkable to remove the pollutant effect.But ozone is prone to decompose, and can not recycle.The absorption method reproducing adsorbent is more loaded down with trivial details.Mine tailing storehouse self-purification method degradation speed is slow.
In recent years, utilize the poisonous and hazardous pollutant of semi-conducting material photocatalytic degradation to become one of popular research topic of comparison.Not only energy consumption is low, easy and simple to handle, reaction condition is gentle, non-secondary pollution for photocatalysis technology, and can effectively organic pollution be converted into inorganic molecules, reaches the purpose of complete inorganicization.Using more photochemical catalyst at present is TiO
2, it has the advantage of photocatalytic activity height, good stability.Yet TiO
2Greater band gap, can only absorb the ultraviolet light of λ≤387nm, the utilization rate of luminous energy is low.Therefore, people transfer to sight gradually has the low energy gap width, can utilize the semiconductor light-catalyst of visible light, to improve the utilization ratio to solar energy.Chinese patent CN101830537A discloses the method for organic principle in a kind of visible light photocatalytic degradation beneficiation wastewater of sulphide ore.This method prepares photochemical catalyst Bi with coprecipitation
2O
3Powder.Its preparation process comprises: the 1. preparation of presoma: with five water bismuth nitrates, red fuming nitric acid (RFNA) and deionized water mixing in polytetrafluoroethylcontainer container according to a certain percentage; Slowly drip KOH solution then and be neutral to pH; Stir while dripping, obtain the solid deposition behind the reaction 1h; With sedimentation and filtration and washing, dry (120 ℃) then, grind, obtain precursor powder; 2. photochemical catalyst Bi
2O
3Preparation: precursor powder is calcined 6h in 303 ℃～800 ℃, obtains Bi
2O
3Powder.Though it is fast that this method has technological reaction speed, remove pollutant obvious results advantage, its semiconductor light-catalyst that relates to preparation is complicated, and cost is high.
Summary of the invention
In view of the deficiency of prior art, the objective of the invention is to the fast simple and low Fe of cost with preparation technology
2O
3The photochemical catalyst beneficiation wastewater of sulphide ore organic principle that is used for degrading, thus the complicated and high problem of cost of existing visible light catalyst preparation solved.
The objective of the invention is to realize like this:
The visible light catalyst preparation method of organic principle in a kind of beneficiation wastewater of sulphide ore of degrading is a raw material with ferric nitrate, malonic acid and water, adopts wet chemistry method to be prepared into alpha-iron oxide nano-powder, promptly gets visible light catalyst.
Preferably, the preparation method of said visible light catalyst comprises the steps:
(1) is raw material with ferric nitrate, malonic acid and water, mixes, be evaporated to pasty state 80 ℃ of water-baths; Wherein, ferric nitrate, the mol ratio of malonic acid and water is: 1:2-8:45-180;
(2) pastel is dry under 105 ℃ of-120 ℃ of conditions;
(3) dry pastel is put into kiln calcining under 200 ℃-500 ℃ and got alpha-iron oxide nano-powder in 2-6 hour.
Further preferably, the preparation method of said visible light catalyst, ferric nitrate wherein, the mol ratio of malonic acid and water is: 1:2-4:47-84.
Further preferably, the preparation method of said visible light catalyst, wherein the calcining heat in the step (3) is 250 ℃-350 ℃, calcination time is 2-3 hour.
Again further preferably, the preparation method of said visible light catalyst, wherein the water of step (1) employing is deionized water or distilled water.
The method of organic principle in a kind of beneficiation wastewater of sulphide ore of degrading comprises alpha-iron oxide nano-powder with method for preparing as visible light catalyst, outstandingly turbidly in beneficiation wastewater of sulphide ore, carries out illumination and penetrates.
Preferably, the method for organic principle in the said degraded beneficiation wastewater of sulphide ore, wherein the ratio in 0.3～2.0g/L waste water adds alpha-iron oxide nano-powder, and irradiation is 150～240 minutes under visible light.
The present invention introduces beneficiation wastewater in the cylindrical quartz photo catalysis reactor, adds the photochemical catalyst Fe of preparation as stated above in the ratio of 0.3～2.0 g/L waste water
2O
3, open magnetic stirring apparatus again and stir, make Fe
2O
3Be suspended state, connect xenon source then, shone 150～240 minutes, utilize Fe
2O
3Organic principle in the photocatalytic degradation waste water.Said xenon lamp places in the quartzy cold-trap, and this cold-trap is fixed on cylindrical quartz reactor central authorities, is connected with cooling water in the interlayer in the cold-trap, eliminates the fuel factor of xenon lamp through the flow of regulating cooling water.Said light source adopts xenon lamp, the following wave spectrum of optical filter elimination 420 nm.This xenon lamp is used for simulated solar spectrum.Also can use solar light irradiation in the present invention.
The visible light catalyst preparation method of the degraded sulphide ore ore dressing organic wastewater that compared with prior art, the present invention relates to has following main advantage and progress:
3. it is remarkable to remove the pollutant effect, and degradation speed is fast,
Description of drawings
Fig. 1 is the XRD figure spectrum of the ferric oxide powder of the embodiment of the invention 1 preparation;
Fig. 2 is the SEM photo of the ferric oxide powder of the embodiment of the invention 1 preparation.
The specific embodiment
Below through the embodiment form foregoing of the present invention is remake further detailed description; But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1:
10.0g nine water ferric nitrates (about 0.03 mol) and 6.3 g malonic acid (about 0.06 mol) are added in 25 mL (the about 1.4 mol) distilled water successively, mix, be evaporated to pasty state 80 ℃ of water-baths.Pastel is dry under 105 ℃ of conditions; Dry pastel is put into kiln calcining under 250 ℃ got ferric oxide powder in 3 hours.The XRD figure spectrum of gained powder is as shown in Figure 1.Can know from Fig. 1, all characteristic peak positions and standard powder diffraction card (
-Fe
2O
3PDF 39-1346) diffraction maximum is consistent, can confirm that the gained powder does
-Fe
2O
3The SEM photo of gained powder is as shown in Figure 2, and this figure shows that the size of gained powder is about 50 nm～100 nm.
Be in the butyl xanthate flotation waste water adding cylindrical quartz photo catalysis reactor of 40.0 mg/L with 40 mL concentration then, add the Fe of embodiment 1 preparation
2O
340 mg, magnetic agitation makes photochemical catalyst be in suspended state always, shines with 300 W xenon lamps then.The following wave spectrum of optical filter elimination 420 nm.At wavelength>after the illumination of 420 nm penetrated 150 min, butyl xanthate concentration changes with time situation was as shown in table 1.Can know that by table 1 behind illumination 150 min, the degradation rate of butyl xanthate is 94.0%.
The Fe of 250 ℃ of preparations of table 1
2O
3Visible light photocatalytic degradation contains butyl xanthate beneficiation wastewater result
Embodiment 2:
10.0g nine water ferric nitrates (about 0.03 mol) and 9.4 g malonic acid (about 0.09 mol) are added in 35 mL (the about 1.9 mol) distilled water successively, mix, be evaporated to pasty state 80 ℃ of water-baths.Pastel is dry under 105 ℃ of conditions; Dry pastel is put into kiln calcining under 300 ℃ got ferric oxide powder in 2 hours.
Be in the butyl xanthate flotation waste water adding cylindrical quartz reactor of 40.0 mg/L with 40 mL concentration then, add the Fe of 40 mg embodiment, 2 preparations
2O
3, magnetic agitation makes photochemical catalyst be in suspended state always, shines with 300 W xenon lamps then.The following wave spectrum of optical filter elimination 420 nm.At wavelength>behind illumination 180 min of 420 nm, the butyl xanthate concentration changes with time is as shown in table 2.Can know that by table 2 behind illumination 180 min, the degradation rate of butyl xanthate is 96.0%.
The Fe of 300 ℃ of preparations of table 2
2O
3Visible light photocatalytic degradation contains butyl xanthate beneficiation wastewater result
Embodiment 3:
10.0g nine water ferric nitrates (about 0.03 mol) and 12.5g malonic acid (about 0.12 mol) are added in the 45 mL distilled water (about 2.5 mol) successively, mix, be evaporated to pasty state 80 ℃ of water-baths.Pastel is dry under 105 ℃ of conditions; Dry pastel is put into kiln calcining under 350 ℃ got ferric oxide powder in 2 hours.
Be in the butyl xanthate flotation waste water adding cylindrical quartz reactor of 40.0 mg/L with 40 ml concentration then, add the Fe of 40 mg embodiment, 3 preparations respectively
2O
3, magnetic agitation makes photochemical catalyst be in suspended state always, shines with the 300W xenon lamp then.The following wave spectrum of optical filter elimination 420 nm.At wavelength>behind illumination 240 min of 420 nm, the butyl xanthate concentration changes with time is as shown in table 3.Can know that by table 3 behind illumination 240 min, the degradation rate of butyl xanthate is 90.0%.
The Fe of 350 ℃ of preparations of table 3
2O
3Visible light photocatalytic degradation contains butyl xanthate beneficiation wastewater result
Claims (8)
1. the visible light catalyst preparation method of organic principle in the beneficiation wastewater of sulphide ore of degrading, it is characterized in that: with ferric nitrate, malonic acid and water is raw material, adopts wet chemistry method to be prepared into alpha-iron oxide nano-powder.
2. according to the preparation method of the said visible light catalyst of claim 1, it is characterized in that comprising the steps:
(1) is raw material with ferric nitrate, malonic acid and water, mixes, be evaporated to pasty state 80 ℃ of water-baths; Wherein, ferric nitrate, the mol ratio of malonic acid and water is: 1:2-8:45-180;
(2) pastel is dry under 105 ℃ of-120 ℃ of conditions;
(3) dry pastel is put into kiln calcining under 200 ℃-500 ℃ and got alpha-iron oxide nano-powder in 2-6 hour.
3. according to the preparation method of the said visible light catalyst of claim 2, it is characterized in that: ferric nitrate, the mol ratio of malonic acid and water is: 1:2-4:47-84.
4. according to the preparation method of the said visible light catalyst of claim 2, it is characterized in that: the calcining heat in the step (3) is 250 ℃-350 ℃, and calcination time is 2-3 hour.
5. according to the preparation method of each said visible light catalyst of claim 1-4, it is characterized in that: the water that step (1) adopts is deionized water or distilled water.
6. the method for organic principle in the beneficiation wastewater of sulphide ore of degrading is characterized in that: comprise alpha-iron oxide nano-powder with each preparation of claim 1-4 as visible light catalyst, outstandingly turbidly in beneficiation wastewater of sulphide ore, carry out illumination and penetrate.
7. according to the method for organic principle in the said degraded beneficiation wastewater of sulphide ore of claim 6, it is characterized in that: the ratio in 0.3 ~ 2.0g/L waste water adds alpha-iron oxide nano-powder, and irradiation is 150～240 minutes under visible light.
8. according to the method for organic principle in the said degraded beneficiation wastewater of sulphide ore of claim 7, it is characterized in that: the light source of said visible light is xenon lamp or sunshine.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830537A (en) * | 2010-03-23 | 2010-09-15 | 武汉理工大学 | Method for degrading organic components in ore-dressing wastewater of sulphide ores by catalysis under visible light |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830537A (en) * | 2010-03-23 | 2010-09-15 | 武汉理工大学 | Method for degrading organic components in ore-dressing wastewater of sulphide ores by catalysis under visible light |
Non-Patent Citations (1)
| Title |
|---|
| 邓庚凤等: "溶胶-凝胶法制备超细氧化铁的工艺研究", 《江西理工大学学报》 * |
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Application publication date: 20121205 |