CN109731546A - Zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation and application - Google Patents
Zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation and application Download PDFInfo
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Abstract
The present invention relates to a kind of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation and application, it is characterised in that: (1) presses FeCl2·4H2O and FeCl3·6H2The mass ratio of O is that 1.47:1 weighs mixing, adds deionized water to make whole dissolutions, by active carbon and FeCl3·6H2The mass ratio of O is 1:0.5-1.0, adds active carbon, and ultrasonic 15-30min is transferred to hydrothermal reaction kettle, 100-150 DEG C of reaction 3-5h is cooling, and deionized water washs to obtain composite material with ammonium hydroxide tune pH >=11；(2) add zinc nitrate hexahydrate in composite material, control itself and quality of activated carbon ratio 2-1:1, with ammonium hydroxide tune pH >=11, ultrasonic 0.5-1h is transferred to hydrothermal reaction kettle, and 160-200 DEG C of reaction 10-12h is cooling, deionized water, dehydrated alcohol washing, drying.Inorganic agent and organic pollutant quality ratio 20-50:1 vibrate 15-30min, 365nm ultraviolet lighting 15-30min, Magnetic Isolation recycling.The invention has the advantages that hydro-thermal method and coprecipitation combine, the waste water treating agent with high adsorption, photocatalytic, Magneto separate and recyclability is made；Easy to use, processing organic pollutant is efficient.
Description
Technical field
The invention belongs to sewage treatment fields, are related to the process field of organic pollutant, and in particular to a kind of zinc oxide/tetra- oxygen
Change three-iron/active carbon nanometer waste water treating agent preparation and application.
Technical background
With rapid development of economy, water pollution is brought while exacerbating shortage of water resources to environmental protection
Baptism.Water pollutant source is wider, wherein the methylene blue of the industries such as papermaking, weaving and printing discharge, methyl orange, hole
The organic pollutants such as sparrow malachite green are particularly acute, these pollutants have that the time is long, range is wide, processing difficulty is big in water, give people
Health care belt seriously threaten.
Currently, sewage water treatment method mainly has absorption method, membrane separation process, oxidation-reduction method etc., these methods respectively have feature
And deficiency.For example, being the absorption method of representative other than there is recycling difficulty using active carbon, there is also reactivate to recycle needs
It carries out the cumbersome post-processing operation step such as eluting, this significantly limits its use scope；And with zinc oxide etc. for representative
Photocatalytic degradation method, have the characteristics that economic, environmental protection, but its disposal efficiency is to be improved, research shows that improve it
The disposal efficiency needs effectively to shift, the light exciton that separation light excitation generates；Photocatalytic system is improved to organic pollutant
Adsorption capacity；There is suitable matrix to fix or support its physical structure.Therefore it provides a kind of have high adsorption, efficiently
The waste water treating agent of catalytic performance has broad application prospects.
Summary of the invention
The invention aims to solve that existing recycling is difficult when the absorption of single-activity charcoal uses, it is cumbersome to be re-activated and without
Ji, using zinc oxide as the photocatalytic degradation method degradation efficiency of representative it is not high the problems such as, a kind of zinc oxide/tetra- oxidations three are provided
Iron/active carbon nanometer waste water treating agent preparation and application.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent, it is characterised in that including walking as follows
It is rapid:
(1) according to FeCl2·4H2O and FeCl3·6H2The mass ratio of O is that 1.47:1 weighs mixing, to FeCl2·4H2O and
FeCl3·6H2In O plus deionized water dissolves it all, according to active carbon and FeCl3·6H2The mass ratio of O is 1:0.5-
1.0, active carbon is added, is ultrasonically treated 15-30 minutes, then the ammonium hydroxide for being 15%-30% with mass concentration adjusts pH value >=11, then
Be transferred in hydrothermal reaction kettle, 100-150 DEG C reaction 3-5 hours, be cooled to room temperature, washed through deionized water after reaction
After obtain ferroso-ferric oxide/activity carbon nanometer composite material；
It (2) is 2-1:1, the ferroso-ferric oxide/active carbon obtained to step (1) according to zinc nitrate hexahydrate and quality of activated carbon ratio
Zinc nitrate hexahydrate (Zn (NO is added in nanocomposite3)2·6H2O), with the ammonium hydroxide of mass concentration 15%-30% adjust pH >=
It after 11, ultrasonic disperse 0.5-1 hours, is transferred in hydrothermal reaction kettle, is reacted 10-12 hours at 160 DEG C -200 DEG C, reaction terminates cold
But it to room temperature, is successively washed with deionized water and dehydrated alcohol, zinc oxide/ferroso-ferric oxide/active carbon can be obtained after dry
Nanometer waste water treating agent.
A kind of application method of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent, it is characterised in that including such as
Lower step:
It is 20-50:1 according to the mass ratio of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent and organic pollutant,
Above-mentioned zinc oxide/tetra- are added into the aqueous solution containing organic pollutant (methylene blue, methyl orange etc. common are machine pollutant)
Fe 3 O/active carbon nanometer waste water treating agent vibrates 15-30 minute, make organic pollutant and zinc oxide/ferroso-ferric oxide/
It is right with UV Light 15-30 minutes of wavelength 365nm after active carbon nanometer waste water treating agent reaches absorption and desorption equilibrium
Organic dyestuff in water carries out light degradation, with magnet to zinc oxide/ferroso-ferric oxide in mixed solution/active carbon nanometer waste water
Inorganic agent carries out Magnetic Isolation, recycling and reusing.
In the ferriferrous oxide nano for combining the active carbon, optically active zinc oxide and magnetic property with high absorption property
On the basis of advantage, the novel nano waste water that high activity has been prepared respectively is combined using hydro-thermal method and coprecipitation for particle
Inorganic agent (zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent), it is final realize novel nano waste water treating agent can
Controlization preparation；The result shows that the inorganic agent has high absorption property and photocatalysis performance, and only it is by the effect of externally-applied magnetic field
It can be achieved to recycle the novel nano waste water treating agent, there is good regenerability, be highly suitable for organic contamination in sewage
The improvement of object, and use value significant to environmental protection and sustainable development.
Advantages of the present invention: 1. solve, subsequent activation processing difficult solely with recycling existing for activated carbon adsorption it is cumbersome and with
Zinc oxide etc. is the low problem of the photocatalytic degradation efficiency of representative；2. it is simple for process, using hydro-thermal method and coprecipitation phase
In conjunction with method；3. having high absorption property, photocatalysis performance, Magneto separate performance and recyclable performance；4. it is easy to use,
There is good treatment effect to organic pollutants such as methylene blue common in waste water, methyl oranges, protect environment.
Detailed description of the invention
Fig. 1 is a kind of TEM figure of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent；
Fig. 2 is a kind of dispersion liquid figure of zinc oxide/ferroso-ferric oxide/activity carbon nanometer composite material in water；
Fig. 3 is 1 Methylene Blue aqueous solution of embodiment through zinc peroxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent light
Figure after catalytic degradation；
Fig. 4 is zinc oxide/ferroso-ferric oxide in embodiment 1/active carbon nanometer waste water treating agent to photocatalytic degradation of methylene blue
Recycle figure.
Specific embodiment
Embodiment 1
1, zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation
(1) by 0.0569 g FeCl3·6H2O and 0.0837 g FeCl2·4H2O is added in 30mL deionized water, and dissolution is simultaneously
It is added 0.1 g active carbon after mixing, after twenty minutes, the ammonium hydroxide for being 15% with mass concentration is by above-mentioned mixed liquor for ultrasonic treatment
PH value be adjusted to 11, be then transferred in hydrothermal reaction kettle, 120 DEG C react 3 hours, be cooled to room temperature after reaction, pass through
Ferroso-ferric oxide/activity carbon nanometer composite material is obtained after deionized water washing；
(2) 0.2 g zinc nitrate hexahydrate is added to ferroso-ferric oxide obtained in step (1)/activity carbon nanometer composite material
In, pH to 11, which is adjusted, with 25% concentrated ammonia liquor is transferred in hydrothermal reaction kettle after ultrasonic disperse 0.5 hour, 160 DEG C of hydro-thermal reactions 10
Hour, reaction terminates to be cooled to room temperature, and is successively washed with deionized water, dehydrated alcohol, and zinc oxide/tetra- oxygen can be obtained after dry
Change three-iron/active carbon nanometer waste water treating agent.
2, photocatalytic degradation MB
It takes 20 mL methylene blue (MB) aqueous solutions (concentration is 15 mg/L) in sample cell, the oxygen that 10 mg steps 1 obtain is added
Change zinc/ferroso-ferric oxide/active carbon nanometer waste water treating agent, puts it on oscillator and vibrate 15 minutes, make zinc oxide/tetra- oxygen
After change three-iron/active carbon nanometer waste water treating agent and MB molecule reach absorption and desorption equilibrium, with ultraviolet lamp (wavelength: 365 nm)
It carries out illumination 20 minutes, light degradation (97 .0% of degradation rate) is carried out to the organic dyestuff in water and obtains mixed liquor.
3, zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent recycles
Zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent in the mixed liquor obtained with magnet to step 2 carries out magnetic
Property separation, which is directly used in (equivalent replacement) step
The light degradation of the aqueous solution of methylene blue (MB) in 2 is tested, useless to investigate the zinc oxide/ferroso-ferric oxide/active carbon nanometer
The cycling and reutilization situation of water treatment agent；The experimental results showed that this nanometer of waste water treating agent be after recycling utilization 6 times,
Still excellent light degradation property and renewable performance are shown, 90% is remained within to the photodegradation rate of methylene blue (MB)
(Fig. 4) above.
Embodiment 2
1, zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation
(1) by 0.06828 g FeCl3·6H2O and 0.1004 g FeCl2·4H2O is added in 35 mL deionized waters, dissolution
And 0.1 g active carbon is added after mixing, ultrasonic treatment is after 25 minutes, and the ammonium hydroxide for being 20% with mass concentration is by above-mentioned mixing
The pH value of liquid is adjusted to 11, is then transferred in hydrothermal reaction kettle, and 135 DEG C are reacted 3.5 hours, is cooled to room temperature after reaction,
Ferroso-ferric oxide/activity carbon nanometer composite material is obtained after deionized water is washed；
(2) 0.2 g zinc nitrate hexahydrate is added to ferroso-ferric oxide obtained in step (1)/activity carbon nanometer composite material
In, pH to 11.5 is adjusted with 25% concentrated ammonia liquor, ultrasonic disperse is transferred in hydrothermal reaction kettle after 1 hour, and it is small that 11 are reacted at 180 DEG C
When, reaction terminates to be cooled to room temperature, and is successively washed with deionized water, dehydrated alcohol, and zinc oxide/tetra- oxidations can be obtained after dry
Three-iron/active carbon nanometer waste water treating agent.
2, photocatalytic degradation MB
It takes 18 mL methylene blue (MB) aqueous solutions (concentration is 15 mg/L) in sample cell, the oxygen that 12 mg steps 1 obtain is added
Change zinc/ferroso-ferric oxide/active carbon nanometer waste water treating agent, puts it on oscillator and vibrate 25 minutes, make zinc oxide/tetra- oxygen
After change three-iron/active carbon nanometer waste water treating agent and MB molecule reach absorption and desorption equilibrium, with ultraviolet lamp (wavelength: 365 nm)
It carries out illumination 25 minutes, light degradation, degradation rate 97.2% is carried out to the organic dyestuff in water.
Embodiment 3
1, zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation
(1) by 0.07397 g FeCl3·6H2O and 0.1088 g FeCl2·4H2O is added in 50 mL deionized waters, dissolution
And 0.1 g active carbon is added after mixing, ultrasonic treatment is after 30 minutes, and the ammonium hydroxide for being 30% with mass concentration is by above-mentioned mixing
The pH value of liquid is adjusted to 11.5, is then transferred in hydrothermal reaction kettle, and 150 DEG C are reacted 5 hours, is cooled to room temperature after reaction,
Ferroso-ferric oxide/activity carbon nanometer composite material is obtained after deionized water is washed；
(2) 0.2 g zinc nitrate hexahydrate is added to ferroso-ferric oxide obtained in step (1)/activity carbon nanometer composite material
In, pH to 12 is adjusted with 25% concentrated ammonia liquor and is transferred in hydrothermal reaction kettle after ultrasonic disperse 1 hour, and 185 DEG C of hydro-thermal reactions 12 are small
When, reaction terminates to be cooled to room temperature, and is successively washed with deionized water, dehydrated alcohol, and zinc oxide/tetra- oxidations three are obtained after dry
Iron/active carbon nanometer waste water treating agent.
2, photocatalytic degradation MB
It takes 20mL methylene blue (MB) aqueous solution (concentration is 15 mg/L) in sample cell, the oxygen that 15 mg steps 1 obtain is added
Change zinc/ferroso-ferric oxide/active carbon nanometer waste water treating agent, puts it on oscillator and vibrate 30 minutes, make zinc oxide/tetra- oxygen
After change three-iron/active carbon nanometer waste water treating agent and MB molecule reach absorption and desorption equilibrium, with ultraviolet lamp (wavelength: 365 nm)
It carries out illumination 30 minutes, effective light degradation, degradation rate 97.5% is carried out to the organic dyestuff in water.
As can be seen from Figure 1 zinc oxide nano-particle (ZnO) and magnetic ferroferric oxide nano-particles (Fe3O4) random
It is grown in activated carbon surface, foring zinc oxide/ferroso-ferric oxide/activity carbon nanometer composite material is produced by the present invention one
Kind zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent；
As can be seen from Figure 2 novel nano sewage-treating agent good dispersion property in water；
As can be seen from Figure 3 the nano water treatment agent is very good to the photocatalytic degradation effect of aqueous solution of methylene blue, degradation
Water afterwards is in colourless；
As can be seen from Figure 4 the nano water treatment agent is after recycling 6 times, and catalytic effect hardly happens variation, still
90% or more so is maintained, shows excellent photocatalysis performance and renewable performance.
Claims (2)
1. a kind of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent preparation method, it is characterised in that including as follows
Step:
(1) according to FeCl2·4H2O and FeCl3·6H2The mass ratio of O is that 1.47:1 weighs mixing, to FeCl2·4H2O and
FeCl3·6H2In O plus deionized water dissolves it all, according to active carbon and FeCl3·6H2The mass ratio of O is 1:0.5-
1.0, active carbon is added, is ultrasonically treated 15-30 minutes, then the ammonium hydroxide for being 15%-30% with mass concentration adjusts pH value >=11, then
Be transferred in hydrothermal reaction kettle, 100-150 DEG C reaction 3-5 hours, be cooled to room temperature, washed through deionized water after reaction
After obtain ferroso-ferric oxide/activity carbon nanometer composite material；
It (2) is 2-1:1, the ferroso-ferric oxide/active carbon obtained to step (1) according to zinc nitrate hexahydrate and quality of activated carbon ratio
Zinc nitrate hexahydrate is added in nanocomposite, adjusts pH >=11, ultrasonic disperse 0.5- with the ammonium hydroxide of mass concentration 15%-30%
It after 1 hour, is transferred in hydrothermal reaction kettle, is reacted 10-12 hours at 160 DEG C -200 DEG C, reaction terminates to be cooled to room temperature, and successively uses
Deionized water and dehydrated alcohol washing, can be obtained zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent after dry.
2. a kind of user of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent obtained according to claim 1
Method, it is characterised in that include the following steps:
It is 20-50:1 according to the mass ratio of zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent and organic pollutant,
Above-mentioned zinc oxide/ferroso-ferric oxide/active carbon nanometer waste water treating agent is added into the aqueous solution containing organic pollutant, vibrates
Used UV Light 15-30 minutes of wavelength 365nm after 15-30 minutes, with magnet to the waste water treating agent in mixed solution into
Row Magnetic Isolation, recycling.
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| CN114344952A (en) * | 2021-12-28 | 2022-04-15 | 内蒙古大学 | Multifunctional demulsifier and preparation method and application method thereof |
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