CN105195150B - One kind prepares efficient Fe3O4/FeAl2O4The methods and applications of composite film class fenton catalyst - Google Patents
One kind prepares efficient Fe3O4/FeAl2O4The methods and applications of composite film class fenton catalyst Download PDFInfo
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Abstract
One kind prepares efficient Fe3O4/FeAl2O4The methods and applications of composite film class fenton catalyst, it is related to a kind of methods and applications for preparing class fenton catalyst.The invention aims to solve existing class fenton catalyst to have the problem of separation and recovery of catalyst is using hardly possible, poor mechanical property.Method：First, carbon steel polishing；2nd, bright carbon steel is connected with positive source, is used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；3rd, plasma electrolysis reaction is adopted, efficient Fe is obtained3O4/FeAl2O4Composite film class fenton catalyst.Fe prepared by the present invention3O4/FeAl2O4The degradation efficiency of composite film class fenton catalyst Pyrogentisinic Acid in 60min is up to 100%.The present invention can obtain one kind and prepare efficient Fe3O4/FeAl2O4The method of composite film class fenton catalyst.
Description
Technical field
The present invention relates to a kind of methods and applications for preparing class fenton catalyst.
Background technology
With economic fast development and the continuous growth of population, the discharge of industrial wastewater, agricultural effluent and sanitary wastewater
Amount and discharge species are continuously increased, and harm of the Organic Pollutants In Water to environment and the mankind is increasingly serious.In order to greatest extent
Ground reduction water pollution, improvement water quality condition, have weight to the advanced treating before discharge of wastewater for the problem of curbing environmental pollution
The meaning wanted.
Fenton oxidation method is mixed as a kind of high-level oxidation technology using a certain amount of ferrous ion with hydrogen peroxide,
Strong oxidizing property hydroxyl radical free radical is produced under certain pH value and carrys out degradable organic pollutant.Because Fenton oxidation method is simple to operate, drop
Efficiency high, device simple are solved, in addition using Fe2+As catalyst, and iron material is abundant, bio-compatibility, with low cost, therefore
Fenton oxidation method is favored extensively.
However, homogeneous Fenton oxidation method is present, pH applications are narrow, produce a large amount of iron cements after reaction, need to be pre-adjusted waste water
The problems such as pH value.In order to overcome the shortcoming that homogeneous Fenton oxidation method is present, class Fenton technology, out-phase class Fenton are further developed
Catalyst applicable pH range is wide can even degrade under near-neutral sulfite deinking, catalyst recoverable, without iron cement generation, H2O2Profit
With rate height by domestic and international extensive concern.
Traditional different in nature class fenton catalyst is mainly powder body material, there is catalyst and recycles difficult, poor mechanical property
Shortcoming
The content of the invention
The invention aims to solve existing class fenton catalyst to there is separation and recovery of catalyst using difficult, mechanical property
Poor the problem of, and one kind is provided and prepares efficient Fe3O4/FeAl2O4The methods and applications of composite film class fenton catalyst.
One kind prepares efficient Fe3O4/FeAl2O4The method of composite film class fenton catalyst, is to complete according to the following steps
's：
First, carbon steel polishing：Use 500 mesh silicon carbide papers, 1000 mesh silicon carbide papers, 1500 mesh water millings successively first
The surface that paper mesh, 2000 mesh silicon carbide papers and 2500 mesh silicon carbide papers carry out being polishing to carbon steel to the surface of carbon steel is minute surface；So
Afterwards using the surface 3 times~5 times of deionized water rinsing carbon steel, the surface 3 times~5 times that absolute ethyl alcohol rinses carbon steel is reused, most
Dried up afterwards using hair-dryer, obtain the carbon steel of light；
2nd, the bright carbon steel obtained in step one is placed in the electrolyte in stainless steel electrolytic groove, bright carbon steel
It is connected with positive source, is used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 1A/cm in current density2~20A/cm2, supply frequency 100Hz~3000Hz,
The pH value of 10 DEG C~50 DEG C of electrolyte temperature and electrolyte is progress plasma electrolytic oxidation reaction under conditions of 8.0~14.0
5min~30min, obtains efficient Fe3O4/FeAl2O4Composite film class fenton catalyst；
Electrolyte described in step 3 is made up of main film forming agent and additive, and solvent is water；Described main film forming agent
Concentration is 1g/L~20g/L；The concentration of described additive is 0.1g/L~2g/L.
Efficient Fe3O4/FeAl2O4Composite film class fenton catalyst is used to handle the waste water containing phenol.
Advantage of the present invention：
First, electrolyte system of the invention is simple, economical and practical, and preparation technology is simple；
2nd, the present invention prepares Fe using plasma electrolysis oxidation method first3O4/FeAl2O4Composite film class Fenton is catalyzed
Agent；
3rd, present invention gained film layer has multistage nested pore structure, and Film color is grey black, and average pore size is 6.4 μm；
4th, efficient Fe prepared by the present invention3O4/FeAl2O4Composite film class fenton catalyst is easily recycled, iron-free
Mud is produced, with excellent stability, and processing cost is cheap, technique simple, thus is had a good application prospect；
5th, the present invention is successfully prepared efficient Fe using plasma electrolysis deposition technique on carbon steel3O4/FeAl2O4It is compound
Film layer class fenton catalyst, can be mass-produced；
6th, Fe prepared by the present invention3O4/FeAl2O4The degraded of composite film class fenton catalyst Pyrogentisinic Acid in 60min
Efficiency is up to 100%.
The present invention can obtain one kind and prepare efficient Fe3O4/FeAl2O4The method of composite film class fenton catalyst.
Brief description of the drawings
Fig. 1 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The XRD spectrum of composite film class fenton catalyst；Figure
" ▲ " represents Fe3O4 diffraction maximums in 1, and "●" represents FeAl2O4Diffraction maximum；
Fig. 2 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The Fe 2p3/2 couple of composite film class fenton catalyst
The XPS spectrum peak answered；
Fig. 3 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst amplifies 1000 times
SEM schemes；
Fig. 4 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The digital photograph of composite film class fenton catalyst；
Fig. 5 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst amplifies 5000 times
SEM schemes；
Fig. 6 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The drop of composite film class fenton catalyst degrading waste water
Solve efficiency versus time curve figure.
Embodiment
Embodiment one：Present embodiment is that one kind prepares efficient Fe3O4/FeAl2O4Composite film class Fenton is catalyzed
The method of agent is completed according to the following steps：
First, carbon steel polishing：Use 500 mesh silicon carbide papers, 1000 mesh silicon carbide papers, 1500 mesh water millings successively first
The surface that paper mesh, 2000 mesh silicon carbide papers and 2500 mesh silicon carbide papers carry out being polishing to carbon steel to the surface of carbon steel is minute surface；So
Afterwards using the surface 3 times~5 times of deionized water rinsing carbon steel, the surface 3 times~5 times that absolute ethyl alcohol rinses carbon steel is reused, most
Dried up afterwards using hair-dryer, obtain the carbon steel of light；
2nd, the bright carbon steel obtained in step one is placed in the electrolyte in stainless steel electrolytic groove, bright carbon steel
It is connected with positive source, is used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 1A/cm in current density2~20A/cm2, supply frequency 100Hz~3000Hz,
The pH value of 10 DEG C~50 DEG C of electrolyte temperature and electrolyte is progress plasma electrolytic oxidation reaction under conditions of 8.0~14.0
5min~30min, obtains efficient Fe3O4/FeAl2O4Composite film class fenton catalyst；
Electrolyte described in step 3 is made up of main film forming agent and additive, and solvent is water；Described main film forming agent
Concentration is 1g/L~20g/L；The concentration of described additive is 0.1g/L~2g/L.
Present embodiment advantage：
First, the electrolyte system of present embodiment is simple, economical and practical, and preparation technology is simple；
2nd, present embodiment prepares Fe using plasma electrolysis oxidation method first3O4/FeAl2O4Composite film class Fenton is urged
Agent；
3rd, film layer obtained by present embodiment has multistage nested pore structure, and Film color is grey black, and average pore size is
6.4 μm；
4th, efficient Fe prepared by present embodiment3O4/FeAl2O4Composite film class fenton catalyst is easily recycled,
Produced without iron cement, with excellent stability, and processing cost is cheap, technique simple, thus has a good application prospect；
5th, present embodiment is successfully prepared efficient Fe using plasma electrolysis deposition technique on carbon steel3O4/FeAl2O4
Composite film class fenton catalyst, can be mass-produced；
6th, Fe prepared by present embodiment3O4/FeAl2O4Composite film class fenton catalyst Pyrogentisinic Acid in 60min
Degradation efficiency is up to 100%.
Present embodiment can obtain one kind and prepare efficient Fe3O4/FeAl2O4The method of composite film class fenton catalyst.
Embodiment two：Present embodiment is with the difference of embodiment one：Described main film forming agent is aluminium
Sour sodium.Other steps are identical with embodiment one.
Embodiment three：One of present embodiment and embodiment one or two difference is：Described addition
Agent is a hydration sodium hypophosphite.Other steps are identical with embodiment one or two.
Embodiment four：One of present embodiment and embodiment one to three difference is：Institute in step one
The carbon steel stated is Q235 carbon steels.Other steps are identical with embodiment one to three.
Embodiment five：One of present embodiment and embodiment one to four difference is：Adopted in step 3
Powered with the pulse power, be 8A/cm in current density2~20A/cm2, supply frequency 100Hz~3000Hz, electrolyte temperature 10
DEG C~50 DEG C and electrolyte ph be to carry out plasma electrolytic oxidation reaction 5min~30min under conditions of 8.0~14.0, obtain
To efficient Fe3O4/FeAl2O4Composite film class fenton catalyst.Other steps are identical with embodiment one to four.
Embodiment six：One of present embodiment and embodiment one to five difference is：Adopted in step 3
Powered with the pulse power, be 10A/cm in current density2~20A/cm2, supply frequency 500Hz~3000Hz, electrolyte temperature
The pH value of 10 DEG C~50 DEG C and electrolyte be carry out under conditions of 8.0~14.0 plasma electrolytic oxidation reaction 5min~
30min, obtains efficient Fe3O4/FeAl2O4Composite film class fenton catalyst.Other steps and the phase of embodiment one to five
Together.
Embodiment seven：One of present embodiment and embodiment one to six difference is：Institute in step 3
The electrolyte stated is made up of main film forming agent and additive, and solvent is water；The concentration of described main film forming agent is 5g/L~20g/L；
The concentration of described additive is 0.5g/L~2g/L.Other steps are identical with embodiment one to six.
Embodiment eight：One of present embodiment and embodiment one to seven difference is：Institute in step 3
The electrolyte stated is made up of main film forming agent and additive, and solvent is water；The concentration of described main film forming agent is 10g/L~20g/L；
The concentration of described additive is 1g/L~2g/L.Other steps are identical with embodiment one to seven.
Embodiment nine：Present embodiment is efficient Fe3O4/FeAl2O4Composite film class fenton catalyst is used to locate
Manage the waste water containing phenol.
Embodiment ten：The difference of present embodiment and embodiment nine is：By efficient Fe3O4/
FeAl2O4Composite film class fenton catalyst is added in the waste water containing phenol, and low whipping speed is 100r/min~500r/
The hydrogen peroxide that mass fraction is 30% is added under min, then low whipping speed is stirring reaction under 100r/min~500r/min
45min~60min, water after being handled；Described efficient Fe3O4/FeAl2O4The geometric surface of composite film class fenton catalyst
Product and the volume ratio (5cm in the waste water containing phenol2~10cm2):50mL；Phenol in the described waste water containing phenol
Concentration is 20mg/L~50mg/L；Described efficient Fe3O4/FeAl2O4The geometric area and matter of composite film class fenton catalyst
The volume ratio for measuring the hydrogen peroxide that fraction is 30% is (5cm2~10cm2):0.034mL.Other are identical with embodiment nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：One kind prepares efficient Fe3O4/FeAl2O4The method of composite film class fenton catalyst is by following step
Suddenly complete：
First, carbon steel polishing：Use 500 mesh silicon carbide papers, 1000 mesh silicon carbide papers, 1500 mesh water millings successively first
The surface that paper mesh, 2000 mesh silicon carbide papers and 2500 mesh silicon carbide papers carry out being polishing to carbon steel to the surface of carbon steel is minute surface；So
Afterwards using the surface 4 times of deionized water rinsing carbon steel, the surface 4 times that absolute ethyl alcohol rinses carbon steel is reused, finally using blowing
Machine is dried up, and obtains the carbon steel of light；
Carbon steel described in step one is Q235 carbon steels；
2nd, the bright carbon steel obtained in step one is placed in the electrolyte in stainless steel electrolytic groove, bright carbon steel
It is connected with positive source, is used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 15A/cm in current density2, supply frequency 2000Hz, 30 DEG C of electrolyte temperature
PH value with electrolyte is progress plasma electrolytic oxidation reaction 15min under conditions of 13.0, obtains efficient Fe3O4/
FeAl2O4Composite film class fenton catalyst；
Electrolyte described in step 3 is made up of main film forming agent and additive, and solvent is water；Described main film forming agent
Concentration is 10g/L；The concentration of described additive is 1.5g/L；
Main film forming agent described in step 3 is sodium aluminate；
Additive described in step 3 is a hydration sodium hypophosphite.
Fig. 1 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The XRD spectrum of composite film class fenton catalyst；Figure
" ▲ " represents Fe3O4 diffraction maximums in 1, and "●" represents FeAl2O4Diffraction maximum；
Composite film necessarily contains Fe as can be seen from Figure 13O4, FeAl may be contained2O4。
Fig. 2 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The Fe 2p3/2 couple of composite film class fenton catalyst
The XPS spectrum peak answered；
As can be seen from Figure 2,709.9eV, 713.4eV correspond to Fe after swarming3O4In Fe2+、Fe3+, 709.9eV, 713.4
EV corresponds to FeAl2O4In Fe2+、Fe3+, thus, it can be known that the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film
Class fenton catalyst composition is by Fe3O4And FeAl2O4Constitute.
Fig. 3 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst amplifies 1000 times
SEM schemes；
Fig. 4 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The digital photograph of composite film class fenton catalyst；
Fig. 5 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst amplifies 5000 times
SEM schemes；
It was found from Fig. 3 and Fig. 5, the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst is
Multistage nesting pore structure, average pore size is 6.4 μm；
As can be seen from Figure 4, the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The color of composite film class fenton catalyst
To show grey black.
By 6cm2Efficient Fe3O4/FeAl2O4Composite film class fenton catalyst is added to 50mL phenol concentrations for 35mg/L
The waste water containing phenol in, low whipping speed is that the hydrogen peroxide that 0.034mL mass fractions are 30% is added under 150r/min, then
Low whipping speed is stirring reaction 0min~60min, water after being handled under 150r/min；As shown in Figure 6.
Fig. 6 is the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4The drop of composite film class fenton catalyst degrading waste water
Solve efficiency versus time curve figure.
As can be seen from Figure 6, the Fe that the step 3 of embodiment one is obtained3O4/FeAl2O4Composite film class fenton catalyst is in 60min
The degradation efficiency of interior Pyrogentisinic Acid is up to 100%.
Claims (1)
1. a kind of efficient Fe3O4/FeAl2O4The application of composite film class fenton catalyst, it is characterised in that efficient Fe3O4/
FeAl2O4Composite film class fenton catalyst is used to handle the waste water containing phenol；
Described efficient Fe3O4/FeAl2O4It is by following step that composite film class fenton catalyst, which is used to handle the waste water containing phenol,
Suddenly complete：
By efficient Fe3O4/FeAl2O4Composite film class fenton catalyst is added in the waste water containing phenol, and low whipping speed is
The hydrogen peroxide that mass fraction is 30% is added under 100r/min~500r/min, then low whipping speed is 100r/min~500r/
Stirring reaction 45min~60min, water after being handled under min；Described efficient Fe3O4/FeAl2O4Composite film class Fenton is urged
The geometric area of agent and the volume ratio (5cm in the waste water containing phenol2~10cm2):50mL；Described is useless containing phenol
The concentration of phenol is 20mg/L~50mg/L in water；Described efficient Fe3O4/FeAl2O4Composite film class fenton catalyst
The volume ratio for the hydrogen peroxide that geometric area is 30% with mass fraction is (5cm2~10cm2):0.034mL；
Described efficient Fe3O4/FeAl2O4The preparation method of composite film class fenton catalyst is completed according to the following steps：
First, carbon steel polishing：Use 500 mesh silicon carbide papers, 1000 mesh silicon carbide papers, 1500 mesh silicon carbide papers successively first
The surface that mesh, 2000 mesh silicon carbide papers and 2500 mesh silicon carbide papers carry out being polishing to carbon steel to the surface of carbon steel is minute surface；Then
Using the surface 4 times of deionized water rinsing carbon steel, the surface 4 times that absolute ethyl alcohol rinses carbon steel is reused, finally using hair-dryer
Drying, obtains the carbon steel of light；
Carbon steel described in step one is Q235 carbon steels；
2nd, the bright carbon steel obtained in step one is placed in the electrolyte in stainless steel electrolytic groove, bright carbon steel and electricity
Source positive pole is connected, and is used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 15A/cm in current density2, supply frequency 2000Hz, 30 DEG C of electrolyte temperature and electricity
The pH value for solving liquid is progress plasma electrolytic oxidation reaction 15min under conditions of 13.0, obtains efficient Fe3O4/FeAl2O4It is multiple
Close film layer class fenton catalyst；
Electrolyte described in step 3 is made up of main film forming agent and additive, and solvent is water；The concentration of described main film forming agent
For 10g/L；The concentration of described additive is 1.5g/L；
Main film forming agent described in step 3 is sodium aluminate；
Additive described in step 3 is a hydration sodium hypophosphite；
Described efficient Fe3O4/FeAl2O4Composite film class fenton catalyst degradation efficiency of Pyrogentisinic Acid in 60min is reachable
100%.
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| CN105536812A (en) * | 2016-01-08 | 2016-05-04 | 清华大学 | Nano Fe3O4/Mn3O4 composite material and preparation method and application thereof |
| CN106345472A (en) * | 2016-08-05 | 2017-01-25 | 哈尔滨工业大学 | Method for preparing high-efficient Fenton-like catalyst of sulphur modified iron-based composite material solid acid ceramic film layer and application |
| CN107245749B (en) * | 2017-06-09 | 2019-03-12 | 哈尔滨工业大学 | A kind of method and application preparing sulfur doping out-phase fenton catalyst in titanium alloy surface |
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| US8808522B2 (en) * | 2011-09-07 | 2014-08-19 | National Chung Hsing University | Method for forming oxide film by plasma electrolytic oxidation |
| CN104437502B (en) * | 2014-12-15 | 2017-01-04 | 南京理工大学 | Magnetic fenton catalyst ferrospinel with Fenton iron containing sludge as source of iron and application |
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