CN105297108B - A kind of utilization plasma electrolytic oxidation method prepares the methods and applications of ceramic film class fenton catalyst on Q235 carbon steels surface - Google Patents
A kind of utilization plasma electrolytic oxidation method prepares the methods and applications of ceramic film class fenton catalyst on Q235 carbon steels surface Download PDFInfo
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- CN105297108B CN105297108B CN201510785645.5A CN201510785645A CN105297108B CN 105297108 B CN105297108 B CN 105297108B CN 201510785645 A CN201510785645 A CN 201510785645A CN 105297108 B CN105297108 B CN 105297108B
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Abstract
A kind of utilization plasma electrolytic oxidation method prepares the methods and applications of ceramic film class fenton catalyst on Q235 carbon steels surface, and it is related to a kind of methods and applications for preparing class fenton catalyst.The problem of the invention aims to solve complicated existing traditional class fenton catalyst separation and recovery and poor mechanical property.Method：First, Q235 carbon steels pre-treatment；2nd, the bright Q235 carbon steels obtained in step one are placed in the electrolyte in stainless steel electrolytic groove, are used as anode；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；3rd, plasma electrolysis reaction is adopted, ceramic film class fenton catalyst is obtained.The degradation efficiency of ceramic film class fenton catalyst Pyrogentisinic Acid in 180min prepared by the present invention is up to 96%；Its tensile strength is up to 14MPa.The present invention can obtain a kind of method that utilization plasma electrolytic oxidation method prepares ceramic film class fenton catalyst on Q235 carbon steels surface.
Description
Technical field
The present invention relates to a kind of methods and applications for preparing class fenton catalyst.
Background technology
With the rapid development of economy, environmental problem is increasingly serious, wherein, the water body that persistent organic pollutants trigger is dirty
Dye becomes increasingly conspicuous.Hardly degraded organic substance pollutant can not thoroughly be gone using traditional means such as flocks, absorption, biological treatment etc.
Remove, and high-level oxidation technology uses the strong oxidizing property hydroxyl radical free radical by the thorough mineralising of persistent organic pollutants for carbon dioxide
And water, therefore have broad application prospects.
Fenton oxidation method utilizes Fe in high-level oxidation technology2+And H2O2It is generation strong oxidizing property hydroxyl between 2~3 to be blended in pH
Base free radical carrys out degradable organic pollutant.Due to its abundant raw material, with low cost, efficiency high and widely paid close attention to.
However, because Fenton oxidation method is present, pH working ranges are narrow, catalyst is Fe2+, need before and after sewage disposal to adjust pH
The shortcomings of producing iron cement in value, degraded, has further developed class fenton catalyst.At present, class fenton catalyst is main with solid
The form presence of powder, but there is separation and recovery complexity in it, in order to solve conventional powder class fenton catalyst separation and recovery hardly possible
Shortcoming, the present invention is prepared for ceramics in silicate electrolyte using plasma electrolytic oxidation method in Q235 carbon steel surface in situ
Film layer class fenton catalyst.
The content of the invention
It is complicated and poor mechanical property the invention aims to solve existing traditional class fenton catalyst separation and recovery
Problem, and a kind of utilization plasma electrolytic oxidation method is provided and prepares ceramic film class fenton catalyst on Q235 carbon steels surface
Methods and applications.
A kind of utilization plasma electrolytic oxidation method prepares the side of ceramic film class fenton catalyst on Q235 carbon steels surface
Method is completed according to the following steps：
First, Q235 carbon steels pre-treatment：Successively using the table of 500# sand paper, 1500# sand paper and 2500# sand paper to Q235 carbon steels
The surface that face carries out being polishing to Q235 carbon steels is minute surface；Using deionized water rinsing Q235 carbon steels surface 3 times~5 times, reuse
Absolute ethyl alcohol rinses Q235 carbon steels surface 3 times~5 times, is finally dried up using hair-dryer, obtains the Q235 carbon steels of light；
2nd, the bright Q235 carbon steels obtained in step one are placed in the electrolyte in stainless steel electrolytic groove, are used as sun
Pole；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 density2~15A/cm2, supply frequency 500Hz~3000Hz,
10 DEG C~50 DEG C of electrolyte temperature and electrolyte ph are progress plasma electrolytic oxidation reaction under conditions of 9.0~14.0
5min~20min, ceramic film class fenton catalyst is obtained on Q235 carbon steels surface, that is, is completed one kind and utilized plasma electrolysis
The method that oxidizing process prepares ceramic film class fenton catalyst on Q235 carbon steels surface；
Electrolyte described in step 3 is made up of sodium metasilicate, sodium hypophosphite and water；Sodium metasilicate in described electrolyte
Concentration be 10g/L~30g/L；The concentration of sodium hypophosphite is 0.5g/L~2g/L in described electrolyte.
Ceramic film class fenton catalyst is used to handle the waste water containing phenol.
Advantages 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 ceramics using plasma electrolysis oxidation method on Q235 carbon steels in silicate electrolyte first
Film layer class fenton catalyst；
3rd, the film layer of ceramic film class fenton catalyst prepared by the present invention is coarse black film layer, and average pore size is
2.5μm；
4th, the present invention can be mass-produced ceramic film class fenton catalyst；
5th, ceramic film class fenton catalyst prepared by the present invention degradation efficiency of Pyrogentisinic Acid in 180min is reachable
96%；
6th, ceramic film class fenton catalyst prepared by the present invention, its tensile strength is up to 14MPa.
The present invention can obtain one kind and ceramic film class sweet smell is prepared on Q235 carbon steels surface using plasma electrolytic oxidation method
The method of catalyst.
Brief description of the drawings
Fig. 1 is the XRD spectrum for the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained；" ▲ " represents in Fig. 1
Fe diffraction maximum；
Fig. 2 is the corresponding XPS spectrum figures of Fe 2p3/2 for the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained；
The corresponding XPS spectrum figures of Si 2p for the ceramic film class fenton catalyst that the step 3 of Fig. 3 embodiments one is obtained；
Fig. 4 is the SEM figures that the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained amplifies 1000 times；
Fig. 5 is the degraded for waste water of the ceramic film class fenton catalyst degraded containing phenol that the step 3 of embodiment one is obtained
The 1 ceramic film class Fenton obtained for the step 3 of embodiment one in efficiency and total iron stripping quantity versus time curve figure, Fig. 5
Catalyst degradation contains the degradation efficiency curve of the waste water of phenol, and 2 be the ceramic film class Fenton that the step 3 of embodiment one is obtained
Total iron stripping quantity versus time curve of catalyst.
Embodiment
Embodiment one：Present embodiment is that one kind utilizes plasma electrolytic oxidation method in Q235 carbon steel surface systems
The method of standby ceramic film class fenton catalyst is completed according to the following steps：
First, Q235 carbon steels pre-treatment：Successively using the table of 500# sand paper, 1500# sand paper and 2500# sand paper to Q235 carbon steels
The surface that face carries out being polishing to Q235 carbon steels is minute surface；Using deionized water rinsing Q235 carbon steels surface 3 times~5 times, reuse
Absolute ethyl alcohol rinses Q235 carbon steels surface 3 times~5 times, is finally dried up using hair-dryer, obtains the Q235 carbon steels of light；
2nd, the bright Q235 carbon steels obtained in step one are placed in the electrolyte in stainless steel electrolytic groove, are used as sun
Pole；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 density2~15A/cm2, supply frequency 500Hz~3000Hz,
10 DEG C~50 DEG C of electrolyte temperature and electrolyte ph are progress plasma electrolytic oxidation reaction under conditions of 9.0~14.0
5min~20min, ceramic film class fenton catalyst is obtained on Q235 carbon steels surface, that is, is completed one kind and utilized plasma electrolysis
The method that oxidizing process prepares ceramic film class fenton catalyst on Q235 carbon steels surface；
Electrolyte described in step 3 is made up of sodium metasilicate, sodium hypophosphite and water；Sodium metasilicate in described electrolyte
Concentration be 10g/L~30g/L；The concentration of sodium hypophosphite is 0.5g/L~2g/L in described electrolyte.
The advantage of present embodiment：
First, the electrolyte system of present embodiment is simple, economical and practical, and preparation technology is simple；
2nd, present embodiment is prepared on Q235 carbon steels using plasma electrolysis oxidation method in silicate electrolyte first
Ceramic film class fenton catalyst；
3rd, the film layer of ceramic film class fenton catalyst prepared by present embodiment is coarse black film layer, average hole
Footpath is 2.5 μm；
4th, present embodiment can be mass-produced ceramic film class fenton catalyst；
5th, ceramic film class fenton catalyst prepared by the present embodiment degradation efficiency of Pyrogentisinic Acid in 180min is reachable
96%；
6th, ceramic film class fenton catalyst prepared by present embodiment, its tensile strength is up to 14MPa.
Present embodiment can obtain one kind and prepare ceramic film on Q235 carbon steels surface using plasma electrolytic oxidation method
The method of class fenton catalyst.
Embodiment two：Present embodiment is with the difference of embodiment one：Using pulse electricity in step 3
Source powers, and is 1A/cm in current density2~12A/cm2, supply frequency 500Hz~2000Hz, 10 DEG C~50 DEG C of electrolyte temperature
With electrolyte ph be 10.0~14.0 under conditions of carry out plasma electrolytic oxidation reaction 10min~20min, you can
Q235 carbon steels surface obtains ceramic film class fenton catalyst, that is, completes one kind using plasma electrolytic oxidation method in Q235 carbon
The method that steel surface prepares ceramic film class fenton catalyst.Other steps are identical with embodiment one.
Embodiment three：One of present embodiment and embodiment one or two difference is：Adopted in step 3
Powered with the pulse power, be 7A/cm in current density2~15A/cm2, supply frequency 2000Hz~3000Hz, electrolyte temperature 10
DEG C~50 DEG C and electrolyte ph be to carry out plasma electrolytic oxidation reaction 10min~20min under conditions of 12.0~14.0,
Ceramic film class fenton catalyst is obtained on Q235 carbon steels surface, that is, completes one kind using plasma electrolytic oxidation method in Q235
The method that carbon steel surface prepares ceramic film class fenton catalyst.Other steps are identical with embodiment one or two.
Embodiment four：One of present embodiment and embodiment one to three difference is：Adopted in step 3
Powered with the pulse power, be 10A/cm in current density2, supply frequency 1000Hz, 30 DEG C of electrolyte temperature and electrolyte ph
To carry out plasma electrolytic oxidation reaction 10min under conditions of 12.0, ceramic film class Fenton is obtained on Q235 carbon steels surface
Catalyst, that is, complete one kind and prepare ceramic film class fenton catalyst on Q235 carbon steels surface using plasma electrolytic oxidation method
Method.Other steps are identical with embodiment one to three.
Embodiment five：One of present embodiment and embodiment one to four difference is：Institute in step 3
The concentration of sodium metasilicate is 20g/L~30g/L in the electrolyte stated.Other steps are identical with embodiment one to four.
Embodiment six：One of present embodiment and embodiment one to five difference is：Institute in step 3
The concentration of sodium metasilicate is 10g/L~20g/L in the electrolyte stated.Other steps are identical with embodiment one to five.
Embodiment seven：One of present embodiment and embodiment one to six difference is：Institute in step 3
The concentration of sodium hypophosphite is 0.5g/L~1g/L in the electrolyte stated.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 concentration of sodium hypophosphite is 1g/L~2g/L in the electrolyte stated.Other steps are identical with embodiment one to seven.
Embodiment nine：Present embodiment is that ceramic film class fenton catalyst is used to handle giving up containing phenol
Water；And described ceramic film class fenton catalyst is reachable to the degradation efficiency of the phenol in wastewater containing phenol in 180min
96%.
Embodiment ten：The difference of present embodiment and embodiment nine is：Ceramic film class Fenton is urged
Agent is used for waste water of the processing containing phenol and completed according to the following steps：
Ceramic film class fenton catalyst is immersed in the phenolic waste water that pH is 4.0, then low whipping speed is 100r/
The hydrogen peroxide that mass fraction is 30%, then low whipping speed are added under min~500r/min under 100r/min~500r/min
Stirring reaction 60min~180min, water after being handled；The geometric area of described ceramic film class fenton catalyst is with containing
Volume ratio (the 5cm of the waste water of phenol2~10cm2):50mL；The concentration of the described phenol in wastewater containing phenol is 20mg/L
~50mg/L；The geometric area of described ceramic film class fenton catalyst and volume ratio of the mass fraction for 30% hydrogen peroxide
For (5cm2~10cm2):0.034mL.Other steps are identical with embodiment nine.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：One kind prepares ceramic film class Fenton on Q235 carbon steels surface using plasma electrolytic oxidation method and urged
The method of agent is completed according to the following steps：
First, Q235 carbon steels pre-treatment：Successively using the table of 500# sand paper, 1500# sand paper and 2500# sand paper to Q235 carbon steels
The surface that face carries out being polishing to Q235 carbon steels is minute surface；Using deionized water rinsing Q235 carbon steels surface 4 times, anhydrous second is reused
Alcohol rinses Q235 carbon steels surface 4 times, is finally dried up using hair-dryer, obtains the Q235 carbon steels of light；
2nd, the bright Q235 carbon steels obtained in step one are placed in the electrolyte in stainless steel electrolytic groove, are used as sun
Pole；Stainless steel electrolytic groove is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 12A/cm in current density2, supply frequency 2000Hz, 30 DEG C of electrolyte temperature
With electrolyte ph be 14.0 under conditions of carry out plasma electrolytic oxidation reaction 20min, made pottery on Q235 carbon steels surface
Porcelain film layer class fenton catalyst, that is, complete one kind and prepare ceramic film on Q235 carbon steels surface using plasma electrolytic oxidation method
The method of class fenton catalyst；
Electrolyte described in step 3 is made up of sodium metasilicate, sodium hypophosphite and water；Sodium metasilicate in described electrolyte
Concentration be 25g/L；The concentration of sodium hypophosphite is 1g/L in described electrolyte.
Fig. 1 is the XRD spectrum for the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained；" ▲ " represents in Fig. 1
Fe diffraction maximum；
The ceramic film class fenton catalyst that the step 3 of embodiment one is obtained as can be seen from Figure 1 is amorphous state, its Fe diffraction
Peak derives from Q235 matrixes.
Fig. 2 is the corresponding XPS spectrum figures of Fe 2p3/2 for the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained；
The ceramic film class fenton catalyst that the step 3 of embodiment one is obtained as can be seen from Figure 2 contains Fe3O4。
The corresponding XPS spectrum figures of Si 2p for the ceramic film class fenton catalyst that the step 3 of Fig. 3 embodiments one is obtained；
The ceramic film class fenton catalyst that the step 3 of embodiment one is obtained as can be seen from Figure 3 contains SiO2。
Fig. 4 is the SEM figures that the ceramic film class fenton catalyst that the step 3 of embodiment one is obtained amplifies 1000 times；
The ceramic film class fenton catalyst surface that the step 3 of embodiment one is obtained as can be seen from Figure 4 is coarse, porous shape
Looks.
By 6cm2The ceramic film class fenton catalyst that the step 3 of embodiment one is obtained is added to the benzene that 50mL pH are 4.0
Phenol concentration is in 35mg/L waste water, low whipping speed is that the dioxygen that 0.034mL mass fractions are 30% is added under 150r/min
Water, then low whipping speed are stirring reaction 0min~180min, water after being handled under 150r/min；As shown in Figure 5.
Fig. 5 is the degraded for waste water of the ceramic film class fenton catalyst degraded containing phenol that the step 3 of embodiment one is obtained
The 1 ceramic film class Fenton obtained for the step 3 of embodiment one in efficiency and total iron stripping quantity versus time curve figure, Fig. 5
Catalyst degradation contains the degradation efficiency curve of the waste water of phenol, and 2 be the ceramic film class Fenton that the step 3 of embodiment one is obtained
Total iron stripping quantity versus time curve of catalyst.
Phenol clearance is up to 96% after degraded 180min as can be seen from Figure 5, and total iron stripping quantity is 0.94mg/L, less than European Union
Defined Fe contents (<2mg/L), the concentration of phenol in wastewater is 1.4mg/L during degraded 180min.
Claims (8)
1. a kind of utilization plasma electrolytic oxidation method prepares the application of ceramic film class fenton catalyst on Q235 carbon steels surface,
It is characterized in that ceramic film class fenton catalyst is used to handle the waste water containing phenol；And described ceramic film class Fenton is urged
Agent is in 180min to the degradation efficiency of the phenol in wastewater containing phenol up to 96%；
Described ceramic film class fenton catalyst is used for waste water of the processing containing phenol and completed according to the following steps：
By ceramic film class fenton catalyst be immersed in pH be 4.0 phenolic waste water in, then low whipping speed be 100r/min~
The hydrogen peroxide that mass fraction is 30%, then low whipping speed are added under 500r/min anti-to be stirred under 100r/min~500r/min
60min~180min is answered, water after being handled；The geometric area of described ceramic film class fenton catalyst is with containing phenol
Volume ratio (the 5cm of waste water2~10cm2):50mL；The concentration of the described phenol in wastewater containing phenol is 20mg/L~50mg/
L；The volume ratio for the hydrogen peroxide that the geometric area of described ceramic film class fenton catalyst is 30% with mass fraction is (5cm2
~10cm2):0.034mL；
The method of described ceramic film class fenton catalyst is completed according to the following steps：
First, Q235 carbon steels pre-treatment：The surface of Q235 carbon steels is entered using 500# sand paper, 1500# sand paper and 2500# sand paper successively
The surface that row is polishing to Q235 carbon steels is minute surface；Using deionized water rinsing Q235 carbon steels surface 3 times~5 times, reuse anhydrous
Alcohol flushing Q235 carbon steels surface 3 times~5 times, is finally dried up using hair-dryer, obtains the Q235 carbon steels of light；
2nd, the bright Q235 carbon steels obtained in step one are placed in the electrolyte in stainless steel electrolytic groove, are used as anode；No
Rust steel electrolytic cell is connected with power cathode, is used as negative electrode；
3rd, powered using the pulse power, be 1A/cm in current density2~15A/cm2, supply frequency 500Hz~3000Hz, electrolysis
10 DEG C~50 DEG C of liquid temperature degree and electrolyte ph be carry out under conditions of 9.0~14.0 plasma electrolytic oxidation reaction 5min~
20min, ceramic film class fenton catalyst is obtained on Q235 carbon steels surface, that is, is completed one kind and utilized plasma electrolytic oxidation method
The method for preparing ceramic film class fenton catalyst on Q235 carbon steels surface；
Electrolyte described in step 3 is made up of sodium metasilicate, sodium hypophosphite and water；Sodium metasilicate is dense in described electrolyte
Spend for 10g/L~30g/L；The concentration of sodium hypophosphite is 0.5g/L~2g/L in described electrolyte.
2. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that powered in step 3 using the pulse power, is 1A/cm in current density2~
12A/cm2, supply frequency 500Hz~2000Hz, 10 DEG C~50 DEG C of electrolyte temperature and electrolyte ph be 10.0~14.0
Under the conditions of carry out plasma electrolytic oxidation reaction 10min~20min, you can ceramic film class is obtained on Q235 carbon steels surface fragrant
Pause catalyst, that is, complete one kind and the catalysis of ceramic film class Fenton is prepared on Q235 carbon steels surface using plasma electrolytic oxidation method
The method of agent.
3. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that powered in step 3 using the pulse power, is 7A/cm in current density2~
15A/cm2, supply frequency 2000Hz~3000Hz, 10 DEG C~50 DEG C of electrolyte temperature and electrolyte ph be 12.0~14.0
Under the conditions of carry out plasma electrolytic oxidation reaction 10min~20min, obtain ceramic film class Fenton on Q235 carbon steels surface and urge
Agent, that is, complete a kind of utilization plasma electrolytic oxidation method and prepare ceramic film class fenton catalyst on Q235 carbon steels surface
Method.
4. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that powered in step 3 using the pulse power, is 10A/cm in current density2, electricity
Source frequency 1000Hz, 30 DEG C of electrolyte temperature and electrolyte ph are progress plasma electrolytic oxidation reaction under conditions of 12.0
10min, ceramic film class fenton catalyst is obtained on Q235 carbon steels surface, that is, is completed one kind and utilized plasma electrolytic oxidation method
The method for preparing ceramic film class fenton catalyst on Q235 carbon steels surface.
5. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that the concentration of sodium metasilicate is 20g/L~30g/ in the electrolyte described in step 3
L。
6. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that the concentration of sodium metasilicate is 10g/L~20g/ in the electrolyte described in step 3
L。
7. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that in the electrolyte described in step 3 the concentration of sodium hypophosphite be 0.5g/L~
1g/L。
8. one kind according to claim 1 prepares ceramic film using plasma electrolytic oxidation method on Q235 carbon steels surface
The application of class fenton catalyst, it is characterised in that in the electrolyte described in step 3 the concentration of sodium hypophosphite be 1g/L~
2g/L。
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| 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 |
| CN111139510B (en) * | 2020-01-15 | 2021-01-19 | 大连海事大学 | Preparation method of marine low-carbon steel anticorrosive coating |
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