CN109806776A - Mix the method for the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material - Google Patents
Mix the method for the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material Download PDFInfo
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- CN109806776A CN109806776A CN201910121470.6A CN201910121470A CN109806776A CN 109806776 A CN109806776 A CN 109806776A CN 201910121470 A CN201910121470 A CN 201910121470A CN 109806776 A CN109806776 A CN 109806776A
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- microfiltration membranes
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Abstract
The invention belongs to catalysis material technical fields, more particularly to a kind of method for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material, this method synthesizes GO nanometer sheet, sol-gal process and high-temperature calcination by modified Hummers method and Fe doping TiO is made2Then the two is mixed with certain proportion by ultrasonic treatment, prepares blended liquid by hydro-thermal method by nano particle, finally by centrifugation, washing, dry, obtained Fe2O3 doping graphene oxide titanic oxide nano compound material.It is modified using surface cladding process to by pretreated micro-filtration film surface, is made and mixes the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material.Microfiltration membranes prepared by the present invention can carry out photocatalytic degradation using visible light, and photocatalytic activity is high.
Description
Technical field
The invention belongs to catalysis material technical fields, and in particular to it is multiple that one kind mixes iron graphene oxide nano titania
The method of the modified microfiltration membranes of condensation material.
Background technique
Titanium dioxide (TiO2) it is most common photochemical catalyst in water process, in addition to having the common trait of nano material
Outside, TiO2Also there is Superhydrophilic, extremely strong surface-active, ultraviolet absorbability, efficient photocatalytic activity etc..TiO2It can
Organic pollutant (such as organic dyestuff, toxic micropollutants, oil) is resolved into carbon dioxide and water completely.It has been found that by TiO2It receives
Rice grain, which is integrated in water filter membrane, can enhance its flux, pollutant removal and resistance tocrocking.However, TiO is used alone2It is made
Photocatalytic activity of the photocatalysis membrana under sunlight it is very low.This is because TiO2Band-gap energy (3.2eV) with higher,
Therefore the electron hole of photocatalysis can only be less than 387nm by wavelength and energy is higher than the ultraviolet photoactivation of 3.2eV.So tool
TiO cannot be excited by having the visible light of longer wavelength2Photocatalytic activity.
Summary of the invention
Invention broadly provides a kind of sides for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material
The microfiltration membranes of method, preparation can carry out photocatalytic degradation using visible light, and photocatalytic activity is high.Its technical solution is as follows:
A method of mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material, comprising the following steps:
(1) by graphite in KMnO4、H2SO4And NaNO3Mixture in aoxidize, filter mixture to collect solid particle,
The solid in deionized water is washed to removing chemical residue by settling flux and centrifuge cycle, using ultrasonic cleaner by GO
Particle suspension liquid ultrasonication is, at GO nanometer sheet, to remove any unpeeled stone finally by centrifugation for graphite oxide removing
The suspension is freeze-dried to obtain pure GO nanometer sheet suspension and obtains GO powder by black residue；
(2) it configures A liquid: measuring dehydrated alcohol and be added to the container, butyl titanate is added into container；
Configuration B liquid: FeCl is taken3, dehydrated alcohol, deionized water and acetic acid mixing, adjust pH value of solution to 2-3；
Fe-TiO2The preparation of particle: B liquid being added in A liquid when stirring A liquid, rear stirring, it is still aging obtain it is transparent solidifying
Glue, then Fe-TiO is obtained by dry, grinding, calcining2Particle；
(3) it disperses GO powder prepared by step (1) in deionized water, is ultrasonically treated, added into deionized water
Enter the Fe-TiO of step (2) preparation2Particle is then sonicated, and obtains blending suspension, and suspension will be blended and carry out pyroreaction,
Then cooling, centrifugation, washing, drying, obtain Fe-GO/TiO2Particle；
(4) microfiltration membranes are impregnated with deionized water, then film is immersed into KMNO4In the mixed solution of NaOH, taken after reaction
It washes out, film becomes yellowish-brown, then film is placed in NaHSO3It is taken off completely in solution to yellowish-brown, takes out washing, then use surface
Activator solution impregnates, and obtains pretreated microfiltration membranes；
(5) Fe-GO/TiO for preparing step (3)2Particle ultrasonic disperse adds in deionized water into the deionized water
Enter pretreated microfiltration membranes, reaction obtains modified microfiltration membranes.
Preferably, FeCl in step (2)3Mass ratio with butyl titanate is 1:15-20.
Preferably, calcining described in step (2) is specifically to be warming up to 450-500 DEG C of calcining 2-3h with 2.5 DEG C/min,
Then 2h is kept the temperature.
Preferably, GO powder and Fe-TiO in step (3)2The mass ratio of particle is 1:15-20.
Preferably, it is 180 DEG C, centrifugal condition 5000rpm that suspension pyroreaction temperature is blended in step (3), is used
Deionized water is washed three times, and drying condition is lower 60 DEG C of vacuum dry 18h.
Preferably, the material of microfiltration membranes described in step (4) is polysulfones, polyether sulfone, polytetrafluoroethylene (PTFE), Kynoar vinegar
Any one of acid cellulose class and polyvinyl chloride.
Preferably, surfactant described in step (4) is neopelex or cetyl trimethyl bromination
Ammonium.
Preferably, Fe-GO/TiO in step (5)2It is 1g/L that particle, which is scattered in turbid liquid concentration obtained in deionized water,.
Preferably, pretreated microfiltration membranes are washed out drying as 3h is kept the temperature at 80 DEG C in suspension in step (5)
?.
Using the above scheme, the invention has the following advantages that
(1) graphene oxide (GO) is the excellent inorganic nano material for membrane modifying, and structure is sheet, containing a large amount of
The oxygen-containing functional groups such as carboxyl, hydroxyl, epoxy group have very strong hydrophily.GO and TiO2It is compound, promotion can be met simultaneously
TiO2The big element of the three of photocatalysis performance: change TiO2Forbidden bandwidth, and then it is expanded to visible absorption range；Reduce photoproduction
The probability of recombination of electron-hole extends the service life of photo-generated carrier, so that photo-generated carrier is sufficiently had an effect；Improve TiO2
To the adsorption capacity of organic pollutant, sufficiently degrade to it；
(2) the modified TiO of iron ion doping2, in TiO2Iron ion is introduced in lattice can cause atom defect and charge defects,
These defects can become the trap in capture electronics or hole, and then extend the service life of photo-generated carrier；And iron ion and TiO2
Combination level is formed, enables first to be transitted to impurity by the electronics excited, then transit to TiO2Conduction band, can both reduce in this way
Be stimulated required energy, and can guarantee the redox ability of electron-hole, to improve photocatalytic activity；
(3) Fe2O3 doping graphene oxide titanium dioxide is modified microfiltration membranes, and microfiltration membranes are as carrier loaded photocatalysis
Agent reduces the loss of photochemical catalyst, meanwhile, so that the water contact angle of microfiltration membranes is substantially reduced, obtain a kind of photocatalytic activity
Height, the composite micro-filtration membrane that can be all increased using visible light, hydrophily and resistance tocrocking.
Detailed description of the invention
Fig. 1 is the X-ray for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material that embodiment 1 obtains
Diffraction pattern；
Fig. 2 is that the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material are mixed in embodiment 1 respectively in difference
To the degradation efficiency figure of methylene blue (MB) under light source.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
The present embodiment mix the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material the preparation method is as follows:
(1) GO nanometer sheet is synthesized by graphite modified Hummers method.Synthesis process includes by graphite in KMnO4, H2SO4With
NaNO3Mixture in aoxidize, filter mixture to collect solid particle (i.e. graphite oxide), pass through settling flux three times and centrifugation
Solid in circulation washing deionized water is to removing chemical residue, using ultrasonic cleaner by GO particle suspension liquid ultrasonic wave
Processing is, at GO nanometer sheet, it is pure to obtain to remove any unpeeled graphite residue finally by centrifugation for graphite oxide removing
The suspension is freeze-dried and obtains GO powder by GO nanometer sheet suspension；
(2) Fe-TiO is prepared using sol-gel method2Nano particle.Firstly, 10mL butyl titanate is added to 20mL
To form solution A in dehydrated alcohol.Solution B is that FeCl is added310mL dehydrated alcohol, 15mL deionized water and 4.5mL acetic acid
Mixture, the pH of solution B is adjusted to 2 with HCl, solution B is slowly dropped in solution A under vigorous stirring.It has titrated
Mixed solution is obtained after, continues to stir 1h or so under the action of magnetic stirring apparatus.Then, still aging 2h forms yellow
Clear gel.Drying composite and yellow crystals are formed in 100 DEG C of baking oven, solid is transformed into white powder by grinding
End.Then 2h is calcined at 500 DEG C, keeps the temperature 2h, completes Fe-TiO2Preparation；
(3) Fe-GO/TiO is prepared using hydro-thermal method2Particle.Firstly, dispersing 0.05gGO in 80mL deionized water, pass through
Ultrasonication 1h.Add 1gFe-TiO2Afterwards, further 1h is needed to be ultrasonically treated.Then, solution is moved into 100mL spy
In the stainless steel autoclave of fluon lining, it is kept into 18h, cooled to room temperature at a high temperature of 180 DEG C.Finally, will hang
Supernatant liquid is centrifuged with 5000rpm, is then washed with deionized at least three times, and be dried in vacuo at 60 DEG C；
(4) PVDF microfiltration membranes are impregnated into 30min in deionized water, then film is immersed into configured KMNO4It is molten with NaOH
In liquid, washing is taken out after reacting 5min, film becomes yellowish-brown at this time.It is put into NaHSO3Solution in necleophilic reaction to yellowish-brown
Color takes off completely, and taking-up is washed with water to neutrality, then impregnates 5min with proper amount of surfactant CTAB solution；
(5) by 0.1gFe-GO/TiO2Nanometer powder is dispersed in 1h in 100mL deionized water by ultrasonic treatment, is formed outstanding
Turbid.Pretreated pvdf membrane is placed in suspension, 3h is kept the temperature at 80 DEG C, takes out washing, drying.
The modified Fe-GO/TiO in surface2Microfiltration membranes X-ray diffractogram is as shown in Figure 1.
Fe-GO/TiO is calculated in laboratory self-control decomposition apparatus using ultraviolet specrophotometer2Microfiltration membranes it is dark,
To the degradation effect of methylene blue (MB) under ultraviolet and solar radiation, as a result as shown in Figure 2.
Embodiment 2
(1) GO nanometer sheet is synthesized by graphite modified Hummers method.Synthesis process includes by graphite in KMnO4, H2SO4With
NaNO3Mixture in aoxidize, filter mixture to collect solid particle (i.e. graphite oxide), pass through settling flux three times and centrifugation
Solid in circulation washing deionized water is to removing chemical residue, using ultrasonic cleaner by GO particle suspension liquid ultrasonic wave
Processing is, at GO nanometer sheet, it is pure to obtain to remove any unpeeled graphite residue finally by centrifugation for graphite oxide removing
The suspension is freeze-dried and obtains GO powder by GO nanometer sheet suspension；
(2) Fe-TiO is prepared using sol-gel method2Nano particle.Firstly, 10mL butyl titanate is added to 20mL
To form solution A in dehydrated alcohol.Solution B is that FeCl is added310mL dehydrated alcohol, 15mL deionized water and 4.5mL acetic acid
Mixture, the pH of solution B is adjusted to 3 with HCl, solution B is slowly dropped in solution A under vigorous stirring.It has titrated
Mixed solution is obtained after, continues to stir 1h or so under the action of magnetic stirring apparatus.Then, still aging 2h forms yellow
Clear gel.Drying composite and yellow crystals are formed in 100 DEG C of baking oven, solid is transformed into white powder by grinding
End.Then 3h is calcined at 450 DEG C, keeps the temperature 2h, completes Fe-TiO2Preparation；
(3) Fe-GO/TiO is prepared using hydro-thermal method2Particle.Firstly, dispersing 0.05gGO in 80mL deionized water, pass through
Ultrasonication 1h.Add 1gFe-TiO2Afterwards, further 1h is needed to be ultrasonically treated.Then, solution is moved into 100mL spy
In the stainless steel autoclave of fluon lining, it is kept into 18h, cooled to room temperature at a high temperature of 180 DEG C.Finally, will hang
Supernatant liquid is centrifuged with 5000rpm, is then washed with deionized at least three times, and be dried in vacuo at 60 DEG C；
(4) PVDF microfiltration membranes are impregnated into 30min in deionized water, then film is immersed into configured KMNO4It is molten with NaOH
In liquid, washing is taken out after reacting 5min, film becomes yellowish-brown at this time.It is put into NaHSO3Solution in necleophilic reaction to yellowish-brown
Color takes off completely, and taking-up is washed with water to neutrality, then impregnates 5min with proper amount of surfactant CTAB solution；
(5) by 0.1gFe-GO/TiO2Nanometer powder is dispersed in 1h in 100mL deionized water by ultrasonic treatment, is formed outstanding
Turbid.Pretreated pvdf membrane is placed in suspension, 3h is kept the temperature at 80 DEG C, takes out washing, drying.
Embodiment 3
(1) GO nanometer sheet is synthesized by graphite modified Hummers method.Synthesis process includes by graphite in KMnO4, H2SO4With
NaNO3Mixture in aoxidize, filter mixture to collect solid particle (i.e. graphite oxide), pass through settling flux three times and centrifugation
Solid in circulation washing deionized water is to removing chemical residue, using ultrasonic cleaner by GO particle suspension liquid ultrasonic wave
Processing is, at GO nanometer sheet, it is pure to obtain to remove any unpeeled graphite residue finally by centrifugation for graphite oxide removing
The suspension is freeze-dried and obtains GO powder by GO nanometer sheet suspension；
(2) Fe-TiO is prepared using sol-gel method2Nano particle.Firstly, 10mL butyl titanate is added to 20mL
To form solution A in dehydrated alcohol.Solution B is that FeCl is added310mL dehydrated alcohol, 15mL deionized water and 4.5mL acetic acid
Mixture, the pH of solution B is adjusted to 2 with HCl, solution B is slowly dropped in solution A under vigorous stirring.It has titrated
Mixed solution is obtained after, continues to stir 1h or so under the action of magnetic stirring apparatus.Then, still aging 2h forms yellow
Clear gel.Drying composite and yellow crystals are formed in 100 DEG C of baking oven, solid is transformed into white powder by grinding
End.Then 3h is calcined at 450 DEG C, keeps the temperature 2h, completes Fe-TiO2Preparation；
(3) Fe-GO/TiO is prepared using hydro-thermal method2Particle.Firstly, dispersing 0.05gGO in 80mL deionized water, pass through
Ultrasonication 1h.Add 0.75gFe-TiO2Afterwards, further 1h is needed to be ultrasonically treated.Then, solution is moved into 100mL
In the stainless steel autoclave of teflon lining, it is kept into 18h, cooled to room temperature at a high temperature of 180 DEG C.Finally, will
Suspension is centrifuged with 5000rpm, is then washed with deionized at least three times, and be dried in vacuo at 60 DEG C；
(4) PVDF microfiltration membranes are impregnated into 30min in deionized water, then film is immersed into configured KMNO4It is molten with NaOH
In liquid, washing is taken out after reacting 5min, film becomes yellowish-brown at this time.It is put into NaHSO3Solution in necleophilic reaction to yellowish-brown
Color takes off completely, and taking-up is washed with water to neutrality, then impregnates 5min with proper amount of surfactant CTAB solution；
(5) by 0.1gFe-GO/TiO2Nanometer powder is dispersed in 1h in 100mL deionized water by ultrasonic treatment, is formed outstanding
Turbid.Pretreated pvdf membrane is placed in suspension, 3h is kept the temperature at 80 DEG C, takes out washing, drying.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (9)
1. a kind of method for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material, it is characterised in that: including
Following steps:
(1) by graphite in KMnO4、H2SO4And NaNO3Mixture in aoxidize, filter mixture to collect solid particle, by again
It suspends with the solid in centrifuge cycle washing deionized water to chemical residue is removed, is hanged GO particle using ultrasonic cleaner
Supernatant liquid ultrasonication is, at GO nanometer sheet, it is remaining to remove any unpeeled graphite finally by centrifugation for graphite oxide removing
The suspension is freeze-dried to obtain pure GO nanometer sheet suspension and obtains GO powder by object；
(2) it configures A liquid: measuring dehydrated alcohol and be added to the container, butyl titanate is added into container；
Configuration B liquid: FeCl is taken3, dehydrated alcohol, deionized water and acetic acid mixing, adjust pH value of solution to 2-3；
Fe-TiO2The preparation of particle: B liquid being added in A liquid when stirring A liquid, rear stirring, it is still aging obtain clear gel, then
Fe-TiO is obtained by drying, grinding, calcining2Particle；
(3) it disperses GO powder prepared by step (1) in deionized water, is ultrasonically treated, step is added into deionized water
Suddenly the Fe-TiO of (2) preparation2Particle is then sonicated, and obtains blending suspension, and suspension will be blended and carry out pyroreaction, then
Cooling, centrifugation, washing, drying, obtain Fe-GO/TiO2Particle；
(4) microfiltration membranes are impregnated with deionized water, then film is immersed into KMNO4In the mixed solution of NaOH, water is taken out after reaction
It washes, film becomes yellowish-brown, then film is placed in NaHSO3It is taken off completely in solution to yellowish-brown, takes out washing, then use surface-active
Agent solution impregnates, and obtains pretreated microfiltration membranes；
(5) Fe-GO/TiO for preparing step (3)2Warp is added into the deionized water in deionized water for particle ultrasonic disperse
Pretreated microfiltration membranes, reaction obtain modified microfiltration membranes.
2. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: FeCl in step (2)3Mass ratio with butyl titanate is 1:15-20.
3. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: calcining described in step (2) is specifically to be warming up to 450-500 DEG C of calcining 2-3h with 2.5 DEG C/min, then
Keep the temperature 2h.
4. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: GO powder and Fe-TiO in step (3)2The mass ratio of particle is 1:15-20.
5. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: step (3) in be blended suspension pyroreaction temperature be 180 DEG C, centrifugal condition 5000rpm, using go from
Three times, drying condition is lower 60 DEG C of vacuum dry 18h to sub- water washing.
6. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: the material of microfiltration membranes described in step (4) is polysulfones, polyether sulfone, polytetrafluoroethylene (PTFE), Kynoar acetic acid fibre
Tie up plain any one of class and polyvinyl chloride.
7. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: surfactant described in step (4) is neopelex or cetyl trimethylammonium bromide.
8. the method according to claim 1 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: Fe-GO/TiO in step (5)2It is 1g/L that particle, which is scattered in turbid liquid concentration obtained in deionized water,.
9. the method according to claim 8 for mixing the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material,
It is characterized by: pretreated microfiltration membranes are washed out drying i.e. as 3h is kept the temperature at 80 DEG C in suspension in step (5)
It can.
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| CN110743379A (en) * | 2019-11-07 | 2020-02-04 | 北京航空航天大学 | Application of mesoporous silica nanosheet composite film in water treatment |
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| CN112221359A (en) * | 2020-11-05 | 2021-01-15 | 江苏理工学院 | Preparation method and application of novel photocatalytic composite membrane |
| CN113069597A (en) * | 2021-06-07 | 2021-07-06 | 中南大学湘雅医院 | Method for preparing titanium dioxide doped ceramic film by sol-gel method |
| CN113550069A (en) * | 2021-08-04 | 2021-10-26 | 安徽锦鼎织造有限公司 | Preparation process of terahertz hot-air cotton |
| CN114177784A (en) * | 2021-06-22 | 2022-03-15 | 苏州优纬膜环保材料科技有限公司 | Preparation method of intelligent self-repairing interface material |
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| CN116130608A (en) * | 2023-04-04 | 2023-05-16 | 山东科技大学 | Method for preparing titanium oxide film flexible electrode by self-assembly technology |
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| CN110743379A (en) * | 2019-11-07 | 2020-02-04 | 北京航空航天大学 | Application of mesoporous silica nanosheet composite film in water treatment |
| CN110743379B (en) * | 2019-11-07 | 2023-11-14 | 北京航空航天大学 | Application of mesoporous silica nano-sheet composite film in water treatment |
| CN111420564A (en) * | 2020-03-05 | 2020-07-17 | 浙江美易膜科技有限公司 | Inorganic composite separation membrane containing graphene oxide, and preparation method and application thereof |
| CN112221359A (en) * | 2020-11-05 | 2021-01-15 | 江苏理工学院 | Preparation method and application of novel photocatalytic composite membrane |
| CN113069597A (en) * | 2021-06-07 | 2021-07-06 | 中南大学湘雅医院 | Method for preparing titanium dioxide doped ceramic film by sol-gel method |
| CN113069597B (en) * | 2021-06-07 | 2021-08-06 | 中南大学湘雅医院 | Method for preparing titanium dioxide doped ceramic film by sol-gel method |
| CN114177784A (en) * | 2021-06-22 | 2022-03-15 | 苏州优纬膜环保材料科技有限公司 | Preparation method of intelligent self-repairing interface material |
| CN113550069A (en) * | 2021-08-04 | 2021-10-26 | 安徽锦鼎织造有限公司 | Preparation process of terahertz hot-air cotton |
| CN113550069B (en) * | 2021-08-04 | 2022-10-14 | 安徽锦鼎织造有限公司 | Preparation process of terahertz hot-air cotton |
| CN114588946A (en) * | 2022-01-13 | 2022-06-07 | 河海大学 | Preparation method and application of ferrous iron-doped Fe-MOF-based composite material |
| CN116130608A (en) * | 2023-04-04 | 2023-05-16 | 山东科技大学 | Method for preparing titanium oxide film flexible electrode by self-assembly technology |
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