CN109759065A - The laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, preparation method and its application in the treatment of waste water - Google Patents
The laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, preparation method and its application in the treatment of waste water Download PDFInfo
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Abstract
The invention discloses the laminated film of the titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide that belong to technical field of waste water processing, preparation method and its applications in the treatment of waste water, this method grows titanium dioxide on Fluorin doped tin dioxide conductive glass using hydro-thermal method, obtain the good nano-stick array thin film of discreteness, ferrous acid nano nickel particles are deposited using the method for dipping calcining on the titanium dioxide and obtain titanium dichloride load ferrous acid nickel composite film, this film has good treatment of Organic Wastewater effect under visible light；With the method deposited oxide graphene film of dipping on titanium dichloride load ferrous acid nickel composite film, the visible light organic wastewater degraded efficiency that this titanium dichloride load nickel ferrite based magnetic loaded compares titanium dichloride load ferrous acid nickel composite film with graphene composite thin film is significantly improved；The processing method is simple, obvious to visible light catalytic performance boost, has wide practical use in wastewater treatment.
Description
Technical field
The invention belongs to technical field for the treatment of of organic waste, and in particular to titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide
Laminated film, preparation method and its application in the treatment of waste water.
Background technique
With the development and progress of society, a large amount of organic wastewater can be generated in production and life, seriously affect human body
Health and natural environment.Common physics and chemical treatment method are high in the presence of such as energy consumption, treatment effeciency is low and is easy to make
The disadvantages of at secondary pollution.Inexpensive, nontoxic, chemical stabilization, efficient photochemical catalyst titanium dioxide can use sunlight conduct
Drive energy provides good solution for the processing of organic wastewater.Since titanium dioxide forbidden bandwidth is on the left side 3.0eV
The right side, can only be using ultraviolet light of the sunlight less than 5% be only accounted for, and improving it is to promote the pass of its application to the utilization efficiency of visible light
Key link.
It is to promote TiO 2 visible light to respond a kind of effective way by the semiconductors coupling of narrow band gap, and in titanium dioxide
One layer of uniform graphene oxide of deposition is then that a kind of new effective promotion titanium dioxide is negative above load nickel ferrite based magnetic loaded composite construction
The method for carrying nickel ferrite based magnetic loaded composite film visible light catalytic efficiency degradation uns-dimethylhydrazine waste water.
Summary of the invention
The object of the present invention is to provide a kind of titanium dichloride load nickel ferrite based magnetic loaded and the laminated films of graphene oxide, preparation side
Method and its application in the treatment of waste water, using infusion process on titanium dichloride load ferrous acid nickel composite film deposition of titanium oxide
Film improves its visible light catalytic efficiency to realize.
In order to achieve the above object, The technical solution adopted by the invention is as follows:
The laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, using the method continuously impregnated in titanium dioxide
Deposited oxide graphene film on nickel ferrite based magnetic loaded film is loaded, titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide THIN COMPOSITE are obtained
Film, titanium deoxid film layer are nanometer stick array structure, and 1~3 micron of array length, nickel ferrite based magnetic loaded is nano particle, graphite oxide
Alkene is layer structure；Laminated film can improve the separative efficiency in light induced electron and hole, realize effective degradation of waste water.
The number of plies of the graphene oxide film is 1-13 layers.
The preparation method of the laminated film of the titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, including walk as follows
It is rapid:
(1) deionized water, concentrated hydrochloric acid, tetra-n-butyl titanate are mixed according to volume ratio 10:10:0.1~10:10:1, is used
Magnetic stirring apparatus is thoroughly mixed uniformly to be clarified to solution completely, obtains reaction precursor liquid；
(2) it successively uses acetone, dehydrated alcohol and deionized water to be cleaned by ultrasonic in Fluorin doped tin dioxide conductive glass, takes out
After be soaked in dehydrated alcohol it is stand-by；
(3) it will be put into polytetrafluoroethylliner liner after the drying of Fluorin doped tin dioxide conductive glass, pour into reaction precursor liquid,
It is completely soaked Fluorin doped tin dioxide conductive glass in reaction precursor liquid, liner is put into autoclave；
(4) autoclave is put into after being reacted in Constant Temp. Oven, takes out cooled to room temperature；
(5) it takes out sample to be rinsed with deionized water, naturally dry obtains titanium dioxide nanorod array film；
(6) iron nitrate solution and nickel nitrate solution are configured, being uniformly mixed becomes reaction solution, by the nano titania of preparation
Rod array film is put into reaction solution after reaction, with taking out after deionized water dipping, is dried；
(7) it calcines 1~3 hour at 350~550 DEG C in tube furnace, is grown on titanium dioxide nanorod array film
Ferrous acid nano nickel particles out obtain titanium dichloride load nickel ferrite based magnetic loaded film；
(8) i.e. that titanium dichloride load nickel ferrite based magnetic loaded is thin film dipped in graphene oxide solution by infusion process, in dioxy
Change deposited oxide graphene on titanium load nickel ferrite based magnetic loaded film, obtains the THIN COMPOSITE of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide
Film.
The percent by volume of concentrated hydrochloric acid is 36.8% in step (1).
Cleaning described in step (2) is successively to carry out electric substrate of glass at ultrasound in acetone, alcohol and deionized water
Manage 15min；The temperature of the Constant Temp. Oven of step (4) is 120~160 DEG C, and the reaction time is 2~8 hours.
The Fluorin doped tin dioxide conductive after drying in step (3) is soaked in down in reaction precursor liquid.
The iron nitrate solution of step (6) configuration and the molar concentration rate 2:1 of nickel nitrate solution, wherein nickel nitrate is molten
The molar concentration of liquid is 0.1~0.5mol/L, and being uniformly mixed according to concentration becomes reaction solution, by the titanium dioxide nano-rod of preparation
Array film is put into reaction solution, after 0.5~3.0 hour, with taking out after deionized water dipping 3~15 seconds, dries.
Step (7) is calcined in tube furnace to be carried out in air atmosphere, and heating and rate of temperature fall are 3~6 DEG C/s, the iron
The size of sour nano nickel particles is 5nm~10nm.
Graphene oxide solution needs ultrasound 1~3 hour in step (8) described infusion process, and dip time is 2~8 seconds, dipping
Number is 1-13 times.
The application of the laminated film of the titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide in the treatment of waste water, will answer
Film merging is closed equipped in the beaker of waste water, is irradiated using xenon lamp simulated solar irradiation, utilizes the photocatalytic of laminated film
It can degradation of organic waste water.
The beneficial effects of the invention are as follows by being sunk on titanium dichloride load ferrous acid nickel composite film with atomic layer deposition method
Product graphene oxide, prepares titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film, graphene oxide layer can be effective
Increase nickel ferrite based magnetic loaded light induced electron and hole separative efficiency, improve the utilization efficiency of light；Graphene oxide has big ratio table
Area can effectively adsorb the organic molecule for needing to degrade, and improve reaction efficiency, the final visible light catalytic for promoting laminated film
Performance, to the maximum lift efficiency of uns-dimethylhydrazine simulated wastewater up to 40%.This method is simple, it is at low cost, effectively improve it is visible
Catalytic efficiency under the conditions of light.
Detailed description of the invention
Fig. 1 is the scanning electron microscope of the titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film that prepare in embodiment 1
Photo.
Fig. 2 is the scanning electron microscope of the titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film that prepare in embodiment 2
Photo.
Fig. 3 is 100mW/cm2Visible light illumination 1 hour, titanium dichloride load nickel ferrite based magnetic loaded that different frequency of depositing obtain and
The degradation rate of graphene composite thin film degradation 20mg/L uns-dimethylhydrazine waste water.
Fig. 4 is 100mW/cm2Visible light illumination different time, the titanium dichloride load that 9 oxide impregnation graphenes obtain
Nickel ferrite based magnetic loaded and graphene composite thin film are compared with the degradation rate of other laminated films degradation 20mg/L uns-dimethylhydrazine waste water.
Specific embodiment
The present invention is illustrated in the following with reference to the drawings and specific embodiments, but not thereby limiting the invention
Protection scope.
Embodiment 1
(1) by volume it is 10:10 by deionized water, concentrated hydrochloric acid (percent by volume 36.8%), tetra-n-butyl titanate:
0.4 is mixed, and is thoroughly mixed with magnetic stirring apparatus and is uniformly clarified completely to solution, and reaction precursor liquid is obtained；
(2) acetone, dehydrated alcohol and deionized water is successively used to be cleaned by ultrasonic in Fluorin doped tin dioxide conductive glass
15min is soaked in dehydrated alcohol stand-by after taking-up；
(3) it will be put into polytetrafluoroethylliner liner after the drying of Fluorin doped tin dioxide conductive glass, pour into reaction precursor liquid,
Fluorin doped tin dioxide conductive is face-down, is completely soaked Fluorin doped stannic oxide in reaction precursor liquid, and liner is put into height
It presses in reaction kettle；
(4) autoclave is put into 150 DEG C of Constant Temp. Ovens, after reaction after 5 hours, taking-up is naturally cooled to
Room temperature；
(5) it takes out sample to be rinsed with a large amount of deionized waters, naturally dry obtains titanium dioxide nanorod array film；
(6) it configures iron nitrate solution (molar concentration 0.3mol/L) and nickel nitrate (molar concentration 0.15mol/L) is molten
Liquid, being uniformly mixed according to volume ratio 1:1 becomes reaction solution, and the titanium dioxide nanorod array film of preparation is put into reaction solution
In, with taking out after deionized water dipping 5 seconds, dry；
(7) it is calcined in tube furnace, calcination temperature is 500 DEG C, and calcination time is 2 hours, and heating and rate of temperature fall are 5
DEG C/min, ferrous acid nano nickel particles are grown on titanium dioxide nanorod array film, obtain titanium dichloride load nickel ferrite based magnetic loaded
Film, nickel ferrite based magnetic loaded granular size are about 5-10nm.
(8) by infusion process deposited oxide graphene in titanium dichloride load nickel ferrite based magnetic loaded, dipping time is 1 time, is obtained
Titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film.Stereoscan photograph is as shown in Figure 1, show successfully to be prepared
The titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film of Rutile Type, wherein the graphene oxide number of plies is 1 layer.
(9) titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film will be prepared in 100mW/cm2Visible light illumination
Under, waste water is intended to the uns-dimethylhydrazine of 20mg/L and carries out Visible Light Induced Photocatalytic, 90min degradation efficiency is shown in Fig. 3, degradation efficiency 11%.
Embodiment 2
(1) by volume it is 10:10 by deionized water, concentrated hydrochloric acid (percent by volume 36.8%), tetra-n-butyl titanate:
1 is mixed, and is thoroughly mixed with magnetic stirring apparatus and is uniformly clarified completely to solution, and reaction precursor liquid is obtained；
(2) acetone, dehydrated alcohol and deionized water is successively used to be cleaned by ultrasonic in Fluorin doped tin dioxide conductive glass
15min is soaked in dehydrated alcohol stand-by after taking-up；
(3) it will be put into polytetrafluoroethylliner liner after the drying of Fluorin doped tin dioxide conductive glass, pour into reaction precursor liquid,
Fluorin doped tin dioxide conductive is face-down, is completely soaked Fluorin doped stannic oxide in reaction precursor liquid, and liner is put into height
It presses in reaction kettle；
(4) autoclave is put into 120 DEG C of Constant Temp. Ovens, after reaction after 8 hours, taking-up is naturally cooled to
Room temperature；
(5) it takes out sample to be rinsed with a large amount of deionized waters, naturally dry obtains titanium dioxide nanorod array film；
(6) it configures iron nitrate solution (molar concentration 1.0mol/L) and nickel nitrate (molar concentration 0.5mol/L) is molten
Liquid, being uniformly mixed according to volume ratio 1:1 becomes reaction solution, and the titanium dioxide nanorod array film of preparation is put into reaction solution
In, with taking out after deionized water dipping 5 seconds, dry；
(7) it is calcined in tube furnace, calcination temperature is 350 DEG C, and calcination time is 3 hours, and heating and rate of temperature fall are 3
DEG C/min, ferrous acid nano nickel particles are grown on titanium dioxide nanorod array film, obtain titanium dichloride load nickel ferrite based magnetic loaded
Film, nickel ferrite based magnetic loaded granular size are about 5-10nm.
(8) by infusion process deposited oxide graphene in titanium dichloride load nickel ferrite based magnetic loaded, dipping time is 5 times, is obtained
Titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film.Stereoscan photograph is as shown in Figure 1, show successfully to be prepared
The titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film of Rutile Type, wherein the graphene oxide number of plies is 5 layers.
(9) titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film will be prepared in 100mW/cm2Visible light illumination
Under, waste water is intended to the uns-dimethylhydrazine of 20mg/L and carries out Visible Light Induced Photocatalytic, 90min degradation efficiency is shown in Fig. 3, degradation rate 32%:
Embodiment 3: titanium dichloride load nickel ferrite based magnetic loaded that different graphene oxide dipping times obtain and graphene oxide
Laminated film.
As shown in figure 3, having investigated the titanium dichloride load nickel ferrite based magnetic loaded and oxidation that different graphene oxide dipping times obtain
The laminated film of graphene is in 90min, light intensity 100mW/cm2Under visible light illumination, the uns-dimethylhydrazine of 20mg/L is simulated useless
The degradation rate of water.With the increase of the graphene oxide number of plies, the degradation rate of uns-dimethylhydrazine waste water is also increased, 9 take second place
After tend to be saturated, this is because excessive graphene oxide will lead to arrive at nickel ferrite based magnetic loaded visible light greatly reduce.
By the titanium dichloride load nickel ferrite based magnetic loaded and graphene composite thin film of 9 deposited oxide graphenes, with dioxy
The catalytic degradation efficiency for changing titanium load ferrous acid nickel composite film and pure titinium dioxide film compares as shown in figure 4, obtaining from figure
Know that its catalytic efficiency compares titanium dichloride load ferrous acid nickel composite film and improves 40%, improves 270% than pure titinium dioxide.
Claims (10)
1. the laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, which is characterized in that using the method continuously impregnated
The deposited oxide graphene film on titanium dichloride load nickel ferrite based magnetic loaded film, obtains titanium dichloride load nickel ferrite based magnetic loaded and graphite oxide
Alkene laminated film, titanium deoxid film layer are nanometer stick array structure, and 1~3 micron of array length, nickel ferrite based magnetic loaded is nano particle,
Graphene oxide is layer structure；Laminated film can improve the separative efficiency in light induced electron and hole, realize effective drop of waste water
Solution.
2. the laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide according to claim 1, which is characterized in that
The number of plies of the graphene oxide film is 1-13 layers.
3. the preparation method of the laminated film of titanium dichloride load nickel ferrite based magnetic loaded described in claim 1 and graphene oxide, special
Sign is, includes the following steps:
(1) deionized water, concentrated hydrochloric acid, tetra-n-butyl titanate are mixed according to volume ratio 10:10:0.1~10:10:1, uses magnetic force
Blender is thoroughly mixed uniformly to be clarified to solution completely, obtains reaction precursor liquid；
(2) it successively uses acetone, dehydrated alcohol and deionized water to be cleaned by ultrasonic in Fluorin doped tin dioxide conductive glass, is soaked after taking-up
It steeps stand-by in dehydrated alcohol；
(3) it will be put into polytetrafluoroethylliner liner after the drying of Fluorin doped tin dioxide conductive glass, pour into reaction precursor liquid, make fluorine
Doping stannic oxide electro-conductive glass is completely soaked in reaction precursor liquid, and liner is put into autoclave；
(4) autoclave is put into after being reacted in Constant Temp. Oven, takes out cooled to room temperature；
(5) it takes out sample to be rinsed with deionized water, naturally dry obtains titanium dioxide nanorod array film；
(6) iron nitrate solution and nickel nitrate solution are configured, being uniformly mixed becomes reaction solution, by the titanium dioxide nano-rod battle array of preparation
Column film is put into reaction solution after reaction, with taking out after deionized water dipping, is dried；
(7) it is calcined 1~3 hour at 350~550 DEG C in tube furnace, tapping is grown on titanium dioxide nanorod array film
Sour nano nickel particles obtain titanium dichloride load nickel ferrite based magnetic loaded film；
(8) i.e. that titanium dichloride load nickel ferrite based magnetic loaded is thin film dipped in graphene oxide solution by infusion process, in titanium dioxide
Deposited oxide graphene on nickel ferrite based magnetic loaded film is loaded, the laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide is obtained.
4. according to the method described in claim 3, it is characterized in that, the percent by volume of concentrated hydrochloric acid is 36.8% in step (1).
5. according to the method described in claim 3, it is characterized in that, described in step (2) cleaning for by electric substrate of glass successively
Ultrasonic treatment 15min is carried out in acetone, alcohol and deionized water；The temperature of the Constant Temp. Oven of step (4) be 120~
160 DEG C, the reaction time is 2~8 hours.
6. according to the method described in claim 3, it is characterized in that, the Fluorin doped stannic oxide after drying in step (3) is led
Electricity is soaked in reaction precursor liquid down.
7. according to the method described in claim 3, it is characterized in that, the iron nitrate solution and nickel nitrate solution of step (6) configuration
Molar concentration rate 2:1, wherein the molar concentration of nickel nitrate solution is 0.1~0.5mol/L, is mixed according to concentration equal
It is even to become reaction solution, the titanium dioxide nanorod array film of preparation was put into reaction solution after 0.5~3.0 hour and uses deionization
Water retting takes out after 3~15 seconds, dries.
8. according to the method described in claim 3, it is characterized in that, step (7) calcined in tube furnace in air atmosphere into
Row, heating and rate of temperature fall are 3~6 DEG C/s, and the size of the ferrous acid nano nickel particles is 5nm~10nm.
9. according to the method described in claim 3, it is characterized in that, graphene oxide solution needs in step (8) described infusion process
Ultrasound 1~3 hour, dip time are 2~8 seconds, and dipping time is 1-13 times.
10. the laminated film of titanium dichloride load nickel ferrite based magnetic loaded described in claim 1 and graphene oxide is in the treatment of waste water
Using, which is characterized in that it by laminated film merging equipped in the beaker of waste water, is irradiated using xenon lamp simulated solar irradiation, benefit
With the photocatalysis performance degradation of organic waste water of laminated film.
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| CN113426434A (en) * | 2021-06-24 | 2021-09-24 | 蚌埠学院 | SnO (stannic oxide)2/Ag2(1-x)NixFe2O4Preparation method of composite film material |
| CN114768787A (en) * | 2022-05-24 | 2022-07-22 | 中国科学院生态环境研究中心 | Carbon fiber loaded three-layer titanium dioxide photocatalyst and preparation method and application thereof |
| CN115369439A (en) * | 2022-04-11 | 2022-11-22 | 天津工业大学 | Self-supporting oxygen evolution electrocatalyst coupling solar photo-thermal and preparation method and application thereof |
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| CN113426434A (en) * | 2021-06-24 | 2021-09-24 | 蚌埠学院 | SnO (stannic oxide)2/Ag2(1-x)NixFe2O4Preparation method of composite film material |
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