CN109046044B - Composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles as well as preparation method and application thereof - Google Patents
Composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles, a preparation method and application thereof; heating and reacting a clean stainless steel mesh with the cobalt-amine mixed solution, and then washing, drying and calcining to obtain a cobaltosic oxide nano needle mesh; dispersing titanium dioxide in water containing sodium hydroxide, and washing after reaction to obtain sodium titanate nanowires; fixing the cobaltosic oxide nano needle net on a sand core filtering device; vacuum filtering the aqueous dispersion of the sodium titanate nanowires to the surface of a cobaltosic oxide nanoneedle net, washing and drying to obtain a composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles; the oil-contaminated wastewater or the oil-in-water emulsion passes through a composite multilayer network membrane based on sodium titanate nanowires and cobaltosic oxide nanoneedles to complete the treatment of the oil-contaminated wastewater or the separation of the oil-in-water emulsion. The composite material with high efficiency for separating the oil stain wastewater is prepared, the emulsion separation efficiency is high, and the reusability is good.
Description
Technical Field
The invention belongs to the technical field of functional materials, particularly relates to preparation of a multilayer network film material with special wettability and extremely low adhesion performance, and efficient separation of oil stain and oil-in-water emulsion, and particularly relates to a composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles, and a preparation method and application thereof.
Background
Due to the frequent occurrence of pollution caused by global industrial wastewater and oil leakage, it has a long-term and serious environmental impact on the marine and lake ecosystems, while having a great impact on the economy. The ultra-wetting film makes great progress in the aspect of oil-water separation, and is helpful for solving the problems of global industrial wastewater pollution and ocean oil spill. But the separation efficiency and the permeation flux of the existing product are poor.
Disclosure of Invention
The invention aims to provide a composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles, and a preparation method and application thereof, such as application in treatment of oil stain wastewater.
In order to achieve the purpose, the specific technical scheme of the invention is as follows:
the preparation method of the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles comprises the following steps:
(1) heating and reacting a clean stainless steel mesh with the cobalt-amine mixed solution, washing and drying the mixture, and then calcining the mixture to obtain a cobaltosic oxide nanoneedle mesh; the cobalt-amine mixed solution comprises cobalt salt and amine compound;
(2) dispersing titanium dioxide in water containing sodium hydroxide, and washing after reaction to obtain sodium titanate nanowires;
(3) fixing the cobaltosic oxide nano needle net on a sand core filtering device; and then filtering the aqueous dispersion of the sodium titanate nanowires to the surface of a cobaltosic oxide nanoneedle net in vacuum, washing and drying to obtain the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles.
A method for treating oil-contaminated wastewater or separating oil-in-water emulsion comprises the following steps:
(1) heating and reacting a clean stainless steel mesh with the cobalt-amine mixed solution, washing and drying the mixture, and then calcining the mixture to obtain a cobaltosic oxide nanoneedle mesh; the cobalt-amine mixed solution comprises cobalt salt and amine compound;
(2) dispersing titanium dioxide in water containing sodium hydroxide, and washing after reaction to obtain sodium titanate nanowires;
(3) fixing the cobaltosic oxide nano needle net on a sand core filtering device; then filtering the aqueous dispersion of the sodium titanate nanowires to the surface of a cobaltosic oxide nanoneedle net in vacuum, washing and drying to obtain a composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles;
(4) the oil-contaminated wastewater or the oil-in-water emulsion passes through a composite multilayer network membrane based on sodium titanate nanowires and cobaltosic oxide nanoneedles to complete the treatment of the oil-contaminated wastewater or the separation of the oil-in-water emulsion.
The invention discloses a preparation method of cobaltosic oxide nano needle net, which comprises the following steps:
(1) heating and reacting a clean stainless steel mesh with the cobalt-amine mixed solution, washing and drying the mixture, and then calcining the mixture to obtain a cobaltosic oxide nanoneedle mesh; the cobalt-amine mixed solution comprises cobalt salt and amine compound.
The invention discloses a preparation method of sodium titanate nanowires, which comprises the following steps: dispersing titanium dioxide in water containing sodium hydroxide, and washing after reaction to obtain the sodium titanate nanowires.
In the technical scheme, the stainless steel net is washed clean and then dried under the vacuum condition to obtain the clean stainless steel net.
In the above technical scheme, the cobalt salt is Co (NO)3）2·6H2O, the amine compound being NH4F; taking Co (NO)3）2·6H2O、NH4F. Dissolving urea in deionized water to obtain a cobalt-amine mixed solution; the Co (NO)3）2·6H2O、NH4F. The mass ratio of the urea to the deionized water is (1.9-2) to (1: 2) to (100-150).
In the technical scheme, the heating reaction is carried out at 120 ℃ for 9 hours; the calcination was carried out at 400 ℃ for 4 hours.
In the technical scheme, the water containing sodium hydroxide is deionized water; the mass ratio of the sodium hydroxide to the titanium dioxide is (55-60) to 1; the reaction for preparing the sodium titanate nano-wire is stirring reaction at 130 ℃ for 24 hours.
The invention also discloses a composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles, a cobaltosic oxide nanoneedle net and the sodium titanate nanowires, which are prepared by the preparation method; and the application of the cobaltosic oxide nano needle net and the sodium titanate nano wire in the preparation of the composite multilayer network film based on the sodium titanate nano wire and the cobaltosic oxide nano needle.
The invention also discloses application of the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles in treatment of oil stain wastewater or separation of oil-in-water emulsions.
The preparation method of the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles can be represented as follows:
1. preparation of cobaltosic oxide nano needle net
Stainless steel net (6 × 6 cm 6)2) And washing and drying under vacuum condition. 0.58 g of Co (NO) is taken3）2·6H2O, 0.3 g NH4F and 0.6 g of urea are dissolved in 40ml of deionized water, and after uniform mixing, the mixed solution is poured into the autoclave and reacted for 9 hours at 120 ℃. After the reaction is finished, the obtained pink mesh is washed and dried. The pink mesh was finally calcined in a muffle furnace at 400 ℃ for 4 hours, the mesh changing from pink to black.
2. Preparation of ultralong sodium titanate nanowires
Dissolve 16g NaOH in 40mL DI water and stir 0.27g nano TiO with magnetic stirring2(P25) the powder was dispersed in NaOH solution, mixed well and stirred in the autoclave at 130 ℃ for 24 hours. After the reaction was completed, it was cooled to room temperature. Finally, the obtained nanowires are washed to be neutral, and the sodium titanate nanowires are stored in 150mL of deionized water.
3. Preparation of composite membranes
And fixing the cobaltosic oxide nano needle net on the sand core filtering device. Dispersing the stock solution containing 3mL of sodium titanate nanowires in 300mL of deionized water, then carrying out vacuum filtration on the surface of the cobaltosic oxide nanowire net, washing and drying.
The invention designs a three-dimensional multilayer network membrane with an economical and simple preparation method, prepares a steel mesh modified by a cobalt oxide nanoneedle by a hydrothermal method and calcination, then prepares ultralong sodium titanate nanowires by the hydrothermal method, and finally prepares a multilayer network membrane separation material with special wettability and extremely low adhesion performance by a vacuum deposition method so as to realize wide application in oil stain treatment and oil-in-water emulsion separation. The membrane is used for the high-efficiency separation of oil-in-water emulsion and micron-scale and nano-scale oil dirt, the membrane takes ultralong (more than 10 mu m) sodium titanate nano filaments as a selective layer and takes a needle forest-shaped cobalt oxide nano needle net-shaped membrane as a supporting layer, and meanwhile, the membrane has the properties of ultrahydrophilicity in air and low viscosity and ultralipophobicity under water, has 99.9 percent of separation efficiency and good permeation flux, and has great advantages in the gravity separation of oil-in-water emulsion and oil-dirt wastewater with the droplet size of more than 400 nm. The result of this work is a new approach to design ultra-thin, efficient and durable separation membranes with three-dimensional multilayer network structures.
The invention has the advantages that:
1. the raw materials are low in cost, the composite membrane is simple and convenient to prepare, precise and expensive instruments are not used in the whole process, and the separation membrane with ultrahigh separation efficiency and circulation efficiency is prepared by a simple method.
2. The multilayer network composite membrane material prepared by the method can efficiently separate the oil stain wastewater, and has good application prospect in the aspects of environmental protection and oil stain wastewater treatment due to the ultrahigh alkali resistance and salt resistance, good reusability and the like of the material.
3. The composite material with high efficiency for separating oil stain waste water is prepared, has high emulsion separation efficiency, good reusability, stable material and physical wear resistance, and can be mainly produced industrially so as to achieve the purpose of treating the oil stain waste water.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a tricobalt tetraoxide nanoneedle mesh, wherein a and b are respectively the shape distribution of the tricobalt tetraoxide nanoneedle mesh under different magnifications;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the sodium titanate nanowires, wherein a and b are the shape distribution of the sodium titanate nanowires under different magnifications respectively;
FIG. 3 is an SEM image of a multilayer network composite membrane, wherein a is a front side appearance SEM image of the composite membrane, and b is a cross section SEM image of the composite membrane;
FIG. 4 is a graph showing the effect of wettability of a composite film material, wherein a is a dynamic wetting process of 3 microliters of water drops on the surface of the composite film, and b-d are the contact angles of water drops in the air and the contact angles of oil drops in water (chloroform) of an original stainless steel mesh, a cobaltosic oxide nanoneedle mesh and the composite film respectively;
FIG. 5 is a diagram showing the separation step and effect of an oil-in-water emulsion;
FIG. 6 is a graph of separation efficiency and flow rate of composite membrane materials for different emulsions.
Detailed Description
The first embodiment is a preparation method of cobaltosic oxide nano needle net, which comprises the following specific steps:
stainless steel net (6 × 6 cm 6)2) The stainless steel mesh was dried under vacuum after being sonicated with acetone, ethanol and 1M HCl solution for 10 minutes and washed with Deionized (DI) water, respectively. 0.58 g of Co (NO) is taken3）2·6H2O, 0.3 g NH4And F and 0.6 g of urea are dissolved in 40ml of deionized water, and the mixture is magnetically stirred for 10 minutes to obtain a cobalt-amine mixed solution.
The cleaned stainless steel net was placed vertically in the center of a 50ml reaction kettle. The cobalt amine mixture was poured into the autoclave. The autoclave was then heated to 120 ℃ for 9 hours. After the reaction was completed, the resulting pink-colored network was taken out of the autoclave and rinsed with deionized water and ethanol, and naturally dried. The pink mesh was finally calcined in a muffle furnace at 400 ℃ for 4 hours, the mesh changing from pink to black.
Fig. 1 is a scanning electron microscope image of a cobaltosic oxide nanoneedle mesh, the morphology and distribution of nanoneedles can be seen through the image, when the nanoneedles are covered on a stainless steel mesh, the pore size of the steel mesh is reduced to 16 microns, and the dense nanoneedles are uniformly and orderly distributed on the steel mesh. Each nanoneedle is built up from countless nanoparticles, forming such a dense porous structure.
The second embodiment is a preparation method of the ultralong sodium titanate nanowires, which comprises the following specific steps:
dissolve 16g NaOH in 40mL DI water and stir 0.27g nano TiO with magnetic stirring2(P25) powder dispersed in NaOH solution and stirring continued 20 minute; the well dispersed solution was then poured into a 50mL autoclave. Then placed in a silicon oil bath at 130 ℃ with continuous stirring for 24 hours. After the reaction was completed, the autoclave was cooled to room temperature under continuous stirring. Finally, the obtained nanowires are washed by deionized water until the pH value is 7, and the sodium titanate nanowires in the deionized water are obtained through centrifugation. The sodium titanate nanowires were stored in 150mL deionized water.
FIG. 2 is a scanning electron microscope image of sodium titanate nanowires, the length, thickness and distribution of the nanowires can be seen through the image, the nanowires are interwoven to form a three-dimensional porous network, the length of the nanowires exceeds 10 microns, and the diameter of the nanowires is about 80 nanometers.
In the third embodiment, the preparation of the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles comprises the following specific steps:
and fixing the cobaltosic oxide nano needle net on the sand core filtering device. 3mL of sodium titanate nanowire stock solution was uniformly dispersed in 300mL of deionized water. The uniformly dispersed nanowire aqueous solution is filtered in vacuum to the surface of the cobaltosic oxide nanoneedle net. The composite membrane (diameter: 4 cm) was then washed several times with deionized water. The film was dried in a vacuum dryer at 60 ℃ to obtain a composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles.
Fig. 3 is an SEM image of the multilayer network composite membrane, which shows the surface morphology and multilayer distribution of the composite membrane, and a view a shows that the sodium titanate nanowires are uniformly deposited on the entire nanoneedle network, and the composite membrane composed of the nanowires and the nanoneedles forms a dense and relatively firm nanoporous membrane. And the figure b is the cross section of the composite membrane, the upper layer is sodium titanate nano filaments, and the lower layer is cobaltosic oxide nano needle net.
Example four: wettability of network composite film
The dynamic change and magnitude of the contact angle of the water drop and oil drop in the air or water are obtained by the measurement of the contact angle tester.
Fig. 4 shows wettability of the composite membrane, and it can be seen by comparison that fig. a is a process diagram of rapid wetting of the composite membrane, fig. b shows that wettability of an original stainless steel mesh is not ideal, a tricobalt tetraoxide nanoneedle mesh (fig. c) is wetted by water in the air (contact angle is 0 °), a contact angle of a droplet of chloroform (3 µ L) in water is 151.5 °, and after vacuum deposition of a sodium titanate nanowire, a contact angle of a droplet of chloroform in water in fig. d is increased to 158.5 °, which proves that the composite membrane has super-oleophobic property under water.
Example five: the emulsion separation test comprises the following specific steps:
1mL of toluene was added to 99 mL of water, followed by addition of 5mg of cetyltrimethylammonium bromide, and ultrasonic vibration was performed for 2 hours, followed by an emulsion separation test.
The composite membrane is fixed in a sand core filter, then 100mL of oil-water emulsion is poured, the attached figure 5 shows the oil-water emulsion separation step and the effect graph, and the clear water flows out quickly after the oil-water emulsion is poured into the sand core filter with the modified network composite membrane, which shows that the composite membrane has good emulsion separation performance.
Example six: and (4) testing the separation efficiency and the flow. The method comprises the following specific steps:
separation efficiency and permeation flux: the separation efficiency of the oil/water emulsion was calculated using the following equation (1):
R（％）=（1-Cp/ Co）×100％ （1）
wherein R (%) is an oil discharge coefficient, CpAnd CoThe concentration of the separated water and oil/water emulsion. The purified water was analyzed by uv-vis spectrophotometry. The water content before and after filtration was determined using Karl Fischer moisture titration.
The flux of the emulsion was determined by calculating the amount of permeation per unit time according to the following equation (2):
Flux = V / At （2）
wherein A (cm)2) Is the effective filtration surface of the membrane, V (L m)-2h-1) Is the volume of permeate, and t (h) is the separation time. For each test, a certain amount is addedThe emulsion of (2) is poured into a filter. Six samples were tested for each system to obtain an average.
FIG. 6 is a diagram showing the effect of the composite membrane on the separation efficiency and flow rate of different oil-water emulsions, and it can be seen from the diagram that the membrane can achieve a higher separation efficiency (over 99%, the separation efficiency of the cobaltosic oxide nanoneedle net is about 80% under the same conditions) for different emulsions at an ideal flow rate.
To summarize:
through the analysis, the multilayer network composite membrane prepared by the hydrothermal method and the calcining method has the function of separating emulsion, and has the advantages of high efficiency, good cyclability, physical durability and the like, and more importantly, the preparation method is simple and convenient, and the raw materials are cheap. Therefore, the method has good application prospect in the aspects of oil stain wastewater treatment and emulsion separation.
Claims (5)
1. The preparation method of the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles comprises the following steps:
(1) heating and reacting a clean stainless steel mesh with the cobalt-amine mixed solution, washing and drying the mixture, and then calcining the mixture to obtain a cobaltosic oxide nanoneedle mesh; the cobalt-amine mixed solution comprises cobalt salt and amine compound; the cobalt salt being Co (NO)3）2·6H2O, the amine compound being NH4F; heating to 120 deg.c for 9 hr; calcining for 4 hours at 400 ℃; the Co (NO)3）2·6H2O、NH4F. The mass ratio of the urea to the deionized water is (1.9-2) to 1: 2 to (100-150);
(2) dispersing titanium dioxide in water containing sodium hydroxide, and washing after reaction to obtain sodium titanate nanowires; the mass ratio of the sodium hydroxide to the titanium dioxide is (55-60) to 1; the reaction for preparing the sodium titanate nano wire is stirring reaction at 130 ℃ for 24 hours;
(3) fixing the cobaltosic oxide nano needle net on a sand core filtering device; and then filtering the aqueous dispersion of the sodium titanate nanowires to the surface of a cobaltosic oxide nanoneedle net in vacuum, washing and drying to obtain the composite multilayer network film based on the sodium titanate nanowires and the cobaltosic oxide nanoneedles.
2. The method according to claim 1, wherein the stainless steel net is washed and dried under vacuum to obtain a clean stainless steel net.
3. The method according to claim 1, wherein Co (NO) is used3）2·6H2O、NH4F. Dissolving urea in deionized water to obtain mixed cobalt-amine solution.
4. The method of claim 1, wherein the water containing sodium hydroxide is deionized water.
5. The composite multilayer network film based on sodium titanate nanowires and cobaltosic oxide nanoneedles prepared by the preparation method according to claim 1.
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