CN109925891B - Small-aperture high-flux carbon nanotube low-pressure membrane and preparation method thereof - Google Patents
Small-aperture high-flux carbon nanotube low-pressure membrane and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carbon nano tube low-pressure membrane with small aperture and high flux and a preparation method thereof. The invention uniformly disperses a certain amount of carbon nano tubes with certain external diameter size and length in an ethanol solution to obtain a carbon nano tube suspension, ultrasonic treatment is carried out on the suspension by using an ultrasonic crusher to disperse the suspension to form a highly uniform carbon nano tube dispersion, a stable carbon nano tube film is formed on a microfiltration membrane supporting layer by using a pressure filtration method, and the carbon nano tube self-supporting low-pressure membrane is prepared by directly taking off the microfiltration membrane and then drying the microfiltration membrane. The pore size and flux of the membrane can be regulated and controlled by optimizing the size of the carbon nano tube and the membrane forming pressure. The invention also provides a self-supporting low-pressure membrane of the carbon nano tube with small aperture and high flux prepared by the preparation method, wherein the aperture of the membrane is 20-10 nm, and the flux is up to about 450 L.m‑2·h‑1·bar‑1Compared with the traditional commercial organic ultrafiltration low-pressure membrane, the membrane has the advantage of higher removal rate of pollutants.
Description
Technical Field
The invention belongs to the crossing field of nano materials and water treatment technology, and relates to a preparation method of a carbon nano tube self-supporting low-pressure membrane capable of optimizing aperture size and flux, and the carbon nano tube self-supporting low-pressure membrane with small aperture and high flux prepared based on the preparation method.
Background
The low-pressure membrane filtration technology can effectively remove particle pollutants and pathogenic microorganisms in water, has relatively low energy consumption compared with the high-pressure membrane filtration technology, and is widely used for feedwater treatment and sewage recycling in recent years. The traditional low-pressure membrane prepared by adopting the organic high-molecular polymer material is limited by the size of the pore diameter of the traditional low-pressure membrane, and has very limited retention capacity on organic pollutants. The organic pollution problem caused by the adsorption and deposition of organic pollutants on the surface or in the pores of the membrane is serious, and the biological pollution of the membrane is further derived and aggravated.
Since their discovery in 1991, carbon nanotubes have been widely regarded for their advantages of good mechanical and adsorptive properties, excellent mechanical and thermal stability, and local antibacterial properties. In recent years, CNTs have become more widely used in the field of water treatment, with the increase in production and rapid decrease in cost of CNTs.
The application of the existing carbon nano tube in the field of water treatment comprises the preparation of a vertically arranged carbon nano tube film and the preparation of a mixed (composite) carbon nano tube film. The mixed (composite) carbon nanotube film is prepared by mixing the carbon nanotube as an additive with a high polymer material by a phase inversion method, has relatively simple process and has the defects that the carbon nanotube is completely wrapped in an organic material and the activity of the carbon nanotube is difficult to exert; the Membrane has a very small pore size, and the flux of the Membrane is more than 3 times that of a common commercial organic ultrafiltration Membrane due to frictionless flow of fluid among carbon nanotubes (Baek et al, High performance and anti-pollution vertical aligned carbon nanotube Membrane for water purification, Journal of Membrane Science 460(2014), 171-177). However, the preparation process is complicated, the operation pressure is high, and the application is always limited.
The carbon nanotube self-supporting film, also called a bucky paper film, is a simplest film structure composed of carbon nanotubes intertwined with each other, and the sheet-type carbon nanotube self-supporting film is a continuous porous network structure like a flexible paper material in appearance. The carbon nanotube self-supporting membrane is used for intercepting pollutants, membrane pores for separating water molecules from other substances are formed by gaps formed by mutual winding of the carbon nanotubes, the pore volume of the membrane pores accounts for 60-70% of the total volume of the membrane pores, and the membrane pores have wide potential application value in the field of advanced treatment of drinking water and sewage.
At present, it has been reported that when a carbon nanotube self-supporting film with a pore diameter of about 40nm (the pore diameter is measured from an SEM image by ImageJ software) prepared by treating purified multi-wall carbon nanotubes by using a microwave technology is used for treating wastewater containing humic acid, the removal rate of the humic acid can reach more than 93 percent, but the flux of the carbon nanotube self-supporting film is only 80 L.m-2·h-1·bar-1. (Yang et al, Removal of natural organic matter in water using functional Carbon not in the hopper, Carbon 59(2013), 160-. Rashid et al have shown that the carbon nanotube self-supporting membrane with a pore diameter of 23 + -3 nm prepared by non-covalent modification of multi-walled carbon nanotubes with biopolymer achieves a 95% removal rate for various trace organic pollutants, however, the membrane flux is only 22 + -4 L.m-2·h-1·bar-1Belonging to the field of nanofiltration membranes. (rashed et al, nanofiltraction applications of tissue MWNT buckypapermembranes conditioning biopolyzers, Journal of Membrane Science 59(2017), 23-34). Therefore, it is necessary to provide a method for preparing a carbon nanotube self-supporting membrane with simple operation and low cost, and the prepared carbon nanotube self-supporting membrane can be widely used as a low-pressure ultrafiltration membrane in the field of advanced treatment of drinking water and sewage, and has small pore diameter and high flux.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a carbon nanotube self-supporting low pressure film, which can prepare a carbon nanotube self-supporting low pressure film with a small aperture and a high flux by optimizing the outer diameter of a carbon nanotube and optimizing the film forming pressure while preparing the carbon nanotube low pressure film.
The invention relates to a preparation method of a small-aperture high-flux carbon nano tube self-supporting low-pressure membrane, which comprises the following steps:
1) preparing a carbon nano tube dispersion liquid: weighing a certain amount of carbon nanotubes, adding the carbon nanotubes into a dispersing agent, and performing ultrasonic treatment to highly disperse the carbon nanotubes to form a dispersion liquid;
2) preparing a carbon nanotube film: and (2) under the drive of constant pressure provided by a full-automatic air source, separating the carbon nano tube from the dispersing agent by using a microfiltration membrane through a dead-end membrane filtering device, and then filtering and cleaning by using ultrapure water to obtain the carbon nano tube membrane covered on the microfiltration membrane.
3) And (3) directly taking off the carbon nanotube layer prepared in the step 2) from the microfiltration membrane, and placing the carbon nanotube layer in an oven for drying to finally prepare the carbon nanotube self-supporting low-pressure membrane with certain strength and flexibility.
The mass of the carbon nano tube is calculated according to the area of the membrane, and the proportion is 5-10 mg/cm2The dispersant is ethanol solution reaching chemical purity, the mass percentage concentration of the dispersant is 95%, and the addition amount is 1mg according to the ratio of the mass of the carbon nano tube to the volume of the ethanol solution: and 3 ml. The ultrasonic treatment uses an ultrasonic crusher, the ultrasonic power is 300-500W, the ultrasonic time is 15-20 min, and the ultrasonic environment is ice bath.
The used microfiltration membrane is a polytetrafluoroethylene membrane, a polyamide membrane, a mixed cellulose ester membrane or a polyvinylidene fluoride membrane, and the pore size of the microfiltration membrane is 0.2-1 mu m. The drying time is 12-24 h.
In the invention, the pore size of the prepared carbon nanotube self-supporting low-pressure membrane can be regulated and controlled by optimizing the outer diameter size and the type of the carbon nanotube, and the regulation and control range is 70 nm-10 nm. Selecting a carbon nano tube with small outer diameter size, and preparing a carbon nano tube self-supporting low-pressure membrane with small aperture, wherein the aperture control range is 70-20 nm; the self-supporting low-pressure film of the carbon nano tube with the aperture range of 20-10 nm can be prepared by selecting the single-walled carbon nano tube.
In the invention, the flux of the prepared carbon nano tube self-supporting low-pressure membrane can be regulated and controlled by optimizing the membrane forming pressure, and the regulation and control range is 120-450 L.m-2·h-1·bar-1. The film forming pressure in the preparation process is increased within the range of 0.05 MPa-0.2 MPa, and the flux of the prepared carbon nano tube self-supporting low-pressure film can be increased.
The preparation method of the low-pressure film of the carbon nano tube with small aperture and high flux provided by the invention has the following beneficial effects:
the preparation process of the carbon nano tube self-supporting low-pressure film is simple and has low cost. The prepared carbon nanotube self-supporting low-pressure membrane has the characteristics of small aperture, high membrane flux and low operation pressure (the operation pressure is 0.5-1 Bar in the membrane filtration water treatment process, and the operation pressure is 1-2 Bar and is hereinafter referred to as the low-pressure membrane), and has wide application value in the field of water treatment.
The pore size of the carbon nano tube self-supporting low-pressure membrane prepared by the method can be regulated and controlled by optimizing the outer diameter size and the type of the carbon nano tube so as to meet different requirements of treating different water quality pollutants on the pore size of the membrane.
The flux of the carbon nanotube self-supporting low-pressure film prepared by the method can be improved by optimizing the film forming pressure, the film forming pressure is increased, and the flux of the prepared carbon nanotube self-supporting low-pressure film can be increased.
Drawings
FIG. 1 is a diagram of a carbon nanotube self-supporting low-pressure film in example 1 of the present invention;
FIG. 2a is a surface SEM image of a carbon nanotube self-supporting low-pressure film prepared by using multi-walled carbon nanotubes with outer diameters of 30-50nm in example 1 of the invention;
FIG. 2b is a surface SEM image of a carbon nanotube self-supporting low-pressure film prepared by using multi-walled carbon nanotubes with outer diameters of 10-20nm in example 1 of the invention;
FIG. 2c is a surface SEM image of a carbon nanotube self-supporting low pressure film prepared with multi-walled carbon nanotubes having an outer diameter of less than 8nm in example 1 of the present invention;
FIG. 2d is a surface SEM image of a carbon nanotube self-supporting low-pressure film prepared with single-walled carbon nanotubes having an outer diameter of less than 8nm in example 1 of the present invention;
FIG. 3 is a graph showing the pore size of the carbon nanotube self-supporting low-pressure film in example 1 of the present invention. Wherein A is prepared from multi-wall carbon nano-tubes with the outer diameter of 30-50 nm; b is prepared from multi-wall carbon nanotubes with the outer diameter of 10-20 nm; c is prepared by multi-wall carbon nano-tubes with the outer diameter less than 8 nm; d is prepared from single-wall carbon nanotubes with the outer diameter less than 8 nm.
FIG. 4 is a graph of flux versus filtration pressure for carbon nanotube free standing low pressure membranes prepared from single walled carbon nanotubes with an outer diameter of less than 8nm at different membrane forming pressures in example 2 of the present invention. Wherein A is the film forming pressure of 0.05 MPa; b is the film forming pressure of 0.10 MPa; c is the film forming pressure of 0.15 MPa; d is the film forming pressure of 0.20 MPa.
Detailed Description
The invention will be further illustrated with reference to the following specific examples.
Example 1
Preparing a carbon nano tube dispersion liquid: respectively weighing 100mg of multi-walled carbon nanotubes with the outer diameter of 30-50nm, 10-20nm, multi-walled carbon nanotubes with the outer diameter of less than 8nm and single-walled carbon nanotubes with the outer diameter of less than 8nm, adding 300ml of ethanol solvent with the concentration of 95% (W/W), and carrying out ultrasonic treatment for 15min under the ultrasonic power of 500W by using an ultrasonic crusher in an ice bath environment to prepare the carbon nanotube dispersion liquid with uniform dispersion height.
Preparing a carbon nanotube film: and (3) under the drive of a constant film forming pressure of 0.05MPa provided by a full-automatic air source, separating the carbon nano tube from the dispersing agent by using a polyvinylidene fluoride micro-filtration membrane with the aperture of 0.45 mu m through a dead-end membrane filtration device, and then filtering and cleaning by using 300ml of ultrapure water to obtain the carbon nano tube membrane covered on the polyvinylidene fluoride micro-filtration membrane.
And directly removing the carbon nanotube layer covered on the polyvinylidene fluoride micro-filtration membrane, and drying in an oven at 80 ℃ for 24h to prepare four carbon nanotube self-supporting low-pressure membranes.
Referring to fig. 1, it can be seen that the carbon nanotube self-supporting low-pressure film prepared by the method of the present invention can be bent in an "S" shape, which shows that the carbon nanotube self-supporting low-pressure film has a stable structure and good flexibility.
FIG. 2 is a surface SEM image of a carbon nanotube self-supporting film prepared from multi-walled carbon nanotubes with outer diameters of 30-50nm, multi-walled carbon nanotubes with outer diameters of 10-20nm, multi-walled carbon nanotubes with outer diameters smaller than 8nm and single-walled carbon nanotubes with outer diameters smaller than 8nm in example 1. As can be seen from fig. 2, the carbon nanotube self-supporting low pressure membrane has a porous nano-network structure, and the nano-network structure becomes denser as the outer diameter of the multi-wall carbon nanotube decreases; the carbon nanotube self-supporting low-pressure film prepared from the single-walled carbon nanotube has the densest nano network structure.
And analyzing the surface SEM image of the carbon nanotube self-supporting low-pressure film by using ImageJ software to obtain the relative aperture size of the carbon nanotube self-supporting low-pressure film.
As can be seen from fig. 3, the pore diameters of the four carbon nanotube self-supporting low-pressure films prepared in example 1 were 66.34nm, 41.38nm, 32.18nm and 17.23nm, respectively. The pore size of the prepared carbon nanotube self-supporting low-pressure membrane can be regulated and controlled by optimizing the outer diameter and the type of the carbon nanotube. The carbon nano tube with small outer diameter size is selected to prepare the carbon nano tube self-supporting low-pressure film with small aperture; the self-supporting low-pressure film of the carbon nano tube with smaller aperture can be prepared by selecting the single-wall carbon nano tube.
Example 2
Preparing a carbon nano tube dispersion liquid: weighing four 100mg portions of single-walled carbon nanotubes with the outer diameter less than 8nm, adding 300ml of 95% ethanol solvent, and carrying out ultrasonic treatment for 15min under the ultrasonic power of 500W by using an ultrasonic crusher in an ice bath environment to prepare the carbon nanotube dispersion liquid with uniform dispersion height.
Preparing a carbon nanotube film: and (3) under the drive of constant film forming pressures of 0.05MPa, 0.10MPa, 0.15MPa and 0.20MPa respectively provided by a full-automatic air source, separating the carbon nano tubes from the dispersing agent by using a polyvinylidene fluoride micro-filtration membrane with the aperture of 0.45 mu m through a dead-end membrane filtration device, and then filtering and cleaning by using 300ml of ultrapure water to obtain a carbon nano tube layer covered on the polyvinylidene fluoride micro-filtration membrane.
And directly removing the carbon nanotube layer covered on the polyvinylidene fluoride micro-filtration membrane, and drying in an oven at 80 ℃ for 24h to obtain four carbon nanotube self-supporting low-pressure membranes prepared under different driving pressures.
The mass of the carbon nano tube self-supporting low-pressure membrane penetrating fluid prepared by the constant-pressure dead-end filtering device and the calculation record connected with the analytical balance is utilized, the volume of the penetrating fluid (the density of a water sample is defaulted to 1kg/L) is obtained after conversion, and a flux-transmembrane pressure relation graph can be obtained after analysis and calculation.
Referring to FIG. 4, the flux of the carbon nanotube self-supporting low pressure film prepared under the film forming pressures of 0.05MPa, 0.10MPa, 0.15MPa and 0.20MPa is 320.4 + -14.3 L.m-2·h-1·bar-1、325.6±17.4L·m-2·h-1·bar-1、383.8±11.36L·m-2·h-1·bar-1And 430.8 + -16.4 L.m-2·h-1·bar-1. The prepared carbon nanotube self-supporting low-pressure membrane has high flux, and the flux of the carbon nanotube self-supporting low-pressure membrane can be improved by increasing the driving pressure in the preparation process.
The pore diameter of the self-supporting low-pressure film of the carbon nano tube with small pore diameter and high flux prepared by the method is 10-20nm at the minimum, and the flux is 430.8 +/-16.4 L.m-2·h-1·bar-1The operation pressure is low, and the method belongs to the category of low-pressure ultrafiltration membranes.
Claims (4)
1. A preparation method of a carbon nano tube self-supporting low-pressure film is characterized by comprising the following steps:
1) preparing a carbon nano tube dispersion liquid: weighing carbon nanotubes, adding the carbon nanotubes into a dispersing agent, and performing ultrasonic treatment to highly disperse the carbon nanotubes to form a dispersion liquid;
2) preparing a carbon nanotube film: the carbon nano tube dispersion liquid prepared by the step 1) is driven by a constant film forming pressure provided by a full-automatic air source, and the film forming pressure is 0.05 MPa-0.2 MPa; separating the carbon nano tube from the dispersing agent by using a microfiltration membrane through a dead-end membrane filtering device, and then filtering and cleaning with ultrapure water to obtain the carbon nano tube covered on the microfiltration membrane;
3) directly taking off the carbon nanotube film prepared in the step 2) from the microfiltration membrane, and placing the carbon nanotube film in an oven for drying to finally prepare the carbon nanotube self-supporting low-pressure film;
the mass of the carbon nano tube weighed in the step 1) is calculated according to the area of the membrane, and the proportion is 5-10 mg/cm2；
The dispersing agent in the step 1) is an ethanol solution reaching chemical purity, the mass percentage concentration is 95%, and the adding amount is 1mg according to the ratio of the mass of the carbon nano tube to the volume of the ethanol solution: calculating 3 ml;
an ultrasonic crusher is used for ultrasonic treatment in the step 1), the ultrasonic power is 300-500W, the ultrasonic time is 15-20 min, and the ultrasonic environment is an ice bath;
the microfiltration membrane used in the step 2) is a polytetrafluoroethylene membrane, a polyamide membrane, a mixed cellulose ester membrane or a polyvinylidene fluoride membrane, and the aperture size of the microfiltration membrane is 0.2-1 mu m;
the drying time in the step 3) is 12-24 hours;
the film forming pressure is increased in the range of 0.05 MPa-0.2 MPa in the preparation process, and the flux of the prepared carbon nano tube self-supporting low-pressure film is increased.
2. The preparation method of claim 1, wherein the operating pressure of the prepared carbon nanotube self-supporting low-pressure membrane in the membrane filtration treatment process is in the range of 0.5-1 bar.
3. The preparation method of claim 1, wherein the pore diameter of the carbon nanotube low pressure membrane is controlled by optimizing the outer diameter size and the type of the carbon nanotube, selecting multi-walled carbon nanotubes and single-walled carbon nanotubes with different outer diameter sizes, and the range of the pore diameter control is 10 nm-70 nm.
4. The method of claim 1, wherein the carbon nanotubes are single-walled carbon nanotubes having an outer diameter of less than 8nm, and the carbon nanotubes are self-supported low-pressure membranes prepared at a membrane forming pressure of 0.2MPa, and have the advantages of small pore diameter of 10-20nm and high flux of 430.8 ± 16.4L-m-2·h-1·bar-1。
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| CN111249912B (en) * | 2020-03-14 | 2022-06-14 | 北京工业大学 | Method for improving performance of composite carbon nano material low-pressure film by layered design |
| CN111375316B (en) * | 2020-03-20 | 2022-04-22 | 北京工业大学 | Preparation method of multi-walled carbon nanotube low-pressure film for strengthening removal of humic acid in water and relieving pollution |
| CN114057184B (en) * | 2020-07-31 | 2023-06-09 | 北京大学 | Density regulation and control method and preparation device of self-supporting carbon nanotube film target |
| CN113049150A (en) * | 2021-02-02 | 2021-06-29 | 诺瑞(深圳)新技术有限公司 | Flexible pressure sensor, preparation method thereof, robot skin and wearable equipment |
| CN113104839A (en) * | 2021-04-14 | 2021-07-13 | 北京工业大学 | Modified multi-walled carbon nanotube, low-pressure membrane thereof, preparation method and application |
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