CN112657474A - Preparation of polypyrrole-polyacrylonitrile nanofiber membrane and application of polypyrrole-polyacrylonitrile nanofiber membrane in adsorption of chromium ions - Google Patents
Preparation of polypyrrole-polyacrylonitrile nanofiber membrane and application of polypyrrole-polyacrylonitrile nanofiber membrane in adsorption of chromium ions Download PDFInfo
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Abstract
The invention provides a preparation method of a polypyrrole-polyacrylonitrile nano-fiber membrane, which is characterized by dissolving polyacrylonitrile in an N, N-dimethylformamide solution to obtain a polyacrylonitrile solution, carrying out electrostatic spinning on the polyacrylonitrile solution, and drying to obtain the polyacrylonitrile nano-fiber membrane; adding the polyacrylonitrile nano-fiber membrane and the pyrrole monomer into water, stirring uniformly, adding a ferric trichloride solution for chemical polymerization, and drying to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane. The preparation method is simple in preparation process and low in cost, and can realize mass production. The polypyrrole-polyacrylonitrile nanofiber membrane provided by the invention combines the polypyrrole with rich nitrogen-containing functional groups with the polyacrylonitrile nanofiber membrane, so that the polypyrrole-polyacrylonitrile nanofiber membrane has a large specific surface area and good adsorption performance, is high in adsorption capacity when used for adsorbing chromium ions in an aqueous solution, is easy to separate from water, and provides a new idea for removing heavy metal ions in the aqueous solution.
Description
Technical Field
The invention relates to a preparation method of a polypyrrole-polyacrylonitrile nanofiber membrane, which is mainly used for adsorbing chromium ions in an aqueous solution and belongs to the technical field of nano composite materials.
Background
Polypyrrole (Ppy) is one of conducting polymers, has the characteristics of convenient preparation, adjustable conductivity, good biocompatibility, good environmental stability and the like, and is widely applied to many fields such as biological detection, super capacitors, antistatic materials, microelectronic devices, battery electrodes and the like. And Ppy has abundant nitrogen-containing functional groups and has the capability of removing various heavy metal ions and dyes from wastewater.
Polyacrylonitrile (PAN) is obtained from the monomer acrylonitrile by free radical polymerization. The acrylonitrile units in the macromolecular chain are linked in a linker-to-tail fashion. The polyacrylonitrile fiber is mainly used for preparing polyacrylonitrile fiber, has the advantages of good weather resistance and sun resistance, and can keep 77% of the original strength after being placed outdoors for 18 months. It is also resistant to chemical agents, in particular inorganic acids, bleaching powders, hydrogen peroxide and organic agents in general.
The nanofiber membrane has the advantages of large volume ratio and ideal porosity, and the electrostatic spinning nanofiber membrane is mainly applied to the aspects of energy storage, air filtration, water treatment, ion exchange membranes and the like. The electrostatic spinning technology has the advantages of simplicity, rapidness, mass production and the like, is widely applied to the production of the nanofiber membrane, and meanwhile, the nanofiber membrane has the characteristics of porous structure, easy surface modification, high specific surface area and the like, and is widely applied to the removal of pollutants in aqueous solution.
Disclosure of Invention
The invention aims to provide a preparation method of a polypyrrole-polyacrylonitrile nanofiber membrane;
another object of the present invention is to provide the use of the above nanofiber membrane for adsorbing chromium ions in an aqueous solution.
Preparation of polypyrrole-polyacrylonitrile nano fiber membrane
The preparation method of the polypyrrole-polyacrylonitrile nanofiber membrane comprises the following steps:
(1) dissolving polyacrylonitrile in an N, N-dimethylformamide solution to obtain a polyacrylonitrile solution, performing electrostatic spinning on the polyacrylonitrile solution, and drying at 50-60 ℃ to obtain the polyacrylonitrile nanofiber membrane. Wherein the weight fraction of the polyacrylonitrile solution is 8-10%; electrostatic spinning conditions: voltage: 19 kV, reception distance: 15 cm, injection speed: 0.003 mm/s.
(2) Adding the polyacrylonitrile nanofiber membrane and the pyrrole monomer into water, uniformly stirring, adding a ferric trichloride solution to carry out chemical polymerization, and drying at 50-60 ℃ to obtain the polypyrrole-polyacrylonitrile nanofiber membrane. Wherein the mass ratio of the pyrrole monomer to the polyethyleneimine-polyacrylonitrile nanofiber membrane is 25: 1-125: 1; the concentration of the ferric trichloride solution is 0.08-0.12 g/mL; the mass ratio of the pyrrole monomer to the ferric trichloride is 1: 1-1: 6.
Structure of polypyrrole-polyacrylonitrile nano fiber membrane
1. Scanning electron microscope image analysis
FIG. 1 (a) is a scanning electron microscope image of a polyacrylonitrile nanofiber membrane. The polyacrylonitrile nanometer fiber membrane has smooth surface and uniform diameter. 1 (b), (c) and (d) are scanning electron micrographs of the polypyrrole-polyacrylonitrile nano-fiber membrane. As can be seen from FIG. 1 (b), there is a Ppy polymer on the surface of the nanofiber membrane when polypyrrole is deposited. Fig. 1 (c) and (d) clearly show that the surface of the nanofiber membrane has protrusions, which indicates that Ppy is well deposited on the surface of the polyacrylonitrile nanofiber membrane, and indicates that the polypyrrole-polyacrylonitrile nanofiber membrane is successfully prepared.
2. BET analysis
The prepared polypyrrole-polyacrylonitrile nano fiber membrane is subjected to BET test to obtain the specific surface area value of 414.916 m2The larger specific surface area provides more adsorption sites for the nanofiber membrane, and is more beneficial to the adsorption of metal ions.
Application of polypyrrole-polyacrylonitrile nanofiber membrane
1. Adsorption performance to chromium ions under different polypyrrole contents
0.01 g of polypyrrole-polyacrylonitrile nanofiber membranes with different polypyrrole contents are added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, after the solution is shaken for 24 hours in a constant-temperature oscillator, supernatant is taken, and the concentration of the residual chromium ions is detected by using a DPC (diphenyl carbonate) method, and the result is shown in 3, and it can be seen that when the mass ratio of the polyacrylonitrile nanofiber membranes to the pyrrole monomers is 1:75, the adsorption of the chromium ions reaches 142 mg/g.
2. Polypyrrole-polyacrylonitrile nanofiber membrane has adsorption performance on chromium ions with different initial concentrations
Adding 0.01 g of polyethyleneimine-polyacrylonitrile-polypyrrole core-shell structure nanofiber membrane (mass ratio of polyacrylonitrile nanofiber membrane to pyrrole monomer is 1: 75) into 25mL of solution of chromium ions with different initial concentrations, adjusting the pH of the solution to 2, shaking in a constant temperature oscillator for 24 hours, taking supernatant, detecting the concentration of the remaining chromium ions by using a DPC (diphenyl carbonate) method, and calculating the adsorption amount of the nanofiber membrane, wherein the result is shown in FIG. 4, and the maximum adsorption amount of the nanofiber membrane to the chromium ions reaches 221 mg/g.
In summary, the present invention has the following advantages over the prior art:
the method firstly prepares the polyacrylonitrile nanofiber membrane through electrostatic spinning, and then deposits polypyrrole on the surface of the polyacrylonitrile nanofiber membrane through a chemical polymerization method to obtain the polypyrrole-polyacrylonitrile nanofiber membrane, so that the preparation process is simple, the cost is low, and mass production can be realized. The polypyrrole and polyacrylonitrile nanofiber membrane with rich nitrogen-containing functional groups is combined with the polyacrylonitrile nanofiber membrane, so that the polypyrrole and polyacrylonitrile nanofiber membrane has a large specific surface area and good adsorption performance, is high in adsorption capacity when used for adsorbing chromium ions in wastewater, is easy to separate from water and recover, and provides a new idea for removing heavy metal ions in an aqueous solution.
Drawings
FIG. 1 is a scanning electron microscope image of a polypyrrole-polyacrylonitrile nanofiber membrane;
FIG. 2 is a BET analysis of a polypyrrole-polyacrylonitrile nanofiber membrane;
FIG. 3 is an adsorption diagram of polypyrrole-polyacrylonitrile nanofiber membranes at different polypyrrole contents on chromium ions with an initial concentration of 100 mg/L;
FIG. 4 is an adsorption diagram of polypyrrole-polyacrylonitrile nanofiber membranes to chromium ions of different initial concentrations.
Detailed Description
The preparation and application of the polypyrrole-polyacrylonitrile nanofiber membrane are described in detail by specific examples below.
Example 1
(1) 1.2 g of polyacrylonitrile was added to 10 mL of N, N-dimethylformamide solution, and stirred at 50 ℃ for 4 hours to obtain a polyacrylonitrile solution. And (3) filling the prepared polyacrylonitrile solution into an injector for electrostatic spinning. Conditions of electrostatic spinning: voltage: 19 kV, reception distance: 15 cm, injection speed: 0.003 mm/s. And (3) drying the polyacrylonitrile nanofiber membrane obtained by electrostatic spinning in a 60 ℃ oven.
(2) Putting dried 0.02g of polyacrylonitrile nano-fiber membrane into a beaker filled with 500 mL of water, adding 0.5 g of pyrrole monomer under the stirring condition, stirring for 30 minutes, slowly adding 30mL of 0.1 g/mL ferric chloride solution, carrying out chemical polymerization for 8 hours at 0-4 ℃, and drying for 2 hours in an oven at 60 ℃ to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane.
(3) 0.01 g of the polypyrrole-polyacrylonitrile nanofiber membrane is added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, and after the solution is shaken in a constant temperature oscillator for 24 hours, the chromium ion adsorption reaches 63 mg/g.
Example 2
(1) The same as example 1;
(2) putting dried 0.02g of polyacrylonitrile nano-fiber membrane into a beaker filled with 500 mL of water, adding 1 g of pyrrole monomer under the stirring condition, stirring for 30 minutes, slowly adding 30mL of 0.1 g/mL ferric chloride solution, carrying out chemical polymerization for 8 hours at 0-4 ℃, and drying in an oven at 60 ℃ to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane;
(3) 0.01 g of the polypyrrole-polyacrylonitrile nanofiber membrane is added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, and after the solution is shaken in a constant temperature oscillator for 24 hours, the chromium ion adsorption reaches 67 mg/g.
Example 3
(1) The same as example 1;
(2) putting 0.02g of dried polyacrylonitrile nano-fiber membrane into a beaker filled with 500 mL of water, adding 1.5 g of pyrrole monomer under the stirring condition, stirring for 30 minutes, slowly adding 30mL of 0.1 g/mL ferric chloride solution, carrying out chemical polymerization at 0-4 ℃ for 8 hours, and drying in an oven at 60 ℃ to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane;
(3) 0.01 g of the polypyrrole-polyacrylonitrile nanofiber membrane is added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, and after the solution is shaken in a constant temperature oscillator for 24 hours, the chromium ion adsorption reaches 123 mg/g. The maximum adsorption capacity of the nanofiber membrane on chromium ions reaches 221 mg/g.
Example 4
(1) The same as example 1;
(2) putting dried 0.02g of polyacrylonitrile nano-fiber membrane into a beaker filled with 500 mL of water, adding 2g of pyrrole monomer under the stirring condition, stirring for 30 minutes, slowly adding 30mL of 0.1 g/mL ferric chloride solution, carrying out chemical polymerization for 8 hours at 0-4 ℃, and drying in an oven at 60 ℃ to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane;
(3) 0.01 g of the polypyrrole-polyacrylonitrile nanofiber membrane is added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, and after the solution is shaken in a constant temperature oscillator for 24 hours, the chromium ion adsorption reaches 98 mg/g.
Example 5
(1) The same as example 1;
(2) putting 0.02g of dried polyacrylonitrile nano-fiber membrane into a beaker filled with 500 mL of water, adding 2.5 g of pyrrole monomer under the stirring condition, stirring for 30 minutes, slowly adding 30mL of 0.1 g/mL ferric chloride solution, carrying out chemical polymerization for 8 hours at 0-4 ℃, and drying in an oven at 60 ℃ to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane;
(3) 0.01 g of the polypyrrole-polyacrylonitrile nanofiber membrane is added into 25mL of chromium ion solution with the initial concentration of 100mg/L, the pH value of the solution is adjusted to be 2, and after the solution is shaken in a constant temperature oscillator for 24 hours, the chromium ion adsorption reaches 54 mg/g.
Claims (8)
1. A preparation method of a polypyrrole-polyacrylonitrile nanofiber membrane comprises the following steps:
(1) dissolving polyacrylonitrile in an N, N-dimethylformamide solution to obtain a polyacrylonitrile solution, performing electrostatic spinning on the polyacrylonitrile solution, and drying to obtain a polyacrylonitrile nanofiber membrane;
(2) adding the polyacrylonitrile nano-fiber membrane and the pyrrole monomer into water, stirring uniformly, adding a ferric trichloride solution for chemical polymerization, and drying to obtain the polypyrrole-polyacrylonitrile nano-fiber membrane.
2. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the step (1), the weight fraction of the polyacrylonitrile solution is 8-10%.
3. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the step (1), electrostatic spinning conditions are as follows: voltage: 19 kV; receiving distance: 15 cm; injection speed: 0.003 mm/s.
4. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the step (2), the mass ratio of the pyrrole monomer to the polyethyleneimine-polyacrylonitrile nanofiber membrane is 25: 1-125: 1.
5. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the step (2), the concentration of the solution of ferric trichloride is 0.08-0.12 g/mL; the mass ratio of the pyrrole monomer to the ferric trichloride is 1: 1-1: 6.
6. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the step (2), the chemical polymerization is carried out for 6-10 hours at the temperature of 0-4 ℃.
7. The method for preparing polypyrrole-polyacrylonitrile nano fiber membrane according to claim 1, wherein: in the steps (1) and (2), the drying temperature is 50-60 ℃.
8. Use of the polypyrrole-polyacrylonitrile nanofiber membrane prepared by the method of claim 1 in adsorbing chromium ions in aqueous solution.
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| CN114887597A (en) * | 2022-03-25 | 2022-08-12 | 西安交通大学 | Aflatoxin surface molecularly imprinted nanofiber membrane adsorbent and preparation method and application thereof |
| CN114950156A (en) * | 2022-07-15 | 2022-08-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fish gill structure-imitated nanofiber composite film, and preparation method and application thereof |
| CN115323784A (en) * | 2022-01-27 | 2022-11-11 | 青岛大学 | Polypyrrole conductive flexible fiber membrane material and preparation method thereof |
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| CN115323784A (en) * | 2022-01-27 | 2022-11-11 | 青岛大学 | Polypyrrole conductive flexible fiber membrane material and preparation method thereof |
| CN114887597A (en) * | 2022-03-25 | 2022-08-12 | 西安交通大学 | Aflatoxin surface molecularly imprinted nanofiber membrane adsorbent and preparation method and application thereof |
| CN114887597B (en) * | 2022-03-25 | 2023-08-22 | 西安交通大学 | Aflatoxin surface molecularly imprinted nanofiber membrane adsorbent and preparation method and application thereof |
| CN114950156A (en) * | 2022-07-15 | 2022-08-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fish gill structure-imitated nanofiber composite film, and preparation method and application thereof |
| CN114950156B (en) * | 2022-07-15 | 2024-01-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nanofiber composite film imitating fish gill structure, preparation method and application thereof |
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