CN107158969B - Functionalized nanofiber filtering material and preparation method and application thereof - Google Patents
Functionalized nanofiber filtering material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a functionalized nanofiber filtering material and a preparation method and application thereof, and belongs to the technical field of air purification materials. The method comprises the following steps: c is to be3N4Adding the nanosheets into a solvent, uniformly dispersing by ultrasonic oscillation, and then adding polymer powder for uniform dissolution to obtain the C-containing nanoparticles3N4Preparing the polymer spinning solution of the nano-sheet on a substrate by an electrostatic spinning technology to obtain the functionalized nano-fiber filtering material; the functional nanofiber filter material obtained by the invention can well filter organic pollutants and can be used as an air filter materialHigh efficiency and low resistance, and greatly improves the air quality.
Description
Technical Field
The invention belongs to the technical field of air purification materials, and particularly relates to a functionalized nanofiber filtering material and a preparation method and application thereof.
Background
Air pollution seriously affects people's health, life, work and social economy. The filtering technology is an effective method for improving the atmospheric environment and improving the indoor quality. At present, the common air filtering material has low efficiency and high resistance, can not meet the requirements of people on air quality, and the development of a functional air filtering material which can efficiently filter particles with low resistance and can remove air pollutants such as formaldehyde is urgently needed.
The electrostatic spinning nanofiber filter material has the most excellent performance in a plurality of filter materials due to the sparse and porous structure and the relatively high specific surface area. However, since it is generally spun from high polymer, most of them can only intercept and electrostatically adsorb suspended particles in the air, and cannot remove bacteria, viruses and organic pollutants in the air. In recent years, many experts and scholars have prepared various composite functionalized electrospun nanofiber membranes by compounding electrospun nanofibers with functionalized materials.
The invention discloses an antibacterial air filter felt and a preparation method and application thereof in a patent of CN 103446803A invention published in 12, 18 and 2013 in China, wherein an electrostatic spinning polymer nano fiber felt is used as a carrier material, a nano antibacterial agent with a certain concentration is loaded in an electrostatic spraying mode, the nano antibacterial agent is selected from a nano silver antibacterial agent, a nano silver antibacterial agent suspension and a polymer spinning solution are prepared firstly during preparation, then the nano fiber felt is prepared by electrostatic spinning and is synchronously and electrostatically sprayed with the loaded nano antibacterial agent, and finally vacuum drying is carried out. The technology has the following defects: the nano antibacterial agent is selected from nano silver antibacterial agents which can play a role in sterilization, but heavy metal silver in the nano silver antibacterial agent can cause inevitable damage to human bodies.
The patent of CN 104785018A invention published in 7, month and 22 of China introduces a PVDF nanofiber functionalized air filter material and a preparation method thereof, the PVDF nanofiber comprises a polypropylene micro fiber layer and a PVDF nanofiber layer, the PVDF nanofiber is prepared from a spinning solution, the polypropylene micro fiber layer is used as a base material, PVDF resin, a mixed solvent and tetrabutyl perchloric acid are stirred and mixed, the base material is hot-pressed by a high-temperature calender roll, and then the base material is fed into an electrostatic spinning device for spraying. The technology has the following defects: the filter material only comprises two materials of PVDF and polypropylene, has no special effects of sterilization and oil particle adsorption, and has complex manufacturing process and higher cost.
The patent of CN104815483A invention published in 8/5.2015 in China introduces a composite antibacterial air filtering material, which comprises an electret fabric layer, an electrostatic spinning fiber membrane layer and a base material non-woven fabric layer which are sequentially bonded, wherein the surfaces of the electrostatic spinning fiber membrane layer and the base material non-woven fabric layer are loaded with chitosan and nano TiO2A photocatalyst. Although the method can play the roles of antibiosis, disinfection and peculiar smell removal, the manufacturing process is too complicated, and the sprayed layer is easy to fall off.
Disclosure of Invention
Aiming at solving the defects and shortcomings of the prior art and removing organic pollutants such as formaldehyde, the invention mainly aims to provide a functionalized nanofiber filtering material.
The invention also aims to provide a preparation method of the functionalized nanofiber filter material.
It is a further object of the present invention to illustrate the use of such a functionalized nanofiber filter material.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a functionalized nanofiber filtering material comprises the following steps:
(1) preparing a polymer spinning solution: c is to be3N4Adding the nanosheets into a solvent, performing ultrasonic oscillation until the nanosheets are uniformly dispersed, adding a polymer, and performing magnetic stirring until the nanosheets are uniformly dissolved to obtain the C-containing material3N4A polymer spinning solution of nanosheets;
(2) electrostatic spinning: and (2) preparing the polymer spinning solution obtained in the step (1) on a substrate by an electrostatic spinning technology to obtain the functionalized nanofiber filtering material.
Preferably, the time of the ultrasonic oscillation in the step (1) is 1 h.
Preferably, the magnetic stirring time in the step (1) is 12 h.
Preferably, the solvent in step (1) is one or more of formic acid, N-N dimethylformamide, tetrahydrofuran, trifluoroacetic acid, dichloromethane, water and acetone.
Preferably, the polymer in step (1) is at least one of polyamide, polycarbonate, polyethylene terephthalate, polybutylene terephthalate, polyurethane, polyvinyl chloride, polystyrene, polyacrylonitrile, polyvinyl alcohol and polylactic acid.
Further preferably, the polymer and the solvent in step (1) correspond to the following:
polyamide: a formic acid solvent;
polycarbonate (C): a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 1: 1;
polyethylene terephthalate: a mixed solvent of trifluoroacetic acid and dichloromethane in a volume ratio of 4: 1;
polybutylene terephthalate: a mixed solvent of trifluoroacetic acid and dichloromethane in a volume ratio of 3: 2;
polyurethane: a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 7: 3;
polyvinyl chloride: a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 1: 1;
polystyrene: N-N dimethylformamide solvent;
polyacrylonitrile: N-N dimethylformamide solvent;
polyvinyl alcohol: a water solvent;
polylactic acid: a mixed solvent of N, N-dimethylformamide and acetone in a mass ratio of 4: 1.
Preferably, C in the polymer spinning solution in the step (1)3N4The content of the nano-sheets is 0.01-20 wt.%.
Preferably, the content of the polymer in the polymer spinning solution in the step (1) is 5-25 wt.%.
Preferably, the substrate in step (2) is a conventional micron fiber filter.
Preferably, the electrostatic spinning process conditions in step (2) are as follows: the voltage is 10-30 kV, the receiving distance is 5-30 cm, the injection speed is 1-5 mL/h, the temperature is 0-35 ℃, and the relative humidity is 0-70%.
The functionalized nanofiber filtering material is prepared by the method.
Preferably, the material consists of a nanofiber membrane and a substrate, wherein the nanofiber membrane consists of a type of general engineering plastic polymer nanofibers and C dispersed in the polymer nanofibers3N4Nano-sheet composition; said C is3N4The nanosheet is prepared from melamine by a high-temperature thermal spalling method; the fiber diameter of the nanofiber membrane is 100-900 nm, and the gram weight of the nanofiber membrane is 0.01-5 g/m2The porosity is more than or equal to 80 percent.
The application of the functionalized nanofiber filter material in air filtration is provided.
The invention introduces C on the surface of the nano fiber3N4Nanosheets, C3N4The non-metallic semiconductor material is composed of C, N elements with high earth content, and has the advantages of acid, alkali and light corrosion resistance, good stability, hardness comparable to that of diamond, and easily controllable structure and performance. C3N4The composite material is a graphite phase laminated structure, gas molecules can pass through the layers, and the interior of the composite material has a plurality of defects from 0.3nm to dozens of nanometers, so that the composite material is beneficial to gas passing, can greatly reduce the pressure drop in the PM2.5 separation process, and improves the filtration efficiency in the air purification process. Furthermore, C3N4The self-carrying amino group (N-H) has a certain amino group, and has good adsorption and separation effects on air pollutants such as formaldehyde, CO, nitrogen oxides and the like.
The functional nanofiber filter material obtained by the invention can be applied to industrial dust filtration systems, indoor air filtration (such as air purifier filter elements, air conditioner filter elements and the like), motor vehicle gas filtration systems (such as vehicle-mounted air purifiers, tail gas filters and the like), screen windows, curtains, door curtains and the like, and can also be used for manufacturing protective clothing, masks and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention firstly adds C into the electrostatic spinning polymer nano-fiber3N4Nanosheet to obtain a functionalized nanofiber filtering material;
(2) c added into the functional nano-fiber filter material3N4The nano-sheet does not contain metal, has good biocompatibility, and can effectively intercept suspended particles in the air and adsorb nitrogen oxide, CO and SO when being used as an air filtering material due to the specific layered structure, defects and amino groups of the nano-sheet2And the like, especially has good filtering effect on organic dyes (methylene blue, methyl orange, rhodamine B and the like) and small molecular compounds (formaldehyde, phenol, 2, 4-dichlorophenol, 2,4, 6-trichlorophenol, decabromodiphenyl ether, acetaldehyde, NO, Cr and the like) in the air, and can greatly improve the air purification effect. In addition, due to the ultrahigh hardness, the mechanical strength of the nanofiber membrane can be well improved, and the nanofiber membrane has the defects of effectively improving the specific surface area of the filter material, reducing the pressure drop, greatly increasing the adsorption capacity of the filter material and improving the filtering efficiency.
(3) C used in the invention3N4The nanosheet has unique two-dimensional material property and unique amino group, so that when the nanosheet is added into spinning fibers, the nanosheet and the polymer generate a synergistic effect, and the nanosheet has a more efficient separation effect on organic pollutants such as small-particle pollutants and formaldehyde.
(4) The preparation method of the functionalized nanofiber filtering material is simple, does not need special devices and equipment, and can be suitable for preparing a series of extensive nanofiber membrane filtering materials;
(5) the functionalized nanofiber filtering material disclosed by the invention is wide in application and has a good application prospect.
Drawings
FIG. 1 is a schematic view showing the structure of an electrospinning apparatus used in the present invention.
FIG. 2 is a schematic structural and functional diagram of the functionalized nanofiber filter material obtained in the present invention.
Fig. 3 is a schematic view of a testing device for performing a filtration test on the functionalized nanofiber filter material obtained in the present invention.
FIG. 4 shows the functionalized PVDF + C obtained by the present invention3N4Scanning Electron Microscope (SEM) images of nanofiber filter materials.
FIG. 5a shows a cross-sectional view of a3N4Atomic Force Microscopy (AFM) images of the nanoplatelets.
FIG. 5b is C used in the present invention3N4Thickness analysis of nanoplates.
FIG. 6 shows the functionalized PVDF + C obtained in example 3 of the present invention3N4Graph comparing the filtration efficiency of nanofiber filter material with the addition of other substances.
FIG. 7 shows the functionalized PVDF + C obtained in example 3 of the present invention3N4Graph of the filtration efficiency of nanofiber filter material on formaldehyde and carbon monoxide.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Fig. 1 is a schematic structural diagram of an electrospinning device used in the present invention, which includes a flat plate receiver 1, a bolus system 2 of an electrospinning apparatus, and an electrostatic high voltage supply system 3.
FIG. 2 is a schematic structural and functional diagram of the functionalized nanofiber filter material obtained in the invention, which comprises a functionalized nanofiber layer 4, a substrate layer 5, nanofibers 6 and C3N4Nanoplatelets 7.
Fig. 3 is a schematic diagram of a testing device for performing a filtration test on the functionalized nanofiber filter material obtained in the present invention, and the testing device comprises a detector 8, an airflow inlet 9, an airflow outlet 10, a chamber 11 and a membrane material 12.
Example 1
A preparation method of a functionalized nanofiber filtering material comprises the following specific steps:
(1) the polylactic acid (PLA) was dried in a vacuum oven at 60 ℃ for 2 h. Accurately weighing 14.235g of N-N dimethylformamide by an electronic balance, placing the weighed 14.235g of N-N dimethylformamide into a 25ml beaker, and then weighing 0.015g of 0.015g C3N4Placing the nanosheet (the atomic force microscopy image and the thickness analysis image of the nanosheet are shown in figures 5a and 5 b) in N-N dimethylformamide, ultrasonically oscillating for 6h, taking out a beaker, accurately weighing 0.75g of dried polylactic acid powder by using an electronic balance, placing the polylactic acid powder in the beaker, magnetically stirring for 24h at normal temperature to prepare uniform and stable C-containing polylactic acid powder3N4A polyacrylonitrile spinning solution of nano sheets.
(2) Preparing the spinning solution obtained in the step (1) on a substrate by an electrostatic spinning technology, specifically performing electrostatic spinning by using an electrostatic spinning device shown in fig. 1, sticking the cut substrate (Hua-filterable woven material HFC30) on a flat receiver, adjusting electrostatic spinning parameters, controlling the translation speed of a pushing injection system to be 120mm/min, the receiving distance to be 30cm, the electrostatic high voltage to be 25kV, the pushing injection speed to be 2mL/h, the temperature to be 25 ℃, and the relative humidity to be 70%, and obtaining the functional nanofiber filtering material, namely the functional polylactic acid + C3N4The nanofiber filter material has the fiber diameter of the nanofiber membrane in 500nm and the gram weight of 0.05g/m2And the porosity is 85 percent.
The structure and function of the functionalized nanofiber filter material obtained in this embodiment are schematically shown in fig. 2, and the scanning electron microscope image of the functionalized nanofiber filter material is shown in fig. 4.
Example 2
A preparation method of a functionalized nanofiber filtering material comprises the following specific steps:
(1) the polyvinyl chloride (PVC) powder was dried in a vacuum oven at 60 ℃ for 2 h. 5.625g N-N dimethylformamide and 5.625g tetrahydrofuran were accurately weighed on an electronic balance into a 50ml beaker, and then 1.5g C was weighed3N4Nanosheet (atom of the nanosheet)Force microscopy and thickness analysis as shown in FIGS. 5a and 5 b), placing in the above mixed solvent, shaking with ultrasonic oscillator for 6 hr, taking out beaker, accurately weighing 2.25g dried polyvinyl chloride powder with electronic balance, placing in the beaker, magnetically stirring at room temperature for 24 hr to obtain uniform and stable C-containing solution3N4Polyvinyl chloride spinning solution of nanosheets.
(2) Preparing the spinning solution obtained in the step (1) on a substrate by an electrostatic spinning technology, specifically performing electrostatic spinning by using an electrostatic spinning device shown in fig. 1, adhering the cut substrate (Hua-filterable woven material HFC30) on a flat receiver, adjusting electrostatic spinning parameters, controlling the translation speed of a pushing injection system to be 120mm/min, the receiving distance to be 30cm, the electrostatic high voltage to be 30kV, the pushing injection speed to be 2mL/h, the temperature to be 15 ℃, and the relative humidity to be 25%, and obtaining the functional nanofiber filtering material, namely the functional polyvinyl chloride + C3N4The nanofiber filter material has the fiber diameter of the nanofiber membrane in 300nm and the gram weight of 2g/m2Porosity 80%, similar to figure 4 in a scanning electron micrograph.
The structure and the functional schematic diagram of the functionalized nanofiber filter material obtained in this example are shown in fig. 2.
Example 3
A preparation method of a functionalized nanofiber filtering material comprises the following specific steps:
(1) polyvinylidene fluoride (PVDF) powder was dried in a vacuum oven at 60 ℃ for 2 h. Accurately weighing 8.25g N-N dimethylformamide by an electronic balance, placing the dimethylformamide in a 50ml beaker, and then weighing 3gC3N4Placing the nanosheet (the atomic force microscopic picture and the thickness analysis picture of the nanosheet are shown in figures 5a and 5 b) in the solvent, oscillating for 5h with an ultrasonic oscillator, taking out a beaker, accurately weighing 3.75g of dried polyvinylidene fluoride powder with an electronic balance, placing the dried polyvinylidene fluoride powder in the beaker, magnetically stirring for 24h at normal temperature to prepare the uniform and stable C-containing powder3N4And (3) a polyvinylidene fluoride spinning solution of a nanosheet.
(2) Preparing the spinning solution obtained in the step (1) on a substrate by an electrostatic spinning technology, and specifically carrying out static spinning by using electrostatic spinning equipment shown in figure 1Electrospinning, namely sticking the cut substrate (Hua-strain woven material HFC30) on a flat plate receiver, adjusting the electrostatic spinning parameters, controlling the translation speed of a pushing injection system to be 100mm/min, the receiving distance to be 30cm, the electrostatic high voltage to be 30kV, the pushing injection speed to be 2mL/h, the temperature to be 20 ℃ and the relative humidity to be 20%, and obtaining the functionalized nano-fiber filtering material, namely the functionalized polyvinylidene fluoride and C3N4The nanofiber filter material has the fiber diameter of the nanofiber membrane in 450nm and the gram weight of 0.01g/m2The porosity was 95%, and the scanning electron micrograph is similar to that of FIG. 4.
The structure and the functional schematic diagram of the functionalized nanofiber filter material obtained in this example are shown in fig. 2.
The functionalized nanofiber filter materials obtained in examples 1, 2 and 3 were used as air filter materials for testing the filtration performance:
the source of the polluted air adopted by the device is two, namely cigarette smoke and combustion smoke of plant materials. It has been shown that the particle size of the PM (suspended particulate matter) contained in cigarette smoke ranges from 0.01 to 10 μm, and it contains about 7000 different chemical substances, most of which are harmful formaldehyde
(HCHO) and CO contaminants. The combustion fumes of plant materials also contain a large particle size range of PM and high concentrations of formaldehyde (HCHO) and CO pollutants. The contaminated air, diluted to a measurable level, was passed into the left chamber of the experimental apparatus and monitored using a particle counter (CEM, DT-9881). Meanwhile, the pressure difference of the membrane gas flow was measured using a pressure gauge (UEi, EM201-B) with the air flow rate controlled at 5.33 cm/s. The filter membrane was cut into a circular shape having a diameter of 10cm, and was held by a jig for filtration test. The filtration efficiency η of the filter membrane can be expressed as
η＝((C0-C1))/C0
In the formula: c0Indicating the amount of air contaminants in the left chamber,
C1indicating the amount of air contaminants in the right hand chamber.
The experimental results show that: the filtration efficiency of the functionalized nanofiber filter materials obtained in examples 1, 2 and 3 used as air filter materials on PM in air is more than 95%, the filtration pressure drop is between 10 Pa and 50Pa, and the results of example 3 are shown in FIG. 6 (the preparation method of PVDF + silicon dioxide, PVDF + barium titanate and PVDF materials in FIG. 6 is the same as that of example 3, except that carbon nitride is changed into silicon dioxide and barium titanate). The filtration efficiency for formaldehyde (HCHO) and CO reached 60-80%, and the results of example 3 are shown in figure 7.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. A functional nanofiber air filter material is characterized in that,
the functionalized nanofiber air filter material consists of a nanofiber membrane and a substrate, wherein the nanofiber membrane consists of polymer nanofibers and C dispersed in the polymer nanofibers3N4Nano-sheet composition; the nanofiber membrane has the fiber diameter of 100-900 nm and the gram weight of 0.01-5 g/m2The porosity is more than or equal to 80 percent;
the functionalized nanofiber air filter material is prepared by the following method:
(1) preparing a polymer spinning solution: c is to be3N4Adding the nanosheets into a solvent, performing ultrasonic oscillation until the nanosheets are uniformly dispersed, adding a polymer, and performing magnetic stirring until the nanosheets are uniformly dissolved to obtain the C-containing material3N4A polymer spinning solution of nanosheets;
(2) electrostatic spinning: preparing the polymer spinning solution obtained in the step (1) on a substrate by an electrostatic spinning technology to obtain a functionalized nanofiber filtering material;
c in the polymer spinning solution in the step (1)3N4The content of the nanosheets is 0.01-20 wt.%;
the content of the polymer in the polymer spinning solution in the step (1) is 5-25 wt.%.
2. The functionalized nanofiber air filter material of claim 1, wherein the solvent of step (1) is one or two of formic acid, N-N dimethylformamide, tetrahydrofuran, trifluoroacetic acid, dichloromethane, water and acetone.
3. The functionalized nanofiber air filter material of claim 1, wherein the polymer of step (1) is at least one of polyamide, polycarbonate, polyethylene terephthalate, polybutylene terephthalate, polyurethane, polyvinyl chloride, polystyrene, polyacrylonitrile, polyvinyl alcohol, and polylactic acid.
4. The functionalized nanofiber air filter material of claim 1, wherein the polymer and the solvent of step (1) correspond to the following:
polyamide: a formic acid solvent;
polycarbonate (C): a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 1: 1;
polyethylene terephthalate: a mixed solvent of trifluoroacetic acid and dichloromethane in a volume ratio of 4: 1;
polybutylene terephthalate: a mixed solvent of trifluoroacetic acid and dichloromethane in a volume ratio of 3: 2;
polyurethane: a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 7: 3;
polyvinyl chloride: a mixed solvent of N-N dimethylformamide and tetrahydrofuran in a mass ratio of 1: 1;
polystyrene: N-N dimethylformamide solvent;
polyacrylonitrile: N-N dimethylformamide solvent;
polyvinyl alcohol: a water solvent;
polylactic acid: a mixed solvent of N, N-dimethylformamide and acetone in a mass ratio of 4: 1.
5. The functionalized nanofiber air filter material as claimed in claim 1, wherein the electrostatic spinning in step (2) is carried out under the following process conditions: the voltage is 10-30 kV, the receiving distance is 5-30 cm, the injection speed is 1-5 mL/h, the temperature is 0-35 ℃, and the relative humidity is 0-70%.
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