CN111249805B - Electret nanofiber filtering material and preparation method thereof - Google Patents
Electret nanofiber filtering material and preparation method thereof Download PDFInfo
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- CN111249805B CN111249805B CN202010129526.5A CN202010129526A CN111249805B CN 111249805 B CN111249805 B CN 111249805B CN 202010129526 A CN202010129526 A CN 202010129526A CN 111249805 B CN111249805 B CN 111249805B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
- B01D39/04—Organic material, e.g. cellulose, cotton
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0618—Non-woven
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0622—Melt-blown
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0627—Spun-bonded
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0631—Electro-spun
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
- Y02A50/2351—Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust
Abstract
The invention provides electret nanofiber filtrationThe material and the preparation method thereof belong to the technical field of new materials, and solve the technical problem that the electret performance of an electret nanofiber filtering material in the prior art is unstable, so that the filtering efficiency of fine particles in air is low. The filter material is prepared from spinning solution through electrostatic spinning, wherein the spinning solution comprises the following components in parts by weight: 5-30 parts of a polymer; 1-10 parts of thiophene dipolar molecule; 60-94 parts of solvent; wherein the thiophene dipolar molecule is a compound with an electron donor-pi conjugated system-electron acceptor dipole structure. The invention prepares high PM through dissolving thiophene dipolar molecule and polymer together and adopting electrostatic spinning technology2.5The air filtering material has the advantages of simple preparation method and low production cost, and has the advantages of filtering performance, low resistance pressure drop and ideal performance stability.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to an electret nanofiber filtering material and a preparation method thereof.
Background
The fine particles in the air refer to particles with the aerodynamic equivalent diameter less than or equal to 2.5 micrometers in the environment, and are also called fine particles, fine particles or PM 2.5, the particle size of the fine particles is small, the fine particles can stay in the atmosphere for a long time, the conveying distance is long, the fine particles can cause great harm to human health, and various diseases such as pneumonia, lung function reduction and the like can be easily caused. The adoption of the air filtering material to protect fine particles in the air is an effective measure.
Currently, conventional air filtration materials primarily include meltblown fibers, glass fibers, and spunbond fibers. However, the conventional air filter material is generally composed of micron-sized fibers, and the diameter of the fibers is large, the pore size between the fibers is large, the specific surface is small, and therefore the filtering efficiency is low. The nanofiber filter material is a trend of development of novel filter materials due to the characteristics of thin filament diameter, small pore diameter and large specific surface area. The nano-fiber in the prior art can be prepared by stretching, template synthesis, phase separation, self-assembly, electrostatic spinning and the like. Compared with the traditional filter material, the electrostatic spinning nanofiber has incomparable advantages in the field of filtration. Electrostatic spinning is a nanofiber preparation technology for spinning by using high voltage electricity, and due to the special performance of electrostatic spinning fibers, particles with the particle size of 1 micron or less can be filtered, so that the application range of filtering is widened. In order to further improve the filtering effect of the filtering material, the polymer air filtering material is usually modified by electret, for example, chinese patent CN104289042B provides a thermal polarization electrostatic spinning nanofiber electret filtering material and its preparation method, which is made by "instant cooling" and nano inorganic particles. However, in the above patent, the preparation method of the electrostatic spinning nanofiber electret filter material is to perform electrostatic spinning on the polymer solution to form electrostatic spinning fibers, and then obtain the electrostatic spinning fiber electret filter material by using a thermal polarization method, so the preparation method is complex, the equipment is complex, the cost is high, and the electret performance is unstable. In addition, the charge generated by the electret in the method is easy to disappear under the action of organic solvents such as isopropanol and the like, so that the filtration efficiency is greatly reduced. In addition, the electret effect can be further improved by adding inorganic nano particles such as tourmaline and the like. However, the compatibility between the inorganic particles and the polymer base material is not good, and the mechanical performance of the air filter material is easy to be reduced.
Disclosure of Invention
The invention aims to provide an electret nanofiber filtering material and a preparation method thereof, and aims to solve the technical problem that the electret performance of the electret nanofiber filtering material in the prior art is unstable, so that the filtering efficiency of fine particles in air is low. In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides an electret nanofiber filtering material which is prepared from spinning solution through electrostatic spinning, wherein the spinning solution comprises the following components in parts by weight:
5-30 parts of a polymer;
1-10 parts of thiophene dipolar molecule;
60-94 parts of solvent;
wherein the thiophene dipolar molecule is a compound with an electron donor-pi conjugated system-electron acceptor dipole structure. I.e. one end of the molecule is an electron donor and the other end is an electron acceptor. Connecting the two is a pi conjugated system.
According to a preferred embodiment, the electron donor of the thiophene-based dipolar molecule is selected from an atom or group with a lone pair of electrons containing an oxygen atom, a nitrogen atom or a sulfur atom; the electron acceptor of the thiophene dipolar molecule is selected from atoms or groups with an electron-withdrawing tendency; the pi conjugated system is a thiophene pi conjugated system.
According to a preferred embodiment, the electron donor is selected from hydroxyl, alkoxy, amine or mercapto; the electron acceptor is selected from nitro, aldehyde group, cyano, sulfonic group, carboxyl, acyl, trifluoromethyl, trichloromethyl or tribromomethyl.
According to a preferred embodiment, the polymer is selected from one or several of the following components: polyacrylonitrile, polyamide, polyurethane, polycarbonate, polyethersulfone, polyphenylene oxide, polyimide, polyvinyl chloride, polyvinylidene fluoride, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polymethyl methacrylate, polyvinyl alcohol, chitosan, or a modified polymer thereof. Preferably, the polymer is selected from polyvinylidene fluoride, polyphenylene oxide or polystyrene. After the polymer is dissolved in the selected solvent, the solution viscosity is moderate, electrostatic spinning emission is facilitated, the emission amount of spinning fibers is large, and the fiber strength is high.
According to a preferred embodiment, the solvent is selected from one or several of the following components: water, formic acid, acetic acid, trifluoroacetic acid, ethanol, N-dimethylformamide, N-dimethylacetamide, dichloroethane, chloroform, tetrahydrofuran, acetone, toluene, butanone, or isopropanol. The solvent selected by the invention can fully and uniformly dissolve the polymer, has small peculiar smell, small toxicity, no corrosion to machinery and low price, and is beneficial to industrial production.
According to a preferred embodiment, the spinning solution comprises the following components in parts by weight:
10-20 parts of a polymer;
1-5 parts of thiophene dipolar molecule;
75-89 parts of solvent;
wherein the thiophene dipolar molecule is thiophene with a dipole structure of an electron donor-pi conjugated system-electron acceptor; the polymer is selected from one or more of polyacrylonitrile, thermoplastic polyimide, polymethyl methacrylate, polyvinylidene fluoride or polystyrene; the solvent is one or two of N, N-dimethylformamide or N, N-dimethylacetamide. By using the formula as a preferable scheme, the spinning solution has more moderate viscosity and larger spinning amount, and better filtering efficiency is obtained.
The invention also provides a preparation method of the electret nanofiber filter material, which is used for preparing the electret nanofiber filter material and at least comprises the following steps:
s1: preparing spinning solution, and respectively weighing polymer, thiophene dipolar molecules and solvent according to weight percentage; stirring and dissolving the thiophene dipolar molecules in the solvent at the temperature of 20-80 ℃, then adding the polymer, and stirring and dissolving to form uniform spinning solution;
s2: and (4) performing electrostatic spinning to obtain an electret nanofiber filter material, and preparing the electret nanofiber filter material by loading the spinning solution obtained in the step S1 on a supporting material by using an electrostatic spinning method. Preferably, the support material of the present invention is a substrate that can be used to support nanofibers and make an air filter material.
According to a preferred embodiment, the support material is a spunbonded, needle-punched or meltblown nonwoven.
According to a preferred embodiment, the support material is a PP meltblown nonwoven, a PP spunbond nonwoven or a PET meltblown nonwoven.
According to a preferred embodiment, said step S2 further comprises: laying the support material on a receiving electrode plate; then, voltage is applied to the transmitting electrode, the receiving electrode plate is grounded or reverse voltage is applied, and the electret nanofiber filtering material loaded with nanofibers with different shapes is prepared by adjusting the pressure difference of positive and negative voltages, the distance between the spinning electrode and the receiving electrode and the temperature and humidity of the environment.
Preferably, the electret nanofiber filter membrane prepared by the preparation method is dried for later use, and other substrate layers can be attached to the electret nanofiber filter membrane to form a multilayer composite structure. Preferably, a composite structure consisting of a substrate layer, an electret nanofiber material and a substrate layer can be further formed.
Based on the technical scheme, the electret nanofiber filter material and the preparation method thereof have the following technical effects:
according to the electret nanofiber filtering material, thiophene dipolar molecules and polymers are dissolved together, a spinning solution is prepared to form nanofibers through an electrostatic spinning method, the thiophene dipolar molecules are polarized under the action of a high-voltage electric field in the electrostatic spinning process, and the orientation of dipole moment of the polarized thiophene dipolar molecules is stabilized by the solidified polymers, so that the prepared nanofibers obtain a good electret effect, the electrostatic effect is effectively improved, the interception effect of electrostatic adsorption force on fine particles is greatly improved, the electret effect is long-lasting, and the interception efficiency of the filtering material on the fine particles is effectively improved. Meanwhile, the thiophene dipolar molecules and the polymer are dissolved together, and the electret nanofiber filtering material which has high PM 2.5 filtering performance, low resistance pressure drop and ideal performance stability is prepared by an electrostatic spinning technology has the advantages of simple preparation method, low production cost and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a surface Scanning Electron Microscope (SEM) image of an electret nanofiber prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
This example 1 provides an electret nanofiber filter material of a preferred embodiment, which is prepared by supporting a spinning solution on a support material of a PP melt-blown nonwoven fabric through an electrospinning method. The spinning solution in the embodiment comprises the following components in parts by weight:
13 parts Polyacrylonitrile (PAN);
3 parts of methyl 2-aminothiophene-3-carboxylate;
and 84 parts of an N, N-dimethylformamide solvent.
The embodiment 1 also provides a preparation method of the material, which comprises the following specific steps:
(1) weighing 3 parts of methyl 2-aminothiophene-3-carboxylate, adding the methyl 2-aminothiophene-3-carboxylate into a container containing 84 parts of N, N-dimethylformamide solvent, heating the container in a water bath at 60 ℃, stirring the mixture in the container until the mixture is dissolved, weighing 13 parts of Polyacrylonitrile (PAN), adding the Polyacrylonitrile (PAN) into the thiophene solution, and preparing into a uniform and transparent solution, namely spinning solution.
(2) Setting electrostatic spinning process parameters: and (3) carrying out electrostatic spinning on the spinning solution obtained in the step (1) on melt-blown cloth for 0.5h, taking down and drying to obtain the electret PAN nanofiber filtering material, wherein the flow rate is 2mL/h, the electrode spacing is 15cm, the voltage difference is 30kV, and the inner diameter of a spinning needle is 0.67 mm.
The performance of the electret nanofiber filter material prepared in this example 1 is as follows: the filtering efficiency of NaCl particles is 99.7 percent and the resistance pressure drop is 88Pa when the filtering efficiency is measured by a TSI 8130 type automatic filter material detector at 85L/min.
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the electret nanofiber filter material has the following properties: the NaCl particulate matter filtration efficiency was 84.3% and the resistance pressure drop was 87Pa (measured at 85L/min using an automatic Filter tester model TSI 8130). Therefore, the filtration effect of the electret nanofiber filter material of the present invention is not greatly reduced even after the treatment with isopropanol, which indicates that the charge generated by the electret of the electret nanofiber filter material prepared by the preparation method of the present invention is not easily lost even after the treatment with isopropanol.
The surface Scanning Electron Microscope (SEM) image of the electret nanofibers produced in this example is shown in FIG. 1. As can be seen from the attached figure 1, the electret nanofiber filter material prepared by the preparation method has the advantages of small fiber diameter, large specific surface area, small pore diameter and high porosity, so that the electret nanofiber filter material has good air permeability.
Comparative example 1
Compared with the filter material provided by the comparative example 1, the filter material has different proportions of the components in the spinning solution, and specifically comprises the following components:
13 parts Polyacrylonitrile (PAN);
and 87 parts of N, N-dimethylformamide.
Under the same conditions, the performance of the filter material prepared in the comparative example 1 is tested as follows: NaCl particulate matter filtration efficiency: 95.8%, resistance pressure drop: 88Pa (measured at 85L/min using an automatic Filter media tester model TSI 8130).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the performance of the filter material is as follows: the NaCl particulate matter filtration efficiency was 65.3% and the resistance pressure drop was 87Pa (measured at 85L/min using an automatic Filter tester model TSI 8130). Therefore, the filtration effect of the spinning solution without thiophene dipolar molecules is greatly reduced after the spinning solution is subjected to electrostatic spinning to form a nanofiber filter material and then is treated by isopropanol, which shows that the electret charge generated by the nanofiber filter material prepared without thiophene dipolar molecules is easy to disappear under the action of isopropanol, and the generated electret effect is unstable.
According to the comparative example, the electret nanofiber filtering material prepared by adding the thiophene dipolar molecule 2-aminothiophene-3-methyl carboxylate into the spinning solution has stable body charge electrostatic adsorption force and good electret effect, and the electret effect is long-lasting, so that the interception effect on fine particles is greatly improved, the interception efficiency of the filtering material on the fine particles is effectively improved, and the resistance pressure drop is reduced.
Example 2
This example 2 provides another preferred embodiment of electret nanofiber filter material, which is prepared by supporting a spinning solution on a PP spunbonded nonwoven support material. The spinning solution in the embodiment comprises the following components in parts by weight:
15 parts of polyvinylidene fluoride (PVDF);
4 parts of 5-amino-2-thiophenecarboxaldehyde;
and 81 parts of an N, N-dimethylacetamide solvent.
The embodiment also provides a preparation method of the material, which comprises the following steps:
(1) weighing 4 parts of 5-methoxy-2-thiophenecarboxaldehyde, adding the 5-methoxy-2-thiophenecarboxaldehyde into a container containing 81 parts of N, N-dimethylacetamide solvent, heating the container in a water bath at 60 ℃, stirring the mixture in the container until the mixture is dissolved, weighing 15 parts of polyvinylidene fluoride (PVDF), adding the PVDF into the thiophene solution, and preparing the uniform and transparent spinning solution.
(2) Setting parameters of an electrostatic spinning process: the flow rate is 2mL/h, the electrode spacing is 15cm, the voltage difference is 28kV, the inner diameter of a spinning needle is 0.67mm, the PVDF spinning solution is subjected to electrostatic spinning on melt-blown cloth for 0.5h, and the melt-blown cloth is taken down and dried to obtain the electret PVDF nanofiber filtering material.
The performance of the electret nanofiber filter material prepared by the embodiment is as follows: the NaCl particulate matter filtration efficiency was 99.5% and the resistance pressure drop was 92Pa (measured at 85L/min using an automatic Filter tester model TSI 8130).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the electret nanofiber filter material has the following properties: the NaCl particulate matter filtration efficiency was 86.8% and the resistance pressure drop was 92Pa (measured at 85L/min using an automatic Filter tester model TSI 8130). Therefore, the filtering effect of the electret nanofiber filter material of the invention is not greatly reduced after the treatment with isopropanol, which shows that the charge generated by the electret of the electret nanofiber filter material prepared by the preparation method of the invention is not easy to disappear even after the treatment with isopropanol.
Comparative example 2
Compared with the embodiment 2, the spinning solution of the comparative example 2 has different component ratios, specifically:
15 parts of polyvinylidene fluoride (PVDF);
and 85 parts of N, N-dimethylacetamide.
Under the same conditions, the performance of the filter material of the comparative example is tested as follows: NaCl particulate matter filtration efficiency: 96.5%, resistance pressure drop: 85Pa (measured at 85L/min using an automated filter material tester model TSI 8130).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the performance of the filter material is as follows: the NaCl particulate matter filtration efficiency was 68.2% and the resistance pressure drop was 86Pa (measured using an automatic Filter tester model TSI 8130 at 85L/min). Therefore, the filtration effect of the spinning solution without thiophene dipolar molecules is greatly reduced after the spinning solution is subjected to electrostatic spinning to form a nanofiber filter material and then is treated by isopropanol, which shows that the electret charge generated by the nanofiber filter material prepared without thiophene dipolar molecules is easy to disappear under the action of isopropanol, and the generated electret effect is unstable.
According to the comparative example, the thiophene dipolar molecule 5-amino-2 thiophene formaldehyde added into the spinning solution has stable body charge electrostatic adsorption force, good electret effect, long-lasting electret effect, and can effectively improve the interception efficiency of the filtering material on fine particles and reduce resistance pressure drop.
Example 3
The embodiment provides another electret nanofiber filter material in a preferred embodiment, which is prepared by loading a spinning solution on a PP melt-blown nonwoven fabric support material, wherein the spinning solution comprises the following components in parts by weight:
22 parts of Polystyrene (PS);
3 parts of dimethyl 4-aminothiophene-2, 3-dicarboxylate;
and 75 parts of an N, N-dimethylacetamide solvent.
The embodiment also provides a preparation method of the material, which comprises the following steps:
(1) weighing 3 parts of 4-aminothiophene-2, 3-dicarboxylic acid dimethyl ester, adding the mixture into a container containing 75 parts of N, N-dimethylacetamide solvent, heating the container in a water bath at 60 ℃, stirring the mixture in the container until the mixture is dissolved, weighing 22 parts of Polystyrene (PS), adding the Polystyrene (PS) into the thiophene solution, and preparing a uniform and transparent solution, namely spinning solution.
(2) Setting parameters of an electrostatic spinning process: the flow rate is 2mL/h, the electrode spacing is 15cm, the voltage difference is 25kV, the inner diameter of a spinning needle is 0.67mm, the PS spinning solution is subjected to electrostatic spinning on melt-blown cloth for 0.5h, and the melt-blown cloth is taken down and dried to obtain the electret PS nanofiber filtering material.
The performance of the electret nanofiber filter material prepared by the embodiment is as follows: the NaCl particulate matter filtration efficiency was 98.7% and the resistance pressure drop was 84Pa (measured using an automatic Filter tester model TSI 8130 at 85L/min).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the electret nanofiber filter material has the following properties: the NaCl particulate matter filtration efficiency was 83.5% and the resistance pressure drop was 83Pa (measured using a model TSI 8130 autofilter tester at 85L/min). Therefore, after the treatment by isopropanol, the filtering effect of the electret nanofiber filtering material provided by the invention is not greatly reduced, which shows that the charge generated by the electret after the treatment by isopropanol of the electret nanofiber filtering material prepared by the preparation method provided by the invention is not easy to disappear.
Comparative example 3
Compared with the embodiment 3, the spinning solution of the comparative example 3 has different solution component ratios, specifically:
22 parts of Polystyrene (PS);
and 78 parts of N, N-dimethylacetamide.
Under the same conditions, the performance of the filter material of the comparative example is tested as follows: NaCl particulate matter filtration efficiency: 93.7%, resistance pressure drop: 82Pa (measured using an automatic Filter media tester model TSI 8130 at 85L/min).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the performance of the filter material is as follows: the NaCl particulate matter filtration efficiency was 58.4% and the resistance pressure drop was 81Pa (measured using a model TSI 8130 autofilter tester at 85L/min). Therefore, the filtration effect of the spinning solution without thiophene dipolar molecules is greatly reduced after the spinning solution is subjected to electrostatic spinning to form a nanofiber filter material and then is treated by isopropanol, which shows that the electret charge generated by the nanofiber filter material prepared without thiophene dipolar molecules is easy to disappear under the action of isopropanol, and the generated electret effect is unstable.
According to the comparative example, the thiophene dipolar molecule 4-aminothiophene-2, 3-dicarboxylic acid dimethyl ester added into the spinning solution has stable body charge electrostatic adsorption force and good electret effect, and the electret effect is long-lasting, so that the interception effect on fine particles is greatly improved, the interception efficiency of the filter material on the fine particles is effectively improved, and the resistance pressure drop is reduced.
Example 4
The present embodiment provides another electret nanofiber filter material according to a preferred embodiment, which is prepared by loading a spinning solution on a PP melt-blown nonwoven fabric support material, wherein the spinning solution in the present embodiment includes the following components in parts by weight:
27 parts of polymethyl methacrylate (PMMA);
4 parts of 2, 5-dibromo-3, 4-dinitrothiophene;
and 69 parts of an N, N-dimethylformamide solvent.
The embodiment also provides a preparation method of the material, which comprises the following steps:
(1) weighing 4 parts of 2, 5-dibromo-3, 4-dinitrothiophene, adding the weighed 2, 5-dibromo-3, 4-dinitrothiophene into a container containing 69 parts of N, N-dimethylformamide solvent, placing the container in a water bath at 60 ℃ for heating, stirring the mixture in the container until the mixture is dissolved, weighing 27 parts of polymethyl methacrylate (PMMA), adding the weighed PMMA into the thiophene solution, and preparing uniform and transparent solution, namely spinning solution.
(2) Setting electrostatic spinning process parameters: the flow rate is 2mL/h, the electrode spacing is 15cm, the voltage difference is 35kV, the inner diameter of a spinning needle is 0.67mm, PMMA is subjected to electrostatic spinning on melt-blown cloth for 0.5h, and the melt-blown cloth is taken down and dried to obtain the electret PMMA nanofiber filtering material.
The performance of the electret nanofiber filter material prepared by the embodiment is as follows: the NaCl particulate matter filtration efficiency was 99.5% and the resistance pressure drop was 86Pa (measured at 85L/min using an automatic Filter tester model TSI 8130).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the electret nanofiber filter material has the following properties: the NaCl particulate matter filtration efficiency was 86.9% and the resistance pressure drop was 85Pa (measured at 85L/min using an automatic Filter tester model TSI 8130). Therefore, after the treatment by isopropanol, the filtering effect of the electret nanofiber filtering material provided by the invention is not greatly reduced, which shows that the charge generated by the electret after the treatment by isopropanol of the electret nanofiber filtering material prepared by the preparation method provided by the invention is not easy to disappear.
Comparative example 4
Compared with example 4, the spinning solution of comparative example 4 has different solution component ratios, specifically:
27 parts of polymethyl methacrylate (PMMA);
and 73 parts of N, N-dimethylformamide.
Under the same conditions, the performance of the filter material of the comparative example was tested as follows: NaCl particulate matter filtration efficiency: 98.8%, resistance pressure drop: 85Pa (measured at 85L/min using an automated filter material tester model TSI 8130).
The surface charges of the filter material are removed by soaking in isopropanol, and after drying, the performance of the filter material is as follows: the NaCl particulate matter filtration efficiency was 62.1% and the resistance pressure drop was 84Pa (measured using an automatic Filter tester model TSI 8130 at 85L/min). Therefore, the filtration effect of the spinning solution without thiophene dipolar molecules is greatly reduced after the spinning solution is subjected to electrostatic spinning to form a nanofiber filter material and then is treated by isopropanol, which shows that the electret charge generated by the nanofiber filter material prepared without thiophene dipolar molecules is easy to disappear under the action of isopropanol, and the generated electret effect is unstable.
According to the comparative example, the thiophene dipolar molecule 2, 5-dibromo-3, 4-dinitrothiophene added into the spinning solution has stable body charge electrostatic adsorption force, good electret effect and long-lasting electret effect, can greatly improve the interception effect on fine particles, effectively improves the interception efficiency of the filter material on the fine particles, and reduces resistance pressure drop.
Example 5
The present example provides another preferred embodiment of an electret nanofiber filter material, which is prepared by loading a spinning solution on a PP melt-blown nonwoven fabric support material through an electrospinning technology, wherein the spinning solution in the present example comprises the following components in parts by weight:
18 Parts of Polyphenylene Oxide (PPO);
4 parts of 5-hydroxy-2-thenoyl trifluoroacetone;
and 78 parts of an N, N-dimethylformamide solvent.
The embodiment also provides a preparation method of the material, which comprises the following steps:
(1) weighing 4 parts of 5-amino-2-thenoyltrifluoroacetone, adding the 5-amino-2-thenoyltrifluoroacetone into a container containing 78 parts of N, N-dimethylformamide solvent, placing the container in a water bath at 60 ℃ for heating, stirring the mixture in the container until the mixture is dissolved, weighing 18 Parts of Polyphenylene Oxide (PPO), adding the polyphenylene oxide (PPO) into the thiophene solution, and preparing into a uniform and transparent solution, namely spinning solution.
(2) Setting electrostatic spinning process parameters: the flow rate is 2mL/h, the electrode spacing is 15cm, the voltage difference is 25kV, the inner diameter of a spinning needle is 0.67mm, the PVA is subjected to electrostatic spinning on melt-blown cloth for 0.5h, and the melt-blown cloth is taken down and dried to obtain the electret nanofiber filtering material.
The performance of the electret nanofiber filter material prepared in the embodiment is as follows: the NaCl particulate matter filtration efficiency was 98.3% and the resistance pressure drop was 91Pa (measured at 85L/min using an automatic Filter tester model TSI 8130).
The surface charges of the filter material are removed by isopropanol vapor, and after drying, the electret nanofiber filter material has the following properties: the NaCl particulate matter filtration efficiency was 84.7% and the resistance pressure drop was 90Pa (measured using a model TSI 8130 autofilter tester at 85L/min). Therefore, after the treatment by isopropanol, the filtering effect of the electret nanofiber filtering material provided by the invention is not greatly reduced, which shows that the charge generated by the electret after the treatment by isopropanol of the electret nanofiber filtering material prepared by the preparation method provided by the invention is not easy to disappear.
Comparative example 5
Compared with example 5, the spinning solution of the comparative example 5 has different solution component ratios, specifically:
17 Parts of Polyphenylene Oxide (PPO);
and 83 parts of an N, N-dimethylformamide solvent.
Under the same conditions, the performance of the filter material of the comparative example is tested as follows: NaCl particulate matter filtration efficiency: 91.8%, resistance pressure drop: 89Pa (measured using an automated filter material tester model TSI 8130 at 85L/min).
The surface charge of the filter material is removed by isopropanol vapor, and after drying, the performance of the filter material is as follows: the NaCl particulate matter filtration efficiency was 55.3% and the resistance pressure drop was 87Pa (measured at 85L/min using an automatic Filter tester model TSI 8130). Therefore, the filtration effect is greatly reduced after the nanofiber filter material is formed by electrostatic spinning of the spinning solution without adding thiophene dipolar molecules and treated by isopropanol, which shows that the electret charge generated by the nanofiber filter material prepared without adding thiophene dipolar molecules is easy to disappear under the action of isopropanol, and the generated electret effect is unstable.
According to the comparative example, the electret nanofiber prepared by adding the thiophene dipolar molecule 5-hydroxy-2-thenoyltrifluoroacetone into the spinning solution has stable body charge electrostatic adsorption force, good electret effect, long-acting and lasting electret effect, can greatly improve the interception effect on fine particles, effectively improve the interception efficiency of the filter material on the fine particles, and reduce resistance pressure drop.
According to the electret nanofiber filtering material, the thiophene dipolar molecules and the polymer are dissolved together, and the spinning solution is prepared to form the electret nanofibers through an electrostatic spinning method, so that the thiophene dipolar molecules are polarized under the action of a high-voltage electric field in the electrostatic spinning process, and the orientation of dipole moment of the polarized thiophene dipolar molecules is stabilized by the solidified polymer, so that the prepared nanofibers have a good electret effect, the electret effect is long-lasting, the electrostatic effect is effectively improved, the interception effect of electrostatic adsorption force on fine particles is greatly improved, and the interception efficiency of the filtering material on the fine particles is effectively improved. In addition, the electret nanofiber filter material has the advantages of simple preparation method, low production cost and the like.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
Claims (8)
1. The electret nanofiber filter material is characterized in that the filter material is prepared by spinning solution through electrostatic spinning, wherein the spinning solution comprises the following components in parts by weight:
5-30 parts of a polymer;
1-10 parts of thiophene dipolar molecule; and
60-94 parts of a solvent;
wherein, the thiophene dipolar molecule is a compound with a dipole structure of an electron donor-pi conjugated system-electron acceptor;
wherein the pi conjugated system is a thiophene pi conjugated system;
wherein the electron donor is selected from hydroxyl, alkoxy, amine or mercapto; the electron acceptor is selected from nitro, aldehyde group, cyano, sulfonic group, carboxyl, acyl, trifluoromethyl, trichloromethyl or tribromomethyl.
2. The electret nanofiber filter material of claim 1, wherein said polymer is selected from one or more of the following: polyacrylonitrile, polyamide, polyurethane, polycarbonate, polyethersulfone, polyphenylene oxide, polyimide, polyvinyl chloride, polyvinylidene fluoride, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polymethyl methacrylate, polyvinyl alcohol, chitosan, or a modified polymer thereof.
3. The electret nanofiber filter material of claim 1, wherein the solvent is selected from one or more of the following: water, formic acid, acetic acid, trifluoroacetic acid, ethanol, N-dimethylformamide, N-dimethylacetamide, dichloroethane, chloroform, tetrahydrofuran, acetone, toluene, butanone, or isopropanol.
4. The electret nanofiber filter material according to any one of claims 1 to 3, wherein the spinning solution comprises the following components in parts by weight:
10-20 parts of a polymer;
1-5 parts of thiophene dipolar molecule; and
75-89 parts of a solvent;
wherein the thiophene dipolar molecule is a thienyl compound with a dipole structure of an electron donor-pi conjugated system-electron acceptor, and the pi conjugated system is a thiophene pi conjugated system; the polymer is selected from one or more of polyacrylonitrile, thermoplastic polyimide, polymethyl methacrylate, polyvinylidene fluoride or polystyrene; the solvent is one or two of N, N-dimethylformamide or N, N-dimethylacetamide.
5. A method for the preparation of an electret nanofiber filter material according to any of claims 1 to 4, comprising at least the steps of:
s1: preparing spinning solution, and respectively weighing polymer, thiophene dipolar molecules and solvent according to weight percentage; stirring and dissolving the thiophene dipolar molecules in the solvent at the temperature of 20-80 ℃, then adding the polymer, and stirring and dissolving to form uniform spinning solution;
s2: and (4) performing electrostatic spinning to obtain an electret nanofiber filter material, and preparing the electret nanofiber filter material by loading the spinning solution obtained in the step S1 on a supporting material by using an electrostatic spinning method.
6. The method of claim 5, wherein the support material is a spunbond, needle-punched or meltblown nonwoven.
7. The method according to claim 5, wherein the support material is a PP meltblown nonwoven fabric, a PP spunbond nonwoven fabric or a PET meltblown nonwoven fabric.
8. The method for preparing a composite material according to claim 5, wherein the step S2 further includes: laying the support material on a receiving electrode plate; and then, applying voltage on the transmitting electrode, grounding the receiving electrode plate or applying reverse voltage, and preparing the electret nanofiber filtering material loaded with nanofibers with different shapes by adjusting the voltage difference between positive and negative voltages, the distance between the spinning electrode and the receiving electrode and the temperature and humidity of the environment.
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