CN107137979B - Micron fiber three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof - Google Patents
Micron fiber three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of textile materials, and discloses a micron fiber three-dimensional framework/polymer nanofiber composite filter material and a preparation method thereof. Preparing polymer nano-fibers by a melt blending method; dispersing the polymer nano-fiber and a cross-linking agent in a solvent to form a suspension, then soaking a micron-fiber non-woven fabric framework in the suspension, freeze-drying to form a solidified block, and removing the solvent to obtain the non-woven material with the polymer nano-fiber aerogel distributed between the micron-fiber frameworks in a gradient manner. The preparation process adopted by the invention is simple, the raw materials are green and environment-friendly, the conditions are mild, the method is suitable for industrial large-scale production, and the product has good flexibility, high-efficiency and low-resistance air filtration performance and can be applied to the field of high-efficiency air purification.
Description
Technical Field
The invention belongs to the field of textile materials, and particularly relates to a microfiber three-dimensional skeleton/polymer nanofiber composite filter material and a preparation method thereof.
Background
In recent years, the industrialization of China is rapidly developed, the urbanization speed is increased continuously, various pollution problems come together, and air pollution becomes a main problem of current environmental pollution. Factory exhaust gas, automobile exhaust, building dust, resident life and the like discharge a large amount of smoke particles, and the particles also provide carriers for bacteria to grow and propagate. Therefore, designing and preparing a filter material which can effectively block fine dust particles in the air and has excellent antibacterial performance is a great subject which is concerned with the human health.
Conventional filter materials are generally non-woven fabrics, and the pore size is generally between ten and several microns and tens of microns, so that only micron-sized particles can be intercepted. The filtering efficiency of the non-woven filtering material on particles of 0.3 micron or smaller can be obviously improved and the resistance pressure drop of the non-woven filtering material can be reduced through the electrostatic electret, but the electrostatic electret has limited effect, higher-level filtering is difficult to realize, and the electrostatic is easily influenced by the environmental humidity to reduce the filtering performance. Compared with the conventional fiber, the nanofiber has larger specific surface area, extremely high porosity and excellent adsorption performance, can block nano-scale particle pollutants, and can obviously reduce resistance pressure drop. With the development of the novel industry with extremely high requirements of electronic, aerospace and precision instruments on indoor air, micron fiber grade filter materials cannot meet the requirements of filter precision, and the use of nano-sized fibers in the structure of the filter materials is an inevitable trend in the development of the filter materials.
The aerogel is a porous material with high porosity formed by removing a solvent of the aerogel through a special means under the condition of keeping a three-dimensional network structure of the aerogel unchanged. The aerogel has high specific surface area (which can reach 200-1000 m)2The porosity is high (reaching 80 to 99.8 percent), and the density is low (about 0.003 to 1 g/cm)2The air density is 0.00129g/cm2) And the like, so that the composite material has wide prospects in the aspects of air purification, heat insulation materials, medical treatment, energy, information and the like.
The nanofiber aerogel material integrates the characteristics of nanofiber and aerogel, and can meet the requirements of high efficiency and low resistance at the same time. Document [ High Performance Air Filters Produced from Fine filtered Wood Pulp: Fiber Network Compression Dual to the free Process [ J ]. Industrial & Engineering Chemistry Research, 2012, 51 (32): 10702-10711 report the preparation of air filters by freeze-drying method using wood pulp fibers as raw material. Literature [ Junji N, Tsuguyuki S, Akira i.simple Freeze-Drying Procedure for Producing nanocell Aerogel-containment, High-Performance Air Filters [ J ]. Acs Applied Materials & Interfaces, 2015, 7 (35): 19809 reports that TEMPO oxidized nano-cellulose is used as a raw material to prepare the air filter material by a freeze drying method. However, the aerogel materials in the above documents generally have a problem of large resistance pressure drop. Patent CN105692588A discloses a preparation method of carbon aerogel for air filtration, which uses biomass as raw material to prepare carbon aerogel through hydrothermal method and freeze drying process. However, the aerogel material disclosed by the invention has the problems of complex preparation process and difficult regulation and control of the material structure.
Disclosure of Invention
In order to solve the problems, the invention provides a microfiber three-dimensional skeleton/polymer nanofiber composite filter material and a preparation method thereof.
The invention discloses a micro-fiber three-dimensional framework/polymer nano-fiber composite filter material which comprises a micro-fiber three-dimensional framework and a polymer nano-fiber aerogel, wherein the polymer nano-fiber aerogel and the micro-fiber three-dimensional framework are combined in a physical entanglement, physical crosslinking or chemical crosslinking mode.
The technical scheme adopted by the invention is as follows: a preparation method of a micron fiber three-dimensional framework/polymer nanofiber composite filter material specifically comprises the following steps:
(1) dispersing polymer nano fibers prepared by melt blending in a solution containing a cross-linking agent, and stirring to form a nano fiber suspension;
(2) soaking the three-dimensional skeleton of the micro-fiber in the nano-fiber suspension obtained in the step (1); and (3) forming a solidified block by adopting a freeze drying method, and removing the solvent to obtain the required micron fiber three-dimensional framework/polymer nano fiber composite filter material.
Specifically, the polymer nanofiber is one of or two of or three of ethylene-vinyl alcohol copolymer, polyethylene terephthalate, polyacrylonitrile, polysulfone, polyethylene octene co-elastomer, nylon 6, polypropylene, polystyrene, polyvinyl chloride and polyvinylidene fluoride.
Specifically, the solvent is one of deionized water, ethanol, tert-butyl alcohol, isopropanol, formic acid, Tetrahydrofuran (THF), dichloromethane, trifluoroacetic acid, N-dimethylformamide, acetone, N-heptane, and Dimethylacetamide (DMAC), or two or three mixed solvents.
Specifically, the crosslinking agent is one of polyacrylic acid, polyvinyl alcohol, genipin and chitosan, or two mixed crosslinking agents or three mixed crosslinking agents.
Specifically, the micron fiber three-dimensional framework is one or more of polypropylene fiber needle-punched non-woven fabric, polyester fiber needle-punched non-woven fabric, aromatic polyamide fiber needle-punched non-woven fabric, pure cotton water-punched non-woven fabric and warp-knitted 3D spacer fabric, wherein the gram weight of the non-woven fabric is 60g/m2～300g/m2。
Specifically, the mass fraction of the polymer nanofibers in the nanofiber suspension in the step (1) is 0.7-3%.
Specifically, the conditions for freezing and solidifying in the step (2) are as follows: treating at-150 to-15 ℃ for 1.5 to 5 hours.
Specifically, the diameter of the polymer nanofiber is 120 nm-500 nm.
The invention has the beneficial effects that:
(1) according to the invention, the nano-fiber is immersed in the micro-fiber non-woven fabric framework to prepare the aerogel material, so that the non-woven fabric base material with a fluffy structure is compounded with the nano-fiber in a three-dimensional space, and the composite material is suitable for combination of different micro-fibers and polymer nano-fibers, the micro-fiber framework not only enhances the mechanical property of the filter material, but also enables the nano-fiber aerogel material to have a higher specific surface area and a fluffy structure, and the purposes of high efficiency, low resistance, filtration efficiency and longer service life are achieved.
(2) The composite filter material has good structure controllability, and can be realized by adjusting the size of the nano-fiber, the structure of the base material, and the dispersion characteristic and concentration of the suspension; and the nano fibers enter the framework in a diffusion mode, and the gradient distribution of the surface of the composite filter material and the nano fibers in the framework can be formed, so that the pore size of the gradient is formed, the gradient filtration of different sizes of particle pollutants is facilitated, and the resistance pressure drop is reduced.
(3) The polymer nano fiber and the micron fiber prepared by the melt blending method are compounded, and the preparation method has the advantages of low cost, mild condition, easiness in control, easiness in obtaining raw materials, environmental friendliness, industrial large-scale production and the like.
Drawings
FIG. 1 is a nanofiber-based three-dimensional framework material;
FIG. 2 is a scanning electron microscope image of the surface layer of the nanofiber-based three-dimensional framework material;
FIG. 3 is a scanning electron microscope image of the inner layer of the nanofiber-based three-dimensional framework material.
Detailed Description
The technical solutions of the present invention are further described below, but not limited thereto, and all the technical solutions of the present invention should be equally replaced or modified without departing from the technical principles and the spirit of the present invention, and the protection scope of the present invention is covered.
Example 1
(1) Dispersing ethylene-vinyl alcohol nanofibers with the average diameter of 150nm in deionized water containing tert-butyl alcohol, and stirring at a high speed by a high-speed stirrer to form a nanofiber suspension;
(2) the mixture is heated to 110g/m2Completely soaking the pure cotton spunlace non-woven fabric into the nanofiber suspension in the step (1); (3) freezing for 1.5h at-15 ℃ to solidify the mixture, and removing the solvent by adopting a freeze drying method to obtain the pure cotton spunlace/ethylene vinyl alcohol composite filter material.
Wherein the mass fraction of the suspension is 1.1 percent, and the mass ratio of the tert-butyl alcohol to the deionized water is 60: 40. The gram weight of the nanofiber layer of the prepared composite filter material is 7g/m2(ii) a The nanofibers and nonwoven fibers are reinforced by physical entanglement, with the performance criteria shown in table 1.
Comparative example 1
Preparation of ethylene vinyl alcohol copolymer nanofiber suspension according to the method of example 1Then freezing for 1.5h at-15 ℃ to solidify the nano-fiber, and removing the solvent by adopting a freeze drying method to obtain the ethylene vinyl alcohol polymer nano-fiber filtering material. Wherein the mass fraction of the suspension is 1.1 percent, the mass ratio of the tert-butyl alcohol to the deionized water is 60:40, and the gram weight of the nanofiber layer of the filter material is 7g/m2The performance index is shown in Table 1.
Example 2
(1) Dispersing nylon 6 nano-fibers with the average diameter of 220nm in a polyacrylic acid solution containing a mixed solvent of formic acid and ethanol, and forming a nano-fiber suspension by a high-speed stirrer;
(2) 130g/m2Completely soaking the PP needled non-woven fabric into the nanofiber suspension;
(3) freezing for 5h at-100 ℃ to solidify the mixture, removing the solvent by adopting a freeze drying method, and then drying for 5min at 80 ℃ for chemical crosslinking to obtain the PP needling/nylon 6 nanofiber composite filter material.
Wherein the mass fraction of the suspension is 0.9%, and the mass ratio of formic acid to ethanol is 25: 75. the gram weight of the nanofiber layer of the composite filter material is 13g/m2(ii) a The nanofibers and nonwoven fibers are reinforced by a combination of physical entanglement and chemical crosslinking, with the performance criteria shown in table 1.
Comparative example 2
Preparing nylon 6 nano-fiber suspension according to the method of example 2, freezing for 5h at-100 ℃ to solidify the suspension, removing the solvent by adopting a freeze drying method, and drying for 5min at 80 ℃ to chemically crosslink the suspension to obtain the nylon 6 nano-fiber filter material. Wherein the mass fraction of the suspension is 0.9%, and the mass ratio of formic acid to ethanol is 25: 75, the nanofiber layer of the filter has a grammage of 13g/m2. The performance index is shown in Table 1.
Example 3
(1) Dispersing polyethylene glycol terephthalate nano-fibers with the average diameter of 170nm in a polyvinyl alcohol solution containing a mixed solvent of dichloromethane and trifluoroacetic acid, stirring at a high speed by a high-speed stirrer to form a nano-fiber suspension, and crosslinking the nano-fiber suspension at the temperature of 30 ℃;
(2) 200g/m2Completely soaking the PP needled non-woven fabric into the nanofiber suspension;
(3) freezing for 4h at-80 ℃ to solidify the mixture, and removing the solvent by adopting a freeze drying method to obtain the PP needling/polyethylene terephthalate nanofiber composite filter material.
Wherein the mass fraction of the suspension is 0.7 percent, the mass ratio of the dichloromethane to the trifluoroacetic acid is 75:25, and the gram weight of the nanofiber layer of the composite filter material is 11g/m2. The nanofibers and nonwoven fibers are reinforced by a combination of physical entanglement and physical crosslinking, with the performance criteria shown in table 1.
Comparative example 3
The polyethylene terephthalate nanofiber suspension was prepared according to the method of example 3, crosslinked at 30 ℃, frozen at-80 ℃ for 4 hours to solidify, and the solvent was removed by freeze-drying to obtain a polyethylene terephthalate nanofiber filter material. Wherein the mass fraction of the suspension is 0.7 percent, the mass ratio of the dichloromethane to the trifluoroacetic acid is 75:25, and the gram weight of the nanofiber layer of the filter material is 11g/m2. The performance index is shown in Table 1.
Example 4
(1) Dispersing polystyrene nano-fibers with the average diameter of 250nm in a mixed solution of DMF and diethyl ether, and stirring at high speed by a high-speed stirrer to form a nano-fiber suspension;
(2) 200g/m2Completely soaking the PET needle punched non-woven fabric into the nanofiber suspension;
(3) freezing for 2h at-80 ℃ to solidify the mixture, and removing the solvent by adopting a freeze drying method to obtain the PET acupuncture/polystyrene nano fiber composite filter material.
Wherein the mass fraction of the suspension is 1 percent, and the mass ratio of DMF to diethyl ether is 80: 20. The gram weight of the nanofiber layer of the composite filter material is 18g/m2(ii) a The nanofibers and nonwoven fibers are reinforced by physical entanglement, with the performance criteria shown in table 1.
Comparative example 4
Polystyrene nanofibers were prepared according to the method of example 4And (3) freezing the vitamin suspension for 2h at-80 ℃ to solidify the vitamin suspension, and removing the solvent by adopting a freeze drying method to obtain the polystyrene nano-fiber filtering material. Wherein the mass fraction of the suspension is 1 percent, and the mass ratio of DMF to diethyl ether is 80: 20. The gram weight of the nanofiber layer of the filter material is 18g/m2. The performance index is shown in Table 1.
Example 5
(1) Dispersing the polyethylene octene co-elastomer nano-fiber with the average diameter of 120nm in a mixed solution of polyvinyl alcohol and genipin, the solvent of which is diethyl ether, stirring at high speed by a high-speed stirrer to form a nano-fiber suspension, and crosslinking the nano-fiber suspension at 50 ℃;
(2) the mixture is mixed with 100g/m2Completely soaking the PP needled non-woven fabric into the nanofiber suspension;
(3) freezing for 2.5h at-120 ℃ to solidify the mixture, and removing the solvent by adopting a freeze drying method to obtain the PP needling/polyethylene octene co-elastomer composite filter material.
Wherein the mass fraction of the suspension is 1.5%. The gram weight of the nanofiber layer of the composite filter material is 15g/m2(ii) a The nanofibers and nonwoven fibers are reinforced by a combination of physical entanglement and physical crosslinking, with the performance criteria shown in table 1.
Comparative example 5
The polyethylene octene co-elastomer nanofiber suspension was prepared according to the method of example 5, crosslinked at 50 ℃, frozen at-120 ℃ for 2.5h to solidify, and the solvent was removed by freeze-drying to obtain a polyethylene octene co-elastomer filter material. Wherein the mass fraction of the suspension is 1.5 percent, and the mass ratio of the petroleum ether to the cyclohexane is 50: 50. The gram weight of the nanofiber layer of the filter material is 15g/m2The performance index is shown in Table 1.
Example 6
(1) Dispersing polypropylene nano-fiber with average diameter of 190nm in chitosan solution with solvent of petroleum ether and cyclohexane, stirring at high speed by a high-speed stirrer to form nano-fiber suspension, and crosslinking at 50 deg.C;
(2) mixing with a stirring mill at 300g/m23D warp knitting interval weaveCompletely soaking the mixture into the nanofiber suspension;
(3) freezing for 2.5h at-150 ℃ to solidify the mixture, and removing the solvent by adopting a freeze drying method to obtain the 3D warp-knitted spacer fabric/polypropylene composite filter material.
Wherein the mass fraction of the suspension is 2.3 percent, and the mass ratio of the petroleum ether to the cyclohexane is 50: 50. The gram weight of the nanofiber layer of the composite filter material is 14g/m2(ii) a The nanofibers and nonwoven fibers are reinforced by a combination of physical entanglement and physical crosslinking, with the performance criteria shown in table 1.
Comparative example 6
The polypropylene nanofiber suspension was prepared according to the method of example 6, crosslinked at 50 ℃, frozen at-150 ℃ for 2.5h to solidify, and the solvent was removed by freeze-drying to obtain a polypropylene filter material. Wherein the mass fraction of the suspension is 2.3 percent, and the mass ratio of the petroleum ether to the cyclohexane is 50: 50. The gram weight of the nanofiber layer of the filter material is 14g/m2The performance index is shown in Table 1.
TABLE 1 tensile Strength and filtration Performance index of Filter materials obtained in examples and comparative examples
The preparation method of examples 7-21 is the same as that of examples 1-6, wherein the structural parameters and performance indexes of nanofiber size, solvent parameters, suspension mass fraction, mechanical properties, air filtration effect and the like are shown in tables 2-4.
TABLE 2 structural parameters and Performance indices of the Filter materials prepared in the examples and comparative examples
TABLE 3 structural parameters and Performance indices of the Filter materials prepared in the examples and comparative examples
TABLE 4 structural parameters and Performance indices of the Filter materials prepared in the examples and comparative examples
As can be seen from tables 1-4, the composite filter material prepared by the invention has the efficiency of more than 99.99 to 0.1-2.5 mu m particles, and the piezoresistance is less than 80Pa, so that the high efficiency and low resistance of the filter material are realized, the production process is simple, the production cost is low, and the large-scale production is easy to realize.
Claims (4)
1. A micron fiber three-dimensional skeleton/polymer nanofiber composite filter material is characterized in that: the composite material comprises a microfiber three-dimensional skeleton and a polymer nanofiber aerogel, wherein the polymer nanofiber aerogel is combined with the microfiber three-dimensional skeleton through physical entanglement, physical crosslinking or chemical crosslinking; the polymer nanofiber is one or two or a mixture of three of ethylene-vinyl alcohol copolymer, polyethylene terephthalate, polyacrylonitrile, polysulfone, polyethylene octene co-elastomer, nylon 6, polypropylene, polystyrene, polyvinyl chloride and polyvinylidene fluoride, and the diameter of the polymer nanofiber is 120 nm-500 nm; the micrometer fiber three-dimensional framework is one or more of polypropylene fiber needle-punched non-woven fabric, polyester fiber needle-punched non-woven fabric, aromatic polyamide fiber needle-punched non-woven fabric, pure cotton needle-punched non-woven fabric and warp-knitted 3D spacer fabric, wherein the gram weight of the non-woven fabric is 60g/m2～300g/m2；
The preparation method comprises the following steps:
(1) dispersing polymer nano fibers prepared by melt blending in a solution containing a cross-linking agent, and stirring to form a nano fiber suspension with the mass fraction of the polymer nano fibers being 0.7-3%;
(2) soaking a microfiber three-dimensional framework in the nanofiber suspension obtained in the step (1), wherein nanofibers in the nanofiber suspension enter the microfiber three-dimensional framework in a diffusion mode to form gradient distribution of nanofibers on the surface of the composite filter material and inside the nanofiber framework, and pore diameters of gradient sizes are formed; and then, forming a solidified block by adopting a freeze drying method, and removing the solvent to obtain the required micron fiber three-dimensional framework/polymer nanofiber composite filter material.
2. The method for preparing the microfiber three-dimensional skeleton/polymer nanofiber composite filter material according to claim 1, wherein the method comprises the following steps: the solvent is one or two or three of deionized water, ethanol, tert-butyl alcohol, isopropanol, formic acid, tetrahydrofuran, dichloromethane, trifluoroacetic acid, N-dimethylformamide, acetone, N-heptane and dimethylacetamide.
3. The method for preparing the microfiber three-dimensional skeleton/polymer nanofiber composite filter material according to claim 1, wherein the method comprises the following steps: the cross-linking agent is one of polyacrylic acid, polyvinyl alcohol, genipin and chitosan, or two mixed cross-linking agents, or three mixed cross-linking agents.
4. The method for preparing the microfiber three-dimensional skeleton/polymer nanofiber composite filter material according to claim 1, wherein the method comprises the following steps: the conditions of freezing, condensing and curing in the step (2) are as follows: treating at-150 to-15 ℃ for 1.5 to 5 hours.
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| CN108677379A (en) * | 2018-03-30 | 2018-10-19 | 厦门保瑞达环保科技有限公司 | A kind of 3 microns of filter material manufacture crafts |
| CN108926910A (en) * | 2018-08-02 | 2018-12-04 | 苏州华龙化工有限公司 | A kind of preparation method of antistatic combined filtration scavenging material |
| CN109046040B (en) * | 2018-08-03 | 2022-01-21 | 武汉纺织大学 | Gradient filter membrane material based on nano-fibers and preparation method thereof |
| CN109012218A (en) * | 2018-08-27 | 2018-12-18 | 中国科学院城市环境研究所 | Four layers of composite micro-nano rice fiber air filter membrane of one kind and its application |
| CN110258127B (en) * | 2019-05-27 | 2022-11-15 | 武汉纺织大学 | Reversible self-repairing thermoplastic polymer nanofiber membrane or aerogel material and preparation method thereof |
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| CN115364692B (en) * | 2022-08-12 | 2023-08-25 | 中国科学院上海高等研究院 | Air filtration composite membrane prepared based on cellulose nanofiber reinforced hydrogel conversion and preparation method thereof |
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