CN118179145A - Superfine mesh fiber filter material and preparation method thereof - Google Patents

Superfine mesh fiber filter material and preparation method thereof Download PDF

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Publication number
CN118179145A
CN118179145A CN202410586803.3A CN202410586803A CN118179145A CN 118179145 A CN118179145 A CN 118179145A CN 202410586803 A CN202410586803 A CN 202410586803A CN 118179145 A CN118179145 A CN 118179145A
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filter material
superfine
fiber filter
mesh
electrostatic spinning
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CN118179145B (en
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蔡容容
张立志
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D46/00Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0001Making filtering elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D46/00Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/54Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
    • B01D46/546Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using nano- or microfibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Nonwoven Fabrics (AREA)
  • Filtering Materials (AREA)

Abstract

The invention discloses a superfine mesh fiber filter material and a preparation method thereof, which belong to the technical field of new materials and new equipment, wherein the superfine mesh fiber filter material is arranged into a three-dimensional mesh structure and is formed by interweaving superfine nano fibers and submicron fibers, and the preparation method of the superfine mesh fiber filter material comprises the following steps: s1, dissolving polymer particles and 1-butyl-3-methylimidazole chloride in hexafluoroisopropanol solvent, and stirring to obtain uniform and stable polymer solution; s2, taking the obtained polymer solution, and adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning under high humidity; s3, obtaining the superfine mesh fiber filter material with stable structure and performance through freeze drying. The invention relates to a superfine reticular fiber filter material and a preparation method thereof, wherein an electrostatic spinning technology is adopted to construct superfine nano fibers and submicron fibers into a filter material with a three-dimensional reticular structure, and the filter material has the advantages of high filter efficiency, low resistance and high dust holding capacity.

Description

Superfine mesh fiber filter material and preparation method thereof
Technical Field
The invention relates to the technical field of new materials and new equipment, in particular to a superfine mesh fiber filter material and a preparation method thereof.
Background
Glass fibers and melt-blown nonwoven fabrics are core media of the existing high-efficiency filter, but have the problems of low filtering efficiency and high filtering resistance to PM0.3 ultrafine particles.
Compared with the traditional filter material, the nanofiber has a nano-scale one-dimensional form and an extremely high specific surface area, and the air filter material formed by the nanofiber has higher capture efficiency on ultrafine particles, so that the nanofiber has important application value in the precise filter fields of industrial ultra-clean rooms, clean operating rooms, human body protection and the like.
The electrostatic spinning technology is a simple method for preparing nano-scale fibers, but the conventional electrostatic spinning nano-scale fibers are mostly in a submicron range, and have the problems of large bulk density, low porosity and the like, so that the filtration resistance is rapidly increased along with the dust holding capacity, the dust holding capacity is small, and the filtration energy consumption is large.
In the invention patent with publication number of CN106984201A and name of nano-cobweb/bead fiber composite air filtering membrane and its preparation method, it is disclosed that the air filtering membrane with sandwich structure is prepared by combining electrostatic spraying technology and electrostatic spinning technology, the filtering efficiency of fine particles of PM 1.0 is up to above 99%, the resistance pressure drop is not more than 120 Pa, in the technology, the air filtering membrane is formed by layering and superposing nano-cobweb and bead fiber layers, the stacking density is still larger, the filtering resistance is higher, the mechanical strength of upper and lower nano-cobweb is low, and the wear is easy; and relates to two processes of electrostatic net spraying and electrostatic spinning, and the preparation process is relatively complex.
In the invention patent with publication number CN111455474B and named as "a wool-like crimped electrostatic spinning nanofiber and a preparation method thereof", the invention discloses that the wool-like crimped electrostatic spinning nanofiber is prepared by carrying out electrostatic spinning on a mixed spinning solution of a high-elasticity polymer and a low-elasticity polymer in a high-humidity environment, and the fiber material has a fluffy structure, but the fiber is still in submicron level, and the filtering efficiency of ultrafine particle PM 0.3 is low; in the patent of the invention with the publication number of CN117563330A and the name of needleless electrostatic spinning nanofiber composite filter material and a preparation method thereof, the three-dimensional form of nanofibers can be maintained by adopting a needleless electrostatic spinning technology and designing various parameters in the spinning process, but the pore diameter of the obtained nanofiber membrane is difficult to regulate and control, and the filtration resistance is still higher.
Based on the above problems, a superfine mesh fiber filter material and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a superfine mesh fiber filter material and a preparation method thereof, wherein an electrostatic spinning technology is adopted to construct superfine nano fibers and submicron fibers into a filter material with a three-dimensional mesh structure, and the filter material has the advantages of high filter efficiency, low resistance and high dust holding capacity.
In order to achieve the aim, the invention provides the superfine mesh fiber filter material, which is of a three-dimensional mesh structure and is formed by interweaving superfine nano fibers and submicron fibers, wherein the porosity of the filter material is more than or equal to 60 percent, the average pore diameter is less than 1.0 mu m, and the gram weight is less than 1.0 g/m 2.
Preferably, the diameter distribution of the superfine nano fibers is 30-60 nm, and the diameter distribution of the submicron fibers is 120-160 nm.
Based on the superfine mesh fiber filter material, a preparation method is provided, which comprises the following steps:
S1, dissolving polymer particles and 1-butyl-3-methylimidazole chloride in hexafluoroisopropanol solvent, and magnetically stirring for 8-12 hours at normal temperature to obtain uniform and stable polymer solution.
S2, taking the obtained polymer solution, adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning under high humidity, and depositing superfine nano-fibers and submicron fibers on a metal net of a receiving roller;
S3, immediately freeze-drying the fiber filter material containing the metal net, then placing the fiber filter material at room temperature for 6-12 hours, and removing the filter material from the surface of the metal net to obtain the superfine net-shaped fiber filter material with stable structure and performance.
Preferably, in the S1, the polymer particles are PA6 or PAN, and the concentration of the 1-butyl-3-methylimidazole chloride salt composed of the polymer particles and the 1-butyl-3-methylimidazole chloride is 2.0-5.0 wt.%; the concentration of the polymer solution is 3.0-6.0 wt.%.
Preferably, in the step S2, the electrostatic spinning voltage is 10-15 KV, the receiving distance is 10-15 cm, and the flow rate of the polymer solution is 0.05-0.25 mm/min;
Preferably, in the step S3, the metal mesh is a copper mesh or a brass mesh with 500-800 meshes, the relative humidity is 75-100%, and the temperature is 5-45 ℃.
Preferably, in the step S3, the freeze-drying temperature is-90 ℃ to-60 ℃ and the time is 10-16 hours.
Therefore, the superfine mesh fiber filter material and the preparation method thereof have the following beneficial effects:
(1) By adding 1-butyl-3-methylimidazole chloride, the ion quantity and the conductivity in textile liquid are improved, the surface energy is reduced, the textile charged jet current is promoted to split, two kinds of fine fibers with different sizes are formed, wherein the superfine nanofiber can be used for constructing the aperture of less than 1.0 mu m, and the PM 0.3 filtering efficiency is improved; the submicron fiber can ensure that the passing air flow is in a near-sliding flow state, and the filtration resistance is reduced.
(2) The nanofiber filter material with the fluffy stacking structure is obtained through electrostatic spinning under the high humidity condition, and the obtained filter material is quickly freeze-dried, residual moisture and solvent are directly sublimated without influencing the physical form of the filter material, so that the obtained filter material has a three-dimensional net structure and high porosity, and compared with the conventional two-dimensional layered stacking filter material, the three-dimensional pore channel can reduce the filtering resistance and improve the dust holding capacity while guaranteeing the filtering efficiency.
(3) The filtering efficiency of the superfine mesh fiber filtering material prepared by the invention on PM 0.3 reaches more than 99.5%, and the resistance of the superfine mesh fiber filtering material does not exceed 130 Pa under the wind speed of 5.3 cm/s.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic structural view of an ultrafine mesh fiber filter material of the present invention;
FIG. 2 is an electron microscope image of embodiment 1 of the present invention;
FIG. 3 is a physical diagram of example 1 of the present invention;
FIG. 4 is an electron microscope image of embodiment 2 of the present invention;
FIG. 5 is an electron microscope image of comparative example 1 of the present invention;
FIG. 6 is an electron microscope image of comparative example 2 of the present invention;
reference numerals:
1. Superfine nanofibers; 2. submicron fibers.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention.
As shown in figure 1, the invention provides a superfine mesh fiber filter material which is of a three-dimensional mesh structure and is formed by interweaving 30-60 nm superfine nano fibers 1 and 120-160 nm submicron fibers 2, wherein the porosity of the filter material is more than or equal to 60%, the average pore diameter is less than 1.0 mu m, and the gram weight is less than 1.0 g/m 2.
Example 1
The embodiment provides a preparation method of an ultrafine mesh fiber filter material, which comprises the following specific steps:
(1) 4.0 g of PA6 particles and 2.4 g of 1-butyl-3-methylimidazole chloride were dissolved in 100 ml hexafluoroisopropanol solvent, and magnetically stirred at room temperature for 8: 8h to obtain a uniform and stable polymer solution.
(2) Taking the obtained polymer solution, and adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning in an environment with relative humidity of 80%; adjusting electrostatic spinning parameters: the electrostatic spinning voltage is 12 KV, the receiving distance is 10 cm, the solution flow rate is 0.10 mm/min, the fibers are received by adopting a copper mesh, and the spinning time is 45 min; a filter material formed by fluffy stacking of ultrafine nano fibers and submicron fibers is obtained.
(3) And (3) immediately placing the fiber filtering material into a freeze dryer for drying at the drying temperature of-80 ℃ for 10 h hours to obtain the superfine mesh fiber filtering material with stable structure and performance.
The diameter of the superfine mesh fiber filter material prepared by the embodiment is intensively distributed in the range of 40-60 nm and 130-160 nm, and the filtering efficiency of PM 0.3 reaches 99.87% as shown in a scanning electron microscope chart of FIG. 2; meanwhile, the porous ceramic membrane has a fluffy structure, as shown in a physical diagram of FIG. 3, the porosity is 63%, the average pore diameter is 0.96 mu m, the filtration resistance is 118 Pa at the surface wind speed of 5.3 cm/s, and the pressure drop only rises to 168 Pa when about 10 g/m 2 NaCl particles are deposited.
Example 2
The embodiment provides a preparation method of an ultrafine mesh fiber filter material, which comprises the following specific steps:
(1) 5.5 g PAN particles and 4.0 g of 1-butyl-3-methylimidazole chloride were dissolved in 100 ml hexafluoroisopropanol solvent, and magnetically stirred at room temperature for 12. 12 h to obtain a uniform and stable polymer solution.
(2) Taking the obtained polymer solution, and adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning in an environment with relative humidity of 95%; adjusting electrostatic spinning parameters: the electrostatic spinning voltage is 15 KV, the receiving distance is 12 cm, the solution flow rate is 0.15 mm/min, the fibers are received by adopting a copper mesh, and the spinning time is 60 min; a filter material formed by fluffy stacking of ultrafine nano fibers and submicron fibers is obtained.
(3) And (3) immediately placing the fiber filtering material into a freeze dryer for drying at the drying temperature of-85 ℃ for 12 h hours to obtain the superfine mesh fiber filtering material with stable structure and performance.
The diameter of the superfine mesh fiber filter material prepared by the embodiment is concentrated and distributed in the range of 30-45 nm and 120-140 nm, and as shown in a scanning electron microscope chart of FIG. 4, the filter efficiency of PM 0.3 reaches 99.98%; meanwhile, the porous ceramic material has a fluffy structure, the porosity is 67%, the average pore diameter is 0.92 mu m, the filtration resistance is 126 Pa at the surface wind speed of 5.3 cm/s, and the pressure drop only rises to 170 Pa when about 10 g/m 2 NaCl particles are deposited.
Comparative example 1
The comparative example provides a preparation method of a superfine fiber filter material, which comprises the following specific steps:
(1) 4.0 g of PA6 particles and 2.4 g of 1-butyl-3-methylimidazole chloride were dissolved in 100 ml hexafluoroisopropanol solvent, and magnetically stirred at room temperature for 8: 8h to obtain a uniform and stable polymer solution.
(2) Taking the obtained polymer solution, and adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning in an environment with relative humidity of 80%; adjusting electrostatic spinning parameters: the electrostatic spinning voltage is 1 KV, the receiving distance is 10cm, the solution flow rate is 0.10 mm/min, the fibers are received by adopting a copper mesh, and the spinning time is 45 min; a filter material formed by fluffy stacking of ultrafine nano fibers and submicron fibers is obtained.
(3) Placing the fiber filtering material in a vacuum drying oven after being placed at the room temperature of 2h, and drying at the temperature of not more than 45 ℃ to obtain the superfine fiber filtering material with stable structure and performance.
The diameters of the superfine fiber filter materials prepared in the comparative example are intensively distributed in the intervals of 30-50 nm and 100-130 nm, and as shown in a scanning electron microscope chart of FIG. 5, the filter efficiency of PM 0.3 reaches 99.87%; however, as the fiber filter material is dried in a vacuum drying oven and a common drying oven, after moisture is evaporated from the fiber filter material, the fiber filter material with a fluffy structure collapses, and each layer of fiber is closely packed, the porosity is reduced to 32 percent, and the average pore diameter is as low as 0.56 mu m, so that the filtration resistance is as high as 308 Pa at the surface wind speed of 5.3 cm/s, and the pressure drop is rapidly increased to 968 Pa when about 10 g/m 2 NaCl particles are deposited.
Comparative example 2
The comparative example provides a preparation method of a fiber filter material, which comprises the following specific steps:
(1) 5.5 g PAN particles were dissolved in 100ml hexafluoroisopropanol solvent and magnetically stirred at room temperature for 12. 12 h to give a uniform and stable polymer solution.
(2) Taking the obtained polymer solution, and adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning under the environment with the relative humidity of 55%; adjusting electrostatic spinning parameters: the electrostatic spinning voltage is 15 KV, the receiving distance is 12 cm, the solution flow rate is 0.15 mm/min, the fibers are received by adopting a copper mesh, and the spinning time is 60 min; a filter material formed by fluffy stacking of ultrafine nano fibers and submicron fibers is obtained.
(3) And (3) immediately placing the fiber filtering material into a freeze dryer for drying at the drying temperature of-85 ℃ for 12 h hours to obtain the superfine mesh fiber filtering material with stable structure and performance.
In the comparative example, as no 1-butyl-3-methylimidazole chloride is added, the conductivity and the ion concentration of the electrostatic spinning solution are relatively small, and the fibers cannot be fully stretched, and the diameters of the prepared fiber filtering materials are intensively distributed in a range of 150-230 nm, as shown in a scanning electron microscope diagram of fig. 6, so that the filtering efficiency of PM 0.3 is only 81.67%. The filter had a porosity of 50% and an average pore size of 1.89 μm and a filtration resistance of 68 Pa at a face wind speed of 5.3 cm/s, and the pressure drop increased to 136 Pa when about 10 g/m 2 NaCl particles were deposited.
By comparison, the filtering efficiency of the superfine mesh fiber filtering material prepared by the invention on PM 0.3 reaches more than 99.5%, and the resistance of the superfine mesh fiber filtering material does not exceed 130 Pa at the wind speed of 5.3 cm/s.
Therefore, the superfine net-shaped fiber filter material and the preparation method thereof adopt the electrostatic spinning technology to construct the superfine nano-fiber and submicron fiber into the filter material with a three-dimensional net-shaped structure, and have the excellent filter performance of high filter efficiency, low resistance and large dust holding capacity.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.

Claims (7)

1. A superfine mesh-like fibrous filter material, characterized in that:
The superfine reticular fiber filter material is arranged into a three-dimensional reticular structure and is formed by interweaving superfine nano fibers and submicron fibers, the porosity of the filter material is more than or equal to 60 percent, and the average pore diameter is less than 1.0 mu m.
2. A superfine mesh-like fiber filter material according to claim 1, wherein: the diameter distribution of the superfine nanofiber is 30-60 nm, and the diameter distribution of the submicron fiber is 120-160 nm.
3. A method for preparing the ultrafine mesh-like fibrous filter material according to any one of claims 1 to 2, comprising the steps of:
S1, dissolving polymer particles and 1-butyl-3-methylimidazole chloride in hexafluoroisopropanol solvent, and magnetically stirring for 8-12 hours at normal temperature to obtain uniform and stable polymer solution;
s2, taking the obtained polymer solution, adopting a multi-needle electrostatic spinning machine to carry out electrostatic spinning under high humidity, and depositing superfine nano-fibers and submicron fibers on a metal net of a receiving roller;
S3, immediately freeze-drying the fiber filter material containing the metal net, then placing the fiber filter material at room temperature for 6-12 hours, and removing the filter material from the surface of the metal net to obtain the superfine net-shaped fiber filter material with stable structure and performance.
4. A method for preparing a superfine mesh fiber filter material according to claim 3, wherein: in the S1, polymer particles are PA6 or PAN, and the concentration of 1-butyl-3-methylimidazole chloride salt formed by mixing the polymer particles and 1-butyl-3-methylimidazole chloride is 2.0-5.0 wt%; the concentration of the polymer solution is 3.0-6.0 wt.%.
5. The method for preparing the superfine mesh fiber filter material according to claim 4, wherein the method comprises the following steps: in the step S2, the electrostatic spinning voltage is 10-15 KV, the receiving distance is 10-15 cm, and the flow rate of the polymer solution is 0.05-0.25 mm/min.
6. The method for preparing the superfine mesh fiber filter material according to claim 5, wherein the method comprises the following steps: in the step S3, the metal net is a copper net or a brass net with 500-800 meshes, the relative humidity is 75-100%, and the temperature is 5-45 ℃.
7. The method for preparing the superfine mesh fiber filter material according to claim 6, wherein the method comprises the following steps: in the step S3, the freeze drying temperature is-90 ℃ to-60 ℃ and the time is 10-16 hours.
CN202410586803.3A 2024-05-13 2024-05-13 Superfine mesh fiber filter material and preparation method thereof Active CN118179145B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102813562A (en) * 2011-06-10 2012-12-12 冯淑芹 Three-dimensional large-aperture nanoscale fibrous scaffold and method for preparing same
US20130052462A1 (en) * 2010-03-18 2013-02-28 National Institute For Materials Science Networked polymeric nanofibers, process for producing same, gas adsorbent, and gas separation material
CN106102863A (en) * 2014-12-23 2016-11-09 盈宗制药有限公司 With the protective mask of coating, the formula constituting described coating and the method making described protective mask that are interweaved by different electrospinning fibres
CN112044406A (en) * 2020-09-09 2020-12-08 大连工业大学 Method for preparing microcrystalline cellulose/graphene oxide aerogel fibers from cotton barks
CN114191888A (en) * 2021-12-14 2022-03-18 青岛华世洁环保科技有限公司 Electrospinning filter material, preparation method thereof and filter cartridge prepared from electrospinning filter material
CN114367149A (en) * 2021-12-15 2022-04-19 佛山佛塑科技集团股份有限公司 Filter material and preparation method and application thereof
CN117160142A (en) * 2023-10-23 2023-12-05 西安工程大学 Aerogel filter material with hierarchical pore structure and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130052462A1 (en) * 2010-03-18 2013-02-28 National Institute For Materials Science Networked polymeric nanofibers, process for producing same, gas adsorbent, and gas separation material
CN102813562A (en) * 2011-06-10 2012-12-12 冯淑芹 Three-dimensional large-aperture nanoscale fibrous scaffold and method for preparing same
CN106102863A (en) * 2014-12-23 2016-11-09 盈宗制药有限公司 With the protective mask of coating, the formula constituting described coating and the method making described protective mask that are interweaved by different electrospinning fibres
CN112044406A (en) * 2020-09-09 2020-12-08 大连工业大学 Method for preparing microcrystalline cellulose/graphene oxide aerogel fibers from cotton barks
CN114191888A (en) * 2021-12-14 2022-03-18 青岛华世洁环保科技有限公司 Electrospinning filter material, preparation method thereof and filter cartridge prepared from electrospinning filter material
CN114367149A (en) * 2021-12-15 2022-04-19 佛山佛塑科技集团股份有限公司 Filter material and preparation method and application thereof
CN117160142A (en) * 2023-10-23 2023-12-05 西安工程大学 Aerogel filter material with hierarchical pore structure and preparation method thereof

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