CN111013255A - A kind of preparation method of micro/nanofiber aerogel composite filter material - Google Patents
A kind of preparation method of micro/nanofiber aerogel composite filter material Download PDFInfo
- Publication number
- CN111013255A CN111013255A CN201911421836.8A CN201911421836A CN111013255A CN 111013255 A CN111013255 A CN 111013255A CN 201911421836 A CN201911421836 A CN 201911421836A CN 111013255 A CN111013255 A CN 111013255A
- Authority
- CN
- China
- Prior art keywords
- micro
- filter material
- fiber
- composite filter
- aerogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 120
- 239000002121 nanofiber Substances 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 239000003658 microfiber Substances 0.000 title claims abstract description 61
- 239000004964 aerogel Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 43
- 239000006185 dispersion Substances 0.000 claims abstract description 35
- 238000001914 filtration Methods 0.000 claims abstract description 35
- 238000000967 suction filtration Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000004108 freeze drying Methods 0.000 claims abstract description 13
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 9
- 238000010008 shearing Methods 0.000 claims abstract description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003546 flue gas Substances 0.000 claims abstract description 6
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 239000003733 fiber-reinforced composite Substances 0.000 claims abstract description 4
- 238000009413 insulation Methods 0.000 claims abstract description 4
- 230000002787 reinforcement Effects 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 3
- 239000004642 Polyimide Substances 0.000 description 23
- 229920001721 polyimide Polymers 0.000 description 23
- 238000009987 spinning Methods 0.000 description 22
- 239000000758 substrate Substances 0.000 description 21
- 239000004734 Polyphenylene sulfide Substances 0.000 description 17
- 229920000069 polyphenylene sulfide Polymers 0.000 description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 239000012528 membrane Substances 0.000 description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000010041 electrostatic spinning Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 229920005594 polymer fiber Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 229920001410 Microfiber Polymers 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000003958 fumigation Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001523 electrospinning Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000002149 hierarchical pore Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920006376 polybenzimidazole fiber Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- D01D5/0023—Electro-spinning characterised by the initial state of the material the material being a polymer melt
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01G—PRELIMINARY TREATMENT OF FIBRES, e.g. FOR SPINNING
- D01G1/00—Severing continuous filaments or long fibres, e.g. stapling
- D01G1/02—Severing continuous filaments or long fibres, e.g. stapling to form staple fibres not delivered in strand form
- D01G1/04—Severing continuous filaments or long fibres, e.g. stapling to form staple fibres not delivered in strand form by cutting
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nonwoven Fabrics (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a preparation method of a micro/nano fiber aerogel composite filter material, belonging to the field of textile materials. The specific preparation method of the invention comprises the following steps: (1) preparing micro/nano fibers; (2) preparing a dispersion liquid from the micro/nano fibers prepared in the step (1) by fiber shearing and crushing; (3) and (3) carrying out freeze-drying molding on the fiber dispersion liquid impregnation base material obtained in the step (2): carrying out suction filtration on the base material and the fiber dispersion liquid by adopting a vacuum suction filtration method to obtain a wet composite material; then, freeze-drying the wet composite material to prepare an aerogel material; (4) and (4) reinforcing the aerogel composite filter material obtained in the step (3) to obtain the micro/nano fiber aerogel composite filter material. The invention adopts a vacuum filtration method to prepare the micro/nano fiber aerogel continuous gradient structure composite filter material, has high filtering efficiency, and is suitable for the fields of high-temperature flue gas filtration, oil/water, heat insulation, sound absorption, fiber reinforced composite materials and the like.
Description
Technical Field
The invention relates to a preparation method of a micro/nano fiber aerogel composite filter material, belonging to the field of textile materials.
Background
The emission of industrial smoke is one of the main causes of haze, and particularly, the fine particulate matters (PM2.5) generated by the smoke can increase the incidence rate of respiratory diseases of human beings. Therefore, the research and development of the high-temperature flue gas filtering material for controlling the emission of the dust-containing flue gas in the industrial furnace and the solution of the key technology are important and hot points of the research in the field of environmental protection in China. However, the high-temperature flue gas filtration has higher requirements on the capture efficiency and the service life of the filter material, and the currently used filter materials are needle-punched, spunlaced or membrane-coated filter materials.
For example, chinese patent CN105220364A discloses a nonwoven material combining dry and wet web forming methods and hydroentangling consolidation, which is a composite web formed by laying an ultra-short fiber surface layer on a dry-laid web substrate and then hydroentangling consolidation. The filter material has a good filtering performance and a small pressure drop, but has a low efficiency of collecting fine particles.
For another example, chinese patent CN105688512A discloses a spunlace precision face-layer filter material, which is composed of a precision face layer, an upper fiber web layer, a substrate layer, and a lower fiber web layer from a dust-facing surface to an air-purifying surface. The filter material has stable structure and high filtering precision, but the preparation process is complicated.
For another example, chinese patent CN108434863A discloses a corrosion-resistant high-gram-weight spunlace filter material, which is prepared by using polyphenylene sulfide fibers with different fineness and length as raw materials to prepare a spunlace substrate, and then performing surface coating with PTFE emulsion and a film-forming agent. The filter material has high filtering precision, but large pressure drop and complex preparation process.
The nanofiber aerogel material has a unique multistage mesh structure, macropores (10-30 mu m) in the material are interconnected through a triangular bonding area, the bonding area is composed of a plurality of small pores (1-2 mu m), the material is in a honeycomb-shaped pore structure, the structure endows the material with good air permeability, and meanwhile, the compression resilience and the durability of the material are superior to those of other fiber aerogel materials with the same volume density.
For example, a micro/nano composite aerogel filter material is disclosed in the literature (Robust polyimide nanoparticles/micro fiber aerogels wet by solution-vacuum for environmental applications), which is obtained by immersing a nonwoven substrate in a nanofiber dispersion, performing ultrasonic treatment, and then performing freeze drying, fumigation and reinforcement. Compared with the nanofiber membrane filter material, the filter material reduces the filtration resistance to a certain extent under the same filtration efficiency. However, after ultrasonic impregnation, the nanofibers are mainly randomly distributed on the upper and lower surfaces of the substrate, only a part of the fibers are embedded in the substrate, and the filtration efficiency of particles below 0.5 μm needs to be improved.
Disclosure of Invention
In order to solve at least one problem, the invention provides a preparation method of a micro/nano fiber aerogel composite filter material, wherein the composite filter material is prepared by preparing fibers with different diameters by adopting a multi-needle electrostatic spinning technology, then carrying out homogeneous shearing, freezing and forming, and then carrying out fumigation and reinforcement to form the aerogel filter material.
In addition, the invention adopts a vacuum filtration method to prepare the micro/nano fiber aerogel continuous gradient structure composite filter material, and the density of the micro/nano fibers is gradually reduced from the dust facing surface to the air purifying surface. The filter material solves the problems of low strength and easiness in damage of the micro/nano fiber aerogel, and improves the filtering efficiency of the base material.
The first purpose of the invention is to provide a preparation method of a micro/nano fiber aerogel composite filter material, which comprises the following steps:
(1) preparing micro/nano fibers;
(2) preparing a dispersion liquid from the micro/nano fibers prepared in the step (1) by fiber shearing and crushing;
(3) and (3) carrying out freeze-drying molding on the fiber dispersion liquid impregnation base material obtained in the step (2): carrying out suction filtration on the base material and the fiber dispersion liquid by adopting a vacuum suction filtration method to obtain a wet composite material; then, freeze-drying the wet composite material to prepare an aerogel material;
(4) and (4) reinforcing the aerogel composite filter material obtained in the step (3) to obtain the micro/nano fiber aerogel composite filter material.
In one embodiment, the micro/nano fiber preparation in step (1) is specifically: the high-temperature resistant polymer fiber is prepared by adopting an electrostatic spinning technology.
In one embodiment, the preparation of the dispersion by shearing and crushing the fibers in the step (2) is specifically as follows: polymer fiber is immersed into a dispersion solvent, and a polymer fiber dispersion liquid with a certain concentration is prepared by a high-speed shearing machine or a crushing machine.
In one embodiment, the reinforcement of the aerogel composite filter material in the step (4) is specifically: and (3) putting the dried and formed aerogel material into volatile organic solvent steam, and preparing the high-temperature-resistant composite filter material by fumigating and reinforcing.
In one embodiment, the parameter setting of the vacuum filtration in the step (3) is specifically as follows: the length-diameter ratio of the micro/nano fibers is 5-40/20-200, the suction filtration time is 5-45 min, and the suction filtration pressure is 0.02-0.1 MPa.
In one embodiment, the parameters of the vacuum filtration in step (3) are set as follows: the mass/volume fraction of the base material and the dispersion liquid is 3.34%, the length-diameter ratio of the micro/nano fibers is 40/150, the suction filtration time is 15min, and the suction filtration pressure is 0.06 MPa.
In one embodiment, the electrospinning technology in step (1) is multi-needle electrospinning, the micro-fibers and the nano-fibers are simultaneously sprayed, and the micro-fiber/nano-fiber membrane with a random packing structure is prepared by regulating the number ratio of the micro-nozzles to the nano-nozzles.
In one embodiment, the high temperature resistant polymer used in step (1) includes polyimide, polyphenylene sulfide, aramid, and other high temperature resistant polymer materials.
In one embodiment, step (1) produces polymer fibers having a diameter of between 100nm and 4 μm.
In one embodiment, the dispersing solvent component in step (2) includes one or more of water, ethanol, tert-butanol, dioxane, and other solvents.
In one embodiment, the mass/volume percent concentration of the fibers in the fiber dispersion in step (2) is 0.05 wt% to 2.0 wt%, i.e., the percentage of fibers in the total solution is 0.05 to 2 wt%.
In one embodiment, the base material in step (3) is a textile fabric product such as a needle-punched non-woven fabric, a knitted fabric and a braided fabric, which is made of one or more fibers selected from polyimide fibers, polyphenylene sulfide fibers, polytetrafluoroethylene fibers and polybenzimidazole fibers.
In one embodiment, the mass/volume ratio of the base material to the dispersion in step (3) is 1.5% to 8%, corresponding to 1.5 to 8g of base material added to 100mL of dispersion.
In one embodiment, the specific parameters of the freeze-drying machine in the step (3) are set as follows: the vacuum degree is 5Pa, and the drying time is 24 h.
In one embodiment, the organic solvent in step (4) is one or more selected from dichloromethane, acetone, tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide, dioxane, trichloromethane and hexafluoroisopropanol.
In one embodiment, the steam concentration in step (4) is 5.0 × 10-3~0.1mol/L。
The second purpose of the invention is to provide a composite filter material prepared by the method.
The third purpose of the invention is the application of the composite filter material in high-temperature flue gas filtration.
In one embodiment, the filter media is used to make a filter bag, which can be used in a bag house filter.
The fourth purpose of the invention is to apply the composite filter material in the fiber reinforced composite material.
The fifth purpose of the invention is the application of the composite filter material in oil/water separation.
The sixth purpose of the invention is the application of the composite filter material in heat insulation and sound absorption materials.
The invention has the beneficial effects that:
(1) the invention compounds the electrostatic spinning micro/nano fiber with the high temperature resistant base material to form the composite high temperature resistant aerogel filter material with the fiber density gradient distribution; from the dust facing side to the air cleaning side, the density of the micro/nano fibers is gradually reduced. The filter material solves the problems of low strength and easiness in damage of the micro/nano fiber aerogel, and improves the filtering efficiency of the base material.
(2) Compared with the prior filter material, the filter material has high porosity which is more than 83 percent, and small filter resistance which is less than 220 Pa; the filtering efficiency of the filtered impurities with the particle size range of more than 0.3 mu m reaches more than 75 percent, the filtering performance is good, multi-level gradient filtering can be realized, the application is not limited, and the composite material can also be used as materials for sound absorption, heat insulation, oil/water separation, fiber reinforced composite materials and the like.
(3) The filter material of the invention can be used for filtering harmful substances, protecting the environment and solving the problem of secondary pollution.
Drawings
FIG. 1 is a flow chart of the preparation process of example 1.
Fig. 2 shows the morphology of the micro/nanofiber membrane in example 1.
Fig. 3 is a schematic structural diagram of the micro/nanofiber composite aerogel filter material in example 1.
FIG. 4 is a topographical view of a micro/nanofiber composite aerogel filter material according to example 1; (a) and (b) SEM images taken for two different locations.
Fig. 5 is an appearance diagram of the micro/nanofiber composite filter of comparative example 2.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
Testing of porosity: calculated from the mass and volume of the material, the formula is as follows:
wherein P is the porosity (%) of the filter material, and V is0Is the volume (cm) of the filter material3) M is the mass (g) of the fiber material, and ρ is the density (g/cm) of the fiber material3)。
Testing of filtration performance: the filtration efficiency and filtration resistance of the filter media were tested with a filter media integration bench ((LZC-H, Huada equipment, Suzhou Co., Ltd.) at an air flow rate of 84L/min.
Example 1
The preparation process of the nano/micron fiber composite aerogel filter material is shown in figure 1: the preparation method comprises the steps of preparing a micro/nano high-temperature-resistant fiber membrane, preparing a fiber dispersion solution, carrying out freeze-drying molding on a dispersion solution impregnation base material and reinforcing an aerogel composite filter material in sequence. The specific implementation mode is as follows:
a micro/nano fiber aerogel composite filter material comprises the following raw materials:
p84 fibers; soluble Polyimide (PI) powder; polyphenylene Sulfide (PPS) needle punched non-woven substrate, 500g/m2(ii) a N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dioxane.
(1) Preparing micro/nano fibers:
and (2) carrying out side-by-side spinning on the PI spinning solution with the concentration of 16% and the PI spinning solution with the concentration of 25% by adopting a multi-needle electrostatic spinning technology, wherein the number ratio of 16% PI/25% PI spray heads is 1: 1. Wherein, the PI spinning solution with the concentration of 16% takes P84 fiber as a raw material, and the ratio of DMF: DMAc 1:1 is spinning solution; the 25% PI spinning solution is prepared from soluble Polyimide (PI) powder as raw material, dioxane: DMF-1: 1 is the spinning solution. In the spinning process, the spinning voltage is 20kV, the spinning distance is 20cm, and the spinning flow is 1 mL/h. The morphology of the spun micro/nanofibers is shown in fig. 2.
(2) Preparation of fiber dispersion: weighing 0.4g of the micro/nano fiber membrane obtained in the step (1), and shearing into pieces of 1 × 1cm2Then, the resulting mixture was put into 400mL of a water/t-butanol (ratio: 1) solution and homogenized at 13000rpm for 30 minutes by a homogenizer to prepare a 0.1% fiber dispersion.
(3) Impregnating the PPS base material with the dispersion liquid, and freeze-drying and molding: cutting a PPS (polyphenylene sulfide) needle-punched non-woven substrate with the diameter of 15cm, putting the PPS needle-punched non-woven substrate into a Buchner funnel, pouring the micro-nano fiber dispersion liquid obtained in the step (2) into the funnel, and promoting the penetration of fibers into the substrate by suction filtration (the specific parameters are set as follows: the mass/volume fraction of the substrate and the dispersion liquid is 3.34%, the length-diameter ratio of micro/nano fibers is 40/150 respectively, the suction filtration time is 15min, and the suction filtration pressure is 0.06 MPa); and then freezing the filtered material at-80 ℃ for 24h, and then putting the frozen material into a freeze dryer for freeze drying for 24h to obtain the freeze-dried material.
(4) And (3) reinforcement of the aerogel composite filter material: dripping 500L of DMF solution into a 150mL sealed tank, and then putting the material freeze-dried in the step (3) into the sealed tank for fumigation for 1 h; the micro/nano fiber aerogel composite filter material can be obtained, and the specific structure is shown in fig. 3 and 4.
FIG. 2 is the morphology of the micro/nanofiber membrane in example 1, and it can be seen that: the micro/nano fiber is interwoven into a film.
Fig. 3 is a schematic structural diagram of the micro/nanofiber composite high-temperature aerogel filter material in example 1, and it can be seen from the diagram that: from the dust facing surface to the air purifying surface, the micro-nano fibers are distributed in a continuous density gradient manner.
Fig. 4 is a morphology diagram of the micro/nanofiber composite aerogel filter material according to example 1, and it can be seen from the diagram that: the micro/nano fibers are embedded into the substrate to form a hierarchical pore structure.
Example 2
A micro/nano fiber aerogel composite filter material comprises the following raw materials:
p84 fibers; soluble Polyimide (PI) powder; polyphenylene Sulfide (PPS) needle punched non-woven substrate, 500g/m2(ii) a N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), dioxane.
(1) Preparing micro/nano fibers:
and (2) carrying out side-by-side spinning on 10% PI spinning solution and 25% PI spinning solution by adopting a multi-needle electrostatic spinning technology, wherein the number ratio of 10% PI to 25% PI spray heads is 3: 1. Wherein, the PI spinning solution with the concentration of 10% takes P84 fiber as a raw material and DMF as a spinning solution; the 25% PI spinning solution is prepared from soluble Polyimide (PI) powder as raw material, dioxane: DMF-1: 1 is the spinning solution. In the spinning process, the spinning voltage is 20kV, the spinning distance is 20cm, and the spinning flow is 1 mL/h.
(2) Preparation of fiber dispersion: weighing 0.4g of the micro/nano fiber membrane obtained in the step (1), and shearing into pieces1×1cm2The resulting mixture was put into 400mL of a tert-butanol solution, and homogenized at 13000rpm for 30min with a homogenizer to prepare a 0.1% fiber dispersion.
(3) Freeze-drying and forming of the dispersion liquid impregnated substrate: cutting the PPS needle-punched non-woven substrate with the diameter of 15cm, putting the PPS needle-punched non-woven substrate into a Buchner funnel, pouring the micro/nano fiber dispersion liquid obtained in the step (2) into the funnel, and promoting the penetration of the fibers into the substrate by suction filtration (the specific parameters are set as follows, the mass/volume fractions of the substrate and the dispersion liquid are 3.34%, the length-diameter ratio of the micro/nano fibers is 40/150 respectively, the suction filtration time is 15min, and the suction filtration pressure is 0.06 MPa); then freezing the filtered material at-20 ℃ for 24h, and then putting the frozen material into a freeze dryer for freeze drying for 24 h.
(4) And (3) reinforcement of the aerogel composite filter material: and (3) dripping 500L DMAc solution into a 150mL sealed tank, and then putting the freeze-dried material into the sealed tank to fumigate for 1h to obtain the micro/nano fiber aerogel composite filter material.
Comparative example 1
The vacuum filtration parameters of example 1 were adjusted to make the mass/volume fractions of the base material and the dispersion 1.18%, the aspect ratio of the micro/nanofiber 62/216, the pressure of filtration 0.15MPa, the time of filtration 15min, and other parameters remained unchanged, to obtain a micro/nanofiber aerogel composite filter.
Comparative example 2
The vacuum filtration parameters of example 1 were adjusted to 3.34% mass/volume fraction of the base material and the dispersion, 40/150% aspect ratio of the micro/nanofiber, 0.01MPa of filtration pressure, 15min of filtration time, and other parameters were kept unchanged to obtain the micro/nanofiber aerogel composite filter material.
Comparative example 3
And (3) adjusting the suction filtration compounding method in the embodiment 1 to change the ultrasonic immersion method into the ultrasonic immersion method for 15min, and keeping other parameters unchanged to obtain the micro/nano fiber aerogel composite filter material.
Comparative example 4
The process of compounding the micro/nano fiber dispersion liquid and the PPS substrate by suction filtration in example 1, namely the PPS substrate, is omitted.
And (3) testing:
the composite filter materials of examples 1 and 2 and comparative examples 1 to 4 were subjected to a performance test, and the specific test results are shown in table 1 below:
table 1 results of performance test on the composite filter materials of examples 1 and 2 and comparative examples 1 to 4
As can be seen from Table 1:
(1) compared with the PPS base material (comparative example 4), the filtration efficiency of the micro/nano composite aerogel filter material (examples 1 and 2) on particles with the particle size of less than 0.5 mu m is improved by 40-50%, and the porosity is improved by 3-7%.
(2) Compared with the composite filter material prepared by an immersion method (comparative example 3), the composite filter materials prepared by a vacuum filtration method (example 1 and example 2) have the advantages that the filtration efficiency of the composite filter material to particles with the particle size of less than 0.5 mu m is improved by about 20 percent and the filtration efficiency of the composite filter material to particles with the particle size of more than 1 mu m is improved by about 0.7 to 6 percent under the same filtration resistance; the porosity is improved by about 4 percent, so that the filtration resistance is not increased while the filtration efficiency is greatly improved.
(3) Compared to example 1 and example 2:
when the length-diameter ratio of the fiber and the suction filtration pressure are too large (comparative example 1), the filtration efficiency of the prepared composite filter material is not obviously improved, but the filtration resistance is more than 3 times higher, because the length-diameter ratio of the micro/nano fiber is large and the micro/nano fiber is densely accumulated on the surface of the base material under the too large pressure.
When the suction filtration pressure and time are too small (comparative example 2), the filtration efficiency of the prepared composite filter material on particles with the particle size of less than 0.5 mu m is lower than that of example 1, and the filtration resistance is higher;
in addition, the fibers in the dispersion were deposited on the dust-facing surface of the PPS substrate, so that the surface of the prepared composite filter material was easily damaged (fig. 5).
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The preparation method of the micro/nano fiber aerogel composite filter material is characterized by comprising the following steps of:
(1) preparing micro/nano fibers;
(2) preparing a dispersion liquid from the micro/nano fibers prepared in the step (1) by fiber shearing and crushing;
(3) and (3) carrying out freeze-drying molding on the fiber dispersion liquid impregnation base material obtained in the step (2): carrying out suction filtration on the base material and the fiber dispersion liquid by adopting a vacuum suction filtration method to obtain a wet composite material; then, freeze-drying the wet composite material to prepare an aerogel material;
(4) and (4) reinforcing the aerogel composite filter material obtained in the step (3) to obtain the micro/nano fiber aerogel composite filter material.
2. The preparation method according to claim 1, wherein the parameter setting of the vacuum filtration in the step (3) is specifically as follows: the length-diameter ratio of the micro/nano fibers is (5-40)/(20-200), the suction filtration time is 5-45 min, and the suction filtration pressure is 0.02-0.1 MPa.
3. The method according to claim 1, wherein the parameters of the vacuum filtration in the step (3) are set as follows: the mass/volume fraction of the base material and the dispersion liquid is 3.34%, the length-diameter ratio of the micro/nano fibers is 40/150, the suction filtration time is 15min, and the suction filtration pressure is 0.06 MPa.
4. The preparation method of claim 1, wherein the reinforcement of the aerogel composite filter material in the step (4) is specifically as follows: and (3) putting the dried and formed aerogel material into volatile organic solvent steam, and preparing the high-temperature-resistant composite filter material by fumigating and reinforcing.
5. The method according to claim 4, wherein the steam concentration in the step (4) is 5.0X 10-3~0.1mol/L。
6. The method of claim 1, wherein the fiber produced in step (1) has a diameter of 100nm to 4 μm.
7. The production method according to claim 1, wherein the mass/volume percentage concentration of the fibers in the fiber dispersion liquid in the step (2) is 0.05 to 2.0 wt%.
8. The micro/nano fiber aerogel composite filter material obtained by the preparation method of any one of claims 1 to 7.
9. Use of the composite filter material of claim 8 in high temperature flue gas filtration.
10. The use of the composite filter material of claim 8 in fiber reinforced composites, oil-water separation, or thermal insulation and sound absorption.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911421836.8A CN111013255B (en) | 2019-12-31 | 2019-12-31 | A kind of preparation method of micro/nanofiber aerogel composite filter material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911421836.8A CN111013255B (en) | 2019-12-31 | 2019-12-31 | A kind of preparation method of micro/nanofiber aerogel composite filter material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111013255A true CN111013255A (en) | 2020-04-17 |
CN111013255B CN111013255B (en) | 2021-06-11 |
Family
ID=70198056
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911421836.8A Active CN111013255B (en) | 2019-12-31 | 2019-12-31 | A kind of preparation method of micro/nanofiber aerogel composite filter material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111013255B (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113856244A (en) * | 2021-10-21 | 2021-12-31 | 国网浙江省电力有限公司检修分公司 | Porous composite material with gradient structure and preparation method and application thereof |
CN114481680A (en) * | 2022-03-10 | 2022-05-13 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same |
WO2022121594A1 (en) * | 2020-12-09 | 2022-06-16 | 青岛科技大学 | Nanofiber/mofs-based preferential alcohol-permeable pervaporation membrane and preparation method thereof |
CN114804805A (en) * | 2022-04-24 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel composite material and preparation method thereof |
Citations (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110266213A1 (en) * | 2010-05-03 | 2011-11-03 | Korea Institute Of Science And Technology | Ultrafine continuous fibrous ceramic filter and method of manufacturing same |
CN104001371A (en) * | 2014-05-30 | 2014-08-27 | 福州大学 | Method for recycling waste dust removal filter material |
CN104941319A (en) * | 2015-06-19 | 2015-09-30 | 合肥工业大学 | Method for preparing manganese-base dedusting and denitration integration function filter material |
CN105536349A (en) * | 2015-12-08 | 2016-05-04 | 张家港万众一芯生物科技有限公司 | Novel nanometer aerogel material for air filtration and preparation method thereof |
CN105821586A (en) * | 2016-04-18 | 2016-08-03 | 广州拜费尔空气净化材料有限公司 | Nano-fiber filtering material and preparation method thereof |
CN106215515A (en) * | 2016-08-19 | 2016-12-14 | 安徽元琛环保科技股份有限公司 | A kind of preparation method of Electrospun nano-fibers glass woven felt filter material |
CN106823563A (en) * | 2017-03-02 | 2017-06-13 | 江南大学 | A kind of preparation of melt Static Spinning polypropylene filter material and structural behaviour regulation and control method |
CN108570882A (en) * | 2017-03-13 | 2018-09-25 | 昆明纳太科技有限公司 | Carbon nanotube composite gradient structure filter paper and preparation method thereof |
CN109046040A (en) * | 2018-08-03 | 2018-12-21 | 武汉纺织大学 | Gradient filtration membrane material based on nanofiber and preparation method thereof |
CN109126290A (en) * | 2018-09-20 | 2019-01-04 | 俞小峰 | A kind of high-strength anti-flaming air filting material and preparation method thereof |
KR20190014563A (en) * | 2019-01-28 | 2019-02-12 | 연세대학교 산학협력단 | Filter apparatus and manufacture method thereof |
US20190308131A1 (en) * | 2016-07-08 | 2019-10-10 | Linde ZHANG | Air filtration device utilizing self-supporting graphene material |
US20190314746A1 (en) * | 2018-04-16 | 2019-10-17 | The Hong Kong Polytechnic University | Electrostatically-charged Nanofiber Media and Fabrication Method Thereof |
CN110461926A (en) * | 2017-01-26 | 2019-11-15 | 蓝移材料有限公司 | Organic polymer aeroge comprising micro-structure |
-
2019
- 2019-12-31 CN CN201911421836.8A patent/CN111013255B/en active Active
Patent Citations (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110266213A1 (en) * | 2010-05-03 | 2011-11-03 | Korea Institute Of Science And Technology | Ultrafine continuous fibrous ceramic filter and method of manufacturing same |
CN104001371A (en) * | 2014-05-30 | 2014-08-27 | 福州大学 | Method for recycling waste dust removal filter material |
CN104941319A (en) * | 2015-06-19 | 2015-09-30 | 合肥工业大学 | Method for preparing manganese-base dedusting and denitration integration function filter material |
CN105536349A (en) * | 2015-12-08 | 2016-05-04 | 张家港万众一芯生物科技有限公司 | Novel nanometer aerogel material for air filtration and preparation method thereof |
CN105821586A (en) * | 2016-04-18 | 2016-08-03 | 广州拜费尔空气净化材料有限公司 | Nano-fiber filtering material and preparation method thereof |
US20190308131A1 (en) * | 2016-07-08 | 2019-10-10 | Linde ZHANG | Air filtration device utilizing self-supporting graphene material |
CN106215515A (en) * | 2016-08-19 | 2016-12-14 | 安徽元琛环保科技股份有限公司 | A kind of preparation method of Electrospun nano-fibers glass woven felt filter material |
CN110461926A (en) * | 2017-01-26 | 2019-11-15 | 蓝移材料有限公司 | Organic polymer aeroge comprising micro-structure |
CN106823563A (en) * | 2017-03-02 | 2017-06-13 | 江南大学 | A kind of preparation of melt Static Spinning polypropylene filter material and structural behaviour regulation and control method |
CN108570882A (en) * | 2017-03-13 | 2018-09-25 | 昆明纳太科技有限公司 | Carbon nanotube composite gradient structure filter paper and preparation method thereof |
US20190314746A1 (en) * | 2018-04-16 | 2019-10-17 | The Hong Kong Polytechnic University | Electrostatically-charged Nanofiber Media and Fabrication Method Thereof |
CN109046040A (en) * | 2018-08-03 | 2018-12-21 | 武汉纺织大学 | Gradient filtration membrane material based on nanofiber and preparation method thereof |
CN109126290A (en) * | 2018-09-20 | 2019-01-04 | 俞小峰 | A kind of high-strength anti-flaming air filting material and preparation method thereof |
KR20190014563A (en) * | 2019-01-28 | 2019-02-12 | 연세대학교 산학협력단 | Filter apparatus and manufacture method thereof |
Non-Patent Citations (2)
Title |
---|
梁玉莹: "纤维改善SiO2气凝胶的力学和隔热性能研究进展", 《硅酸盐通报》 * |
申莹等: "Robust polyimide nano/microfibre aerogels welded by solvent-vapour for environmental applications", 《ROYAL SOCIETY OPEN SCIENCE》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022121594A1 (en) * | 2020-12-09 | 2022-06-16 | 青岛科技大学 | Nanofiber/mofs-based preferential alcohol-permeable pervaporation membrane and preparation method thereof |
CN113856244A (en) * | 2021-10-21 | 2021-12-31 | 国网浙江省电力有限公司检修分公司 | Porous composite material with gradient structure and preparation method and application thereof |
CN114481680A (en) * | 2022-03-10 | 2022-05-13 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same |
CN114481680B (en) * | 2022-03-10 | 2023-08-22 | 咸宁优维科技有限公司 | Preparation method of aramid fiber material, aerogel and pumping filter membrane material |
CN114804805A (en) * | 2022-04-24 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel composite material and preparation method thereof |
CN114804805B (en) * | 2022-04-24 | 2023-08-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel composite material and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN111013255B (en) | 2021-06-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Yang et al. | Multifunctional composite membrane based on BaTiO3@ PU/PSA nanofibers for high-efficiency PM2. 5 removal | |
CN111013255B (en) | A kind of preparation method of micro/nanofiber aerogel composite filter material | |
Deuber et al. | Exploration of ultralight nanofiber aerogels as particle filters: capacity and efficiency | |
Yang et al. | Electrospun polymer composite membrane with superior thermal stability and excellent chemical resistance for high-efficiency PM2. 5 capture | |
Su et al. | Multilevel structured PASS nanofiber filter with outstanding thermal stability and excellent mechanical property for high-efficiency particulate matter removal | |
CN107137979B (en) | Micron fiber three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof | |
JP5037034B2 (en) | Filter filter medium, its production method and method of use, and filter unit | |
CN103894077B (en) | A kind of various dimensions pore structure composite filtering film and preparation method thereof | |
Xu et al. | Preparation of a novel poly (ether ether ketone) nonwoven filter and its application in harsh conditions for dust removal | |
Wang et al. | Multilevel‐layer‐structured polyamide 6/poly (trimethylene terephthalate) nanofibrous membranes for low‐pressure air filtration | |
CN109012218A (en) | Four layers of composite micro-nano rice fiber air filter membrane of one kind and its application | |
Li et al. | Three-layer composite filter media containing electrospun polyimide nanofibers for the removal of fine particles | |
CN103505942A (en) | Nanofiber filter material | |
CN107158969A (en) | A kind of functionalized nano-fiber filtering material and its preparation method and application | |
Xu et al. | Preparation and properties of PTFE hollow fiber membranes for the removal of ultrafine particles in PM 2.5 with repetitive usage capability | |
CN112522856A (en) | Metal organic framework and electrospun nanofiber composite protective cover film and preparation | |
Liu et al. | Hierarchical micro/nanofibrous filter for effective fine-particle capture | |
CN109157915A (en) | A kind of micro/nano-fibre composite filter material and preparation method thereof | |
CN111282342B (en) | Long-acting electret nanofiber filtering material and preparation method thereof | |
Zhu et al. | Metal-organic framework decorated polyimide nanofiber aerogels for efficient high-temperature particulate matter removal | |
Gao et al. | Enhanced air filtration performance under high-humidity condition through electrospun membranes with optimized structure | |
Wei et al. | Self-assembly-dominated hierarchical porous nanofibrous membranes for efficient high-temperature air filtration and unidirectional water penetration | |
CN112263877A (en) | Air filter material and filter element and use | |
CN112774457A (en) | Polymer microfiltration membrane and preparation method and application thereof | |
Shao et al. | Electrospun PS/PAN nanofiber membranes formed from doped carbon nanotubes with a fluffy and multi-scale construction for air-filtration materials |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |