CN111589229B - Composite air filter material capable of being washed repeatedly and preparation method thereof - Google Patents

Composite air filter material capable of being washed repeatedly and preparation method thereof Download PDF

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Publication number
CN111589229B
CN111589229B CN202010503971.3A CN202010503971A CN111589229B CN 111589229 B CN111589229 B CN 111589229B CN 202010503971 A CN202010503971 A CN 202010503971A CN 111589229 B CN111589229 B CN 111589229B
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filter material
polypropylene
polycarbonate
zinc nitrate
nitrate hexahydrate
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CN111589229A (en
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李婷婷
岑喜喜
林佳弘
楼静文
张莹
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Shandong Cornell Material Technology Co ltd
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Tianjin Polytechnic University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H13/00—Other non-woven fabrics
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • 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

Abstract

The invention discloses a composite air filter material capable of being repeatedly washed by water and a preparation method thereof, belonging to the field of industrial textiles and comprising the following specific steps: step 1, drying and mixing polypropylene and polycarbonate, and preparing a bi-component polypropylene/polycarbonate mixed master batch by a single-screw granulator; step 2, blowing the master batch prepared in the step 1 to form a polypropylene-polycarbonate melt-blown filter material (PPC); step 3, growing a zeolite imidazole ester framework on the PPC prepared in the step 2 by using zinc nitrate hexahydrate, 2-methylimidazole and anhydrous methanol through an in-situ growth method to prepare a polypropylene-polycarbonate/zeolite imidazole ester framework melt-blown filter material (PPC/ZIF-8); step 4, preparing zinc nitrate hexahydrate, 2-methylimidazole and anhydrous methanol into zeolite imidazolate framework (ZIF-8) nanocrystals according to a molar ratio of 9.08: 72.35: 6292.13; and 5, compounding the polyvinylidene fluoride spinning solution containing the ZIF-8 nanocrystals with the PPC/ZIF-8 filter material prepared in the step 3 to prepare the composite filter material (PPC/PVDF/ZIF-8) capable of being repeatedly washed by water. The PPC/PVDF/ZIF-8 air filter material prepared by the invention can effectively enhance the filtering efficiency on the premise of high efficiency and low resistance, and PM after meeting water 2.5 The filtering performance is stable.

Description

Composite air filter material capable of being washed repeatedly and preparation method thereof
The technical field is as follows:
the invention relates to the field of industrial textiles, in particular to a polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazolate framework melt-blown electrostatic spinning composite air filter material and a preparation method thereof, which are suitable for the air filtration industry.
Background art:
in recent years, serious air pollution problems have seriously threatened human health, especially in the air, fine Particulate Matter (PM) having an aerodynamic diameter of 2.5 μm or less 2.5 ). At present, PM is removed efficiently 2.5 The air fiber filter material mainly comprises a common non-woven fiber filter material, an ultrafine glass fiber filter material, an electrostatic spinning fiber filter material and an electret fiber filter material. The electret fiber filter material is widely researched and applied by people because the electret fiber filter material can effectively improve the filtering efficiency and does not influence the pressure drop value. However, although the filtering performance of the electret fiber filtering material is obviously improved compared with the traditional filtering material, the depth of the charge injection trap has certain limitation, so that the charges residing on the filtering material can be rapidly dissipated after being wetted. Thus, preparation of post-water PM 2.5 The high-efficiency low-resistance air filter material with stable filtering performance becomes an important breakthrough.
The diameter of the fiber of the filter material prepared by the electrostatic spinning process is generally between 100 and 500nm, and the fiber has larger specific surface area, surface energy and smaller pore diameter, but the compact fiber net structure can increase the filter pressure drop value and is not favorable for the comfort of the filter material when being worn. The fiber filter material prepared by adopting the melt-blown process has the advantages of high porosity, long filtering channel, low pressure drop, high yield, high strength and the like, but the fiber diameter is mostly in micron-scale, the pore diameter among the fibers is larger, and the PM is difficult to realize 2.5 The high-efficiency filtration is realized. Therefore, the performance advantages of the melt-blowing process and the electrostatic spinning process can be effectively exerted by combining the melt-blowing process and the electrostatic spinning process.
The zeolite imidazolate framework (ZIF-8) is a novel porous hybrid material, has the characteristics of high porosity, high hydrothermal resistance, high specific surface area, highly adjustable pore diameter and the like, and has great application potential in the fields of gas storage and separation, catalysis, electronics, sensors and medicines. At present, four methods are mainly used for effectively loading ZIF-8 on a supporting material, namely a mechanical method, an adhesive method, an electrostatic spinning method and an in-situ growth method. The in-situ growth method can effectively maintain the original structure and activity of the ZIF-8 and has advantages in exerting the performance of the ZIF-8. However, according to the existing research, the air filter material prepared by the conventional in-situ growth method can effectively improve the filtering efficiency but greatly increase the pressure drop value, and the reactions are finished in an autoclave and are not suitable for mass production.
In order to overcome the defects of the conventional air filter material and the conventional ZIF-8 in-situ growth method, the invention adopts a melt-blown electrospinning composite process and a ZIF-8 in-situ growth method which has mild preparation conditions and is suitable for mass production, so that the prepared PM has good stability and long service life 2.5 The air filter material has the advantages of high efficiency, low resistance and stable filtering performance after meeting water.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problem of providing a polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazolate framework melt-blown electrostatic spinning composite air filter material and a preparation method thereof.
The technical scheme for solving the technical problems of the method is to provide a preparation method of a polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazolate framework melt-blown electrospun composite air filter material, which is characterized by comprising the following steps:
step 1, mixing polypropylene and polycarbonate polymer in a ratio of 99 percent to 1-93 percent to 7 percent to prepare bi-component polypropylene/polycarbonate master batch;
step 2, drying the polypropylene/polycarbonate master batch obtained in the step 1 by using an air-blast drying oven at the drying temperature of 50-80 ℃ for 3-6 h; adopting a single-screw extruder, fully melting the master batch obtained in the step (1) under the action of high temperature and shearing force of a screw, sequentially passing through a pipeline, a metering pump and a die head, and then blowing the polymer from the die head to a collecting net curtain with an air suction device under the action of high-speed hot air in a hot air pipe; finally, winding the filter material on a cloth roller to prepare a polypropylene-polycarbonate melt-blown filter material (PPC); wherein the hot air temperature is 200-.
Step 3, dissolving zinc nitrate hexahydrate in anhydrous methanol, and then soaking the PPC filter material prepared in the step 2 in a zinc nitrate hexahydrate-methanol mixed solution to ensure that the filter material is completely contacted with the solution; dissolving 2-methylimidazole in anhydrous methanol, and pouring into a zinc nitrate hexahydrate methanol solution soaked with a PPC filter material; after full reaction, taking out the PPC filter material, washing with fresh anhydrous methanol, and drying to obtain a polypropylene-polycarbonate/zeolite imidazole ester framework melt-blown filter material (PPC/ZIF-8); wherein zinc nitrate hexahydrate, 2-methylimidazole and anhydrous methanol are prepared into a ZIF-8 precursor solution in a molar ratio of 1: 50-105: 800-9100; the drying temperature is 50-80 ℃, and the drying time is 3-6 h.
Step 4, respectively dissolving zinc nitrate hexahydrate and 2-methylimidazole in anhydrous methanol at the temperature of 20-25 ℃; slowly pouring the mixed solution containing 2-methylimidazole/anhydrous methanol into a methanol solution containing zinc nitrate hexahydrate; after standing, centrifuging the product, washing with fresh methanol, and drying to obtain zeolite imidazole ester framework (ZIF-8) nanocrystal; wherein, the standing time is 12-24 h; the centrifugal speed is 3500-8000 rpm;
step 5, carrying out ultrasonic dispersion on the ZIF-8 nanocrystal prepared in the step 4 and an N, N-dimethylformamide solvent, adding polyvinylidene fluoride, heating and stirring in a water bath to prepare an electrostatic spinning solution; fixing the PPC/ZIF-8 melt-blown filter material prepared in the step 3 on a winding roller of electrostatic spinning equipment; injecting the electrostatic spinning solution into a double-injector, and spinning the spinning solution on the surface of the filter material under the action of a positive high-voltage power supply to prepare the polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazole ester framework melt-blown electrostatic spinning composite filter material (PPC/PVDF/ZIF-8). Preparing the zeolite imidazole ester framework, polyvinylidene fluoride and N, N-dimethylformamide into electrostatic spinning solution according to the mass ratio of 0-0.8: 0-7.2: 0-92.
The technical scheme for solving the technical problem of the material is to provide the composite air filter material which can be repeatedly washed by water according to the method. It is characterized in that the filter material can filter PM in air with high efficiency and low resistance 2.5 And PM after meeting water 2.5 The filtering performance is stable.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention combines melt-blown technology and electrostatic spinning technology, and the prepared PPC melt-blown filter material effectively exerts the performance advantages of the melt-blown filter material and the electrostatic spinning technology, and achieves the primary aim of high efficiency and low resistance.
(2) The invention adopts polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazole ester as a framework structure to prepare the composite filter material, thereby obviously improving PM after meeting water 2.5 And (4) filtering and stabilizing performance.
(3) The method adopted by the invention has the advantages of simple process and mild preparation conditions, and is suitable for batch production.
Drawings
FIG. 1 is a schematic illustration of the preparation of a re-washable composite air filter material (PPC/ZIF-8) according to one embodiment of the present invention;
FIG. 2 is a schematic representation of a zeolitic imidazolate framework (ZIF-8) nanocrystal preparation of one embodiment of the present invention;
FIG. 3 is a graph of the fiber surface topography of (a) a polypropylene-polycarbonate melt blown filter material and (b) a polypropylene-polycarbonate/zeolitic imidazolate framework melt blown filter material in accordance with one embodiment of the present invention;
FIG. 4 shows the polypropylene-polycarbonate/zeolitic imidazolate framework meltblown filter media at different zeolitic imidazolate framework precursor concentrations of an embodiment of the present invention (a) filtration efficiency at different PM particle sizes, (b) PM 2.5 And PM 5 Filtration efficiency, (c) pressure drop and (d) PM 2.5 Filtering the quality factor graph;
FIG. 5 is a graph of (a) filtration efficiency, pressure drop, and (d) quality factor for a PPC/ZIF8-9 meltblown filter of one embodiment of the present invention after a filter-wash-dry cycle;
FIG. 6 is a graph of (a) fiber surface topography, (b) average fiber diameter, and (c) fiber distribution of a re-washable composite filter of an embodiment of the present invention;
FIG. 7 shows an embodiment of the invention of (a) PM of a polypropylene-polycarbonate/polyvinylidene fluoride/zeolitic imidazolate framework meltblown electrospun composite filter 2.5 Filtration efficiency, (b) pressure drop, and (c) quality factor graph;
fig. 8 is (a) a graph of filtration efficiency, pressure drop, and (b) a graph of quality factor for a PPC/PVDF/ZIF8-3 meltblown electrospun composite filter after a filtration-washing-drying cycle in accordance with an embodiment of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention aims to solve the technical problem of inventing a preparation method of a composite air filter material capable of being repeatedly washed by water.
Step 1, respectively drying polypropylene and polycarbonate polymer with a mass ratio of 97: 3 in a forced air drying oven, wherein the melt index and the melting point of the polypropylene are respectively 35g/10min and 169 ℃, and the melt index and the melting point of the polycarbonate are respectively 14.4g/10min and 250 ℃; after drying, uniformly mixing the polycarbonate and the polypropylene, and granulating by a single-screw granulator to prepare bi-component polypropylene/polycarbonate master batches;
step 2, drying the polypropylene/polycarbonate master batch prepared in the step 1 by using an air-blast drying oven; after the single-screw melt-blowing equipment reaches the preset temperature and is stable, pouring polypropylene/polycarbonate master batches into a feeding cylinder of the melt-blowing equipment, enabling the molten polymer to sequentially pass through a pipeline, a metering pump and a die head, and blowing the polymer onto a collecting net curtain with an air suction device from the die head under the action of high-speed hot air in a hot air pipe; and finally, winding the filter material on a cloth roller to prepare the polypropylene-polycarbonate melt-blown filter material (PPC).
Step 3, continuously stirring the zinc nitrate hexahydrate for 30-60min at the stirring speed of 400-600r/min so as to completely dissolve the zinc nitrate hexahydrate in the anhydrous methanol; pouring the mixed solution of zinc nitrate hexahydrate and anhydrous methanol into a culture dish, completely soaking the PPC melt-blown filter material prepared in the step 2 in the mixed solution for 12-24 hours to ensure that the melt-blown filter material is completely contacted with the solution so as to firmly load Zn on the surface of the fiber 2+ Ions; 2-methylimidazole is stirred for 30-60min at the stirring speed of 400-600r/min to be completely dissolved in the anhydrous methanol; slowly pouring the 2-methylimidazole/anhydrous methanol mixed solution into a culture dish containing the PPC melt-blown filter material, fully reacting with a methanol solution containing zinc nitrate hexahydrate for 1-2 hours, and gradually changing the mixed solution into a milky shape along with the increase of the reaction time; taking the PPC melt-blown filter material after reaction out of the culture dish, and washing the filter material for 8 to 10 times by using fresh anhydrous methanol to remove unreacted substances; finally, drying the polypropylene-polycarbonate melt-blown filter material with the ZIF-8 nanocrystal grown therein at room temperature to prepare the polypropylene-polycarbonate/zeolite imidazolate framework composite melt-blown filter material (PPC/ZIF-8)). Wherein, zinc nitrate hexahydrate, 2-methylimidazole and absolute methanol are prepared into ZIF-8 precursor with the concentration of 0-15: 0-105: 0-9100 molar ratio;
step 4, continuously stirring the zinc nitrate hexahydrate and the 2-methylimidazole at the stirring speed of 400-600r/min at room temperature for 30-60min so as to fully dissolve the zinc nitrate hexahydrate and the 2-methylimidazole in the anhydrous methanol; slowly pouring the mixed solution containing 2-methylimidazole/anhydrous methanol into the methanol solution containing zinc nitrate hexahydrate, and stirring at the stirring speed of 400-600r/min for 3-4h, wherein all operations are carried out at room temperature; after standing for 12-24h, centrifuging the product, washing the product for 3-5 times by using fresh methanol, and then drying the product in a vacuum drying oven to prepare a zeolite imidazole ester framework (ZIF-8) nanocrystal; wherein the molar ratio of the zinc nitrate hexahydrate, the 2-methylimidazole and the anhydrous methanol is 9.08: 72.35: 6292.13.
Step 5, ultrasonically dispersing the zeolite imidazole ester framework prepared in the step 4 and an N, N-dimethylformamide solvent for 2-3 hours; adding polyvinylidene fluoride into a zeolite imidazole ester framework/N, N-dimethylformamide solvent, heating and stirring in a water bath kettle for 6-8 hours to prepare an electrostatic spinning solution; fixing the PPC/ZIF-8 melt-blown filter material prepared in the step 3 on a winding roller of electrostatic spinning equipment; and injecting the spinning solution into a double injector, and loading the spinning solution on the surface of a melt-blown filter material containing ZIF-8 nanocrystals at a positive high-voltage power supply of 23-25kV, a moving distance of 155-160cm and an injection pump speed of 0.8-0-9mm/l to prepare the polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazole ester framework melt-blown electrostatic spinning composite filter material (PPC/PVDF/ZIF-8). Wherein the zeolite imidazole ester framework, the polyvinylidene fluoride and the N, N-dimethylformamide are prepared into the electrostatic spinning solution according to the mass ratio of 0-0.8: 0-7.2: 0-92.

Claims (6)

1. A preparation method of a composite air filter material capable of being repeatedly washed by water is characterized by comprising the following steps:
step 1, mixing polypropylene and polycarbonate polymer according to a mass ratio of 99:1-93:7 to prepare bi-component polypropylene/polycarbonate master batch;
step 2, drying the polypropylene/polycarbonate master batch obtained in the step 1 by using an air-blast drying oven at the drying temperature of 50-80 ℃ for 3-6 h; adopting a single-screw extruder, fully melting the master batch obtained in the step (1) under the action of high temperature and shearing force of a screw, sequentially passing through a pipeline, a metering pump and a die head, and then blowing the polymer from the die head to a collecting net curtain with an air suction device under the action of high-speed hot air in a hot air pipe; finally, winding the mixture on a cloth roller to prepare a polypropylene-polycarbonate melt-blown filter material; wherein the hot air temperature is 200-;
step 3, dissolving zinc nitrate hexahydrate in anhydrous methanol, and then soaking the polypropylene-polycarbonate melt-blown filter material prepared in the step 2 in a mixed solution of zinc nitrate hexahydrate and methanol to ensure that the filter material is completely contacted with the solution; dissolving 2-methylimidazole in anhydrous methanol, and pouring into a zinc nitrate hexahydrate-methanol solution in which a polypropylene-polycarbonate melt-blown filter material is soaked; after full reaction, taking out the polypropylene-polycarbonate melt-blown filter material, washing with fresh anhydrous methanol, and drying to prepare the polypropylene-polycarbonate/zeolite imidazole ester framework melt-blown filter material; wherein, zinc nitrate hexahydrate, 2-methylimidazole and absolute methanol are mixed in a weight ratio of 1: 50-105: preparing a zeolite imidazole ester framework precursor solution at a molar ratio of 700-; drying at 50-80 deg.C for 3-6 h;
step 4, respectively dissolving zinc nitrate hexahydrate and 2-methylimidazole in anhydrous methanol at the temperature of 20-25 ℃; slowly pouring the 2-methylimidazole/anhydrous methanol mixed solution into a methanol solution containing zinc nitrate hexahydrate; after standing, centrifuging the product, washing with fresh methanol, and drying to obtain zeolite imidazole ester skeleton nanocrystal; wherein, the standing time is 12-24 h; the centrifugal speed is 3500-8000 rpm;
step 5, ultrasonically dispersing the zeolite imidazole ester framework nano crystal prepared in the step 4 and an N, N-dimethylformamide solvent, adding polyvinylidene fluoride, heating and stirring in a water bath to prepare electrostatic spinning solution; fixing the polypropylene-polycarbonate/zeolite imidazolate framework melt-blown filter material prepared in the step 3 on a winding drum of electrostatic spinning equipment; and (3) injecting the electrostatic spinning solution into a double-injector, and spinning the spinning solution on the surface of the filter material under the action of a positive high-voltage power supply to prepare the polypropylene-polycarbonate/polyvinylidene fluoride/zeolite imidazole ester framework melt-blown electrostatic spinning composite filter material.
2. The preparation method of the repeatedly washable composite air filter material as recited in claim 1, wherein in step 3, the materials of the zeolite imidazolate framework in-situ growth precursor solution are respectively zinc nitrate hexahydrate, 2-methylimidazole and anhydrous methanol, and the reaction is carried out at normal temperature; the stirring speed and the stirring time of the zinc nitrate hexahydrate or the 2-methylimidazole and the anhydrous methanol are respectively 400-600r/min and 30-60 min.
3. The method for preparing the repeatedly washable composite air filter material as claimed in claim 1, wherein in the step 3, the time for completely soaking the melt-blown filter material in the zinc nitrate hexahydrate/anhydrous methanol mixed solution is 12-24 hours; slowly pouring the 2-methylimidazole/anhydrous methanol mixed solution into a culture dish containing the polypropylene-polycarbonate melt-blown filter material, and reacting with a methanol solution containing zinc nitrate hexahydrate for 1-2 hours; washing the polypropylene-polycarbonate melt-blown filter material after reaction with fresh anhydrous methanol for 8-10 times, and then drying at room temperature; wherein, zinc nitrate hexahydrate, 2-methylimidazole and absolute methanol are mixed in a weight ratio of 1: 50-105: preparing a precursor solution of the zeolite imidazole ester framework in a molar ratio of 800-9100.
4. The method for preparing the repeatedly washable composite air filter material as claimed in claim 1, wherein in step 4, the stirring speed and the stirring time of zinc nitrate hexahydrate or 2-methylimidazole with anhydrous methanol are 400-600r/min and 30-60min respectively; stirring the mixed solution of 2-methylimidazole/anhydrous methanol and zinc nitrate hexahydrate/anhydrous methanol at the stirring speed of 400-600r/min for 3-4h, and standing for 12-24 h; centrifuging the product and washing with fresh methanol for 3-5 times; wherein the molar ratio of zinc nitrate hexahydrate, 2-methylimidazole and anhydrous methanol is 1: 8:690.
5. The preparation method of the repeatedly washable composite air filter material as claimed in claim 1, wherein in step 5, the zeolite imidazolate framework nanocrystals and the N, N-dimethylformamide solvent are ultrasonically dispersed for 2-3h, and polyvinylidene fluoride is added and then heated and stirred in a water bath for 6-8h to prepare an electrostatic spinning solution; the spinning solution amount in the double injector is 3 ml, the voltage of a high-voltage power supply and the moving distance are 23-25kV and 155-160cm respectively; the electrostatic spinning solution is prepared from the zeolite imidazole ester framework nanocrystal, polyvinylidene fluoride and N, N-dimethylformamide according to the mass ratio of 0-0.8: 0-7.2: 0-92, wherein the mass of the zeolite imidazole ester framework nanocrystal, the polyvinylidene fluoride and the N, N-dimethylformamide are not 0.
6. A repeatedly washable composite air filter material obtained according to any one of claims 1 to 5, which is characterized in that the filter material can effectively enhance the filtering efficiency on the premise of high efficiency and low resistance, and PM after meeting water 2.5 The filtering performance is stable, and the filtering performance is still in a higher level even after 5 times of filtering, washing and drying.
CN202010503971.3A 2020-06-05 2020-06-05 Composite air filter material capable of being washed repeatedly and preparation method thereof Active CN111589229B (en)

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