CN113244787B - Preparation method of efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane - Google Patents

Preparation method of efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane Download PDF

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CN113244787B
CN113244787B CN202110438181.6A CN202110438181A CN113244787B CN 113244787 B CN113244787 B CN 113244787B CN 202110438181 A CN202110438181 A CN 202110438181A CN 113244787 B CN113244787 B CN 113244787B
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polyimide
zno
zif
membrane
nanofiber
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CN113244787A (en
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张兴双
李钰
张延青
孙佩佩
王猛
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Shandong Aobo Environmental Protection Technology Co ltd
New Material Institute of Shandong Academy of Sciences
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Shandong Aobo Environmental Protection Technology Co ltd
New Material Institute of Shandong Academy of Sciences
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/58Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • B01D71/62Polycondensates having nitrogen-containing heterocyclic rings in the main chain
    • B01D71/64Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
    • 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
    • B01D46/543Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/008Supramolecular polymers

Abstract

The invention discloses a preparation method of a high-efficiency high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane, wherein the air filter membrane is a composite nanofiber prepared by semi-embedding a ZIF-8 nanoparticle layer wrapping 20-50 nm on the surface of a polyimide nanofiber with the diameter of 50-400 nm and prepared by electrostatic spinning. The invention belongs to the technical field of polyimide nanofiber membranes, and has the advantages that: the ZIF-8 nano particles uniformly distributed on the surface of the fiber can be obtained by activating and regrowing the seeds, the grown ZIF-8 is semi-embedded, the appearance is controllable, the repeatability is good, and meanwhile, the semi-embedded structure can enhance the mechanical property and the PM adsorption property of the nano fiber, thereby being beneficial to the application of subsequent air filtration; the preparation method adopted by the invention is simple, strong in operability, low in cost, environment-friendly and high in PM filtering efficiency, can be used as a method for large-scale batch production of the polyimide/ZIF-8 nanofiber membrane, is easy for industrial production, and has strong universality.

Description

Preparation method of efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane
Technical Field
The invention relates to the technical field of new materials, in particular to a preparation method of a high-efficiency high-temperature-resistant polyimide/ZIF-8 composite fiber air filtering membrane.
Background
The harmful effects of airborne very fine Particulate Matter (PM) are of increasing concern because PM can stay in the atmosphere for long periods of time, and has a long propagation distance, can carry a large number of toxic and harmful substances and microorganisms such as bacteria and viruses, can enter the lungs through the respiratory tract, and is absorbed and ultimately colonized in the human body. The hazards posed by PM are numerous, for example, PM less than 10um in diameter (PM)10) Can pass through human tissues to cause lung diseases; PM (PM) with diameter less than 2.5um2.5) Can cause the increase of the deposition of arterial plaque, cause vascular inflammation and atherosclerosis, and further cause cardiovascular problems such as heart attack and the like; PM (PM) with diameter less than 0.3um0.3) Because of smaller particles, the particle size is stronger than that of PM in penetrability, air retention time and spreading extent2.5. And PM0.3Not only can reach deep part of lung, but also can enter olfactory region in brain via nasal cavity, and the harm degree to health is far greater than PM2.5. The main sources of PM are pollution sources such as combustion of fossil fuel and high-temperature gas discharged by transportation vehicles such as factories and automobiles, so that effective high-temperature resistant filtering PM is produced0.3The filtering membrane has important significance for the healthy and living environment of people.
Conventional filter materials are directed to very fine particulate matter PM0.3、PM2.5The removal effect of (a) is not significant. Porous membranes and fibrous membranes are two common filtration membranes at present, and the latter is a more effective strategy due to the advantages of energy conservation, low cost, various material types and the like. The nanofiber membrane has the advantages of large specific surface area, high aperture ratio, interconnected porous structures, flexible functions and the like, so that the nanofiber membrane can be widely applied as an air filtering membrane. As a novel method for preparing micro/nano fibers, electrostatic spinning is the most general and effective technology for preparing continuous nano fibers with controllable form, structure and functional components. Has wide application prospect in the aspect of air filtration.
Polyimide (PI) is a polymer of imide monomers, having good chemical resistance, excellent mechanical properties, and excellent thermal stability at high temperatures. Polyimide (PI) as a high performance material has good comprehensive properties, especially mechanical properties and thermal stability, and also has a high dipole moment (6.2D), and can provide a strong PM adsorption site. Since the application of polyimide as an air filtration membrane, in order to improve the filtration efficiency, related workers have developed a plurality of methods for preparing composite nanofiber membranes by modifying polyimide. In order to improve the filtration efficiency of the polyimide nanofiber membrane, a ZIF-8 organic metal framework is introduced, so that the polyimide nanofiber membrane has the characteristics of MOFs (surface area is large, structure and pore diversity and functional adjustability), and good thermal stability and chemical stability, which are rarely found in other MOF materials. In addition, the introduction of ZIF-8 can also influence the appearance of the fiber to form superfine fiber, which is beneficial to intercepting smaller fine particle pollutants.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to prepare a mixed precursor solution by taking polyamic acid as a precursor solution and adding ZnO seeds into the precursor solution, prepare a nanofiber membrane by an electrostatic spinning technology, perform thermal imidization, and grow ZIF-8 on the surface of polyimide fiber by an activation and in-situ growth two-step method.
In order to achieve the purpose, in the technical scheme of the invention, nano ZnO is adopted as a seed, and before the polyamic acid solution is prepared by a two-step method, the nano ZnO is uniformly dispersed by ultrasonic. And (2) electrospinning and thermal imidizing the synthesized precursor solution to obtain a polyimide-ZnO nanofiber membrane with uniformly distributed ZnO nanoparticles, soaking the PI-ZnO nanofiber membrane in a dimethyl imidazole solution by using a dipping method to activate ZnO seeds, and growing the seeds on the surface and in the fibers into ZIF-8 by using a hydrothermal method to finally obtain the polyimide/ZIF-8 nanofiber membrane.
The technical scheme provided by the invention is as follows: the preparation method of the efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filtering membrane is characterized in that the air filtering membrane is prepared by electrostatic spinning and has a diameter of 50-400 nmThe composite nanofiber membrane formed by wrapping a 20-50 nm ZIF-8 nanoparticle layer in a semi-embedded mode has a specific surface area of 0.5-1.02 m2(iv) g, tensile strength of 0.334-0.454N/m; the preparation method of the polyimide/ZIF-8 composite fiber air filtering membrane comprises the following steps:
s1: synthesis of polyamic acid/ZnO precursor solution
Firstly, adopting a two-step method to synthesize polyamide acid; weighing m1g Dimethylacetamide (DMAc) was placed in a flask and m was added2g, nano ZnO, and ultrasonically distributing the nano ZnO uniformly; weighing m3Adding 4,4 '-diaminodiphenyl ether (ODA) into a three-neck flask, fixing the flask in which the 4,4' -diaminodiphenyl ether (ODA) and the nano ZnO are dissolved, starting a mechanical (magnetic) stirrer, and mechanically stirring for 15 minutes to completely dissolve monomers; then m is weighed4And adding pyromellitic dianhydride (PMDA) (molar ratio ODA: PMDA is 1: 1-1.02) into the flask in 8-10 times, wherein the adding amount is reduced along with the increase of the times, and the time interval is about 20 minutes after the PMDA which needs to be added is completely dissolved. After the addition was complete, the mixture was rapidly stirred mechanically for one hour to allow the monomers to react fully.
S2: preparing a polyamic acid/ZnO nanofiber membrane by an electrostatic spinning method; carrying out program-controlled heating thermal imidization treatment on the untreated nanofiber membrane, heating the untreated nanofiber membrane from room temperature to 300-350 ℃, and keeping the temperature for 1-2 hours to obtain a polyimide/ZnO nanofiber membrane;
s3: and (3) performing soaking activation and hydrothermal regrowth on nano ZnO seeds of the polyimide/ZnO nanofiber membrane to obtain the semi-embedded polyimide/ZIF-8 nanofiber membrane.
Further, the diameter of the nano ZnO in S1 is 20-50 nm, and the concentration of the monomer nano ZnO in the polyamic acid precursor solution is 5-10 wt%; the pyromellitic dianhydride (PMDA) monomer is added 8-10 times after 4,4' -diaminodiphenyl ether (ODA) monomer is completely dissolved in DMAc.
Further, the electrostatic spinning process in S2 is as follows: collecting the nano-fibers by using a cylindrical roller receiver with the diameter of 12cm and the length of 30cm, and placing a metal grid receiving substrate on the receiver; adjusting parameters: the rotating speed is 100 r/min-200 r/min, the distance from the spinning nozzle to the receiving surface of the roller is 18 cm-22 cm, the voltage of a high-voltage power supply is 18 kV-22 kV, the material pushing speed is 0.0010 mm/s-0.0015 mm/s, the spinning nozzle transversely swings from the center position, the swing amplitude is 30cm, and the swing speed is 0.5 cm/min.
Further, the electrospun polyamic acid/ZnO is removed from the metal grid, and the temperature rise program of the muffle furnace is set as follows: and heating the polyimide/ZnO nano-fiber film from room temperature to 300-350 ℃ at a speed of 3 ℃/min, preserving heat for 1-2 hours, and naturally cooling the polyimide/ZnO nano-fiber film to room temperature to obtain the polyimide/ZnO nano-fiber film.
Further, in S3, the seed activation solution is a dimethyl imidazole solution with a concentration of 0.5mol/L, and the regrowth solution is a methanol solution of zinc nitrate hexahydrate, dimethyl imidazole and sodium acetate.
Further, ZnO seed activation: preparing 50ml of 0.5mol/L dimethyl imidazole aqueous solution, putting the annealed polyimide/ZnO nanofiber membrane into the solution, heating and standing for 2 hours at 50 ℃, and activating ZnO seeds; regrowing ZnO seeds: 30ml of regrowth solution was prepared with 2mmol of Zn (NO)3)2·6H2Dissolving O, 3mmol of dimethyl imidazole and 2mmol of HCOONa in 30ml of methanol solution, magnetically stirring until a clear and transparent solution is formed, transferring the activated polyimide/ZnO nanofiber membrane and the regrowth solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 2 hours at 100 ℃.
Compared with the prior art, the invention has the advantages that: (1) according to the invention, nano ZnO seeds are introduced into the polyimide nano fibers by an electrostatic spinning method, and the ZIF-8 uniformly distributed on the surfaces of the fibers can be obtained through subsequent activation and regrowth. The ZIF-8 grown is semi-embedded, the appearance is controllable, and the repeatability is good. Meanwhile, the semi-embedded structure can enhance the mechanical property of the nano fiber and the adsorption property to PM, and is beneficial to the application of the nano fiber filtering membrane in air filtration.
(2) The preparation method adopted by the invention is simple, strong in operability, low in cost, environment-friendly, high in finished product filtering efficiency, strong in universality, easy for industrial production, and capable of producing the polyimide/ZIF-8 nanofiber filtering membrane in large scale and in batch.
(3) The preparation method can be further popularized to effective regulation and synthesis of the electrospun nanofiber/MOF composite nanomaterial, and the type of the MOF material on the surface of the nanofiber can be regulated by changing the seed layer. The appearance of the nanofiber can be adjusted by adjusting electrospinning parameters (voltage, material pushing speed, temperature, humidity, receiver rotating speed and the like) in the electrospinning process. The MOF material modified polyimide nanofiber membranes with different diameter distributions can be adjusted and grown by adjusting the hydrothermal time and the solution concentration. The principle of filtering PM by using the polyimide/ZIF-8 composite nanofiber filtering membrane disclosed by the invention is as follows: according to known filtration theory, the mechanism of PM particle capture by nanofibers is six: sieving, inertial impaction, interception, diffusion, electrostatic attraction, and gravitational effects. For PM particles of different diameters, one or more of the trapping mechanisms play a major role, while the other mechanisms work synergistically.
The invention prepares the high-temperature resistant polyimide/ZIF-8 composite fiber membrane by an electrostatic spinning method, and the filter membrane is used for treating PM in high-temperature gas0.3The highest filtering efficiency can reach 100 percent. The resistance pressure drop at an air flow rate of 14L/min was only 97.1Pa, and a filtration efficiency of 99.9% or more was maintained. The composite nanofiber membrane has the advantages of simple preparation method, high filtration efficiency, low resistance pressure drop, good mechanical property, high temperature resistance and the like, is an ideal air filtration material with good application prospect, can be widely applied to filtration of high-temperature pollution source gas, and is beneficial to effectively adsorbing PM particles from the source.
Drawings
FIG. 1 is a schematic diagram of a nanofiber membrane prepared by an electrospinning technique (wherein: 1: an injector; 2: nanofibers; 3: a metal mesh receiving substrate; 4: a high voltage power supply).
FIG. 2 is a scanning electron micrograph of a polyimide/ZnO composite nanofiber film prepared according to example 1 at 30000 times magnification.
FIG. 3 is a scanning electron micrograph of an activated polyimide/ZnO composite nanofiber film prepared according to example 2 at 30000 magnification.
FIG. 4 is a scanning electron micrograph of a polyimide/ZIF-8 composite nanofiber membrane prepared according to example 3, at 20000 times magnification.
FIG. 5 is a graph showing the results of thermal stability tests of polyimide/ZIF-8 nanocomposite fiber membranes prepared according to examples of the present invention.
FIG. 6 is a polyimide/ZIF-8 nanocomposite fiber membrane vs PM made according to an example of the invention0.3The result of the filtration performance test of (1).
FIG. 7 is a polyimide/ZIF-8 nanocomposite fiber membrane vs PM made according to an example of the invention0.5The result of the filtration performance test of (1).
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings.
Example 1 (Synthesis of polyimide/ZnO composite nanofiber film)
Referring to FIG. 2, 36.99g of dimethylacetamide (DMAc) was weighed into a flask, 0.70455g of nano ZnO was added, and the mixture was sonicated for 30min to make the distribution uniform. 3.3375g of 4,4' -diaminodiphenyl ether (ODA) and 3.708g of pyromellitic dianhydride (PMDA) were weighed in a monomer molar ratio of 1:1 to 1.02(ODA: PMDA), respectively, and the ODA was placed in a three-necked flask. The flask in which the ODA and the nano ZnO were dissolved was fixed, and a mechanical stirrer was started to mechanically stir for 15 minutes to completely dissolve the monomers. The PMDA is added into the flask for 8-10 times, the adding amount is reduced along with the increase of the times, and the time interval is about 20 minutes after the added PMDA is completely dissolved. And (3) after the addition is finished, quickly and mechanically stirring for one hour to ensure that the monomers fully react to generate 16 wt% of polyamic acid/ZnO precursor solution, wherein the doped ZnO accounts for 10 wt%.
Setting the discharge parameters as follows: the voltage is 20KV, the rotating speed is 100r/min, the temperature is 30 ℃, the humidity is 65%, the material returning speed is 0.0010mm/s, the distance between the needle point and the grid receiving base is 20cm, the needle point swings at the center position, the swing amplitude is 30cm, the swing speed is 0.5mm/s, the electrospinning time is 60min, and after a sample is taken, the sample is dried in an oven at 120 ℃ for 12 h. Placing the mixture into a muffle furnace at a temperature of 3 ℃/min, and heating the mixture from room temperature to 350 ℃. Keeping the temperature at 350 ℃ for 1h, and then naturally cooling to room temperature to obtain the polyimide/ZnO nanofiber membrane.
Example 2 (activated polyimide/ZnO composite nanofiber film)
Referring to FIG. 3, 50ml of 0.5mol/L aqueous solution of dimethylimidazole was prepared, and 2.0222g of dimethylimidazole was dissolved in 50ml of water and mechanically stirred for 30 minutes to distribute the solution uniformly. And (3) putting the annealed film into the solution, and heating and standing for 2h at 50 ℃ to activate the ZnO seeds.
Example 3 (preparation of polyimide/ZIF-8 composite nanofiber Membrane)
Referring to fig. 4, the activated polyimide/ZnO composite nanofiber membrane is cleaned by removing methanol. 0.595g of Zn (NO) are weighed out3)2·6H2O, 0.7389g of dimethylimidazole, 0.408g of HCOONa were dissolved in 30ml of methanol. Mechanically stirring for 30min, transferring to a reaction kettle, and putting the activated membrane into the reaction kettle. The oven is set to 100 ℃ for hydrothermal growth for 2 h. After completion of the hydrothermal treatment, the mixture was washed 3 times with deionized water and dried at 50 ℃ overnight.
PM Filter Performance test
Referring to fig. 5, the main basis for evaluating the filtration performance of the filtration air membrane is to consider the pressure loss of the gas before and after slippage on the fiber surface in addition to the filtration efficiency. The overall filtration performance of an air filtration membrane is therefore usually evaluated by a quality factor Q [ -ln (1- η)/Δ P ], where η is the filtration efficiency and Δ P is the pressure drop. Compared with the traditional filter material, the electrospun nanofiber membrane has higher filtering efficiency and lower resistance pressure drop, so that the electrospun nanofiber membrane has higher quality factor Q, namely the polyimide/ZIF-8 nanofiber has better filtering performance.
The PM filtering membranes prepared in examples 1-3 were subjected to a filtration efficiency test. And (3) placing the prepared polyimide/ZIF-8 composite nanofiber membrane in an improved G506 automatic filter material tester to test the membrane. The instrument emits particles with the diameter of 0.3-10um through an aerosol generator (capable of emitting oily and salt particles), and a high-pressure fan ensures that airflow stably passes through a test filter membrane to simulate pollutant particles in the air. Pollutant particles before and after air flow filtration are tested through a particle counter to calculate the filtration efficiency, and meanwhile, the equipment can test the pressure drop and the air permeability of an instrument to be tested.
Thermal stability test
Referring to fig. 6 and 7, thermogravimetric analysis of the polyimide film and the polyimide/ZIF-8 nanofiber film shows that the introduction of ZIF-8 significantly improves the thermodynamic stability.
The polyimide/ZIF-8 nanofiber composite membrane prepared by the seed method has high temperature resistance, high efficiency filtration efficiency and low resistance pressure drop. The invention has lower production cost and wide application, and can adsorb PM particles from a high-temperature gas emission source to realize the air purification effect.
The present invention and the embodiments thereof have been described above, and the description is not restrictive, and the embodiments shown in the detailed description are only a part of the embodiments of the present invention, not all embodiments, and the actual configuration is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (4)

1. The preparation method of the high-efficiency high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane is characterized by comprising the following steps of: the air filter membrane is a composite nanofiber membrane prepared by electrostatic spinning and formed by wrapping a 20-50 nm ZIF-8 nanoparticle layer on the surface of a polyimide nanofiber with the diameter of 50-400 nm in a semi-embedded mode, and the specific surface area of the composite nanofiber membrane is 0.5-1.02 m2(iv) g, tensile strength of 0.334-0.454N/m; the preparation method of the polyimide/ZIF-8 composite fiber air filtering membrane comprises the following steps:
s1: synthesizing polyamic acid/ZnO precursor solution; uniformly dispersing nano ZnO in a dimethylacetamide (DMAc) solvent by ultrasonic, and then adding 4,4' -diaminodiphenyl ether (ODA): preparing a polyamic acid/ZnO solution with the mass percent of 16-20 wt% according to the molar ratio of pyromellitic dianhydride (PMDA) to 1: 1-1.02;
s2: preparing a polyamic acid/ZnO nanofiber membrane by an electrostatic spinning method; carrying out program-controlled heating thermal imidization treatment on the untreated nanofiber membrane, heating the untreated nanofiber membrane from room temperature to 300-350 ℃, and keeping the temperature for 1-2 hours to obtain a polyimide/ZnO nanofiber membrane;
s3: performing soaking activation and hydrothermal regrowth on nano ZnO seeds of the polyimide/ZnO nanofiber membrane to obtain a semi-embedded polyimide/ZIF-8 nanofiber membrane;
ZnO seed activation: preparing 50ml of 0.5mol/L dimethyl imidazole aqueous solution, putting the annealed polyimide/ZnO nanofiber membrane into the solution, heating and standing for 2 hours at 50 ℃, and activating ZnO seeds;
regrowing ZnO seeds: 30ml of regrowth solution was prepared with 2mmol of Zn (NO)3)2·6H2Dissolving O, 3mmol of dimethyl imidazole and 2mmol of HCOONa in 30ml of methanol solution, magnetically stirring until a clear and transparent solution is formed, transferring the activated polyimide/ZnO nanofiber membrane and the regrowth solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 2 hours at 100 ℃.
2. The preparation method of the high-efficiency high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filtration membrane as claimed in claim 1, wherein the preparation method comprises the following steps: the diameter of the nano ZnO in S1 is 20-50 nm, and the concentration of the monomer nano ZnO in the polyamic acid precursor solution is 5-10 wt%; the pyromellitic dianhydride (PMDA) monomer is added for 8-10 times after 4,4' -diaminodiphenyl ether (ODA) monomer is completely dissolved in dimethylacetamide (DMAc).
3. The preparation method of the efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filtration membrane as claimed in claim 1, wherein the electrospinning process in S2 is as follows: collecting the nano-fibers by using a cylindrical roller receiver with the diameter of 12cm and the length of 30cm, and placing a metal grid receiving substrate on the receiver; adjusting parameters: the rotating speed is 100 r/min-200 r/min, the distance from the spinning nozzle to the receiving surface of the roller is 18 cm-22 cm, the voltage of a high-voltage power supply is 18 kV-22 kV, the material pushing speed is 0.0010 mm/s-0.0015 mm/s, the spinning nozzle transversely swings from the center position, the swing amplitude is 30cm, and the swing speed is 0.5 cm/min.
4. The preparation method of the high-efficiency high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filtration membrane as claimed in claim 3, wherein the preparation method comprises the following steps: and (3) removing the electrospun polyamic acid/ZnO from the metal grid, and setting a muffle furnace temperature-rising program as follows: and heating the polyimide/ZnO nano-fiber film from room temperature to 300-350 ℃ at a speed of 3 ℃/min, preserving heat for 1-2 hours, and naturally cooling the polyimide/ZnO nano-fiber film to room temperature to obtain the polyimide/ZnO nano-fiber film.
CN202110438181.6A 2021-04-22 2021-04-22 Preparation method of efficient high-temperature-resistant polyimide/ZIF-8 composite nanofiber air filter membrane Active CN113244787B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521678A (en) * 2016-11-01 2017-03-22 华南协同创新研究院 Preparation method of polymer fiber-based ZnO nanowire fiber
CN109195700A (en) * 2016-05-31 2019-01-11 Eth苏黎世公司 self-supporting MOF film
CN111653717A (en) * 2020-07-10 2020-09-11 东莞市魔方新能源科技有限公司 Preparation method of composite diaphragm, composite diaphragm and lithium ion battery

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019210159A1 (en) * 2018-04-26 2019-10-31 Texas A&M University In situ fabrication of metal-organic framework films and mixed-matrix membranes

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109195700A (en) * 2016-05-31 2019-01-11 Eth苏黎世公司 self-supporting MOF film
CN106521678A (en) * 2016-11-01 2017-03-22 华南协同创新研究院 Preparation method of polymer fiber-based ZnO nanowire fiber
CN111653717A (en) * 2020-07-10 2020-09-11 东莞市魔方新能源科技有限公司 Preparation method of composite diaphragm, composite diaphragm and lithium ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
静电纺PMDA-ODA制备聚酰亚胺(PI)纤维及表面功能化的研究;曾静;《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》;20170315;第13-14、44-55页 *

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