CN113668093A - Polyimide nano spider-web fiber filtering membrane and preparation method thereof - Google Patents
Polyimide nano spider-web fiber filtering membrane and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/546—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using nano- or microfibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
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- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
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- 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
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Abstract
The invention discloses a polyimide nano-cobweb fiber filtering membrane and a preparation method thereof, belonging to the field of polyimide fiber preparation. Dissolving 4, 4' -diaminodiphenyl ether in a solvent, continuously and slowly adding pyromellitic dianhydride, and then reacting to obtain a polyamic acid precursor solution; adding lithium chloride into the obtained polyamic acid precursor solution, and uniformly mixing to obtain a solution to be spun; spinning the obtained spinning solution into a film to obtain a polyimide fiber film with a spider-web structure; and removing the solvent from the obtained polyimide fiber membrane with the spider-web structure, and then carrying out imidization treatment to obtain the polyimide nano spider-web fiber filtering membrane. The prepared polyimide nano spider-web fiber filtering membrane has a spider-web structure, has high filtering efficiency and high temperature resistance, can filter fine particles and can be recycled for multiple times.
Description
Technical Field
The invention belongs to the field of polyimide fiber preparation, and relates to a polyimide nano-cobweb fiber filtering membrane and a preparation method thereof.
Background
The sources of air pollution are many, including harmful gas, fine liquid drop and solid particulate matter, and along with further advancing of industrialization, air pollution is more and more abusive, seriously harming physical and mental health of human beings at present. The problem of air pollution is one of the important environmental problems to be solved urgently, so that the research and development of the high-efficiency air filtering material have important significance for maintaining human health and environmental sustainable development.
The research of the high-performance filter material with the cobweb structure provides a novel solution for the problems. The traditional filtering material is generally not high in temperature resistance and poor in filtering efficiency, and the problem of high-temperature and high-efficiency filtering is difficult to solve. Polyimide (PI) is one of organic polymer materials with the best comprehensive performance, and the PI fiber has excellent thermal stability due to the special imide ring on the main chain of the PI fiber, namely high strength, corrosion resistance, self-extinguishing and radiation resistance, particularly high conjugated structure and high aromaticity, so that the PI fiber has great advantages in preparing the filter material by taking PI as a raw material. The filtering efficiency of the filtering membrane prepared by polyimide alone is poor, and the problem that how to improve the filtering efficiency of the polyimide filtering membrane is needed to be solved urgently is solved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a polyimide nano-cobweb fiber filtering membrane and a preparation method thereof, which effectively solve the problem of low filtering efficiency under the current high-temperature condition.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a polyimide nano-cobweb fiber filtering membrane, which comprises the following steps: dissolving 4, 4' -diaminodiphenyl ether in a solvent, continuously and slowly adding pyromellitic dianhydride, and then carrying out low-temperature polycondensation reaction to obtain a polyamic acid precursor solution; adding lithium chloride into the obtained polyamic acid precursor solution, and uniformly mixing to obtain a solution to be spun; spinning the obtained spinning solution into a film to obtain a polyimide fiber film with a spider-web structure; and removing the solvent from the obtained polyimide fiber membrane with the spider-web structure, and then carrying out imidization treatment to obtain the polyimide nano spider-web fiber filtering membrane.
Preferably, the reaction charge ratio of the 4, 4' -diaminodiphenyl ether, the pyromellitic dianhydride and the solvent is 10-30 g: 10.5-31.5 g: 100-300 mL.
Preferably, the low-temperature polycondensation reaction parameters of the polyamic acid precursor solution include: reacting for 12-24 h at 0-4 ℃.
Preferably, the reaction charge ratio of the polyamic acid precursor solution to lithium chloride is 10 mL: 0.003 to 0.01 g.
Preferably, the operating parameters for spinning the obtained solution to be spun into a film comprise: and putting the spinning solution into an injector, wherein the voltage is 25-30 kV, and the speed of a propeller is 0.2-0.5 mL/h.
Preferably, the polyimide fiber membrane with the spider-web structure is dried at 60 ℃ for 12-24 hours to remove the solvent.
Preferably, the temperature of the imidization treatment is 25 to 300 ℃.
Preferably, the solvent is N, N-dimethylformamide.
The invention discloses a polyimide nano-cobweb fiber filtering membrane prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of a polyimide nano-cobweb fiber filtering membrane, which is characterized in that multifunctional polyimide with excellent performances in all aspects is prepared by low-temperature polycondensation, the multifunctional polyimide is used as a matrix, lithium chloride is used as an important substance for preparing a nano-cobweb structure, and after electrostatic spinning, the polyimide nano-fiber membrane with the cobweb structure is formed by high-temperature imidization in a tubular furnace.
Further, by controlling the spinning conditions such as applied voltage and advancing speed, the formed spider web area can be made larger and the filtering performance can be made higher.
The invention also discloses a polyimide nano-cobweb fiber filtering membrane prepared by the preparation method, which is prepared from polyimide and lithium chloride as raw materials, has a cobweb structure, has high filtering efficiency and high temperature resistance, and can filter PM2.5Fine particles can be used repeatedly; in the specific embodiment of the present invention, it is found that the filtration efficiency of the polyimide nano-spider web fiber filtration membrane can reach 99% or more.
Drawings
FIG. 1 is an SEM image of a polyimide nanoweb fiber filtration membrane of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention provides a preparation method of a polyimide nano-cobweb fiber filtering membrane with excellent high-temperature high-efficiency filtering performance, which comprises the following specific steps:
(1) dissolving 4, 4' -diaminodiphenyl ether (ODA) 10-30 g in N, N-Dimethylformamide (DMF) 100-300 mL, slowly adding pyromellitic dianhydride (PMDA) 10.5-31.5 g, stirring at 0-4 ℃ for 12-24 h, and carrying out low-temperature polycondensation reaction to obtain a polyamic acid (PAA) precursor solution;
(2) adding 0.003-0.01 g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) 3-10 mL of the spinning solution is placed in an injector, the voltage is 25-30 kV, the speed of a propeller is 0.2-0.5 mL/h, and spinning is carried out to form a film, so as to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at the temperature of 60 ℃ for 12-24 hours to remove redundant solvent;
(5) and (3) carrying out temperature programming imidization on the polyimide fiber membrane with the spider-web structure obtained in the step (4) for 3-4 h at the temperature of 25-300 ℃ in a tubular furnace, and successfully obtaining the high-temperature and high-efficiency filtering polyimide nano spider-web fiber filtering membrane.
The polyimide nano-cobweb fiber filtering membrane prepared by the preparation method has high filtering efficiency, high temperature resistance and certain cycle performance, and related tests show that the filtering efficiency can reach 99.52-99.98%. And has certain cyclicity, particularly, the filtering efficiency can be maintained to be more than 97 percent after the filtering film is used for more than 60 min.
The present invention is described in further detail below with reference to specific examples:
example 1
(1) Dissolving 10g of 4, 4' -diaminodiphenyl ether (ODA) in 100mL of N-N Dimethylformamide (DMF), slowly adding 10.5g of pyromellitic dianhydride (PMDA), and stirring at 4 ℃ for 12h to prepare a polyamic acid (PAA) precursor solution;
(2) adding 0.003g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) putting 4mL of the spinning solution into an injector, wherein the voltage is 28kV, the speed of a propeller is 0.3mL/h, and spinning to form a film to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at 60 ℃ for 24 hours to remove excessive solvent;
(5) imidizing the polyimide fiber membrane with the spider-web structure obtained in the step (4) for 3 hours at 25 ℃ in a tubular furnace to successfully obtain the polyimide nano spider-web fiber filtering membrane with high-temperature and high-efficiency filtration.
The filtration test shows that the filter has excellent filtration performance, the highest filtration efficiency can reach 99.52 percent, and the cycle number can reach 6 times.
Example 2
(1) Dissolving 30g of 4, 4' -diaminodiphenyl ether (ODA) in 300mL of N-N Dimethylformamide (DMF), slowly adding 20g of pyromellitic dianhydride (PMDA), and stirring at 0 ℃ for 24h to prepare a polyamic acid (PAA) precursor solution;
(2) adding 0.01g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) 3mL of the spinning solution to be spun is placed in an injector, the voltage is 30kV, the speed of a propeller is 0.2mL/h, and spinning is carried out to form a film, so as to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at 60 ℃ for 12 hours to remove excessive solvent;
(5) imidizing the polyimide fiber membrane with the spider-web structure obtained in the step (4) for 4 hours at the temperature of 300 ℃ in a tubular furnace to successfully obtain the polyimide nano spider-web fiber filtering membrane with high-temperature and high-efficiency filtration.
The filtration test shows that the filter has excellent filtration performance, the highest filtration efficiency can reach 99.76 percent, and the cycle number can reach 6 times.
Example 3
(1) Dissolving 20g of 4, 4' -diaminodiphenyl ether (ODA) in 150mL of N-N Dimethylformamide (DMF), slowly adding 31.5g of pyromellitic dianhydride (PMDA), and stirring at 1 ℃ for 22h to prepare a polyamic acid (PAA) precursor solution;
(2) adding 0.008g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) putting 8mL of spinning solution into an injector, wherein the voltage is 25kV, the speed of a propeller is 0.4mL/h, and spinning to form a film to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at 60 ℃ for 18 hours to remove excessive solvent;
(5) imidizing the polyimide fibrous membrane with the spider-web structure obtained in the step (4) for 3.5 hours at 50 ℃ in a tubular furnace to successfully obtain the polyimide nano spider-web fibrous filtering membrane with high-temperature and high-efficiency filtration.
The filtration test shows that the filter has excellent filtration performance, the highest filtration efficiency can reach 99.67 percent, and the cycle number can reach 6 times.
Example 4
(1) Dissolving 15g of 4, 4' -diaminodiphenyl ether (ODA) in 200mL of N-N Dimethylformamide (DMF), slowly adding 18g of pyromellitic dianhydride (PMDA), and stirring at 2 ℃ for 18h to prepare a polyamic acid (PAA) precursor solution;
(2) adding 0.005g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) 10mL of the spinning solution to be spun is placed in an injector, the voltage is 28kV, the speed of a propeller is 0.5mL/h, and spinning is carried out to form a film, so as to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at 60 ℃ for 20 hours to remove excessive solvent;
(5) imidizing the polyimide fibrous membrane with the spider-web structure obtained in the step (4) for 3.5h at 100 ℃ in a tubular furnace to successfully obtain the polyimide nano-spider-web fibrous filtering membrane with high-temperature and high-efficiency filtration.
The filtration test shows that the filter has excellent filtration performance, the highest filtration efficiency can reach 99.92 percent, and the cycle number can reach 6 times.
Example 5
(1) Dissolving 25g of 4, 4' -diaminodiphenyl ether (ODA) in 260mL of N-N Dimethylformamide (DMF), slowly adding 24g of pyromellitic dianhydride (PMDA), and stirring at 3 ℃ for 15h to prepare a polyamic acid (PAA) precursor solution;
(2) adding 0.003g of lithium chloride into 10mL of polyamic acid precursor solution, and uniformly mixing to form a solution to be spun;
(3) 6mL of the spinning solution to be spun is placed in an injector, the voltage is 25kV, the speed of a propeller is 0.3mL/h, and spinning is carried out to form a film, so as to prepare the polyimide fiber film with the spider-web structure;
(4) drying the polyimide fiber membrane with the spider-web structure prepared in the step (3) in an oven at 60 ℃ for 15 hours to remove excessive solvent;
(5) imidizing the polyimide fiber membrane with the spider-web structure obtained in the step (4) for 3h at 200 ℃ in a tubular furnace to successfully obtain the polyimide nano spider-web fiber filtering membrane with high-temperature and high-efficiency filtration.
The filtration test shows that the filter has excellent filtration performance, the highest filtration efficiency can reach 99.98 percent, and the cycle number can reach 6 times.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, it can be clearly seen that there is a uniformly distributed spider-web structure between the main fibers, and the structure is dense, so that the specific surface area of the filter fiber membrane is increased, the porosity is increased, and the filter fiber membrane is favorable for further intercepting and capturing impurity particles. This mode of action involves primarily physical contact between the particles of the body and the fibers, and is the most common mode of screening. Therefore, the formation of the spider web structure plays a crucial role in improving the filtration efficiency of the nanofiber filtration membrane.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a polyimide nano-cobweb fiber filtering membrane is characterized by comprising the following steps:
dissolving 4, 4' -diaminodiphenyl ether in a solvent, continuously and slowly adding pyromellitic dianhydride, and then carrying out low-temperature polycondensation reaction to obtain a polyamic acid precursor solution; adding lithium chloride into the obtained polyamic acid precursor solution, and uniformly mixing to obtain a solution to be spun;
spinning the obtained spinning solution into a film to obtain a polyimide fiber film with a spider-web structure; and removing the solvent from the obtained polyimide fiber membrane with the spider-web structure, and then carrying out imidization treatment to obtain the polyimide nano spider-web fiber filtering membrane.
2. The preparation method of the polyimide nano-cobweb fiber filtering membrane according to claim 1, wherein the reaction charge ratio of 4, 4' -diaminodiphenyl ether, pyromellitic dianhydride and solvent is 10-30 g: 10.5-31.5 g: 100-300 mL.
3. The method for preparing a polyimide nano-spider web fiber filtering membrane according to claim 1, wherein the low temperature polycondensation reaction parameters of the polyamic acid precursor solution comprise: reacting for 12-24 h at 0-4 ℃.
4. The preparation method of the polyimide nano-spider web fiber filtering membrane according to claim 1, wherein the reaction charge ratio of the polyamic acid precursor solution to the lithium chloride is 10 mL: 0.003 to 0.01 g.
5. The preparation method of the polyimide nano-cobweb fiber filtering membrane according to claim 1, wherein the operating parameters for spinning the obtained spinning solution to form the membrane comprise: and putting the spinning solution into an injector, wherein the voltage is 25-30 kV, and the speed of a propeller is 0.2-0.5 mL/h.
6. The method for preparing the polyimide nano spider web fiber filtering membrane according to claim 1, wherein the polyimide fiber membrane with the spider web structure is dried at 60 ℃ for 12-24 h.
7. The method for producing a polyimide nano-spider web fiber filtration membrane according to claim 1, wherein the temperature of the imidization treatment is 25 to 300 ℃.
8. The method for preparing a polyimide nano spider web fiber filtering membrane according to claim 1, wherein the solvent is N, N-dimethylformamide.
9. A polyimide nano-spider web fiber filtering membrane prepared by the preparation method of any one of claims 1 to 8.
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140137735A1 (en) * | 2012-11-20 | 2014-05-22 | General Electric Company | Polyimide membranes and method of production |
CN104752665A (en) * | 2015-03-31 | 2015-07-01 | 渤海大学 | Method for preparing polyimide porous nanofiber electrode diaphragm |
CN106984201A (en) * | 2017-05-08 | 2017-07-28 | 河北科技大学 | Nanometer spider web/beading fiber composite air-filtering membrane and preparation method thereof |
CN108365151A (en) * | 2018-01-31 | 2018-08-03 | 青岛蓝科途膜材料有限公司 | A kind of polyimide high temperature-resistant lithium battery diaphragm and preparation method thereof |
CN108894050A (en) * | 2018-05-04 | 2018-11-27 | 河南工程学院 | The preparation method and application of high efficiency filter hollow-fibre membrane non-woven material |
CN111514659A (en) * | 2020-05-04 | 2020-08-11 | 南通大学 | Nano cobweb antibacterial composite air filtering material and preparation method thereof |
CN112516806A (en) * | 2020-10-12 | 2021-03-19 | 宁波方太厨具有限公司 | Preparation method of electrostatic spinning fiber membrane |
CN113005642A (en) * | 2021-03-01 | 2021-06-22 | 南京工业大学 | Preparation method of nano-cobweb fiber membrane |
-
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- 2021-09-10 CN CN202111064449.0A patent/CN113668093B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140137735A1 (en) * | 2012-11-20 | 2014-05-22 | General Electric Company | Polyimide membranes and method of production |
CN104752665A (en) * | 2015-03-31 | 2015-07-01 | 渤海大学 | Method for preparing polyimide porous nanofiber electrode diaphragm |
CN106984201A (en) * | 2017-05-08 | 2017-07-28 | 河北科技大学 | Nanometer spider web/beading fiber composite air-filtering membrane and preparation method thereof |
CN108365151A (en) * | 2018-01-31 | 2018-08-03 | 青岛蓝科途膜材料有限公司 | A kind of polyimide high temperature-resistant lithium battery diaphragm and preparation method thereof |
CN108894050A (en) * | 2018-05-04 | 2018-11-27 | 河南工程学院 | The preparation method and application of high efficiency filter hollow-fibre membrane non-woven material |
CN111514659A (en) * | 2020-05-04 | 2020-08-11 | 南通大学 | Nano cobweb antibacterial composite air filtering material and preparation method thereof |
CN112516806A (en) * | 2020-10-12 | 2021-03-19 | 宁波方太厨具有限公司 | Preparation method of electrostatic spinning fiber membrane |
CN113005642A (en) * | 2021-03-01 | 2021-06-22 | 南京工业大学 | Preparation method of nano-cobweb fiber membrane |
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