CN111850824A - Preparation method of submicron composite film - Google Patents

Preparation method of submicron composite film Download PDF

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Publication number
CN111850824A
CN111850824A CN202010761114.3A CN202010761114A CN111850824A CN 111850824 A CN111850824 A CN 111850824A CN 202010761114 A CN202010761114 A CN 202010761114A CN 111850824 A CN111850824 A CN 111850824A
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CN
China
Prior art keywords
composite film
submicron
proper amount
solution
preparing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202010761114.3A
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Chinese (zh)
Inventor
周年荣
何潇
张林山
谭向宇
黄星
李月梅
闫永梅
杨莉
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Electric Power Research Institute of Yunnan Power Grid Co Ltd
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Electric Power Research Institute of Yunnan Power Grid Co Ltd
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Application filed by Electric Power Research Institute of Yunnan Power Grid Co Ltd filed Critical Electric Power Research Institute of Yunnan Power Grid Co Ltd
Priority to CN202010761114.3A priority Critical patent/CN111850824A/en
Publication of CN111850824A publication Critical patent/CN111850824A/en
Withdrawn legal-status Critical Current

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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/42Non-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
    • D04H1/4382Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/94Monocomponent 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
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-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
    • D04H1/72Non-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
    • D04H1/728Non-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

Abstract

The invention discloses a preparation method of a submicron composite film, which comprises the steps of firstly mixing a proper amount of N, N-dimethylformamide and N-methylpyrrolidone, adding a proper amount of polyetherimide solution while stirring, adding a proper amount of silicon dioxide nano particles after uniformly stirring, and then obtaining the composite film by adopting an electrostatic spinning mechanism after uniformly stirring. The method has simple preparation process and lower cost of raw materials, and the prepared composite membrane has the diameter of nanometer scale and controllable bulk density; the filter has high porosity, can effectively filter micro-and nano-scale impurities, and improves the filtering precision and the filtering efficiency; has good thermal stability, chemical stability and hydrolytic stability. The paint has super-hydrophobicity, self-cleaning property and oil-water separation property, prolongs the service life and reduces the maintenance frequency; has higher charge storage capacity, can continuously display the stationary polarity and improves the filtration efficiency of small particles.

Description

Preparation method of submicron composite film
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a preparation method of a submicron composite film.
Background
In the electrical field, insulating oil is widely used, but the problem of filtering and regenerating the insulating oil still is one of the technical problems in the industry. A large amount of nano-scale particles and acidic colloid are dissolved in the used insulating oil, and the conventional filtering method cannot filter fine particles with the particle diameter due to large gaps and uncontrollable stacking density of the conventional filtering membrane, so that the process of recovering and regenerating the insulating oil is complex and troublesome, and the insulating oil is wasted. The fiber membrane technology is undoubtedly a relatively energy-saving and cost-effective approach to enable efficient and low-cost separation of insulating oil, and it is important to invent a novel fiber membrane with good heat resistance, chemical stability, hydrolytic stability, and which must also have good charge retention, controllable bulk density, and high porosity.
Disclosure of Invention
The invention aims to overcome the defects of large gaps and uncontrollable stacking density of the existing fiber membrane and provide a preparation method of a submicron composite membrane.
The specific scheme is as follows:
the preparation method of the submicron composite membrane is characterized by comprising the following steps:
s1, adding a proper amount of N, N-dimethylformamide and N-methylpyrrolidone into a polyetherimide solution, and uniformly mixing to form a mixed solution A;
s2, adding a proper amount of silicon dioxide nano particles into the mixed solution A, and stirring for more than 2-4 hours to obtain a mixed solution B;
s3, simulating the mixed solution B by using an electrostatic spinning machine to obtain a submicron composite film;
preferably, in step S1, the mass fraction of the N, N-dimethylformamide and N-methylpyrrolidone is 1%, and the mass fraction of the polyetherimide solution is 20%.
Preferably, the mass fraction of the silica nanoparticles in step S2 is 2%.
Preferably, the electrospinning device in step S3 has a spinning voltage of 25kV, a take-up distance of 8-12cm, a solution feed rate of 1mL/h, and a rotation speed of the take-up drum of 45-55 rpm.
Preferably, the composite membrane prepared in step S3 is dried in a vacuum oven for 2-4h to remove the residual solvent.
Preferably, in step S1, the N, N-dimethylformamide and N-methylpyrrolidone are mixed and then placed on a magnetic stirrer, and then the polyetherimide solution is added while stirring and stirred uniformly.
Has the advantages that: the preparation method of the submicron composite film has the advantages of simple preparation process, low cost of raw materials, nano-scale diameter of the prepared composite film and controllable bulk density; the filter has high porosity, can effectively filter micro-and nano-scale impurities, and improves the filtering precision and the filtering efficiency; has good thermal stability, chemical stability and hydrolytic stability. The paint has super-hydrophobicity, self-cleaning property and oil-water separation property, prolongs the service life and reduces the maintenance frequency; has higher charge storage capacity, can continuously display the stationary polarity and improves the filtration efficiency of small particles.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 shows a field emission electron microscope observing PEI-SiO prepared by the invention2And (5) a surface topography of the composite film.
Detailed Description
The invention is explained in more detail below with reference to the examples and the figures:
example (b): a preparation method of a submicron composite film comprises the following steps:
s1, firstly, mixing a proper amount of N, N-dimethylformamide and N-methylpyrrolidone, then placing the mixture on a magnetic stirrer, adding a polyetherimide solution while stirring, and uniformly stirring to form a mixed solution A, wherein the mass fraction of the N, N-dimethylformamide and the N-methylpyrrolidone in the mixed solution A is 1%, and the mass fraction of the polyetherimide solution is 20%;
s2, adding a proper amount of silicon dioxide nano particles into the mixed solution A, and stirring for more than 2-4 hours to obtain a mixed solution B, wherein the mass fraction of the silicon dioxide nano particles in the mixed solution B is 2%. (ii) a
S3, imitating the mixed solution B by using an electrostatic spinning machine to obtain a submicron composite membrane, wherein the spinning voltage of the electrostatic spinning machine is 25kV, the receiving distance is 8-12cm, the solution supply speed is 1mL/h, the rotating speed of a receiving roller is 45-55rpm, and then putting the prepared product into a vacuum box with the temperature of 22-26 ℃ for drying for 2-4h to remove the residual solvent.
As shown in figure 2, the diameter of the submicron composite membrane prepared by the method is in a nanoscale, the submicron composite membrane has high porosity, micro-scale and nano-scale impurities can be effectively filtered, and the filtering precision and the filtering efficiency are improved; has good thermal stability, chemical stability and hydrolytic stability; the paint has super-hydrophobicity, self-cleaning property and oil-water separation property, prolongs the service life and reduces the maintenance frequency; has higher charge storage capacity, can continuously display the stationary polarity and improves the filtration efficiency of small particles.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.

Claims (6)

1. A preparation method of a submicron composite film is characterized by comprising the following steps:
s1, adding a proper amount of N, N-dimethylformamide and N-methylpyrrolidone into a polyetherimide solution, and uniformly mixing to form a mixed solution A;
s2, adding a proper amount of silicon dioxide nano particles into the mixed solution A, and stirring for more than 2-4 hours to obtain a mixed solution B;
and S3, imitating the mixed solution B by using an electrostatic spinning machine to obtain a submicron composite film.
2. The method of preparing a submicron composite film according to claim 1, wherein: in step S1, the mass fraction of the N, N-dimethylformamide and N-methylpyrrolidone is 1%, and the mass fraction of the polyetherimide solution is 20%.
3. The method of preparing a submicron composite film according to claim 1 or 2, characterized in that: the mass fraction of the silica nanoparticles in step S2 was 2%.
4. A method for preparing a sub-micron composite membrane according to claim 3, wherein: in step S3, the electrostatic spinning machine has a spinning voltage of 25kV, a receiving distance of 8-12cm, a solution supply speed of 1mL/h, and a receiving drum rotation speed of 45-55 rpm.
5. The method of preparing a submicron composite film according to claim 1, wherein: the composite membrane prepared in the step S3 is dried in a vacuum oven for 2-4h to remove the residual solvent.
6. The method of preparing a submicron composite film according to claim 1, wherein: in the step S1, the N, N-dimethylformamide and N-methylpyrrolidone are mixed and then placed on a magnetic stirrer, and then the polyetherimide solution is added while stirring and stirred uniformly.
CN202010761114.3A 2020-07-31 2020-07-31 Preparation method of submicron composite film Withdrawn CN111850824A (en)

Priority Applications (1)

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CN202010761114.3A CN111850824A (en) 2020-07-31 2020-07-31 Preparation method of submicron composite film

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CN202010761114.3A CN111850824A (en) 2020-07-31 2020-07-31 Preparation method of submicron composite film

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CN111850824A true CN111850824A (en) 2020-10-30

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130078882A1 (en) * 2011-09-27 2013-03-28 Samsung Electro-Mechanics Co., Ltd. Porous sheet and method for manufacturing the porous sheet
CN104911814A (en) * 2015-06-24 2015-09-16 哈尔滨理工大学 Preparation method of high-heatproof polymer nanometer composite fiber film
CN106757483A (en) * 2016-11-14 2017-05-31 安徽名杰净化科技有限公司 Standby electret PEI boehmite composite fibre filtering material of a kind of electro-spinning and preparation method thereof
CN107761250A (en) * 2017-10-18 2018-03-06 上海恩捷新材料科技股份有限公司 A kind of preparation method of energy storage electrostatic spinning nano perforated membrane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130078882A1 (en) * 2011-09-27 2013-03-28 Samsung Electro-Mechanics Co., Ltd. Porous sheet and method for manufacturing the porous sheet
CN104911814A (en) * 2015-06-24 2015-09-16 哈尔滨理工大学 Preparation method of high-heatproof polymer nanometer composite fiber film
CN106757483A (en) * 2016-11-14 2017-05-31 安徽名杰净化科技有限公司 Standby electret PEI boehmite composite fibre filtering material of a kind of electro-spinning and preparation method thereof
CN107761250A (en) * 2017-10-18 2018-03-06 上海恩捷新材料科技股份有限公司 A kind of preparation method of energy storage electrostatic spinning nano perforated membrane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李小崎: ""驻极聚醚酰亚胺-二氧化硅纳米纤维膜在空气过滤中的应用"", 《中国优秀硕士学位论文全文数据库(电子期刊)工程科技Ⅰ辑》 *

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