CN111691060B - High polymer fiber based on instantaneous pressure-release spinning method, and preparation method and application thereof - Google Patents
High polymer fiber based on instantaneous pressure-release spinning method, and preparation method and application thereof Download PDFInfo
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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
- D04H1/4282—Addition polymers
- D04H1/4291—Olefin series
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- 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
- D01D1/00—Treatment of filament-forming or like material
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- 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
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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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
- 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
- D01F6/90—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 polyamides
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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
- 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
- D01F6/92—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 polyesters
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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
- D04H1/4326—Condensation or reaction polymers
- D04H1/4334—Polyamides
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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
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
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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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/007—Addition polymers
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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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/009—Condensation or reaction polymers
-
- 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
- D04H3/009—Condensation or reaction polymers
- D04H3/011—Polyesters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of high polymer fiber based on an instantaneous pressure-release spinning method, which comprises the steps of conveying a high polymer and a plasticizing auxiliary agent into a supercritical kettle in a metering manner, introducing supercritical carbon dioxide in a stirring state, stirring and stabilizing to form supercritical spinning fluid, carrying out phase separation on the supercritical spinning fluid in an open atmosphere environment instantaneously released by a spinning nozzle to convert the supercritical spinning fluid into carbon dioxide gas, the plasticizing auxiliary agent and a solidified high polymer, and forming the high polymer fiber by the solidified high polymer under the actions of plasticizing auxiliary agent replacement and instantaneous pressure-release differential drafting. The invention also discloses the high polymer fiber prepared by the method and application thereof. The preparation method provided by the invention can obtain higher spinning pressure difference and spinning spraying speed than those obtained by a flash evaporation method, can also avoid the recovery and treatment of an organic solvent, and the fiber diameter of the prepared high polymer fiber is 0.5-5 mu m. The invention belongs to the technical field of preparation of high polymer non-woven fabrics, and is suitable for the field of limited medical protective clothing.
Description
Technical Field
The invention belongs to the technical field of preparation of high polymer non-woven fabrics, and relates to preparation of high polymer fibers, in particular to high polymer fibers based on an instantaneous pressure-release spinning method, and a preparation method and application thereof.
Background
A nonwoven fabric is a fabric formed without the need for a spun woven fabric by simply orienting or randomly arranging the textile staple fibers or filaments to form a web structure, which is then consolidated mechanically, thermally, or chemically. Nonwoven fabrics are novel fibrous articles having a soft, air-permeable and planar structure formed directly from high polymer chips, staple fibers or filaments by various web forming methods and consolidation techniques.
The use of non-woven fabrics is very wide, and the main uses can be roughly divided into: relates to medical and sanitary cloth, home decoration cloth, clothing cloth, industrial cloth, agricultural cloth and the like. The medical sanitary cloth relates to operating gowns, protective clothing, disinfection wrapping cloth, masks, diapers, women sanitary napkins and the like.
The new coronavirus pneumonia epidemic situation outbreak in 2020 spreads to the world and is in a gradually worsening trend, and the outbreak of the epidemic situation makes the demand of the mask and the protective clothing rise sharply. The production of various raw materials for masks and protective clothing, especially nonwoven fabrics, is an important factor that limits the production rate of both. Meanwhile, medical work puts high demands on the barrier property, the steam permeability comfort and the reusability of the mask and the protective clothing.
Researches show that the problems of barrier property, vapor permeability comfort and reusability of the medical protective clothing can be systematically solved by regulating and controlling the fiber fineness of the non-woven fabric. When the diameter of the non-woven fabric reaches submicron size, a nanometer effect can be formed on the solid-gas interface and the solid-liquid interface of the fiber and the outside, and a single-direction wet guide film is formed. Specifically, vapor molecules can be discharged through the fiber membrane, and large-scale substances such as particles, liquid drops and the like can be effectively blocked. Therefore, for high-end medical protective clothing, the development of microfiber non-woven fabrics (UFN) is the core for improving the key performances of medical protective clothing, such as filtration barrier property, comfort and the like, and is also the focus of the research field of fiber and non-woven materials at home and abroad at present. At present, it is difficult to construct a high barrier microfiber aggregate by a method for industrially producing a nonwoven fabric, such as a spunbond method, a sea-island or orange-petal type composite spinning, a melt-blowing method, and the like. The UFN is constructed by methods such as electrostatic spinning, solution jet spinning and the like, the product needs to be processed in multiple steps or compounded with other materials, the mechanical property is poor, and the production efficiency is low. Centrifugal spinning and super-drawing methods can also be used for constructing UFN, but are still in the laboratory exploration stage, and industrial conversion is difficult to realize in a short period of time. Therefore, the UFN one-step forming method which is simple, convenient and easy to implement, wide in application range and excellent in product performance is established, and the method has important significance for the industrial promotion of UFN and the active response to the epidemic situation of the novel coronavirus and the important safety and sanitation events.
The flash evaporation method is a method for preparing non-woven fabric by dissolving polyethylene in an organic solvent (such as toluene, xylene and the like) at high temperature and high pressure and adopting a solution spinning dry process, and the technical process of DuPont company is strictly kept secret. Only a few colleges and enterprises have conducted exploratory studies. For example, the Mark a, mcHugh group of john hopkins university in the united states has made a certain study on the supercritical solubility and phase equilibrium rule of polymers in solvent systems such as alkanes and halogenated hydrocarbons, etc., and summarizes the thermodynamic rule of the phase change of polymer solutions; the Kim group of korean institute of science and technology prepared L-lactide filaments with a fiber diameter of 0.32-0.47mm by flash evaporation spinning. In addition, the flash evaporation method has the problems of large solvent pollution and controllable fiber appearance in the production process of the non-woven fabric.
Aiming at the high-end requirement of the medical protective clothing capable of being repeatedly used, if a safety protective material with high barrier, high wear resistance and high moisture permeability can be manufactured, powerful technical support can be provided for the comfort and the repeated use of the medical mask and the protective clothing.
Disclosure of Invention
The invention aims to provide a preparation method of high polymer fiber based on an instantaneous pressure-release spinning method, which adopts a mode of preparing supercritical high polymer fluid to prepare the high polymer fiber and solves the problems of large solvent pollution and controllability of fiber morphology in the production process of non-woven fabrics by a flash evaporation method;
the second object of the present invention is to provide a high polymer fiber prepared based on the above preparation method;
the invention also aims to provide application of the high polymer fiber to preparation of a high-barrier, high-wear-resistance and high-moisture-permeability safety protection material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high polymer fiber based on an instantaneous pressure-release spinning method comprises the following steps:
1. conveying the high polymer and the plasticizing auxiliary agent into a supercritical kettle, introducing supercritical carbon dioxide under a stirring state, and forming supercritical spinning fluid after stabilization;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released through a spinning nozzle at the speed of 200-300 m/s, the supercritical spinning fluid is quickly subjected to phase separation from a supercritical state under the high-power pressure difference of 100-200 to be converted into carbon dioxide gas, a plasticizing auxiliary agent and a solidified high polymer, and in the process, the solidified high polymer forms high polymer fibers under the actions of plasticizing auxiliary agent displacement and instantaneous pressure-release differential pressure drafting.
As a limitation: the mass ratio of the high polymer to the plasticizing auxiliary agent is 70-95.
As a second limitation: the high polymer is polyolefin, polyester or polyamide;
the polyolefin is one of polypropylene and polyethylene;
the polyester is one of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, polylactic acid, polyhydroxyalkanoate, polyglycolic acid and polybutylene succinate;
the polyamide is one of polyamide 6, polyamide 66, polyamide 56 and polyamide 1010.
As a third limitation: the plasticizing auxiliary agent is one or two of dioxane, cyclohexane, dichloromethane, isopropanol and ethylene glycol monomethyl ether.
As a fourth limitation: the temperature environment of the supercritical kettle is 110-190% o C。
As a fifth limitation: the pressure of the supercritical fluid is 8-18 MPa.
The invention also provides a high polymer fiber which is prepared by the preparation method of the high polymer fiber based on the instantaneous pressure-release spinning method.
As a limitation: the diameter of the high polymer fiber is 0.5-5 μm.
The invention further provides an application of the high polymer fiber, and the high polymer fiber is used for preparing the high polymer non-woven fabric.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the technical progress that:
(1) The instantaneous pressure-release spinning method is based on the fact that the supercritical fluid of the high polymer is used as spinning solution, the spinning pressure difference and the spinning spraying speed which are higher than those obtained by a flash evaporation method can be obtained, and the recovery and treatment of an organic solvent can be effectively reduced or even avoided;
(2) The supercritical spinning fluid is separated in the spraying process, and the fibers of the generated high polymer non-woven fabric have higher vapor permeability and barrier property and good wear resistance, and are particularly suitable for preparing limited medical protective clothing;
(3) The fiber diameter of the high polymer non-woven fabric reaches 0.5-5 mu m;
(4) The preparation method of the invention does not cause solvent pollution in the production process, and the prepared fiber has controllable shape and micro-structure.
The invention is suitable for the technical field of high polymer superfine non-woven fabrics and is used for preparing non-woven fabrics with the particle size of 0.5-5 mu m.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic view of the structure of an apparatus according to embodiments 1 to 10 of the present invention;
FIG. 2 is a scanning electron microscope image of the polyethylene micro-nano fiber of example 1 of the present invention;
fig. 3 is a real object diagram of the polyethylene micro-nano fiber nonwoven fabric in embodiment 1 of the invention.
In the figure: 1. supercritical gas input port, 2, raw material port, 3, supercritical kettle, 4, air amplifier, 5, first collecting roller, 6, godet roller, 7 and second collecting roller.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.
Example 1 preparation method of polyethylene micro-nano fiber based on instantaneous pressure-release spinning method
This example was carried out in the following sequence of steps:
1. as shown in FIG. 1, 90kg of high-density polyethylene and 10kg of cyclohexane, which is a plasticizing auxiliary, were measured and transferred from a raw material port 2 to a port 150 o C, introducing supercritical carbon dioxide from a supercritical gas inlet 1 to 18MPa in a supercritical kettle 3 under a stirring state, and stabilizing for 2h to form supercritical spinning fluid;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released at a speed of 200m/s through a circular nozzle, the supercritical spinning fluid is rapidly subjected to phase separation from a supercritical state under 150 times of pressure difference manufactured by an air amplifier 4 and is converted into carbon dioxide gas, cyclohexane gas and solidified high-density polyethylene, and in the process, the solidified high-density polyethylene forms polyethylene micro-nano fibers under the action of plasticizing auxiliary agent displacement and instantaneous pressure release external force drafting.
As shown in fig. 2, which is a scanning electron microscope image of the polyethylene micro-nano fiber prepared in this embodiment, it can be seen that the polyethylene micro-nano fiber prepared in this embodiment is circular, the diameter thereof is about 0.8 to 3 μm, and the prepared fiber has a controllable morphology and fine structure.
In this embodiment, the high-density polyethylene may be replaced by high-density polypropylene, and the polypropylene micro-nano fiber is finally prepared.
Example 2 preparation method of polyamide 6 micro-nano fiber based on instantaneous pressure-release spinning method
This example was carried out in the following sequence of steps:
1. as shown in FIG. 1, 70kg of polyamide 6 chips, 15kg as a plasticizing adjuvant and 15kg of methylene chloride were measured and transferred from a raw material port 2 to a container 130 o C, introducing supercritical carbon dioxide from a supercritical gas inlet 1 to 12MPa in a supercritical kettle 3 under a stirring state, and stabilizing for 3h to form supercritical spinning fluid;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released at a speed of 250m/s through a circular nozzle, the supercritical spinning fluid is rapidly subjected to phase separation from a supercritical state under a high-power pressure difference of 180 degrees manufactured by an air amplifier 4 and is converted into carbon dioxide gas, isopropanol gas, dichloromethane gas and solidified polyamide 6, and in the process, the solidified polyamide 6 forms polyamide 6 micro-nano fibers under the action of plasticizing auxiliary agent replacement and instantaneous pressure-release external force drafting.
Through detection, the polyamide 6 micro-nano fiber prepared by the embodiment has a circular structure, and the diameter is about 0.5-2 μm.
Example 3 preparation method of polylactic acid micro-nano fiber based on instantaneous pressure-release spinning method
This example was carried out in the following sequence of steps:
1. as shown in FIG. 1, 95kg of polylactic acid chips and 5kg of a plasticizer-assistant dioxane were measured and transferred from a raw material port 2 to a discharge port 110 o C, introducing supercritical carbon dioxide from a supercritical gas inlet 1 to 8MPa in a supercritical kettle 3 under a stirring state, and stabilizing for 2h to form supercritical spinning fluid;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released at a speed of 200m/s through a circular nozzle, the supercritical spinning fluid is rapidly subjected to phase separation from a supercritical state under a high pressure difference of 100 manufactured by an air amplifier 4 to be converted into carbon dioxide gas, dioxane gas and solidified polylactic acid, and in the process, the solidified polylactic acid forms polylactic acid micro-nano fibers under the action of plasticizing auxiliary agent replacement and instantaneous pressure release external force drafting.
Through detection, the polylactic acid micro-nano fiber prepared by the embodiment has a circular structure, and the diameter is about 0.5-3 μm.
Example 4 preparation method of polyethylene terephthalate micro-nano fiber based on instantaneous pressure-release spinning method
This example was carried out in the following sequence of steps:
1. as shown in FIG. 1, 85kg of polyethylene terephthalate chips and 15kg of a plasticizing auxiliary agent ethylene glycol monomethyl ether were measured and transferred from a raw material port 2 to 190 o C, introducing supercritical carbon dioxide from a supercritical gas inlet 1 to 12MPa in a supercritical kettle 3 under a stirring state, and stabilizing for 3h to form supercritical spinning fluid;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released at a speed of 300m/s through a circular nozzle, the supercritical spinning fluid is rapidly subjected to phase separation from a supercritical state under a high-power pressure difference of 200 produced by an air amplifier 4 and is converted into carbon dioxide gas, ethylene glycol monomethyl ether gas and solidified polyethylene terephthalate, and in the process, the solidified polyethylene terephthalate forms polyethylene terephthalate micro-nano fibers under the action of plasticizing auxiliary agent displacement and instantaneous pressure-release external force drafting.
Through detection, the polyethylene terephthalate micro-nano fiber prepared by the embodiment has a circular structure, and the diameter is about 1-5 μm.
Example 5 preparation method of polybutylene succinate micro-nano fiber based on instantaneous pressure-release spinning method
This example was carried out in the following sequence of steps:
1. as shown in FIG. 1, 85kg of polybutylene succinate chips and 15kg of a plasticizing auxiliary methylene chloride were measured and transferred from a raw material port 2 to a feed port 130 o C, introducing supercritical carbon dioxide from a supercritical gas inlet 1 to 10MPa in a supercritical kettle 3 under a stirring state, and stabilizing for 2h to form supercritical spinning fluid;
2. in an open atmosphere environment where supercritical spinning fluid is instantaneously released at a speed of 200m/s through a circular nozzle, the supercritical spinning fluid is rapidly subjected to phase separation from a supercritical state under a high-power pressure difference of 130 produced by an air amplifier 4 to be converted into carbon dioxide gas, dichloromethane gas and solidified poly (butylene succinate), and in the process, the solidified poly (butylene succinate) forms poly (butylene succinate) micro-nano fibers under the action of plasticizing auxiliary agent replacement and instantaneous pressure-release external force drafting.
Through detection, the poly (butylene succinate) micro-nano fiber prepared by the embodiment has a circular structure, and the diameter is about 1-5 μm.
In examples 1-5, only five polymers are used as raw materials, and the polymers used in actual production can be replaced by polytrimethylene terephthalate, polybutylene terephthalate, polyhydroxyalkanoates, polyglycolic acid, polyamide 66, polyamide 56, and polyamide 1010, and finally corresponding polymer micro-nano fibers are prepared.
Similarly, the plasticizing adjuvant used can be replaced by isopropanol or a composite adjuvant consisting of any two of dioxane, cyclohexane, dichloromethane, isopropanol and ethylene glycol monomethyl ether.
The embodiment provides an application of the polyethylene micro-nano fiber prepared in the embodiment 1. As shown in fig. 1, the polyethylene micro-nano fiber can be used for obtaining a high-density polyethylene non-woven fabric through electrostatic fiber opening and hot rolling, in the preparation process, the polyethylene micro-nano fiber forms the high-density polyethylene non-woven fabric on a conveyor belt driven by a first collecting roller 5, and is further sorted and collected under the driving of a godet roller 6 and a second collecting roller 7.
FIG. 3 shows a non-woven fabric of high density polyethylene prepared in this example. Tests show that the average water permeability of the high-density polyethylene non-woven fabric is 19.5 kPa, the synthetic blood permeation and penetration resistance reaches 4 grades, and the moisture permeability of a finished product reaches 9170 g/(m) 2 *d)。
Embodiment 7 application of polyamide 6 micro-nano fiber
The embodiment provides an application of the polyamide 6 micro-nano fiber prepared in the embodiment 2. As shown in fig. 1, the polyamide 6 micro-nano fiber can be used for obtaining a polyamide 6 non-woven fabric through electrostatic fiber opening and hot rolling, in the preparation process, the polyamide 6 micro-nano fiber forms a polyamide 6 non-woven fabric on a conveyor belt driven by a first collecting roller 5, and is further arranged and collected under the driving of a godet roller 6 and a second collecting roller 7.
Tests show that the polyamide 6 non-woven fabric has the average water permeability resistance of 12.5kPa, the synthetic blood permeation and penetration resistance of 3 grades, and the moisture permeability of a finished product reaches 10240 g/(m) 2 *d)。
Embodiment 8 application of polylactic acid micro-nano fiber
The embodiment provides an application of the polylactic acid micro-nano fiber prepared in the embodiment 3. As shown in fig. 1, the polylactic acid micro-nano fiber can be used for obtaining a polylactic acid non-woven fabric through electrostatic fiber opening and hot rolling, in the preparation process, the polylactic acid micro-nano fiber forms the polylactic acid non-woven fabric on a conveyor belt driven by a first collecting roller 5, and is further sorted and collected under the drive of a godet roller 6 and a second collecting roller 7.
Tests show that the polylactic acid non-woven fabric has the average water permeability resistance of 13.5kPa, the synthetic blood permeation and penetration resistance of 3 grades, and the moisture permeability of a finished product reaches 9150 g/(m) 2 *d)。
Embodiment 9 application of polyethylene terephthalate micro-nano fiber
The embodiment provides an application of the polyethylene terephthalate micro-nano fiber prepared in the embodiment 3. As shown in fig. 1, the polyethylene terephthalate micro-nano fiber can be used for obtaining a polyethylene terephthalate non-woven fabric through electrostatic fiber opening and hot rolling, in the preparation process, the polyethylene terephthalate micro-nano fiber forms a polyethylene terephthalate non-woven fabric on a conveyor belt driven by a first collecting roller 5, and is further sorted and collected under the driving of a godet roller 6 and a second collecting roller 7.
Tests show that the water permeability resistance of the polyethylene terephthalate non-woven fabric is 14.1kPa on average, the synthetic blood permeation and penetration resistance reaches 3 grades, and the moisture permeability of a finished product reaches 10250 g/(m) 2 *d)。
Embodiment 10 application of poly (butylene succinate) micro-nano fibers
The embodiment provides an application of the polybutylene succinate micro-nano fiber prepared in the embodiment 3. As shown in fig. 1, the olybuthylenesuccinate micro-nano fiber can be used for obtaining a poly buthylenesuccinate non-woven fabric through electrostatic fiber opening and hot rolling, in the preparation process, the poly buthylenesuccinate micro-nano fiber forms the poly buthylenesuccinate non-woven fabric on a conveyor belt driven by a first collecting roller 5, and is further sorted and collected under the driving of a godet roller 6 and a second collecting roller 7.
Tests prove that the average water permeability resistance of the poly (butylene succinate) non-woven fabric is 16.3kPa, the synthetic blood permeation and penetration resistance reaches 3 grades, and the moisture permeability of a finished product reaches 11130 g/(m) 2 *d)。
The nonwovens prepared in examples 6-10 can be used to prepare limited-use protective garments.
Claims (6)
1. A preparation method of high polymer fiber based on an instantaneous pressure-release spinning method is characterized by comprising the following steps in sequence:
1. conveying the high polymer and the plasticizing auxiliary agent into a supercritical kettle, introducing supercritical carbon dioxide under a stirring state, and forming supercritical spinning fluid after stabilization;
2. the supercritical spinning fluid is instantaneously released into an open atmosphere environment at the speed of 200-300 m/s through a spinning nozzle, the supercritical spinning fluid is quickly subjected to phase separation from a supercritical state under the high-power pressure difference of 100-200 manufactured by an air amplifier and is converted into carbon dioxide gas, a plasticizing auxiliary agent and a solidified high polymer, and in the process, the solidified high polymer forms a high polymer fiber which is in a circular structure and has the diameter of 0.5-5 mu m under the actions of plasticizing auxiliary agent displacement and instantaneous pressure-release differential drafting;
the average water permeability resistance of the high polymer fiber non-woven fabric is 12.5-19.5 kPa, the penetration resistance of the synthetic blood reaches 3-4 grades, and the moisture permeability of the finished product reaches 9170-11130 g/(m) 2 *d)；
The temperature environment of the supercritical kettle is 110-190 ℃;
the high polymer is polyolefin, polyester or polyamide;
the polyolefin is one of polypropylene and polyethylene;
the polyester is one of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, polylactic acid, polyhydroxyalkanoate, polyglycolic acid and polybutylene succinate;
the polyamide is one of polyamide 6, polyamide 66, polyamide 56 and polyamide 1010.
2. The method for preparing a high polymer fiber based on an instant pressure-release spinning method according to claim 1, wherein: the mass ratio of the high polymer to the plasticizing auxiliary agent is 70-95.
3. The method for preparing a high polymer fiber based on the instant pressure-release spinning method according to claim 1 or 2, wherein: the plasticizing auxiliary agent is one or two of dioxane, cyclohexane, dichloromethane, isopropanol and ethylene glycol monomethyl ether.
4. The method for preparing a high polymer fiber based on the instant pressure-release spinning method according to claim 1 or 2, wherein: the pressure of the supercritical spinning fluid is 8-18 MPa.
5. A high polymer fiber characterized by: the polymer fiber is prepared by the method for preparing the polymer fiber based on the instant pressure-release spinning method according to any one of claims 1 to 4.
6. A use of the polymer fiber according to claim 5, wherein: the high polymer fiber is used for preparing a safety protection material with high barrier property, high wear resistance and high moisture permeability.
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| CN112477328A (en) * | 2020-11-24 | 2021-03-12 | 东华大学 | Protective article fabric with double-layer structure and preparation method and application thereof |
| CN114150439A (en) * | 2021-11-29 | 2022-03-08 | 厦门当盛新材料有限公司 | Drawing device of flash spinning tow net and flash spinning equipment |
| CN114892288B (en) * | 2022-04-28 | 2023-02-28 | 上海迅江科技有限公司 | Enhanced flash evaporation/electrostatic spinning composite spinning equipment |
| CN115323628B (en) * | 2022-09-20 | 2024-02-27 | 厦门当盛新材料有限公司 | Antistatic flash-spun composite non-woven fabric and preparation method thereof |
| CN116103771A (en) * | 2023-03-07 | 2023-05-12 | 东华大学 | Continuous supercritical fluid spinning method |
| CN116005282A (en) * | 2023-03-07 | 2023-04-25 | 东华大学 | Uniform and continuous micro-nanofiber supercritical spinning method |
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