CN116219636B - A method for preparing high-strength and high-toughness degradable melt-blown nonwoven material - Google Patents
A method for preparing high-strength and high-toughness degradable melt-blown nonwoven material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 239000004750 melt-blown nonwoven Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims description 19
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 80
- 239000004626 polylactic acid Substances 0.000 claims abstract description 80
- 239000000835 fiber Substances 0.000 claims abstract description 48
- 239000004631 polybutylene succinate Substances 0.000 claims abstract description 32
- 229920002961 polybutylene succinate Polymers 0.000 claims abstract description 32
- -1 polybutylene succinate Polymers 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000010008 shearing Methods 0.000 claims abstract description 5
- 239000000853 adhesive Substances 0.000 claims abstract description 3
- 239000012943 hotmelt Substances 0.000 claims abstract description 3
- 238000000465 moulding Methods 0.000 claims abstract description 3
- 229920001410 Microfiber Polymers 0.000 claims description 10
- 239000003658 microfiber Substances 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000011161 development Methods 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000007664 blowing Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 239000002918 waste heat Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 229920001046 Nanocellulose Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000006855 networking Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—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 by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
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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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/55—Polyesters
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/12—Physical properties biodegradable
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2505/00—Industrial
- D10B2505/04—Filters
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a preparation method of a high-strength high-toughness degradable melt-blown nonwoven material, which comprises the following steps of S1, premixing, S2, melt blending, S3, extruding the prepared polylactic acid/polybutylene succinate premixed slice into a fine-flow melt through a metering pump and a clothes hanger die head, and S3, hot-melt molding, namely, stretching and shearing the melt through high-temperature high-speed air flow to obtain fibers, and collecting the fibers through a self-adhesive synthetic net by a receiving device to obtain the polylactic acid melt-blown nonwoven material with different structures. The preparation method provided by the invention only needs one-time blending, and can realize the improvement of the toughness of the polylactic acid melt-blown nonwoven material without an additional device. In addition, the polylactic acid and the polybutylene succinate are used as raw materials, so that the full-degradable environment-friendly material can be fully degradable, and meets the requirement of sustainable development.
Description
Technical Field
The invention belongs to the technical field of non-woven fabrics, and particularly relates to a preparation method of a high-strength high-toughness degradable melt-blown non-woven material.
Background
The melt blown nonwoven process utilizes high velocity hot air to draw a polymer melt stream extruded through a die orifice, thereby forming microfibers and condensing on a web curtain or drum and bonding to itself to form a nonwoven. The melt-blown nonwoven material prepared by the process has the characteristics of large specific surface area, high porosity, fluffy structure and the like, and is widely applied to the fields of filtration, heat preservation, medical treatment, health and the like. However, the melt-blown nonwoven materials at present are mostly mainly made of polypropylene raw materials, which belong to non-renewable resources, waste is not easy to degrade, and the resources and the environment are burdened. With the continuous enhancement of ecological consciousness and environmental consciousness of people, degradable melt-blown nonwoven materials become research hot spots.
Polylactic acid is a thermoplastic aliphatic polyester and is recognized as a degradable material with the highest potential to replace polypropylene, but polylactic acid melt-blown nonwoven materials have the defects of high brittleness and poor mechanical properties due to high glass transition temperature and slow crystallization rate of polylactic acid, so that the polylactic acid melt-blown nonwoven materials are difficult to produce and apply on a large scale. Various modifications to polylactic acid materials have been made by researchers, and there have been reported the following in order to obtain polylactic acid melt-blown nonwoven fabrics excellent in properties.
Chinese patent (publication No. CN 105088542B) discloses a high-elongation modified polylactic acid SMS composite nonwoven material and a preparation method thereof, and specifically discloses the following technical scheme that 5-30 parts by mass of polyamide elastomer and 70-95 parts by mass of polylactic acid are used as raw materials, and the polylactic acid blending melt-blown nonwoven material is obtained through melt-blowing. The obtained melt-blown nonwoven material has a longitudinal strength of 40-150N/5cm and a longitudinal elongation at break of 60-130%. The material produced by this method has excellent toughness, but the non-degradable properties of polyamide are ignored.
Chinese patent (publication No. CN 113293517B) discloses a polylactic acid elastic superfine fiber nonwoven material, a preparation method and application thereof, and specifically discloses the following technical scheme that 10-20 parts of polyethylene glycol, 10-20 parts of nanocellulose, 20-40 parts of bio-based elastomer and 60-70 parts of polylactic acid are taken as raw materials by mass, and the polylactic acid blending melt-blown nonwoven material is obtained through melt blowing. The obtained melt-blown nonwoven material has a longitudinal strength of 50-80N/5cm and a longitudinal elongation at break of 56-75%. The material manufactured by the method has high toughness, but the method has complex process, time consumption and high cost, and needs to be subjected to three times of blending and a multistage heat drafting device.
The prior modified polylactic acid melt-blown non-woven fabric mainly focuses on adding reinforcing and toughening materials at the same time and improving phase interfaces, and can achieve the effect of reinforcing and toughening, but has complex procedures, long time consumption and high cost, and the problem of solvent volatilization is caused by frequently neglecting the degradability of the added materials. Therefore, how to produce a fully degradable, high-strength and high-toughness polylactic acid melt-blown nonwoven material by a simple process has become an urgent problem to be solved by the industry.
The morphology of the dispersed phase in the blend has a great influence on the mechanical properties. The dispersed phase morphology of the binary blend is mainly divided into a single-phase continuous structure, a two-phase staggered structure and a two-phase continuous structure. The in-situ microfiber structure and the two-phase continuous structure in the single-phase continuous structure are popular fields of polymer blending research. The in-situ microfiber structure refers to a structure that a disperse phase exists in a matrix in a microfiber form, the higher orientation of the microfiber is beneficial to the increase of mechanical strength, and the two-phase continuous structure refers to a network structure that polymer systems mutually penetrate, so that the stress conduction is facilitated. However, no research report on strengthening and modifying the polylactic acid melt-blown nonwoven material by controlling the morphology and structure of the disperse phase exists at present.
Polybutylene succinate (PBS) is a completely biodegradable high polymer material, has good biocompatibility and good toughness.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a polylactic acid melt-blown nonwoven material which has the advantages of simple preparation process, no toxicity, no harm, full degradability and high strength and toughness.
In order to achieve the above object, the present invention adopts the following technical scheme
A preparation method of a high-strength and high-toughness polylactic acid melt-blown nonwoven material comprises the following steps:
S1, premixing, namely premixing a polylactic acid slice and a polybutylene succinate slice serving as raw materials under a certain condition to prepare a polylactic acid/polybutylene succinate premixed slice;
s2, melt blending, namely injecting the prepared polylactic acid/polybutylene succinate premixed slice into a double-screw extruder for melting, and extruding the polylactic acid/polybutylene succinate premixed slice into a trickle melt through a metering pump and a clothes hanger die head;
S3, hot melt molding, namely stretching and shearing the prepared fine flow melt by high-temperature high-speed airflow to obtain fibers, and collecting the fibers by a receiving device through a self-adhesive synthetic net to obtain the polylactic acid melt-blown nonwoven material.
Preferably, in step S1, a drying treatment is required before premixing the polylactic acid slice and the polybutylene succinate slice.
Preferably, the drying treatment is vacuum drying, the temperature of the vacuum drying is 40-100 ℃, and the time of the vacuum drying is 12-72h.
Preferably, in step S1, the temperature of the premixing is room temperature, and the premixing time is 10-40min.
Preferably, in the step S2, the screw extruder is divided into four temperature areas, wherein the temperatures of the four temperature areas are 170-200 ℃, 180-210 ℃, 190-230 ℃ and 220-250 ℃ respectively.
Preferably, in step S2, the temperature of the hanger-type die is 230-260 ℃.
Preferably, in the step S2, the melt extrusion amount of the combined device of the double-screw extruder and the clothes hanger type die head is 20-90g/min;
Preferably, in the step S3, the temperature of the high-temperature high-speed air flow is 240-290 ℃, the speed of the high-temperature high-speed air flow is 100-300m/S, and the receiving distance of the receiving device is 5-40cm.
Preferably, the mass ratio of the polylactic acid slice to the polybutylene succinate slice is 20-95:5-80 in parts by mass.
The second purpose of the invention is to provide the high-strength and high-toughness polylactic acid melt-blown non-woven material prepared by the preparation method, wherein the high-strength and high-toughness polylactic acid melt-blown non-woven material is any one of an in-situ microfiber structure, a two-phase continuous structure or a sea-island structure.
Preferably, the high strength, high toughness polylactic acid melt blown nonwoven material has an average diameter of 3 to 15 μm.
The invention also aims to provide the application of the high-strength high-toughness polylactic acid melt-blown non-woven material in the protection field.
The invention has the following beneficial effects:
(1) The invention aims to construct different disperse phase morphological structures by utilizing stress characteristics of different stages of a melt-blowing process and high cooling rate (the melt-blowing process) so as to strengthen and toughen the polylactic acid melt-blown non-woven material. The high-strength and high-toughness polylactic acid melt-blown nonwoven material is prepared by taking polylactic acid slices and polybutylene succinate slices as raw materials and sequentially carrying out premixing, melt extrusion, high-temperature and high-speed air flow stretching, shearing and self-adhesion networking working procedures, and simultaneously controlling the proportion of a matrix material and a reinforcing material and the temperature and the speed of the high-temperature and high-speed air flow. Specifically, the PBS is firstly dispersed in PLA in the form of spherical droplets by utilizing the shearing force in the screw, and then the spherical droplets of the PBS are evolved into specific structures (such as an in-situ microfiber structure, a two-phase continuous structure and a sea-island structure) with different forms in the PLA matrix under the action of extrusion of a die head under specific conditions and hot air flow. The preparation method provided by the invention only needs one-time blending, and can realize the improvement of the toughness of the polylactic acid melt-blown nonwoven material without an additional device.
(2) The preparation method has no solvent volatilization problem, namely no pollution problem in the preparation process, and the polylactic acid and the polybutylene succinate are selected as raw materials, so that the full-degradable product can be realized, and the final product is carbon dioxide and water, thereby meeting the requirement of sustainable development.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of the structure of a melt-blown nonwoven apparatus used in example 1 of the present invention;
FIG. 2 is a schematic illustration of the formation of different structures of polylactic acid-blended meltblown fibers;
FIG. 3 is a SEM image of the cross-sectional morphology of the polylactic acid blended meltblown fibers prepared in examples 1-3, wherein FIG. 3a is a SEM image of the meltblown fibers prepared in example 1 parallel to the fiber direction;
FIG. 3b is an SEM image of the meltblown fibers produced in example 2 parallel to the fiber direction, FIG. 3c is an SEM image of the meltblown fibers produced in example 3 parallel to the fiber direction, FIG. 3d is an SEM image of the meltblown fibers produced in example 1 perpendicular to the fiber direction, FIG. 3e is an SEM image of the meltblown fibers produced in example 2 perpendicular to the fiber direction, and FIG. 3f is an SEM image of the meltblown fibers produced in example 3 perpendicular to the fiber direction.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth such as the particular system architecture, techniques, etc., in order to provide a thorough understanding of the embodiments of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present invention with unnecessary detail.
Example 1
Referring to fig. 1, a method for preparing a high-strength and high-toughness polylactic acid melt-blown nonwoven material comprises the following steps:
S1, drying a polylactic acid slice with a weight average molecular weight of 70000 and a polybutylene succinate slice with a weight average molecular weight of 65000 for 24 hours under a vacuum condition at 50 ℃, and then weighing 8kg of the dried polylactic acid slice and 2kg of the polybutylene succinate slice for premixing in a high-speed mixer for 20 minutes;
s2, injecting the premixed slices into a double-screw extruder for melting, extruding the premixed slices into melt trickles through a metering pump and a clothes hanger type die head, wherein the temperatures of four temperature areas of the double-screw extruder are 170 ℃,190 ℃,215 ℃ and 250 ℃ in sequence, the temperature of the clothes hanger type die head is 250 ℃, and the extrusion amount is 40g/min;
And S3, placing the extruded melt trickle under high-temperature high-speed air flow with the temperature of 260 ℃ and the speed of 150m/S to form fibers, and self-bonding a synthetic net by utilizing the waste heat of a fiber sheath layer on a receiving device with the receiving distance of 10cm to obtain the polylactic acid melt-blown nonwoven material.
The production process flow chart of the high-strength high-toughness polylactic acid melt-blown nonwoven material is shown in fig. 1, and the meaning of the marks in fig. 1 is as follows, namely 1, a feed inlet, 2, a motor, 3, a double-screw extruder, 4, a filter, 5, a metering pump, 6, a clothes hanger type die head, 7, a spinneret orifice, 8, a gas orifice and 9, and a receiving device.
SEM observations were made on the morphology of the (polylactic acid) melt-blown (nonwoven) fibers prepared in this example, both parallel to the fiber direction and perpendicular to the fiber direction, as shown in fig. 3a and 3 d. As can be seen from the results of fig. 3a and 3d, the (polylactic acid) melt-blown (nonwoven) fiber prepared in the examples has an in-situ microfiber structure (see fig. 2), i.e., polybutylene succinate exists in the form of microfibers in the polylactic acid matrix. The nonwoven material had a machine direction strength of 65N/5cm and an elongation at break of 24.62% measured according to standard GB/T3923.1-2013.
Example 2
The preparation method of the high-strength high-toughness polylactic acid melt-blown nonwoven material comprises the following steps:
S1, drying a polylactic acid slice with a weight average molecular weight of 70000 and a polybutylene succinate slice with a weight average molecular weight of 65000 for 24 hours at a temperature of 50 ℃ under a vacuum condition, weighing 5kg of the dried polylactic acid slice and 5kg of the polybutylene succinate slice, and premixing for 20min in a high-speed mixer;
s2, injecting the premixed slices into a double-screw extruder for melting, extruding the premixed slices into melt trickles through a metering pump and a clothes hanger type die head, wherein the temperatures of four temperature areas of the double-screw extruder are 170 ℃,190 ℃,215 ℃ and 250 ℃ in sequence, the temperature of the clothes hanger type die head is 260 ℃, and the extrusion amount is 50g/min;
And S3, placing the extruded melt trickle under the air flow with the temperature of 280 ℃ and the speed of 220m/S to form fibers, and self-bonding the fibers into a net by utilizing the waste heat of a fiber sheath on a receiving device with the receiving distance of 10cm to obtain the polylactic acid melt-blown nonwoven material.
SEM observations were made on the morphology of the prepared (polylactic acid) meltblown (nonwoven) fibers parallel to the fiber direction and perpendicular to the fiber direction, as shown in fig. 3b and 3 e. As can be seen from the results of fig. 3b and 3e, the (polylactic acid) melt-blown (nonwoven) fiber obtained in this example has a two-phase continuous structure (see fig. 2), i.e., polybutylene succinate and polylactic acid penetrate each other to form a network structure. The nonwoven material had a machine direction strength of 53N/5cm and an elongation at break of 40.54% measured according to standard GB/T3923.1-2013.
Example 3
The preparation method of the high-strength high-toughness polylactic acid melt-blown nonwoven material comprises the following steps:
S1, taking a polylactic acid slice with a weight average molecular weight of 70000 and a polybutylene succinate slice with a weight average molecular weight of 65000, and drying under a vacuum condition at a drying temperature of 50 ℃ for 24 hours;
s2, taking 4kg of dried polylactic acid slices and 6kg of polybutylene succinate slices, and premixing the dried polylactic acid slices and the 6kg of polybutylene succinate slices in a high-speed mixer for 20min;
S3, injecting the premixed slices into a double-screw extruder for melting, extruding the premixed slices into melt trickles through a metering pump and a hanger type melt-blowing die head, wherein the temperatures of four temperature areas of the extruder are 170 ℃,190 ℃,215 ℃ and 250 ℃ in sequence, the temperature of the hanger type die head is 250 ℃, and the extrusion amount is 60g/min;
S4, placing the extruded melt trickle under the air flow with the temperature of 270 ℃ and the speed of 180m/S to form fibers, and self-adhering the fibers on a receiving device with the receiving distance of 10cm by using the waste heat of the fiber skin layer to form a net so as to obtain the polylactic acid melt-blown nonwoven material.
SEM observations were made on the morphology of the prepared (polylactic acid) meltblown (nonwoven) fibers parallel to the fiber direction and perpendicular to the fiber direction, as shown in fig. 3c and 3 f. As can be seen from the results of fig. 3c and 3f, the (polylactic acid) melt-blown (nonwoven) fiber obtained in this example has a sea-island structure (see fig. 2), i.e., polylactic acid exists in the form of spherical droplets in the polybutylene succinate matrix. The nonwoven material had a machine direction strength of 21N/5cm and an elongation at break of 4.49% measured according to standard GB/T3923.1-2013.
Comparative example 1
Substantially the same as in example 1, except that the content of the polylactic acid chips was 2kg and the content of the polybutylene succinate chips was 8.5kg.
As a result of the experiment, it was difficult to form continuous fibers and spinning was impossible, and the temperatures of the die and the air stream were further increased to 265℃and 285℃respectively, and the polylactic acid-blended melt-blown nonwoven material obtained on a receiving device having a receiving distance of 10cm had many spots caused by fibers under-drawn.
The resulting nonwoven material had a machine direction strength of 5N/5cm and an elongation at break of 1.01% measured according to standard GB/T3923.1-2013. The results of this comparative example demonstrate that when the proportion of polybutylene succinate is large, melt extrusion is difficult and spinnability is poor in the spinning temperature range of the pure polylactic acid melt-blown nonwoven material.
Comparative example 2
Substantially the same as in example 2 was found except that the air flow rate was 300m/s.
As a result of the experiment, the meltblown nonwoven was almost free of strength.
The results of this comparative example show that when the air flow velocity is too high, long fibers cannot be formed and spinnability is poor.
Comparative example 3
Substantially the same as in example 3, except that the temperature of the gas stream was 235 ℃.
As a result of the experiment, the fibers were thicker and the doubling was severe, making the meltblown nonwoven stiffer to the touch.
The results of this comparative example demonstrate that when the air flow temperature is too low, the polymer is not sufficiently drawn and the resulting meltblown nonwoven is less skin friendly.
Comparative example 4
S1, drying a polylactic acid slice with a weight average molecular weight of 70000 for 24 hours at a temperature of 50 ℃ under a vacuum condition;
S2, weighing 10 kg of dried polylactic acid slices, injecting into a double-screw extruder for melting, extruding into melt trickles through a metering pump and a clothes hanger type die head, wherein the temperatures of four temperature areas of the extruder are 170 ℃,190 ℃,215 ℃ and 250 ℃ in sequence, and the temperature of the clothes hanger type die head is 250 ℃ and the extrusion amount is 50g/min;
s3, forming fibers by the extruded melt trickle under the action of air flow with the temperature of 270 ℃ and the speed of 150m/S, and self-bonding the fibers into a net by utilizing the waste heat of a fiber sheath on a receiving device with the receiving distance of 10cm to obtain the polylactic acid melt-blown nonwoven material.
The nonwoven material had a machine direction strength of 14N/5cm and an elongation at break of 1.28% measured according to standard GB/T3923.1-2013. Comparative example 4 illustrates that the strength and toughness of the pure polylactic acid melt blown nonwoven material are poor.
The present invention is not limited to the above-described specific embodiments, and various modifications may be made by those skilled in the art without inventive effort from the above-described concepts, and are within the scope of the present invention.
Claims (6)
1. A method for preparing a high-strength and high-toughness degradable melt-blown nonwoven material, which is characterized by comprising the following steps:
S1, premixing, namely premixing a polylactic acid slice and a polybutylene succinate slice serving as raw materials under a certain condition to prepare a polylactic acid/polybutylene succinate premixed slice;
s2, melt blending, namely injecting the prepared polylactic acid/polybutylene succinate premixed slice into a double-screw extruder for melting, and extruding the polylactic acid/polybutylene succinate premixed slice into a trickle melt through a metering pump and a clothes hanger die head;
S3, hot melt molding, namely stretching and shearing the prepared fine flow melt by high-temperature high-speed airflow to obtain fibers, and collecting the fibers by a receiving device through a self-adhesive synthetic net to obtain the polylactic acid melt-blown nonwoven material;
in the step S2, the screw extruder is divided into four temperature areas, wherein the temperatures of the four temperature areas are 170-200 ℃, 180-210 ℃, 190-230 ℃ and 220-250 ℃ respectively;
the temperature of the clothes hanger type die head is 230-260 ℃, and the melting extrusion amount of the combined device of the double-screw extruder and the clothes hanger type die head is 20-90g/min;
In the step S3, the temperature of the high-temperature high-speed air flow is 240-290 ℃, the speed of the high-temperature high-speed air flow is 100-300m/S, and the receiving distance of the receiving device is 5-40cm;
The mass ratio of the polylactic acid slice to the polybutylene succinate slice is 20-95:5-80.
2. The method of claim 1, wherein in step S1, the polylactic acid chips and the polybutylene succinate chips are dried before premixing.
3. The method for preparing the high-strength high-toughness degradable melt-blown nonwoven material according to claim 2, wherein the drying treatment condition is vacuum drying, the temperature of the vacuum drying is 40-100 ℃, and the time of the vacuum drying is 12-72h.
4. The method of claim 1, wherein in step S1, the temperature of the premixing is room temperature and the premixing time is 10-40min.
5. The high-strength and high-toughness polylactic acid melt-blown nonwoven material prepared by the preparation method according to any one of claims 1 to 4, wherein the high-strength and high-toughness polylactic acid melt-blown nonwoven material is any one of an in-situ microfiber structure, a two-phase continuous structure or an island structure, and the average diameter of the high-strength and high-toughness polylactic acid melt-blown nonwoven material is 3 to 15 μm.
6. The use of the high strength and high toughness polylactic acid melt-blown nonwoven material according to claim 5 in the field of protection.
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CN101824708A (en) * | 2010-05-10 | 2010-09-08 | 豆丁乐园(南京)婴儿用品有限公司 | Fully-degradable polylactic acid fiber melt-blowing nonwoven and preparation method thereof |
CN106009559A (en) * | 2016-05-18 | 2016-10-12 | 贵州大学 | Preparation method of high-strength and high-toughness PLA (polylactic acid) and in-situ nanofiber composite |
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KR20090087517A (en) * | 2006-12-15 | 2009-08-18 | 킴벌리-클라크 월드와이드, 인크. | Biodegradable Polylactic Acid for Fiber Formation |
EP2064261A1 (en) * | 2006-12-15 | 2009-06-03 | Kimberly-Clark Worldwide, Inc. | Biodegradable polylactic acids for use in forming fibers |
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