CN112239897B - Island-in-island fiber and application thereof in PU leather - Google Patents

Island-in-island fiber and application thereof in PU leather Download PDF

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CN112239897B
CN112239897B CN202011014992.5A CN202011014992A CN112239897B CN 112239897 B CN112239897 B CN 112239897B CN 202011014992 A CN202011014992 A CN 202011014992A CN 112239897 B CN112239897 B CN 112239897B
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island
polymer
fiber
phase
islands
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CN112239897A (en
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赵鸿凯
段伟东
孙向浩
杜明兵
胡锦文
杨艳彪
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Shanghai Huafeng Super Fiber Technology Co ltd
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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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • 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
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Multicomponent Fibers (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention relates to an island-in-island fiber and application thereof in PU leather, wherein the island-in-island fiber comprises a sea phase and an island phase, the island phase comprises a fixed island and an indefinite island, the indefinite islands are distributed around the fixed island, the surface of the island fiber in the island basically does not contain island phase components, and the island phase basically does not contain components, namely, under a scanning electron microscope of 2000 times, the proportion of the sum of the exposed areas of the island phase to the surface area of the island fiber in the island is less than 5%; the sea phase component is a polymer A and a polymer B, the fixed island component is a polymer C, the indefinite island component is a polymer D, and the melt viscosity relationship of each polymer is as follows: polymer C or polymer D > polymer A > polymer B; the application is as follows: preparing non-woven fabric from island fibers in the island, impregnating polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, grinding, dyeing and post-finishing. The invention effectively solves the problem of exposure of the adventitious islands in the prior art, and the prepared PU leather has higher peeling load, tearing load, tensile load and density.

Description

Island-in-island fiber and application thereof in PU leather
Technical Field
The invention belongs to the technical field of sea-island fibers, relates to a sea-island fiber, and particularly relates to a sea-island fiber containing fixed islands and indefinite islands, and application thereof in PU (polyurethane) leather.
Background
The island-in-island fiber refers to a special island structure which is obtained by island fiber and is distributed with a plurality of small islands around the large island, the technology of combining composite spinning and blended spinning is usually adopted, the large island is a fixed island structure, the small islands are indefinite island structures, and the fiber denier of the large island is larger than that of the small islands.
As early as 1970, related patents have reported such composite filaments of island-in-island structure, specifically a bundle of composite filaments comprising a plurality of synthetic polymer filaments extending substantially parallel to each other along the length of the bundle, and a plurality of synthetic polymer fibrils extending discontinuously along the length of the bundle and distributed in the spaces between the filaments. Fibrils are much finer than filaments and may or may not be attached to them. These bundles are formed of composite filaments of the "island-in-island" type, having filaments embedded in the sea formed by a mixture of 50 to 93% by weight of a main component and 7 to 50% by weight of a secondary component, the filaments being dispersed in the main component. These composite filaments are treated by a process that removes only the major component of the "sea", leaving behind a bundle of filaments. The "island" components preferably constitute from 15 to 75% by weight of the composite filament and may themselves be formed from a blend, rather than from pure homopolymer. Examples are given of composite filaments made from polyethylene terephthalate or nylon 6 as the "island" component, either of which is blended with polystyrene as the "sea" component. In these examples, polystyrene is the major "sea" component and is removed by dissolution with trichloroethylene or tetrachloroethylene. Filaments having polyethylene terephthalate as the island phase component and mixed with a greater proportion of nylon 6 as the sea phase component are also illustrated. In this case, the nylon 6 was removed by treatment with formic acid. The composite filaments are made of "islands" and a minor "sea".
The process greatly improves the respective performances and processing disadvantages of the island fibers and the island fibers, for example, in terms of performances, the filament part can enable the composite fibers to have higher toughness and strength, the short fibers can enable the composite fibers to have soft touch and release stress, and the two fibers are entangled or bonded to form the whole composite fiber; in processing, the sea phase is a blending system, so that the melt viscosity can be increased, and the island phase component is not easy to separate from the sea phase component in composite spinning.
However, there are still some problems to be solved, such as that before removing the sea phase component, the island-fixed component is relatively controllable in both fiber size and position distribution, while the island-fixed component is not controllable in both fiber size and position distribution, especially when preparing the sea-island fiber with high island content, it is easy to expose the island-fixed component at the edge of the sea-island fiber, and the island-fixed component exposed at the edge of the fiber will not be beneficial to the heat setting of the sea-island fiber because the thermal properties of the island-fixed component and the sea phase component are very different. The shape and distribution of the islands in the island fibers prepared by the prior art are often uncontrollable in the spinning process, the obtained fixed islands and the obtained indefinite islands have an incompact structure, and the like, and the improvement of the fiber performance enters the bottleneck.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an island-in-island fiber and a preparation method thereof, and specifically comprises the following steps:
it is an object of the present invention to provide a novel island-in-island fiber which is substantially free of island phase components on the fiber surface;
another object of the present invention is to provide a method for preparing a novel island-in-island fiber, which uses at least two polymers having different melt viscosities as sea phase components, wherein one of the polymers can form a stable and uniformly distributed sea-island structure with the island phase components, and the other polymer is easy to flow to the fiber surface during spinning and easy to block during heat setting.
In view of the fact that the novel island-in-island fibers prepared by the method are easy to adhere during heat setting and the sea phase component can be dissolved, the method also tries to prepare the novel island-in-island fibers into PU leather.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an island-in-island fiber comprises a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, the surface of the island-in-island fiber basically does not contain island phase components, and basically does not contain the island phase components, namely, under a scanning electron microscope of 2000 times, the proportion of the sum of the exposed areas of the island phases to the surface area of the island-in-island fiber is less than 5% (when the sum of the exposed areas of the island phases is 0%, namely, no island phase is visible on the surface of the island-in-island fiber);
the sea phase component is a polymer A and a polymer B, the fixed island component is a polymer C, the indefinite island component is a polymer D, the polymer A and the polymer B are the same or different polymers and can be dissolved in an organic solvent, water or alkali liquor, the polymer C and the polymer D are the same or different polymers and can not be dissolved in a solvent for dissolving the sea phase component, and the melt viscosity relationship of each polymer is as follows: polymer C or Polymer D > Polymer A > Polymer B.
According to the invention, the polymer A and the polymer B form a sea phase component of island fibers in islands, the polymer C and the polymer D respectively form a fixed island component and an indefinite island component of the island fibers in the islands, and the melt viscosity of the polymer B is greatly different from that of the polymer D, so that the mutual diffusion tendency of chain segments of the two polymers is very small, and a micro-phase is formed; the "micro-phase" refers to that in the process that a spinning melt composed of a polymer a, a polymer B and a polymer D enters a spinning filter, a melt pipeline and a spinneret and is spun by a spinneret under the condition of being separated from a screw rod and mechanically stirred, in a melt flow channel, due to the difference of fluidity of a blend, the high-fluidity polymer B in the center of the flow channel flows towards the wall of the flow channel, so that the content of the polymer B in a sea phase component from outside to inside of the fiber is remarkably reduced, the content of the polymer B in the sea phase component in the center of the flow channel is low (mainly polymer a), the sea phase component and an adventitious island component (polymer D) have a small melt viscosity difference, the adventitious island component can be stably dispersed in the sea phase component, the content of the polymer B in the sea phase component in the wall of the flow channel is high, the sea phase component and the adventitious island component (polymer D) have a large melt viscosity difference, so that the two-phase interfacial tension is too large, the adventitious island component in the original fiber is difficult to diffuse into the sea phase component close to the outer wall of the fiber, and the adventitious island component in the original fiber is difficult to disperse in the sea phase component, and the sea component, and the island component close to the outer wall of the fiber, so that the island component is not stably dispersed in the island component, but can be stably dispersed in the fiber, and can be generated. Therefore, the adventitious island component tends to be distributed in the sea phase component containing less polymer B in the fiber to form a certain differential phase, and the diffusion of the adventitious island component to the outer wall of the fiber can be effectively avoided.
As a preferred technical scheme:
one island-in-island fiber as described above, polymer a having a melt index of 20 to 50g/10min (ASTM D1238-13) under a test condition of 190 ℃ by 2.16Kg, polymer B having a melt index of 60 to 75g/10min (ASTM D1238-13) under a test condition of 190 ℃ by 2.16Kg, polymer C or polymer D having a melt index of 7 to 26g/10min (ASTM D1238-13) under a test condition of 235 ℃ by 2.16 Kg; the melt index MI is inversely proportional to the melt viscosity of the polymer, the higher the MI, the lower the melt viscosity of the polymer; in the composite spinning system, the melt viscosity relationship of each polymer is as follows: polymer C or polymer D > polymer A > polymer B; in the invention, the viscosity compounding of the polymer A, the polymer B and the polymer D is the key to influence the forming micro-phase of the blend; when the melt index of the polymer A under the test condition of 190 ℃ by 2.16Kg is less than 20g/10min, and the melt index of the polymer B under the test condition of 190 ℃ by 2.16Kg is more than 75g/10min, although the formation of a more obvious micro-phase sea phase component is facilitated, the viscosity difference of the sea phase component from the center of the fiber to the outer wall of the fiber is too large to change, the spinnability is influenced, and the island merging of the indefinite island component is serious; when the melt index of the polymer A under the test condition of 190 ℃ by 2.16Kg is more than 50g/10min, and the melt index of the polymer B under the test condition of 190 ℃ by 2.16Kg is less than 60g/10min, the viscosity difference of the polymer A and the polymer B is too small, the flowability of the polymer A and the polymer B is similar, a micro-phase structure is not sufficiently formed, and the spinnability problem is caused because the viscosity of the central sea phase component is too small; the spinning quality is influenced by too small or too large melt index of the polymer D, and when the melt index is too small, the melt viscosity difference between the sea phase component and the adventitious island component is too large, the island diameter is large, the distribution is poor, and the spinnability is poor; when the melt index is too large, the difference in melt viscosity between the sea phase component and the amorphous island component is too small, and the sea-island structure stability is poor.
One island-in-island fiber as described above, polymer B having a vicat softening point of 90 to 105 ℃ (test standard GB/T1633-2000, test condition 10n × 50 ℃/h); because the polymer B is mainly concentrated on the surface of island fibers in an island, the influence of the Vicat softening point of the polymer B on the heat setting capability and the processability of the island fibers in the island of the system is researched through experiments, and when the polymer B with the Vicat softening point of 90-105 ℃ is selected, the fact that the surfaces of the fibers are easy to adhere through a hot pressing process when the island fibers in the island are used for preparing a non-woven fabric is found, so that the island fibers in the island show excellent adhesion in a heat setting process; when the Vicat softening point of the polymer B on the surface of the island fiber in the island is less than 90 ℃, the spinnability of the fiber is influenced; when the vicat softening point of the polymer B on the surface of the island fibers in the island is more than 105 ℃, the improvement on the heat-setting effect is not significant.
One island in island fiber as described above, polymer a and polymer B being both LDPE (low density polyethylene), more stable island in island fiber structures can be obtained using the same polymer sea component than using two different polymer sea components; both polymer C and polymer D are PA (polyamide).
An island-in-island fiber as described above, the island-in-island fiber further comprising a compatibilizer.
One island-in-island fiber as described above, the compatibilizer is LDPE-g-MAH (maleic anhydride grafted polyethylene) having a melt index of 5 to 15g/10min (ASTM D1238-13, 190 ℃ c. 2.16 Kg) under the test condition of 190 ℃ c. 2.16Kg and a grafting ratio of 0.8 to 1.2%; the addition of the compatilizer can effectively improve the dispersion and distribution of the adventitious island component in the sea phase component and can refine the island diameter, because the compatilizer contains a maleic anhydride reaction functional group and can react with the active end group of the polymer D, and the compatilizer also contains a polyethylene chain segment and can generate stronger intermolecular force with the polymer A, so the compatilizer can reduce the interfacial tension between the polymer A and the polymer D; compared with a single sea phase, the compatilizer is added into the mixed sea phase in the system to optimize the form and distribution of the indefinite islands, so that the advantages are better, because the melt viscosity of the sea phase along the fiber center to the fiber edge is gradually reduced, when the suitable compatilizer is added to modify the island phase polymer, the island phase and the sea phase interface have better wettability, and the wettability of the fiber edge to the center is gradually improved; the sea phase component in the center of the fiber has higher viscosity and longer molecular chain, and forms stronger intermolecular acting force with LDPE-g-MAH, the indefinite islands from the edge to the center of the fiber are gradually compacted and refined and are better and stably distributed around the definite islands, and the obtained sea-island fiber is more compact in ultrafine fiber bundles and thinner in island diameter of the indefinite islands after fiber opening, is easier to arrange along the direction of the definite islands, and has better mechanical property;
however, the effect of the compatibilizer on the micro-phase formation of the spinning system needs to be considered in the process of selecting the compatibilizer, and excessive compatibilization modification can expose the formed indefinite islands of the polymer D; the grafting rate of the compatilizer is preferably 0.8-1.2%, and the excessively high grafting rate greatly improves the interfacial tension between the polymer D and the mixed sea phase consisting of the polymer C and the polymer D, and when the interfacial tension between the polymer D and the sea phase at the outer wall of the fiber is reduced to be capable of mutual diffusion, the risk of island phase exposure is generated, so that the grafting rate of the compatilizer needs to be strictly controlled to avoid the condition that the addition of the compatilizer damages the micro-phase state of the system; meanwhile, the grafting rate of the compatilizer is not low, the effect of improving the interfacial tension of the polymer A and the polymer D is not large due to low grafting rate, and the island diameter and the distribution thereof cannot be effectively refined; the melt index of the compatilizer is preferably 5-15 g/10min (ASTM D1238-13, 190 ℃ C. X2.16 Kg), and an excessively high melt index causes the viscosity of the system to be excessively high, which is not beneficial to influencing the spinnability, and simultaneously increases the entanglement between the compatilizer and the polymer B, thereby destroying the micro-phase separation state of the system; when the melt index is too low, the effect of the compatibilizer in improving the interfacial tension between the polymer a and the polymer D is reduced, because the polyethylene chain segment is too short and the intermolecular force generated by the polymer D is weak, and the island diameter and distribution cannot be well refined.
The mass ratio of the polymer A to the polymer B is 8; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 20 to 50, the ratio of the sum of the masses of polymer a and polymer B to the mass of polymer D is 50 to 85.
The invention also provides a method for preparing the island-in-island fiber, which adopts a method combining composite spinning and blended spinning, wherein the sea phase component comprises a polymer A and a polymer B, the fixed island component comprises a polymer C, the indefinite island component comprises a polymer D, the polymer A and the polymer B are the same or different polymers and can be dissolved in an organic solvent, water or alkali liquor, the polymer C and the polymer D are the same or different polymers and can not be dissolved in a solvent for dissolving the sea phase component, and the melt viscosity relationship of each polymer is as follows: polymer C or Polymer D > Polymer A > Polymer B.
As a preferred technical scheme:
the method comprises the following specific processes: melting and blending a polymer A, a polymer B, a polymer D and a compatilizer I (more uniform indefinite islands can be obtained by adding the compatilizer I into a blend of a sea phase component and an indefinite island component), forming a blend of the sea phase component and the indefinite island component, melting and blending a polymer C and the compatilizer II (the compatilizer II is added into a definite island component, high-content islands can be stably obtained, and merging islands among the definite islands and the indefinite islands is avoided) to form a plurality of strands of fine flows, mixing the fine flows with the blend of the sea phase component and the indefinite island component in a spinning assembly, and discharging filaments from a spinneret plate to obtain island fibers in the islands; the compatilizer I and the compatilizer II are the same in kind.
In the method, the spinning process parameters comprise: the temperature of cooling air is 15-20 ℃, the spinning speed is 500-800 m/min, the concentration of oil agent is 1.5wt% when winding and bundling are carried out, the winding speed is 500-800 m/min, the temperature of a first drawing water bath is 80-82 ℃, the temperature of a second drawing water bath is 82-90 ℃, the speed of a first drawing machine is 20-25 m/min, the speed of a second drawing machine is 50-70 m/min, the concentration of oil agent in an oil agent tank is 3-6 wt%, the temperature of an oil agent tank is 45-55 ℃, the speed of a third drawing machine is 60-80 m/min, the total drawing multiple is 2.5-3.5, the temperature of a tow entering a crimping machine is 45-55 ℃, the speed of the crimping machine is 60-80 m/min, the temperature of loose heat setting is 50-65 ℃, the time of loose heat setting is 8-12 min, the speed of the cutting machine is 50-70 m/min, and the cutting length is 51mm; the concentration of oil agent and the winding speed are winding bundling technological parameters when winding bundling; the first drafting water bath temperature, the second drafting water bath temperature, the first drafting machine speed, the second drafting machine speed, the oiling agent concentration of an oiling agent groove, the oiling agent groove temperature, the third drafting machine speed and the total drafting multiple are drafting technological parameters; the temperature of the tows entering the crimping machine and the speed of the crimping machine are crimping technological parameters; setting parameters of the relaxation heat setting temperature and the relaxation heat setting time are set process parameters; the speed of the cutting machine and the cutting length of 51mm are cutting technological parameters.
The invention also provides the application of the island-in-island fibers in the PU leather, the island-in-island fibers are made into non-woven fabrics and impregnated with polyurethane slurry, and the PU leather is prepared by curing (curing refers to the process of changing the state of polyurethane from liquid to solid after the solvent in the polyurethane slurry is removed; in the industry, waterborne polyurethane is generally called as curing, solvent polyurethane is generally called as solidifying, and the solvent polyurethane is not distinguished and is generally called as curing), fiber opening, drying, splitting, buffing, dyeing and post-finishing; the PU leather prepared by the method has the PU content of 40wt percent, and the physical property data is as follows: the product with a thickness of 0.9mm has a peel load of 80N or more (sample width 3 cm), a tear load of 70N or more (sample width 3 cm), a tensile load of 120N or more (sample width 1 cm), and a density of 0.48g/cm 3 Compared with PU leather made of common PA6 microfiber base cloth, the PU leather has higher peeling load, tearing load, tensile load and density.
As a preferred technical scheme:
according to the application, before the polyurethane slurry is impregnated, the non-woven fabric is subjected to heating and rolling sizing treatment in sequence to improve the bonding fastness between fibers.
The application is that the PU content in the PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 83-92N when the width of a sample is 3cm, the latitudinal peeling load is 80-88N when the width of the sample is 3cm, the radial tearing load is 75-85N when the width of the sample is 3cm, the latitudinal tearing load is 70-76N when the width of the sample is 3cm, the radial tensile load is 148-178N when the width of the sample is 1cm, the latitudinal tensile load is 120-146N when the width of the sample is 1cm, and the density is 0.48-0.60 g/cm 3 。
Has the beneficial effects that:
(1) The invention researches the melt flow behavior of two polymers with different melt viscosities when preparing island fibers in an island, and forms a 'micro-phase' in the mixed spinning melt processing process by adopting the difference, avoids the problem of island phase exposure existing in the traditional manufacturing method by the viscosity difference of sea phase components between the fiber surface and the center and selecting the proper viscosity difference of the sea phase and the island phase, and simultaneously ensures the stability of the sea phase and the island phase structure, wherein the island phase polymer can be well dispersed in the mixed sea phase with high melt viscosity, and the high-flow sea phase can easily flow to the outer wall to form the low-melt-viscosity polymer mixed sea phase which does not contain the island phase on the fiber surface;
(2) The invention forms a structure similar to the island in the outer sheath core by the material selection design of the sea phase component, the indefinite island component and the definite island component, solves the problem of poor fiber surface thermal cohesiveness when producing island fibers in the prior art, and compared with composite spinning, the method obviously reduces the processing investment;
(3) The invention selects the polymer B with high fluidity and low softening point as one part of the sea phase component, during spinning, the polymer B flows to the outer wall of a spinning die more easily, and a layer of polymer with low softening point is formed on the surface of the fiber, so that the obtained island fiber in the island has excellent cohesiveness, the obtained island fiber is used as the fiber raw material of the non-woven fabric, the obtained non-woven fabric has high fiber cohesiveness after being heated by an oven and rolled for shaping, the non-woven fabric with high density can be obtained according to the requirement, and the prepared finished product has high density and fine and smooth velvet feeling;
(4) According to the invention, the compatilizer LDPE-g-MAH with proper melt index and grafting rate is added into the spinning system, so that the influence of the addition of the compatilizer on the fluidity of each component of the spinning system is taken into consideration while the island diameter and the distribution of the indefinite islands are adjusted, the fiber structure of the island phase fully coated by the sea phase component is ensured to be obtained, the island diameter, the number and the distribution of the indefinite islands are effectively improved, and the strength of the fiber can be remarkably improved.
Drawings
FIG. 1 is a schematic illustration of island fibers in an island;
FIG. 2 is an SEM image of the island-in-island fibers of example 1, at 2000 magnifications, with smooth fiber surfaces and no apparent exposure of adventitious islands;
FIG. 3 is an SEM image of the island-in-island fibers prepared in comparative example 1 at a magnification of 2000 with a significant exposure of the adventitious islands visible on the fiber surface;
FIG. 4 shows the shaping effect of the nonwoven fabric prepared from the island fibers in the island produced in example 1 after heating in an oven (140 ℃,6 min) and rolling by a ironing roller at 80 ℃, and the surface is relatively flat and obviously adhered;
FIG. 5 shows the setting effect of the nonwoven fabric prepared from the island fibers in the island produced in comparative example 1 after heating in an oven (140 ℃,6 min) and rolling by a ironing roller at 80 ℃, the surface is loose and the adhesion is not obvious;
wherein, 1-sea phase I (mainly polymer B), 2-sea phase II (mainly polymer A), 3-fixed island and 4-indefinite island.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
The test method adopted by the invention is as follows:
1) Adopting the microscopic form of a scanning electron microscope watch needle material, wherein the scanning electron microscope is characterized in that: PURE, feina; observing the surface exposure condition of the island phase by using 20 random samples, measuring the exposure radius of the island phase, and cumulatively calculating the exposure area divided by the total area of the visual field;
2) The GB/T14337-2008 standard is adopted to test the fiber strength, and the test instrument is a fiber strength extensometer, the model is as follows: XQ-1A, shanghai Lipu institute of applied science and technology;
3) The linear density of the fiber is tested by adopting the GB/T16256-2008 standard, and the tested instrument is a fiber fineness instrument with the model number: XD-1, shanghai Lipu institute for science and technology of application;
4) The tensile load, the tearing load and the peeling load of the PU leather are tested by adopting the GB/T8949-2008 standard, the thickness of the sample is 0.9mm, the width of the sample is 1cm when the tensile load is measured, the width of the sample is 3cm when the tearing load and the peeling load are measured, and a tested instrument is a computer system tensile testing machine with the model number: AI-7000-S, taiwan high-speed railway;
5) PU leather density test: cutting PU leather product to obtain 10cm-10cm sample, weighing m (unit g), measuring thickness S (unit mm), and measuring density rho = m/10S (unit g/cm) 3 )。
Example 1
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer A, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 1: 100), forming a blend of a sea-phase component and an adventitious island component, melt-blending polymer C and compatibilizer II (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer II to polymer C is 1.5: 100) into a plurality of fine streams, mixing the fine streams with the blend of the sea-phase component and the adventitious island component in a spinning assembly, and discharging filaments from a spinneret to obtain island fibers in an island;
the mass ratio of the polymer A to the polymer B is 8; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 25;
the polymer A is LDPE (the manufacturer is Yanshan petrochemical and the brand is 1I 20A) with the melt index of 20g/10 min; the polymer B is LDPE with a melt index of 75G/10min and a Vicat softening point of 90 ℃ (the manufacturer is Nippon Sumitomo company, and the brand is G807); the polymer C is PA with a melt index of 12g/10min (manufacturer is Meida, new Conn., brand number M32800); the polymer D is PA with a melt index of 12g/10min (the manufacturer is Meida, new Conn., brand M32800); all the compatilizers are LDPE-g-MAH (manufacturer is Shenghao, brand name is PE-12L) with the melt index of 8g/10min and the grafting ratio of 0.8 percent;
the spinning process parameters comprise: the cooling air temperature is 18 ℃, the spinning speed is 650m/min, the concentration of an oiling agent is 1.5wt% when the bundle is wound, the winding speed is 650m/min, the first drawing water bath temperature is 80 ℃, the second drawing water bath temperature is 85 ℃, the speed of a first drawing machine is 20m/min, the speed of a second drawing machine is 50m/min, the concentration of an oiling agent in an oiling agent tank is 5wt%, the temperature of an oiling agent tank is 45 ℃, the speed of a third drawing machine is 60m/min, the drawing total multiple is 3, the temperature of a tow entering a crimping machine is 45 ℃, the speed of the crimping machine is 60m/min, the relaxation heat setting temperature is 50 ℃, the relaxation heat setting time is 12min, the speed of a cutting machine is 65m/min, and the cutting length is 51mm.
The finally prepared island-in-island fiber comprises a sea phase and an island phase as shown in figure 1, wherein the sea phase consists of a sea phase I1 and a sea phase II 2, the sea phase I1 is mainly polymer B mixed with partial polymer A, the sea phase II 2 is mainly polymer A mixed with a small amount of polymer B, the island phase consists of fixed islands 3 and indefinite islands 4, the indefinite islands 4 are distributed around the fixed islands 3, the edges of the fiber are basically free of island phase components, and the proportion of the sum of the exposed areas of the island phases to the surface area of the island fiber in the island is 0.5 percent under a 2000-time scanning electron microscope; the linear density of the island fibers in the island was 4.81dtex, and the strength was 3.42cN/dtex.
Comparative example 1
A method for preparing island-in-island fibers, which is substantially the same as that of example 1, and is different from the method only in that: polymer B was not added during the preparation.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and the proportion of the sum of the exposed areas of the island phases to the surface area of the island fibers in the islands is 18 percent under a scanning electron microscope of 2000 times; the linear density of the island fibers in the island was 4.83dtex, and the strength was 3.02cN/dtex.
Comparing example 1 with comparative example 1, it can be seen that when the surface condition of the fiber is observed by SEM (see fig. 2 and 3), island fibers in the islands obtained in comparative example 1 have a significant exposure of the island phase.
The non-woven fabrics made of the island fibers in the island of the example 1 and the island fibers of the comparative example 1 are heated in an oven (140 ℃,6 min), and then are rolled by a ironing roller (80 ℃) to compare the setting effect, the comparison result is shown in fig. 4 and fig. 5, the non-woven fabric of the example 1 is ironed, the adhesion effect among the fibers is excellent, the compactness of the non-woven fabric is excellent, and the adhesion effect among the fibers is general and the compactness is general after the non-woven fabric of the comparative example 1 is ironed. The difference between the two is that the sea-island fiber obtained in example 1 has substantially no exposure of the island phase because the sea-island phase is not dispersed in the tube wall but is apt to diffuse into the fiber because the difference between the viscosity of the sea phase and the viscosity of the island phase is the largest and the interfacial tension is the largest in the fiber, the melt viscosity difference is generated inside and outside the sea phase in the fiber due to the difference in the flow characteristics, the viscosity difference between the sea phase and the island phase is the largest in the fiber, and the island phase is not stably dispersed in the tube wall during the spinning process, while the polymer B is not added in example 1, and has low viscosity and high fluidity. In addition, polymer B, which is preferred in example 1 to have a specific vicat softening point, can further improve the blocking property between fibers, and it can be seen that the surface of the fibers is significantly flattened.
The mechanical property of the fiber prepared in the example 1 is superior to that of the fiber prepared in the comparative example 1, although the compatilizer is adopted for refining and improving the island diameter of the adventitious islands, the sea phase with the melt viscosity gradually reduced from the center to the edge of the fiber and the island phase modified by the compatilizer LDPE-g-MAH present different wetting properties at different positions, the sea phase in the center of the fiber has longer molecular chains and has higher intermolecular interaction with the LDPE in the compatilizer, so that the adventitious islands from the edge to the center of the fiber are gradually densified and refined and are better and stably distributed around the fixed islands, and after fiber opening, the obtained sea-island fiber has more densified ultrafine fiber bundles, thinner island diameters of the adventitious islands and is more easily distributed along the direction of the fixed islands, and the obtained fiber has better mechanical property.
Example 2
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer A, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 1.3 to 100) to form a blend of a sea-phase component and an adventitious island component, melt-blending polymer C and compatibilizer II (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer II to polymer C is 0.5 to 100) to form a plurality of fine streams, mixing the fine streams with the blend of the sea-phase component and the adventitious island component in a spinning assembly, and discharging from a spinneret to obtain island-in-island fibers;
the mass ratio of the polymer A to the polymer B is 7; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 50;
the polymer A is LDPE (the manufacturer is Yanshan petrochemical and the brand is 1I 20A) with the melt index of 20g/10 min; the polymer B is LDPE with a melt index of 75G/10min and a Vicat softening point of 90 ℃ (the manufacturer is Japan Sumitomo company, the brand number is G807); polymer C was PA (manufactured by Nippon Confucius, inc., brand M33200) having a melt index of 7g/10 min; polymer D was PA with a melt index of 26g/10min (manufacturer: meida, new Congress, brand M2400); all compatibilizers were LDPE-g-MAH with a melt index of 15g/10min and a grafting yield of 1% (Correct from the manufacturer under the designation HC 218);
the spinning process parameters comprise: the cooling air temperature is 15 ℃, the spinning speed is 800m/min, the concentration of an oiling agent is 1.5wt% when winding and bundling are carried out, the winding speed is 800m/min, the first drawing water bath temperature is 81 ℃, the second drawing water bath temperature is 82 ℃, the speed of a first drawing machine is 25m/min, the speed of a second drawing machine is 55m/min, the concentration of an oiling agent in an oiling agent tank is 3wt%, the temperature of the oiling agent tank is 46 ℃, the speed of a third drawing machine is 63m/min, the total drawing multiple is 2.5, the temperature of a tow entering a crimping machine is 48 ℃, the speed of the crimping machine is 63m/min, the relaxation heat setting temperature is 53 ℃, the relaxation heat setting time is 10min, the speed of the cutting machine is 60m/min, and the cutting length is 51mm.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and the proportion of the exposed area sum of the island phases to the surface area of the island fibers in the islands is 0% under a scanning electron microscope of 2000 times; the linear density of the island fibers in the island was 4.83dtex, and the strength was 3.28cN/dtex.
Example 3
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer a, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 0.5 to 100) to form a blend of the sea-phase component and the adventitious island component, melt-blending polymer C and compatibilizer II (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer II to polymer C is 2 to 100) to form a plurality of streams, mixing the streams with the blend of the sea-phase component and the adventitious island component in a spinning assembly, and discharging filaments from a spinneret to obtain island-in-island fibers;
the mass ratio of the polymer A to the polymer B is 3; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 20;
the polymer A is LDPE with the melt index of 35g/10min (the manufacturer is Japan department, and the mark is J3519); the polymer B is LDPE (manufactured by Kanuos and sold under the trademark LD 6622) with the melt index of 70g/10min and the Vicat softening point of 93 ℃; the polymer C is PA with a melt index of 12g/10min (manufacturer is Meida, new Conn., brand number M32800); the polymer D is PA with a melt index of 7g/10min (manufacturer is Meida, new Congress, brand number M33200); all the compatilizers are LDPE-g-MAH (manufacturer is Shenghao, and the brand is PE-12L) with the melt index of 8g/10min and the grafting rate of 0.8 percent;
the spinning process parameters comprise: the cooling air temperature is 16 ℃, the spinning speed is 700m/min, the concentration of an oiling agent is 1.5wt% when the yarn is wound and bunched, the winding speed is 700m/min, the first drawing water bath temperature is 82 ℃, the second drawing water bath temperature is 84 ℃, the first drawing machine speed is 24m/min, the second drawing machine speed is 60m/min, the concentration of an oiling agent in an oiling agent tank is 4wt%, the temperature of the oiling agent tank is 48 ℃, the third drawing machine speed is 68m/min, the total drawing multiple is 2.8, the temperature of the filament bundle entering a crimping machine is 50 ℃, the speed of the crimping machine is 68m/min, the relaxation heat setting temperature is 55 ℃, the relaxation heat setting time is 8min, the speed of the cutting machine is 50m/min, and the cutting length is 51mm.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and the proportion of the sum of the exposed areas of the island phases to the surface area of the island fibers in the island is 2 percent under a scanning electron microscope of 2000 times; the island fibers in the islands had a linear density of 4.79dtex and a strength of 3.52cN/dtex.
Example 4
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer A, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 3;
the mass ratio of the polymer A to the polymer B is 5; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 40;
the polymer A is LDPE with the melt index of 35g/10min (the manufacturer is Japan department, and the mark is J3519); the polymer B is LDPE (manufactured by Kanuos and sold under the trademark LD 6622) with the melt index of 70g/10min and the Vicat softening point of 93 ℃; the polymer C is PA with a melt index of 26g/10min (manufacturer is Meida, new Conn., brand number M2400); the polymer D is PA with a melt index of 7g/10min (manufacturer is Meida, new Congress, brand number M33200); all the compatilizers are LDPE-g-MAH (manufacturer is Shenghao, and the mark is SH-12L) with the melt index of 5g/10min and the grafting rate of 1.2 percent;
the spinning process parameters comprise: the cooling air temperature is 17 ℃, the spinning speed is 600m/min, the concentration of an oiling agent is 1.5wt% when winding and bundling are carried out, the winding speed is 600m/min, the first drawing water bath temperature is 81 ℃, the second drawing water bath temperature is 86 ℃, the first drawing machine speed is 23m/min, the second drawing machine speed is 65m/min, the concentration of an oiling agent in an oiling agent tank is 5wt%, the temperature of an oiling agent tank is 50 ℃, the third drawing machine speed is 72m/min, the total drawing multiple is 3.1, the temperature of a tow entering a crimping machine is 52 ℃, the speed of the crimping machine is 72m/min, the relaxation heat setting temperature is 58 ℃, the relaxation heat setting time is 10min, the speed of the cutting machine is 68m/min, and the cutting length is 51mm.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and the proportion of the exposed area sum of the island phases to the surface area of the island fibers in the islands is 1% under a scanning electron microscope of 2000 times; the island fibers in the island had a linear density of 4.82dtex and a strength of 3.35cN/dtex.
Example 5
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer A, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 2: 100), forming a blend of sea-phase component and adventitious island component, melt-blending polymer C and compatibilizer II (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer II to polymer C is 1: 100) into a plurality of fine streams, mixing the fine streams with the blend of sea-phase component and adventitious island component in a spinning assembly, and discharging filaments from a spinneret to obtain island fibers;
the mass ratio of the polymer A to the polymer B is 2; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 35;
polymer A is LDPE (LG from the manufacturer under the brand name MB 9500) with a melt index of 50g/10 min; the polymer B is LDPE (the manufacturer is Yanshan petrochemical and the brand is 1I 60A) with the melt index of 60g/10min and the Vicat softening point of 105 ℃; the polymer C is PA with a melt index of 12g/10min (manufacturer is Meida, new Conn., brand number M32800); the polymer D is PA with a melt index of 12g/10min (manufacturer is Meida, new Conn., brand number M32800); all compatibilizers were LDPE-g-MAH with a melt index of 15g/10min and a grafting yield of 1% (Correct from the manufacturer under the designation HC 218);
the spinning process parameters comprise: the cooling air temperature is 18 ℃, the spinning speed is 550m/min, the concentration of an oiling agent is 1.5wt% when winding and bundling are carried out, the winding speed is 550m/min, the first drawing water bath temperature is 82 ℃, the second drawing water bath temperature is 88 ℃, the first drawing machine speed is 24m/min, the second drawing machine speed is 70m/min, the concentration of an oiling agent in an oiling agent tank is 5.5wt%, the temperature of an oiling agent tank is 53 ℃, the third drawing machine speed is 77m/min, the total drawing multiple is 3.2, the temperature of a tow entering a crimping machine is 54 ℃, the speed of the crimping machine is 77m/min, the relaxation heat setting temperature is 60 ℃, the relaxation heat setting time is 12min, the speed of a cutting machine is 70m/min, and the cutting length is 51mm.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and the proportion of the exposed area sum of the island phases to the surface area of the island fibers in the islands is 2.5 percent under a scanning electron microscope of 2000 times; the island fibers in the island had a linear density of 4.8dtex and a strength of 3.38cN/dtex.
Example 6
A preparation method of island-in-island fibers comprises the following specific steps: melt-blending polymer a, polymer B, polymer D and compatibilizer I (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer I to polymer D is 2.4 to 100) to form a blend of the sea-phase component and the adventitious island component, melt-blending polymer C and compatibilizer II (the melt-blending temperature is controlled to be higher than the melting points of all raw materials to ensure complete melt-blending, and the mass ratio of compatibilizer II to polymer C is 0.5 to 100) to form a plurality of fine streams, mixing the fine streams with the blend of the sea-phase component and the adventitious island component in a spinning assembly, and discharging from a spinneret to obtain island-in-island fibers;
the mass ratio of the polymer A to the polymer B is 6; the ratio of the sum of the masses of polymer a and polymer B to the sum of the masses of polymer C and polymer D is 30;
polymer A is LDPE (LG from the manufacturer under the brand name MB 9500) with a melt index of 50g/10 min; the polymer B is LDPE (the manufacturer is Yanshan petrochemical and the brand is 1I 60A) with the melt index of 60g/10min and the Vicat softening point of 105 ℃; polymer C was PA (manufactured by Nippon Confucius, inc., brand M33200) having a melt index of 7g/10 min; the polymer D is PA with a melt index of 7g/10min (manufacturer is Meida, new Congress, brand number M33200); all the compatilizers are LDPE-g-MAH (the manufacturer is Shenghao, and the mark is SH-12L) with the melt index of 5g/10min and the grafting rate of 1.2 percent;
the spinning process parameters comprise: the cooling air temperature is 20 ℃, the spinning speed is 500m/min, the concentration of an oiling agent is 1.5wt% when the bundle is wound, the winding speed is 500m/min, the first drawing water bath temperature is 82 ℃, the second drawing water bath temperature is 90 ℃, the first drawing machine speed is 23m/min, the second drawing machine speed is 60m/min, the concentration of an oiling agent in an oiling agent tank is 6wt%, the temperature of the oiling agent tank is 55 ℃, the third drawing machine speed is 80m/min, the total drawing multiple is 3.5, the temperature of the tow entering a crimping machine is 55 ℃, the crimping machine speed is 80m/min, the relaxation heat setting temperature is 65 ℃, the relaxation heat setting time is 11min, the speed of a cutting machine is 68m/min, and the cutting length is 51mm.
The finally prepared island-in-island fibers comprise a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, the indefinite islands are distributed around the fixed islands, and under a scanning electron microscope of 2000 times, the proportion of the sum of the exposed areas of the island phases to the surface area of the island fibers in the islands is 4.2%; the island fibers in the island had a linear density of 4.82dtex and a strength of 3.4cN/dtex.
Example 7
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers prepared in example 1, heating the non-woven fabrics at 140 ℃ and rolling and shaping the non-woven fabrics in sequence, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 89N when the width of a sample is 3cm, the latitudinal peeling load is 83N when the width of the sample is 3cm, the radial tearing load is 80N when the width of the sample is 3cm, the latitudinal tearing load is 73N when the width of the sample is 3cm, the radial tensile load is 165N when the width of the sample is 1cm, the latitudinal tensile load is 142N when the width of the sample is 1cm, and the density is 0.58g/cm 3 。
Comparative example 2
A method for preparing PU leather, which is substantially the same as example 7, except that: the island-in-island fibers used were derived from comparative example 1.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 73N when the width of a sample is 3cm, and the weft peeling load is 3cmThe separation load was 69N, the radial tear load was 68N when the specimen width was 3cm, the weft tear load was 61N when the specimen width was 3cm, the radial tensile load was 130N when the specimen width was 1cm, the weft tensile load was 115N when the specimen width was 1cm, and the density was 0.4g/cm 3 。
Comparing example 7 with comparative example 2, it can be seen that the properties of the island fibers in different islands determine the properties of the PU leather produced therefrom, and as previously mentioned, the fibers obtained in example 1 have two advantages over the fibers obtained in comparative example 1: 1) The surface of the fiber does not basically contain exposed island phases, the heat setting performance is good, the fibers are adhered to each other after being rolled by the ironing roller, and the non-woven fabric is compact, so that the obtained PU leather has higher density, can reach the density of genuine leather and has draping feeling; 2) The fiber has high mechanical property, so that the stripping load, the tearing load and the tensile load of the PU leather obtained by the method are obviously improved.
Example 8
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers in islands prepared in example 2, sequentially heating the non-woven fabrics (the temperature is 140 ℃) and rolling and shaping, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 86N when the width of a sample is 3cm, the latitudinal peeling load is 84N when the width of the sample is 3cm, the radial tearing load is 78N when the width of the sample is 3cm, the latitudinal tearing load is 70N when the width of the sample is 3cm, the radial tensile load is 158N when the width of the sample is 1cm, the latitudinal tensile load is 136N when the width of the sample is 1cm, and the density is 0.6g/cm 3 。
Example 9
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers prepared in example 3, heating the non-woven fabrics at 140 ℃ and rolling and shaping the non-woven fabrics in sequence, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content of the finally prepared PU leather is 40wt%, and the thickness of a finished product is 0.9mm, a peel load in the radial direction of 91N when the specimen width was 3cm, a peel load in the weft direction of 88N when the specimen width was 3cm, a tear load in the radial direction of 82N when the specimen width was 3cm, a tear load in the weft direction of 75N when the specimen width was 3cm, a tensile load in the radial direction of 167N when the specimen width was 1cm, a tensile load in the weft direction of 140N when the specimen width was 1cm, and a density of 0.52g/cm 3 。
Example 10
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers prepared in example 4, heating the non-woven fabrics at 140 ℃ and rolling and shaping the non-woven fabrics in sequence, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 92N when the width of a sample is 3cm, the latitudinal peeling load is 85N when the width of the sample is 3cm, the radial tearing load is 75N when the width of the sample is 3cm, the latitudinal tearing load is 70N when the width of the sample is 3cm, the radial tensile load is 148N when the width of the sample is 1cm, the latitudinal tensile load is 120N when the width of the sample is 1cm, and the density is 0.55g/cm 3 。
Example 11
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers prepared in example 5, heating the non-woven fabrics at 140 ℃ and rolling and shaping the non-woven fabrics in sequence, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 83N when the width of a sample is 3cm, the latitudinal peeling load is 80N when the width of the sample is 3cm, the radial tearing load is 77N when the width of the sample is 3cm, the latitudinal tearing load is 72N when the width of the sample is 3cm, the radial tensile load is 153N when the width of the sample is 1cm, the latitudinal tensile load is 128N when the width of the sample is 1cm, and the density is 0.5g/cm 3 。
Example 12
A preparation method of PU leather comprises the steps of preparing non-woven fabrics from island fibers in islands prepared in example 6, sequentially heating the non-woven fabrics (the temperature is 140 ℃) and rolling and shaping, impregnating the non-woven fabrics with polyurethane slurry, and preparing the PU leather through curing, splitting, drying, splitting, buffing, dyeing and after-finishing.
The PU content in the finally prepared PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peeling load is 90N when the width of a sample is 3cm, the latitudinal peeling load is 86N when the width of the sample is 3cm, the radial tearing load is 85N when the width of the sample is 3cm, the latitudinal tearing load is 76N when the width of the sample is 3cm, the radial tensile load is 178N when the width of the sample is 1cm, the latitudinal tensile load is 146N when the width of the sample is 1cm, and the density is 0.48g/cm 3 。

Claims (7)

1. The island-in-island fiber comprises a sea phase and an island phase, wherein the island phase comprises fixed islands and indefinite islands, and the indefinite islands are distributed around the fixed islands, and the island-in-island fiber is characterized in that the surface of the island fiber in the island is basically free of island phase components, i.e. the total exposed area of the island phase accounts for less than 5% of the surface area of the island fiber in the island under a scanning electron microscope of 2000 times;
the sea phase component is a polymer A and a polymer B, the fixed island component is a polymer C, the indefinite island component is a polymer D, the polymer A and the polymer B are the same or different polymers and can be dissolved in an organic solvent, water or alkali liquor, the polymer C and the polymer D are the same or different polymers and can not be dissolved in a solvent for dissolving the sea phase component, and the melt viscosity relationship of each polymer is as follows: polymer C or polymer D > polymer A > polymer B;
the melt index of the polymer A under the test condition of 190 ℃ for 2.16Kg is 20 to 50g/10min, the melt index of the polymer B under the test condition of 190 ℃ for 2.16Kg is 60 to 75g/10min, and the melt index of the polymer C or the polymer D under the test condition of 235 ℃ for 2.16Kg is 7 to 26g/10min;
the island-in-island fibers further comprise a compatibilizer; the compatilizer is LDPE-g-MAH, the melt index of the compatilizer is 5 to 15g/10min under the test condition of 190 ℃ and 2.16Kg, and the grafting rate is 0.8 to 1.2 percent.
2. The island-in-island fiber according to claim 1, wherein the Vicat softening point of the polymer B is 90 to 105 ℃.
3. The island-in-island fiber according to claim 1, wherein both polymer a and polymer B are LDPE; polymer C and Polymer D are both PA.
4. The island-in-island fiber according to claim 1, wherein the mass ratio of the polymer A to the polymer B is 8 to 6; the ratio of the mass sum of the polymer A and the polymer B to the mass sum of the polymer C and the polymer D is 20 to 50, and the ratio of the mass sum of the polymer A and the polymer B to the mass sum of the polymer D is 50 to 85.
5. The application of the island-in-island fibers in PU leather according to any one of claims 1 to 4, wherein the island-in-island fibers are prepared into a non-woven fabric, impregnated with polyurethane slurry, and then subjected to curing, fiber opening, drying, splitting, buffing, leather polishing, dyeing and after-finishing to prepare the PU leather.
6. The use of claim 5, wherein the nonwoven fabric is subjected to heating and roll-forming treatment before the polyurethane slurry is impregnated.
7. The application of claim 5, wherein the PU content in PU leather is 40wt%, the thickness of a finished product is 0.9mm, the radial peel load is 83 to 92N when the width of a sample is 3cm, the weft peel load is 80 to 88N when the width of the sample is 3cm, the radial tear load is 75 to 85N when the width of the sample is 3cm, the weft tear load is 70 to 76N when the width of the sample is 3cm, the radial tensile load is 148 to 178N when the width of the sample is 1cm, the weft tensile load is 120 to 146N when the width of the sample is 1cm, and the density is 0.48 to 0.60g/cm 3 。
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CN113089124B (en) * 2021-03-30 2023-01-17 上海华峰超纤科技股份有限公司 Anti-hair-falling figured sea-island fiber for PU (polyurethane) microfiber leather and preparation and application thereof

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CN102168321A (en) * 2011-04-09 2011-08-31 禾欣可乐丽超纤皮(嘉兴)有限公司 Sea-island type composite fiber manufacture method
CN102650081A (en) * 2011-02-25 2012-08-29 上海华峰超纤材料股份有限公司 Color fixed island composite short fiber and preparation method thereof
CN103788636A (en) * 2014-02-20 2014-05-14 安安(中国)有限公司 High polymer blending system for manufacturing high-fineness high-strength non-figured PA6 superfine fibers
CN110923849A (en) * 2019-12-21 2020-03-27 上海华峰超纤科技股份有限公司 Fixed island/indefinite island type superfine fiber, superfine fiber synthetic leather and preparation method

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CN102650081A (en) * 2011-02-25 2012-08-29 上海华峰超纤材料股份有限公司 Color fixed island composite short fiber and preparation method thereof
CN102168321A (en) * 2011-04-09 2011-08-31 禾欣可乐丽超纤皮(嘉兴)有限公司 Sea-island type composite fiber manufacture method
CN103788636A (en) * 2014-02-20 2014-05-14 安安(中国)有限公司 High polymer blending system for manufacturing high-fineness high-strength non-figured PA6 superfine fibers
CN110923849A (en) * 2019-12-21 2020-03-27 上海华峰超纤科技股份有限公司 Fixed island/indefinite island type superfine fiber, superfine fiber synthetic leather and preparation method

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