CN115747988A - Preparation method of superfine fiber taking modified PVA as sea - Google Patents
Preparation method of superfine fiber taking modified PVA as sea Download PDFInfo
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Abstract
The invention discloses a preparation method of sea superfine fiber by using modified PVA, which takes nylon (PA 6)/polyvinyl alcohol (PVA) as two phases, wherein the PVA is a sea component, and the PA6 is an island component, and the preparation method comprises the following steps of S1: pre-crystallization of PVA: the pre-crystallization temperature of the PVA master batch is maintained between 105 ℃ and 145 ℃, the pre-crystallization time is 20 min to 23min, crystals with the crystallinity of 37 percent to 40 percent are obtained, and the crystals are sliced. The invention realizes melt co-extrusion in different temperature zones in the same extruder through a multi-temperature zone screw extruder, effectively avoids the problem that two-phase melt temperature is different and the problem that PVA of the PVA can be decomposed when meeting high-temperature PA and can not be melt compounded for spinning due to conjugate compounding.
Description
Technical Field
The invention relates to the technical field of superfine fibers, in particular to a preparation method of a superfine fiber taking modified PVA as sea.
Background
The superfine fiber is attracted by people due to the properties of high coverage, soft hand feeling, comfortable wearing, soft luster, good adsorbability and the like, and is widely applied to the fields of clothes, artificial leather, building materials, adsorption and filter materials and the like.
Island-in-sea fibers are fibers in which one polymer is dispersed in another polymer, the dispersed phase is in the form of "islands" in the fiber cross-section, and the matrix corresponds to "sea", where one component is surrounded by another component in a finely dispersed state as if there were many islands in the sea when viewed in the cross-section of the fiber.
The existing superfine fiber is compounded and extruded into filaments after the sea phase and the island phase are melted, but after the sea phase and the island phase are mixed according to a proportion, the bonding effect between the two phases is poor due to different melting temperatures of the sea phase and the island phase, if the sea phase and the island phase are respectively extruded into filaments and then spun into filaments for forming, the two phases cannot be well uniform due to the fact that the two phases need to be stretched and shaped for multiple times to be compounded, and the island phase distribution effect is poor when the sea phase is subsequently dissolved.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of sea superfine fiber by using modified PVA.
The invention provides a method for preparing sea superfine fiber by using modified PVA, which is characterized in that the sea superfine fiber by using the modified PVA is prepared by using nylon (PA 6)/polyvinyl alcohol (PVA) as two phases, the PVA is a sea component, the PA6 is an island component, and the superfine fiber with the outgoing line density of 0.11-0.35dtex is prepared by conjugate composite spinning and alkali decrement treatment, and the method for preparing the sea superfine fiber by using the modified PVA is carried out according to the following steps:
s1: pre-crystallization of PVA: maintaining the pre-crystallization temperature of the PVA master batch at 105-145 ℃, wherein the pre-crystallization time is 20-23min, obtaining crystals with the crystallinity of 37-40%, and slicing the crystals;
s2: drying the PVA slices and the PA6 slices: the PVA slice is dried continuously by hot air, the drying temperature is required to be between 150 ℃ and 165 ℃, the drying time is controlled to be between 6.0 and 7.5 hours, the water content of the PVA dry slice is between 65 and 70 mu g/g, meanwhile, the PA6 slice can be dried by low dew point (-80 ℃) and low temperature air, the drying time is controlled to be between 6.0 and 7.2 hours, and the water content of the PA6 dry slice is between 75 mu g/g and 85 mu g/g;
s3: melt extrusion: respectively extruding and melting PVA dry slices and PA6 dry slices in a multi-temperature-zone screw extruder, respectively feeding two dry slice melts into a melt pipeline for heating, wherein the heating temperature of the two dry slice melts is set to ensure that islands and sea are formed after the two raw material melts are respectively contacted by a distribution pipeline of a temperature zone in the multi-temperature-zone screw extruder, and the water-soluble PVA is not subjected to thermal decomposition to be standard;
wherein the distribution of the PVA dry slices in the temperature zones of the multi-temperature zone screw extruder from the input end to the output end is 106-108 ℃ in the first zone, 116-118 ℃ in the second zone, 130-133 ℃ in the third zone, 140-142 ℃ in the fourth zone and 150-152 ℃ in the fifth zone in sequence;
wherein the temperature distribution of the PA6 dry slices in the multi-temperature-zone screw extruder from the input end to the output end is sequentially a first zone of 212-215 ℃, a second zone of 230-232 ℃, a third zone of 240-242 ℃, a fourth zone of 252-254 ℃ and a fifth zone of 261-263 ℃;
s4: composite spinning: respectively feeding two raw material melts into a spinning machine arranged at the tail end of a multi-temperature-zone screw extruder, accurately metering by a metering pump, extruding, distributing into a composite assembly in a spinning box body, uniformly distributing island components into sea components through a distribution pipeline in the composite assembly, spraying out from the same spinneret orifice, and carrying out composite spinning to obtain sea-island nascent fibers taking PA as the island components and PVA as the sea components, wherein the fiber ratio of PVA/PA6 accurately metered by the metering pump in the spinning box body is 30/70-35/65, and the spinning pressure is 8.5-10.0MPa;
s5: removing sea phases: stretching and shaping the prepared sea-island nascent fiber to obtain a sea-island fiber filament, placing the sea-island fiber filament in anhydrous methanol or anhydrous ethanol, then quickly pouring the sea-island fiber filament into purified water, homogenizing the sea-island nascent fiber in the purified water for 5 to 10 minutes, gradually heating to 80 ℃, and keeping the temperature for 45 to 50 minutes, so that the sea component PVA in the sea-island fiber filament can be completely dissolved, and the cluster island component superfine fiber can be obtained, wherein the fiber linear density of the cluster island component superfine fiber is 0.30 to 0.60 dtex;
s6: stretching and shaping: and oiling, redrawing and shaping the superfine fibers with the island phase dissolved completely to obtain superfine fibers with target line-out density, wherein the linear density of the redrawn cluster-shaped island phase component superfine fibers is between 0.11 and 0.35 dtex.
Further: the multi-temperature-zone screw extruder in the S3 comprises a driving unit, a hot melting unit and an extruding piece, wherein the driving unit is connected to the end part of the hot melting unit, the other end of the hot melting unit is connected with the outer wall of the spinning box body, the extruding piece is installed at the joint of the hot melting unit and the driving unit, and the outer wall of the extruding piece is provided with a feeding hopper.
Further: the hot melt unit includes first conveying pipeline, second conveying pipeline, heating ring and crowded flange altogether, first conveying pipeline, second conveying pipeline parallel arrangement, and the same side tip of first conveying pipeline, second conveying pipeline is connected to the inside of crowded flange altogether, a plurality of heating ring distributes on the outer wall of first conveying pipeline, second conveying pipeline, and the outer wall of first conveying pipeline, second conveying pipeline still installs temperature sensor, equal electric connection between temperature sensor's signal end and a plurality of heating ring.
Further: the heating ring comprises an electric heating coil, a heat conducting cavity and a fan, the fan is installed on the outer wall of the bottom end of the heat conducting cavity, and the electric heating coil is installed above the connecting position of the heat conducting cavity and the fan.
Further: the extruding part comprises an extruding cylinder and extruding screw rods, the extruding cylinder comprises two symmetrical cavities, the extruding screw rods are respectively arranged in the two cavities, and the end parts of the two extruding screw rods are respectively connected with the driving unit.
Further: spinning manifold in S4 includes thermal-insulated casing, composite set, through dish, blowout flange and goes the sea unit, composite set installs in the one end inner wall of thermal-insulated casing, the blowout flange is installed on the tip outer wall of thermal-insulated casing, and locates between composite set and the blowout flange through the dish, go the sea unit and install on the outer wall of thermal-insulated casing, and go the sea unit and be used for getting rid of sea component PVA.
Further: the sea removing unit comprises a plurality of liquid inlet pipes and liquid outlet pipes, and the liquid inlet pipes and the liquid outlet pipes are distributed on the outer wall of the heat insulation shell.
Further: the composite component comprises an extrusion piece, a bracket, a pressing seat and an extrusion unit, wherein the bracket and the pressing seat are symmetrically distributed on two sides of the extrusion piece, and the extrusion unit drives the pressing seat to extrude the extrusion piece along the vertical direction.
Further: the extrusion unit comprises a driving motor, a cam, an ejector rod and a reset spring, an output shaft of the driving motor is installed at the axis of the cam, a pressing plate is installed at the top of the pressing seat, the reset spring is installed on the outer walls of the two ends of the pressing plate, the ejector rod is installed on the outer wall of the top end of the pressing plate, and the bottom end of the cam is abutted to the outer wall of the top end of the ejector rod.
Further: the extrusion piece comprises a capsule body and inner guide pieces, wherein the inner guide pieces are annularly distributed on the inner wall of the capsule body, and the inner guide pieces are of sheet structures bent along spiral arcs.
The beneficial effects of the invention are as follows:
this PVA carries out the pre-crystallization, it is more stable to get rid of impurity and make its melting temperature interval simultaneously, through multi-temperature-zone screw extruder, different warm areas realize the melting coextrusion in same extruder, the problem that double-phase melting temperature is different has effectively been avoided, conjugate recombination makes its PVA meet the PA of high temperature and take place to decompose and the problem of unable melting composite spinning, when crowded adoption utricule extrudees repeatedly simultaneously, make the spinning spout fast, draw and draw to passing through dish surface screw channel, make its surface fully expose, can improve the acceleration of sea phase and dissolve out, the spinning rapid prototyping that extrudes through the utricule, dissolve out island phase stretch forming simultaneously, make its island phase distribute evenly, the tensile strength and the play linear density of superfine fiber all obtain the improvement.
Drawings
FIG. 1 is a flow chart of the preparation method of sea microfiber modified PVA according to the present invention;
FIG. 2 is a schematic structural view of a multi-temperature zone screw extruder for the method for preparing sea microfiber by using modified PVA according to the present invention;
FIG. 3 is a schematic structural view of the fuse unit of FIG. 2;
FIG. 4 is a schematic structural diagram of a spinning manifold of a method for preparing sea microfiber by using modified PVA according to the present invention;
FIG. 5 is a schematic view of the composite assembly of FIG. 4;
fig. 6 is a schematic view of the extruded structure of fig. 5.
In the figure: 100. a base; 200. a drive unit; 300. a feed hopper; 400. a heat-melting unit; 410. an extrusion member; 420. a first feed delivery pipe; 430. a second delivery pipe; 440. a heating ring; 450. a temperature sensor; 460. co-extruding a flange; 500. spinning manifold; 510. a composite component; 511. an extrusion member; 511a, a capsule body; 511b, an inner guide sheet; 512. a bracket; 513. pressing a plate; 514. pressing a base; 515. a return spring; 516. a cam; 517. a drive motor; 518. a top rod; 520. passing through the disc; 530. a thermally insulated housing; 540. ejecting a flange; 550. a liquid inlet pipe; 560. a liquid outlet pipe; 570. and (7) a temperature controller.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, a method for preparing sea superfine fiber from modified PVA, wherein the sea superfine fiber is prepared from nylon (PA 6)/polyvinyl alcohol (PVA) as two phases, the PVA is a sea component, the PA6 is an island component, and the superfine fiber with the outgoing line density of 0.11-0.35dtex is prepared by conjugate composite spinning and alkali weight reduction treatment, and the method for preparing sea superfine fiber from modified PVA is carried out according to the following steps:
s1: pre-crystallization of PVA: maintaining the pre-crystallization temperature of the PVA master batch at 105-145 ℃, wherein the pre-crystallization time is 20-23min, obtaining crystals with the crystallinity of 37-40%, and slicing the crystals;
s2: drying the PVA slices and the PA6 slices: the PVA slices are dried by hot air continuously, the drying temperature is required to be between 150 and 165 ℃, the drying time is controlled to be between 6.0 and 7.5 hours, the water content of the PVA dry slices is between 65 and 70 mu g/g, meanwhile, the PA6 slices can be dried by low dew point (-80 ℃) and low temperature air, the drying time is controlled to be between 6.0 and 7.2 hours, and the water content of the PA6 dry slices is between 75 mu g/g and 85 mu g/g;
s3: melt extrusion: respectively extruding and melting PVA dry slices and PA6 dry slices in a multi-temperature-zone screw extruder, respectively feeding two dry slice melts into a melt pipeline for heating, wherein the heating temperature of the two dry slice melts is set to ensure that islands and sea are formed after the two raw material melts are respectively contacted by a distribution pipeline of a temperature zone in the multi-temperature-zone screw extruder, and the water-soluble PVA is not subjected to thermal decomposition to be standard;
wherein the temperature distribution of the PVA dry slices in the multi-temperature-zone screw extruder is that a first zone is 106-108 ℃, a second zone is 116-118 ℃, a third zone is 130-133 ℃, a fourth zone is 140-142 ℃ and a fifth zone is 150-152 ℃ from the input end to the output end;
wherein the temperature distribution of the PA6 dry slices in the multi-temperature-zone screw extruder from the input end to the output end is sequentially a first zone of 212-215 ℃, a second zone of 230-232 ℃, a third zone of 240-242 ℃, a fourth zone of 252-254 ℃ and a fifth zone of 261-263 ℃;
s4: composite spinning: respectively feeding the two raw material melts into a spinning machine arranged at the tail end of a multi-temperature-zone screw extruder, accurately metering by a metering pump, extruding, distributing into a composite assembly 510 in a spinning manifold 500, uniformly distributing island components into sea components through a distribution pipeline in the composite assembly 510, spraying out from the same spinneret orifice, and carrying out composite spinning to obtain sea-island type nascent fibers taking PA as the island components and PVA as the sea components, wherein the fiber ratio of PVA/PA6 accurately metered by the metering pump in the spinning manifold 500 is 30/70-35/65, and the spinning pressure is 8.5-10.0MPa;
s5: removing sea phases: stretching and shaping the prepared sea-island nascent fiber to obtain a sea-island fiber filament, placing the sea-island fiber filament in anhydrous methanol or anhydrous ethanol, then quickly pouring the sea-island fiber filament into purified water, homogenizing the sea-island nascent fiber in the purified water for 5 to 10 minutes, gradually heating to 80 ℃, and keeping the temperature for 45 to 50 minutes, so that the sea component PVA in the sea-island fiber filament can be completely dissolved, and the cluster island component superfine fiber can be obtained, wherein the fiber linear density of the cluster island component superfine fiber is 0.30 to 0.60 dtex;
s6: stretching and shaping: and oiling, redrawing and shaping the superfine fibers with the island phase dissolved completely to obtain the superfine fibers with the target outlet density, wherein the linear density of the redrawn cluster-shaped island phase component superfine fibers is between 0.11 and 0.35 dtex.
Referring to fig. 2 to 6, in the S3 step, the multi-temperature zone screw extruder includes a driving unit 200, a hot melting unit 400, and an extruding member 410, the driving unit 200 is connected to an end of the hot melting unit 400, and the other end of the hot melting unit 400 is connected to an outer wall of the spinning beam 500, the extruding member 410 is installed at a connection position of the hot melting unit 400 and the driving unit 200, and the outer wall of the extruding member 410 is installed with the feeding hopper 300.
It should be added that the multi-temperature zone screw extruder is further provided with a base 100, and the driving unit 200, the hot melting unit 400 and the extruding piece 410 are all installed above the base 100;
The extruding part 410 includes an extruding cylinder and an extruding screw, the extruding cylinder includes two symmetrical cavities, the extruding screws are respectively installed in the two cavities, and the end portions of the two extruding screws are respectively connected with the driving unit 200.
It should be added that a partition board is arranged in the feed hopper 300, PVA and PA6 are respectively put into two sides of the partition board, and two sides of the bottom end of the feed hopper 300 are respectively communicated with the cavity;
in step S4, the spinning beam 500 includes a heat insulation housing 530, a composite assembly 510, a pass through plate 520, a blowing flange 540, and a sea removal unit, wherein the composite assembly 510 is mounted on an inner wall of one end of the heat insulation housing 530, the blowing flange 540 is mounted on an outer wall of an end portion of the heat insulation housing 530, and is disposed between the composite assembly 510 and the blowing flange 540 through the plate 520, the sea removal unit is mounted on an outer wall of the heat insulation housing 530, and the sea removal unit is used for removing the sea component PVA.
The sea-going unit comprises a plurality of liquid inlet pipes 550 and liquid outlet pipes 560, and the liquid inlet pipes 550 and the liquid outlet pipes 560 are distributed on the outer wall of the heat insulation shell 530.
The composite assembly 510 includes an extrusion 511, a bracket 512, a pressing base 514, and a pressing unit, wherein the bracket 512 and the pressing base 514 are symmetrically disposed on two sides of the extrusion 511, and the pressing unit drives the pressing base 514 to extrude the extrusion 511 along a vertical direction.
The extrusion unit comprises a driving motor 517, a cam 516, a push rod 518 and a return spring 515, an output shaft of the driving motor 517 is installed at the axis of the cam 516, a pressing plate 513 is installed at the top of a pressing seat 514, the return spring 515 is installed on the outer walls of the two ends of the pressing plate 513, the push rod 518 is installed on the outer wall of the top end of the pressing plate 513, and the bottom end of the cam 516 abuts against and is connected to the outer wall of the top end of the push rod 518.
The extruding member 511 includes a capsule body 511a and inner guide pieces 511b, the inner guide pieces 511b are annularly distributed on the inner wall of the capsule body 511a, and the inner guide pieces 511b are sheet structures curved along a spiral arc.
It should be added, in the step S3, the PVA dry slices and the PA6 dry slices enter the extrusion part 511 through the feeding hopper 300, are pushed into the first conveying pipe 420 and the second conveying pipe 430 through the extrusion screw, and sequentially pass through the heating rings 440 with different temperatures through the extrusion process, wherein the distribution of the PVA dry slices in the temperature zones of the multi-temperature zone screw extruder is sequentially from the input end to the output end, namely, from one zone 106 to 108 ℃, from two zones 116 to 118 ℃, from three zones 130 to 133 ℃, from four zones 140 to 142 ℃ and from five zones 150 to 152 ℃, wherein the distribution of the PA6 dry slices in the temperature zones of the multi-temperature zone screw extruder is sequentially from the input end to the output end, from one zone 212 to 215 ℃, from two zones 230 to 232 ℃, from three zones 240 to 242 ℃, from four zones 252 to 254 ℃ and from five zones 261 to 263 ℃, and are then extruded through the co-extrusion flange 460, and the extruded fibers enter the spinning manifold 500;
it should be further noted that, after entering the spinning manifold 500, step S4 is performed, before entering the spinning manifold 500, the purified water is metered and extruded by a metering pump, and when entering the composite assembly 510, in the capsule 511a, the driving motor 517 continuously rotates to rotate, so as to drive the cam 516 structure to rotate around the output shaft of the driving motor 517, the cam 516 structure is in a heart shape, so when rotating, through the larger outer diameter part of the cam 516, the ejector 518 is pressed down, and the smaller inner diameter part of the cam 518 is continuously abutted against the smaller inner diameter part of the cam 516 under the action of the return spring 515, so that the pressing plate 513 is sprung up, the pressing seat 514 does not press the capsule 511a any more, one cycle is two times of pressing and one time of springback, so as to form a mixture in the capsule 511a, the inner diameter of the nozzle hole formed at the end of the capsule 511a is between 10 μm and 50 μm, and simultaneously enters the heat insulation shell 530, continuously passes through the threaded channel on the disc 520, ethanol is first input through one of the liquid inlet pipe 550, after soaking, the purified water is extracted, then the purified water is injected, the temperature controller 570 is gradually detected, and the purified water is extracted until the purified water is gradually, the purified water is extracted, and the purified water is gradually, and the purified water is discharged through the island-shaped purified water collection flange 540 after the temperature is increased, and the purified water is discharged, and the purified water collection flange 540, and the purified water is discharged through the purified water collection;
the preparation method adopts a conjugate compounding method, so that PVA of the composite fiber can be decomposed when meeting high-temperature PA and can not be fused and compounded with spinning, meanwhile, when a capsule body 511a is adopted for coextrusion and repeated extrusion, the spinning is quickly sprayed and is pulled to pass through a thread channel on the surface of a disc 520, the surface of the disc 520 is fully exposed, the accelerated dissolution of sea phases can be improved, the spinning extruded from the capsule body 511a is quickly formed, dissolution islands are simultaneously formed in a stretching mode, the island phases are uniformly distributed, and the tensile strength and the line outlet density of the superfine fiber are improved.
Example two
Referring to fig. 1, a method for preparing sea superfine fibers from modified PVA, wherein the sea superfine fibers are prepared from nylon (PA 6)/polyvinyl alcohol (PVA) as two phases, the PVA is a sea component, the PA6 is an island component, and the superfine fibers with the outgoing line density of 0.11 to 0.35dtex through conjugate composite spinning and alkali decrement treatment, comprises the following steps:
s1: pre-crystallization of PVA: maintaining the pre-crystallization temperature of the PVA master batch at 105-145 ℃, wherein the pre-crystallization time is 20-23min, obtaining crystals with the crystallinity of 37-40%, and slicing the crystals;
s2: drying PVA slices and PA6 slices: the PVA slices are dried continuously by hot air, the drying temperature is required to be between 150 ℃ and 165 ℃, particularly 160 ℃, the drying time is controlled to be between 6.0 and 7.5 hours, particularly 6.5 hours, the water content of the PVA dry slices is between 65 and 70 mu g/g, meanwhile, the PA6 slices can be dried by low dew point (-80 ℃) and low temperature air, the drying time is controlled to be between 6.0 and 7.2 hours, particularly 6.8 hours, and the water content of the PA6 dry slices is between 75 mu g/g and 85 mu g/g;
s3: melt extrusion: respectively extruding and melting PVA dry slices and PA6 dry slices in a multi-temperature-zone screw extruder, respectively feeding the two dry slice melts into melt pipelines for heating, wherein the heating temperature of the two dry slice melts is set to ensure that an island and a sea are formed after the two raw material melts are respectively contacted through distribution pipelines of temperature zones in the multi-temperature-zone screw extruder, and the water-soluble PVA is not subjected to thermal decomposition to meet the standard;
wherein the distribution of the PVA dry slices in the temperature zones of the multi-temperature zone screw extruder from the input end to the output end is 106-108 ℃ in the first zone, 116-118 ℃ in the second zone, 130-133 ℃ in the third zone, 140-142 ℃ in the fourth zone and 150-152 ℃ in the fifth zone in sequence;
specifically, the temperature of a first area is 106 ℃, a second area is 117 ℃, a third area is 131 ℃, a fourth area is 140 ℃ and a fifth area is 150 ℃;
wherein the temperature distribution of the PA6 dry slices in the multi-temperature-zone screw extruder from the input end to the output end is sequentially a first zone of 212-215 ℃, a second zone of 230-232 ℃, a third zone of 240-242 ℃, a fourth zone of 252-254 ℃ and a fifth zone of 261-263 ℃;
specifically, the temperature of the first zone is 214 ℃, the temperature of the second zone is 230 ℃, the temperature of the third zone is 242 ℃, the temperature of the fourth zone is 253 ℃ and the temperature of the fifth zone is 262 ℃;
s4: composite spinning: respectively feeding the two raw material melts into a spinning machine arranged at the tail end of a multi-temperature-zone screw extruder, accurately metering the melts by a metering pump, extruding the melts, distributing the melts into a composite component 510 in a spinning manifold 500, uniformly distributing an island component into a sea component through a distribution pipeline in the composite component 510, and spraying the sea component from the same spinneret orifice to perform composite spinning to obtain sea-island type nascent fibers with PA as the island component and PVA as the sea component, wherein the fiber ratio of PVA/PA6 accurately metered by the metering pump in the spinning manifold 500 is 30/70-35/65, specifically 30/70, and the spinning pressure is 8.5-10.0MPa;
s5: removing sea phases: stretching and shaping the prepared sea-island nascent fiber to obtain a sea-island fiber filament, placing the sea-island fiber filament in anhydrous methanol or anhydrous ethanol, then quickly pouring the sea-island fiber filament into purified water, homogenizing the sea-island nascent fiber in the purified water for 5 to 10 minutes, gradually heating to 80 ℃, and keeping the temperature for 45 to 50 minutes, so that the sea component PVA in the sea-island fiber filament can be completely dissolved, and the cluster island component superfine fiber can be obtained, wherein the fiber linear density of the cluster island component superfine fiber is 0.30 to 0.60 dtex;
s6: stretching and shaping: and oiling, redrawing and shaping the superfine fibers with the island phase dissolved completely to obtain the superfine fibers with the target outlet density, wherein the linear density of the redrawn cluster-shaped island phase component superfine fibers is between 0.11 and 0.35 dtex.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. A modified PVA is the superfine fiber preparation method of the sea, the superfine fiber of this modified PVA is the superfine fiber of sea, this modified PVA is that nylon (PA 6)/polyvinyl alcohol (PVA) are two-phase, its PVA is "sea" component, PA6 is "island" component, the superfine fiber of the outgoing line density that is prepared out through conjugate composite spinning and alkali decrement treatment is 0.11-0.35dtex, characterized by, this modified PVA is the superfine fiber preparation method of the sea, go on according to the following step:
s1: pre-crystallization of PVA: maintaining the pre-crystallization temperature of the PVA master batch at 105-145 ℃, wherein the pre-crystallization time is 20-23min, obtaining crystals with the crystallinity of 37-40%, and slicing the crystals;
s2: drying the PVA slices and the PA6 slices: the PVA slices are dried by hot air continuously, the drying temperature is required to be between 150 and 165 ℃, the drying time is controlled to be between 6.0 and 7.5 hours, the water content of the PVA dry slices is between 65 and 70 mu g/g, meanwhile, the PA6 slices can be dried by low dew point (-80 ℃) and low temperature air, the drying time is controlled to be between 6.0 and 7.2 hours, and the water content of the PA6 dry slices is between 75 mu g/g and 85 mu g/g;
s3: melt extrusion: respectively extruding and melting PVA dry slices and PA6 dry slices in a multi-temperature-zone screw extruder, respectively feeding the two dry slice melts into melt pipelines for heating, wherein the heating temperature of the two dry slice melts is set to ensure that an island and a sea are formed after the two raw material melts are respectively contacted through distribution pipelines of temperature zones in the multi-temperature-zone screw extruder, and the water-soluble PVA is not subjected to thermal decomposition to meet the standard;
wherein the distribution of the PVA dry slices in the temperature zones of the multi-temperature zone screw extruder from the input end to the output end is 106-108 ℃ in the first zone, 116-118 ℃ in the second zone, 130-133 ℃ in the third zone, 140-142 ℃ in the fourth zone and 150-152 ℃ in the fifth zone in sequence;
wherein the temperature distribution of the PA6 dry slices in the multi-temperature-zone screw extruder from the input end to the output end is sequentially a first zone of 212-215 ℃, a second zone of 230-232 ℃, a third zone of 240-242 ℃, a fourth zone of 252-254 ℃ and a fifth zone of 261-263 ℃;
s4: composite spinning: respectively feeding the two raw material melts into a spinning machine arranged at the tail end of a multi-temperature-zone screw extruder, extruding after accurately metering by a metering pump, distributing into a composite component (510) in a spinning manifold (500), uniformly distributing island components into sea components through a distribution pipeline in the composite component (510), spraying out from the same spinneret orifice, and carrying out composite spinning to obtain sea-island type nascent fibers taking PA as the island components and PVA as the sea components, wherein the fiber ratio of PVA/PA6 accurately metered by the metering pump in the spinning manifold (500) is 30/70-35/65, and the spinning pressure is 8.5-10.0MPa;
s5: removing sea phases: stretching and shaping the prepared sea-island nascent fiber to obtain a sea-island fiber filament, placing the sea-island fiber filament in anhydrous methanol or anhydrous ethanol, then quickly pouring the sea-island fiber filament into purified water, homogenizing the sea-island nascent fiber in the purified water for 5 to 10 minutes, gradually heating to 80 ℃, and keeping the temperature for 45 to 50 minutes, so that the sea component PVA in the sea-island fiber filament can be completely dissolved, and the cluster island component superfine fiber can be obtained, wherein the fiber linear density of the cluster island component superfine fiber is 0.30 to 0.60 dtex;
s6: stretching and shaping: and oiling, redrawing and shaping the superfine fibers with the island phase dissolved completely to obtain the superfine fibers with the target outlet density, wherein the linear density of the redrawn cluster-shaped island phase component superfine fibers is between 0.11 and 0.35 dtex.
2. The method for preparing sea microfiber of modified PVA according to claim 1, wherein the multi-temperature zone screw extruder in S3 comprises a driving unit (200), a hot melting unit (400) and an extruding piece (410), wherein the driving unit (200) is connected to the end of the hot melting unit (400), the other end of the hot melting unit (400) is connected with the outer wall of the spinning beam (500), the extruding piece (410) is installed at the joint of the hot melting unit (400) and the driving unit (200), and the outer wall of the extruding piece (410) is provided with the feed hopper (300).
3. The method as claimed in claim 2, wherein the hot melting unit (400) comprises a first material delivery pipe (420), a second material delivery pipe (430), heating rings (440) and a co-extrusion flange (460), the first material delivery pipe (420) and the second material delivery pipe (430) are arranged in parallel, the ends of the first material delivery pipe (420) and the second material delivery pipe (430) on the same side are connected to the inside of the co-extrusion flange (460), the heating rings (440) are distributed on the outer walls of the first material delivery pipe (420) and the second material delivery pipe (430), the outer walls of the first material delivery pipe (420) and the second material delivery pipe (430) are further provided with temperature sensors (450), and the signal ends of the temperature sensors (450) are electrically connected with the heating rings (440).
4. The method for preparing superfine sea fiber PVA of claim 3, wherein the heating ring (440) comprises an electric heating coil, a heat conducting cavity and a fan, the fan is arranged on the outer wall of the bottom end of the heat conducting cavity, and the electric heating coil is arranged above the joint of the heat conducting cavity and the fan.
5. The method for preparing superfine sea fiber PVA according to claim 2, wherein the extruding part (410) comprises an extruding cylinder and an extruding screw, the extruding cylinder comprises two symmetrical cavities, the extruding screws are respectively arranged in the two cavities, and the ends of the two extruding screws are respectively connected with the driving unit (200).
6. The method of claim 1, wherein the spinning beam (500) in the step S4 comprises a heat insulation shell (530), a composite assembly (510), a through disc (520), a spraying flange (540) and a sea removing unit, wherein the composite assembly (510) is installed on an inner wall of one end of the heat insulation shell (530), the spraying flange (540) is installed on an outer wall of an end of the heat insulation shell (530), the spraying flange is arranged between the composite assembly (510) and the spraying flange (540) through the disc (520), the sea removing unit is installed on an outer wall of the heat insulation shell (530), and the sea removing unit is used for removing the sea component PVA.
7. The method for preparing superfine sea fiber PVA according to claim 1, wherein the sea removing unit comprises a plurality of liquid inlet pipes (550) and liquid outlet pipes (560), and the liquid inlet pipes (550) and the liquid outlet pipes (560) are distributed on the outer wall of the heat insulation shell (530).
8. The method for preparing superfine fiber with modified PVA as sea according to claim 1, wherein the composite assembly (510) comprises an extrusion piece (511), a bracket (512), a pressing seat (514) and a squeezing unit, the bracket (512) and the pressing seat (514) are symmetrically distributed on two sides of the extrusion piece (511), and the squeezing unit drives the pressing seat (514) to squeeze the extrusion piece (511) along the vertical direction.
9. The method for preparing the ultrafine fiber with the modified PVA being as the sea, as recited in claim 1, wherein the extrusion unit comprises a driving motor (517), a cam (516), a push rod (518) and a return spring (515), an output shaft of the driving motor (517) is installed at an axial center of the cam (516), a press plate (513) is installed on the top of the press seat (514), the return spring (515) is installed on outer walls of two ends of the press plate (513), the push rod (518) is installed on an outer wall of a top end of the press plate (513), and a bottom end of the cam (516) is connected against an outer wall of the top end of the push rod (518).
10. A method for preparing ultrafine fibers according to claim 1, wherein the said extrusion member (511) comprises a capsule body (511 a) and an inner guide sheet (511 b), the said inner guide sheet (511 b) is distributed annularly on the inner wall of the capsule body (511 a), and the said inner guide sheet (511 b) is a sheet structure curved along a spiral arc.
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| CN108396435A (en) * | 2018-04-24 | 2018-08-14 | 青岛大学 | A kind of Novel super-thin fabric lining based on modified PVA sea-island fibre |
| CN108532027A (en) * | 2018-04-24 | 2018-09-14 | 山东科贝尔非织造材料科技有限公司 | PA/PVA sea-island fibres and its production technology with water-soluble marine facies |
| CN108589028A (en) * | 2018-04-24 | 2018-09-28 | 山东科贝尔非织造材料科技有限公司 | A kind of novel island fiber synthetic leather base cloth and its production technology |
| CN111733480A (en) * | 2020-07-07 | 2020-10-02 | 上海市合成纤维研究所有限公司 | Sea-island fiber with PA6 as island component, preparation method thereof and superfine fiber formed by same |
| CN115094538A (en) * | 2022-06-06 | 2022-09-23 | 明新旭腾新材料股份有限公司 | Preparation method of superfine sea-island fiber taking efficient water-soluble modified PVA as sea |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396435A (en) * | 2018-04-24 | 2018-08-14 | 青岛大学 | A kind of Novel super-thin fabric lining based on modified PVA sea-island fibre |
| CN108532027A (en) * | 2018-04-24 | 2018-09-14 | 山东科贝尔非织造材料科技有限公司 | PA/PVA sea-island fibres and its production technology with water-soluble marine facies |
| CN108589028A (en) * | 2018-04-24 | 2018-09-28 | 山东科贝尔非织造材料科技有限公司 | A kind of novel island fiber synthetic leather base cloth and its production technology |
| CN111733480A (en) * | 2020-07-07 | 2020-10-02 | 上海市合成纤维研究所有限公司 | Sea-island fiber with PA6 as island component, preparation method thereof and superfine fiber formed by same |
| CN115094538A (en) * | 2022-06-06 | 2022-09-23 | 明新旭腾新材料股份有限公司 | Preparation method of superfine sea-island fiber taking efficient water-soluble modified PVA as sea |
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