CN111519276A - High-shrinkage polyamide fiber and preparation method and application thereof - Google Patents
High-shrinkage polyamide fiber and preparation method and application thereof Download PDFInfo
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- CN111519276A CN111519276A CN201910107548.9A CN201910107548A CN111519276A CN 111519276 A CN111519276 A CN 111519276A CN 201910107548 A CN201910107548 A CN 201910107548A CN 111519276 A CN111519276 A CN 111519276A
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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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/04—Melting filament-forming substances
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
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Abstract
The invention relates to a high-shrinkage polyamide fiber, a preparation method and application thereof. The high-shrinkage polyamide fiber is a polyamide 6/polyamide 56 blend fiber; the boiling water shrinkage rate of the high-shrinkage polyamide fiber is 30-60%, and the high-shrinkage polyamide fiber contains 20-80 wt% of polyamide 56 and 80-20 wt% of polyamide 6. The high-shrinkage polyamide fiber provided by the invention not only adopts bio-based materials as main raw materials and is green and environment-friendly, but also has the characteristics of high shrinkage, softness and the like of the polyamide 56/polyamide 6 blend fiber, is suitable for high-shrinkage fabrics, has extremely high quality, and can be applied to high-grade clothing and the like.
Description
Technical Field
The invention belongs to the technical field of polyamide materials, and relates to a high-shrinkage polyamide fiber, and a preparation method and application thereof.
Background
High-Shrinkage Fiber (HSF) is a Fiber prepared by physical (mainly blending or compounding) or chemical (mainly copolymerization modification) modification, and generally refers to a chemical Fiber with boiling water Shrinkage or dry heat Shrinkage higher than 25%. The high shrinkage fiber has the characteristic that the shrinkage rate of the fiber can reach 25-70% during heat treatment, and various fabrics with special styles can be produced by utilizing the characteristic. The high-shrinkage fiber is interlaced with other fibers, coated and woven by mixed fibers, and after the fabric is processed, the fabric has the advantages of full and smooth hand feeling, good drapability and compact fabric structure. In recent years, with the development and utilization of composite superfine fibers and new composite fibers, the high-shrinkage fibers have wider application and increasingly wider use amount, and particularly can be interwoven with the composite superfine fibers to produce high-grade suede fabrics, peach-skin-like fabrics, high-density fabrics and silk-like fabrics.
The patent CN 105887218A discloses a nylon high-shrinkage fiber and a preparation method thereof, wherein copolymerized photo-sliced nylon 6 and nylon 66 are used as raw materials, the nylon 6 accounts for 50-80%, the nylon 66 accounts for 20-50%, the raw materials are fed into a screw extruder under the protection of nitrogen for melting and mixing, spinning is carried out on a spinning machine on the basis, the boiling water shrinkage rate is 27-30%, and the boiling water shrinkage rate of the nylon high-shrinkage fiber is smaller; patent CN 101646812B discloses a high shrinkage fiber, which is composed of nylon MXD6 polymer and nylon 6 polymer, wherein the weight ratio of each polymer is 35: 65-70: 30, the breaking strength is 4.0CN/dtex or more, the MXD6 is semi-aromatic polyamide, the spinning is difficult, and the production consumption is large.
Patent CN 106676673A discloses a polyamide fibre high shrinkage fiber, polyamide fibre high shrinkage fiber includes first high shrinkage component and the high shrinkage component of second, first high shrinkage component includes polyamide fibre 6 component and antistatic component, the high shrinkage component of second includes polyamide fibre 66 component and antistatic component, and first high shrinkage component carries out melt extrusion through twin-screw extruder with the high shrinkage component of second, produces into skin core type high shrinkage fiber, high shrinkage fiber adopts compound spinning technique, and equipment investment is great, and manufacturing cost is higher, and the operation is complicated.
Patent CN 104018246A discloses a method for preparing polyester-nylon composite superfine fiber with high shrinkage, which comprises the steps of drying a high shrinkage polyester slice, melting the polyester slice in a first screw extruder to obtain a first spinning melt, drying a nylon-6 slice, melting the polyamide slice in a second screw extruder to obtain a second spinning melt, carrying out composite spinning on the first spinning melt and the second spinning melt to obtain POY, and producing DTY through an elasticizer, wherein the boiling water shrinkage of the fiber is more than 15%, the high shrinkage fiber also adopts a composite spinning technology, the equipment investment is large, the production cost is high, and the operation is complex.
Japanese patent laid-open No. 8-209444 reports a high shrinkage nylon fiber with a boiling water shrinkage of 30% or more, which is mainly prepared by copolymerization, and has complicated copolymerization modification process and high production cost.
It can be seen that the above-mentioned conventional polyamide fibers still have many drawbacks, and further improvements are desired.
Disclosure of Invention
A first object of the present invention is to provide a high shrinkage polyamide fiber.
The second object of the present invention is to provide a method for preparing the high shrinkage polyamide fiber.
The third purpose of the invention is to provide the application of the high-shrinkage polyamide fiber.
In order to achieve the above purpose, the solution of the invention is as follows:
[ high shrinkage Polyamide fiber ]
In one aspect of the present invention, there is provided a high shrinkage polyamide fiber, which is a blend fiber of polyamide 6 and polyamide 56;
wherein the boiling water shrinkage rate of the high-shrinkage polyamide fiber is 30-60%;
the high-shrinkage polyamide fiber contains 20-80 wt% of polyamide 56 and 80-20 wt% of polyamide 6.
In a preferred embodiment of the invention, the weight ratio of the polyamide 56 to the polyamide 6 in the high shrinkage polyamide fiber is 25:75 to 75: 25; more preferably 35:65 to 70:30, even more preferably 40:60 to 65:35, and even more preferably 45:55 to 60:40, for example, the weight ratio of polyamide 56 to polyamide 6 is 28:72, 32:68, 42:58, or 76: 24.
The 1, 5-pentanediamine which is one of the raw materials of the polyamide 56 is prepared from a bio-based raw material by a fermentation method or an enzyme conversion method.
The high shrinkage polyamide fiber may further contain an additive, as the case may be. The additives may include: any one or more of a delustering agent, a flame retardant, an antioxidant, an ultraviolet absorbent, an infrared absorbent, a crystallization nucleating agent, a fluorescent brightener or an antistatic agent. The additive can be added in an amount of 0.001-10% of the total weight of the raw materials.
In a preferred embodiment of the present invention, the boiling water shrinkage ratio of the high shrinkage polyamide fiber is 30 to 57%, preferably 30 to 55%, more preferably 32 to 53%, and still more preferably 32 to 48%.
In a preferred embodiment of the present invention, the breaking strength of the high shrinkage polyamide fiber is 2.5 to 10.0cN/dtex, preferably 3.0 to 8.5cN/dtex, more preferably 3.5 to 6.0cN/dtex, and still more preferably 4.0 to 5.7 cN/dtex.
In a preferred embodiment of the present invention, the elastic recovery rate of the high shrinkage polyamide fiber under 10% stretching condition is 96% or more, preferably 96-100%; and/or the elastic recovery rate of the high-shrinkage polyamide fiber under 20% stretching condition is more than 85.5%, and more preferably 86-90%.
In a preferred embodiment of the present invention, the fineness of the high shrinkage polyamide fiber is 1.0 to 3000dtex, preferably 3 to 1000dtex, more preferably 5 to 500dtex, still more preferably 10 to 300dtex, and still more preferably 10 to 150 dtex.
In a preferred embodiment of the invention, the modulus of the high shrinkage polyamide fiber is 20 to 45cN/dtex, preferably 25 to 40cN/dtex, and more preferably 30 to 40 cN/dtex.
The cross section of the high-shrinkage polyamide fiber is in any one shape of a circle, a trilobal shape, a cross shape, a triangular shape, a hollow triangular shape, an I shape, a T shape, a Y shape, a flat shape, a pentagonal shape, a hexagonal shape, an octagonal shape, an I shape or a dumbbell shape.
The high-shrinkage polyamide fiber comprises civil filaments, industrial filaments, bulked textured yarns, monofilaments and short fibers.
[ Process for producing high-shrinkage Polyamide fiber ]
In another aspect of the present invention, there is provided a method for preparing the high shrinkage polyamide fiber, the method comprising the steps of:
(1) polyamide 56 and polyamide 6 resin raw materials are uniformly mixed according to a certain proportion and then dried;
(2) heating the blended polyamide resin obtained by drying in the step (1) to a molten state to form a polyamide melt, and extruding to form a primary yarn;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
In the step (1), the mixing is carried out in a mixing bin; and/or the presence of a gas in the gas,
the drying is carried out in a vacuum drum dryer or a continuous nitrogen filling dryer; and/or the presence of a gas in the gas,
the relative viscosity of the polyamide 56 resin raw material is 2.4-3.5, preferably 2.5-3.3, more preferably 2.6-3.2, and further preferably 2.7-3.1; and/or the presence of a gas in the gas,
the relative viscosity of the polyamide 6 resin raw material is 2.2-3.5, preferably 2.3-3.3, more preferably 2.4-3.0, and further preferably 2.5-2.8; and/or the presence of a gas in the gas,
the drying temperature is 60-120 ℃, and the drying time is 8-30 h; and/or the presence of a gas in the gas,
the water content of the dried blended polyamide resin is less than or equal to 1000ppm, preferably 200-900 ppm, more preferably 300-800 ppm, and further preferably 400-600 ppm.
In the step (2), the step (c),
the extrusion is carried out through a spinneret; and/or the presence of a gas in the gas,
the heating is carried out in a screw extruder which is divided into five zones for heating;
wherein the temperature of the first zone is 220-250 ℃; and/or the presence of a gas in the gas,
the temperature of the second zone is 240-300 ℃; and/or the presence of a gas in the gas,
the temperature of the three zones is 250-320 ℃; and/or the presence of a gas in the gas,
the temperature of the fourth zone is 260-310 ℃; and/or the presence of a gas in the gas,
the temperature of the fifth area is 270-300 ℃; and/or the presence of a gas in the gas,
the second zone temperature is greater than the first zone temperature; and/or the presence of a gas in the gas,
the three zone temperature, the four zone temperature, and/or the five zone temperature is greater than the first zone temperature and/or the second zone temperature;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn;
the temperature of the spinning manifold is 270-310 ℃, preferably 275-300 ℃, more preferably 280-295 ℃, and further preferably 285-290 ℃; and/or the presence of a gas in the gas,
the pressure of a spinning assembly of the spinning manifold is 10-25 MPa, preferably 13-20 MPa, and more preferably 16-18 MPa.
The stretching heat setting treatment in the step (3) is completed on two pairs of hot rollers, and the stretching ratio of the stretching heat setting is 1-2.8 times, preferably 1.2-1.8 times, more preferably 1.3-1.6 times, and even more preferably 1.4-1.6 times; and/or the presence of a gas in the gas,
the heat setting temperature is 60-150 ℃, more preferably 65-95 ℃, further preferably 70-93 ℃, and further preferably 80-90 ℃.
[ use of high shrinkage Polyamide fiber ]
In another aspect of the invention, the invention also provides application of the high-shrinkage polyamide fiber in preparing fabrics such as high-grade suede fabrics, peach-skin-like fabrics, high-density fabrics, silk-like fabrics and/or different-shrinkage mixed-fiber fabrics.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the selected polyamide 56 resin is made by a biological method, is a green material, does not depend on petroleum resources, does not cause serious pollution to the environment, and can reduce the emission of carbon and reduce the generation of greenhouse effect.
Secondly, the high shrinkage polyamide fiber of the present invention has high shrinkage performance in addition to the strength of general polyamide fiber.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The detection method of the performance parameters related in the invention is as follows:
1) relative viscosity:
concentrated sulfuric acid method by Ubbelohde viscometer: the dried polyamide 56 chips or their short fiber samples were accurately weighed at 0.25. + -. 0.0002g, dissolved by adding 50mL of concentrated sulfuric acid (96%), and the time t0 for the concentrated sulfuric acid to flow through and the time t for the polyamide sample solution to flow through were measured and recorded in a thermostatic water bath at 25 ℃.
Viscosity number calculation formula: relative viscosity t/t0
t-solution flow time;
t 0-time of solvent flow.
2) Breaking strength:
the determination of the breaking strength can refer to a GB/T14344-2008 chemical fiber filament tensile property test method; applying a pretension of 0.05 +/-0.005 cN/dtex, a holding distance of 500mm and a drawing speed of 500 mm/min.
Modulus is the breaking strength corresponding to 1% elongation at break x 100.
3) Shrinkage in boiling water:
the boiling water shrinkage rate is measured by reference to GB/T6505-2008 'test method for the thermal shrinkage rate of chemical fiber filaments', which specifically comprises the following steps: taking a section of high-shrinkage polyamide fiber, pre-tensioning the high-shrinkage polyamide fiber by 0.05 +/-0.005 cN/dtex, marking 50.00cm at the two ends of the middle of the section of high-shrinkage polyamide fiber, wrapping the section of high-shrinkage polyamide fiber by gauze, putting the gauze into boiling water, boiling for 30min, drying a sample, and measuring the length change of the sample before and after boiling.
4) Elastic recovery rate:
an electronic single yarn strength tester YG061 is adopted, and parameters are set by referring to a GB/T14344-2003 test method. The ambient temperature is 23 ℃ and the humidity is 65%. The gauge was 500mm, the pre-tension was 0.1cN/dtex, the stretching speed was 500mm/min, the stretching was carried out to a set elongation (E10%, 20%), the apparatus was stopped from stretching and relaxed for 60s, and then recovered, the number of measurements was 10.
Elastic recovery rate ═ ((L-L1)/(L-L0)). 100%
Wherein, L0 is the original length of the sample, L is the length of the sample after stretching to a fixed extension, and L1 is the length of the sample after resetting.
Example one
(1) Uniformly mixing polyamide 56 resin and polyamide 6 resin in a mixing bin according to a mass ratio of 80:20, and drying in a vacuum drum dryer at the drying temperature of 80 ℃ for 20 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.7, the relative viscosity of the polyamide 6 resin was 2.4, and the water content of the blended polyamide resin after drying was 400 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 230 ℃; the temperature of the second zone is 250 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the fifth zone is 290 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 285 ℃, and the pressure of the spinning assembly is 12.5 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching multiple of the primary raw silk is 1.3 times, and the heat setting temperature is 85 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Example two
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 70:30, and then are dried in a vacuum drum dryer, wherein the drying temperature is 95 ℃, and the drying time is 15 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.8, the relative viscosity of the polyamide 6 resin was 2.7, and the water content of the polyamide resin blend after drying was 600 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 240 ℃; the temperature of the second zone is 260 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the fifth zone is 290 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 290 ℃, and the pressure of the spinning assembly is 17.0 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.5 times, and the heat setting temperature is 95 ℃.
The properties of the products obtained are shown in tables 1 and 2.
EXAMPLE III
(1) Uniformly mixing polyamide 56 resin and polyamide 6 resin in a mixing bin according to a mass ratio of 60:40, and drying in a vacuum drum dryer at the drying temperature of 110 ℃ for 13 h;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.6, the relative viscosity of the polyamide 6 resin was 2.5, and the water content of the polyamide resin blend after drying was 500 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 235 ℃; the temperature of the second zone is 245 ℃; the temperature of the three zones is 265 ℃; the temperature of the fourth zone is 275 ℃; the temperature of the fifth zone is 285 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 280 ℃, and the pressure of the spinning assembly is 20.0 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.7 times, and the heat setting temperature is 98 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Example four
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 50:50, and then are dried in a vacuum drum dryer, wherein the drying temperature is 90 ℃, and the drying time is 18 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 3.0, the relative viscosity of the polyamide 6 resin was 2.8, and the water content of the polyamide resin blend after drying was 500 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 245 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 290 ℃; the temperature of the fourth zone is 305 ℃; the temperature of the fifth area is 300 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 295 ℃, and the pressure of the spinning assembly is 18.5 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching multiple is 1.4 times, and the heat setting temperature is 88 ℃.
The properties of the products obtained are shown in tables 1 and 2.
EXAMPLE five
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 35:65, and then are dried in a vacuum drum dryer, wherein the drying temperature is 120 ℃, and the drying time is 10 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.7, the relative viscosity of the polyamide 6 resin was 2.7, and the water content of the polyamide resin blend after drying was 700 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 220 ℃; the temperature of the second zone is 240 ℃; the temperature of the three zones is 260 ℃; the temperature of the fourth zone is 270 ℃; the temperature of the fifth zone is 280 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the manifold was 275 ℃ and the pressure of the spinning pack was 12.5 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.6 times, and the heat setting temperature is 80 ℃.
The properties of the products obtained are shown in tables 1 and 2.
EXAMPLE six
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 30:70, and then are dried in a vacuum drum dryer, wherein the drying temperature is 80 ℃, and the drying time is 20 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 3.2, the relative viscosity of the polyamide 6 resin was 3.0, and the water content of the polyamide resin blend after drying was 800 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 250 ℃; the temperature of the second zone is 280 ℃; the temperature of the three zones is 310 ℃; the temperature of the fourth zone is 305 ℃; the temperature of the fifth area is 300 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 300 ℃, and the pressure of the spinning assembly is 16.0 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.2 times, and the heat setting temperature is 90 ℃.
The properties of the products obtained are shown in tables 1 and 2.
EXAMPLE seven
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 30:70, and then are dried in a vacuum drum dryer, wherein the drying temperature is 80 ℃, and the drying time is 14 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.7, the relative viscosity of the polyamide 6 resin was 2.8, and the water content of the polyamide resin blend after drying was 280 ppm.
The heating in step (2) is carried out in a screw extruder, which is preferably divided into five zones of heating; wherein the temperature of the first zone is 245 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 295 ℃; the temperature of the fourth zone is 305 ℃; the temperature of the fifth zone is 298 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 280 ℃, and the pressure of the spinning assembly is 11.0 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching ratio is 2.8 times, and the heat setting temperature is 150 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Example eight
(1) Uniformly mixing polyamide 56 resin and polyamide 6 resin in a mixing bin according to the mass ratio of 20:80, and drying in a vacuum drum dryer at the drying temperature of 70 ℃ for 25 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.5, the relative viscosity of the polyamide 6 resin was 2.5, and the water content of the polyamide resin blend after drying was 900 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 230 ℃; the temperature of the second zone is 250 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the five zones is 275 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 270 ℃, and the pressure of the spinning assembly is 14.0 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching multiple is 1.3 times, and the heat setting temperature is 75 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example 1
(1) Uniformly mixing polyamide 56 resin and polyamide 6 resin in a mixing bin according to a mass ratio of 85:15, and drying in a vacuum drum dryer at the drying temperature of 80 ℃ for 20 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.7, the relative viscosity of the polyamide 6 resin was 2.4, and the water content of the polyamide resin blend after drying was 400 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 230 ℃; the temperature of the second zone is 250 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the fifth zone is 290 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 285 ℃, and the pressure of the spinning assembly is 12.5 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.3 times, and the heat setting temperature is 85 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example No. two
(1) Polyamide 56 resin and polyamide 6 resin are uniformly mixed in a mixing bin according to the mass ratio of 10:90, and then are dried in a vacuum drum dryer, wherein the drying temperature is 95 ℃, and the drying time is 15 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.8, the relative viscosity of the polyamide 6 resin was 2.7, and the water content of the polyamide resin blend after drying was 600 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 240 ℃; the temperature of the second zone is 260 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the fifth zone is 290 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 290 ℃, and the pressure of the spinning assembly is 17.0 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.5 times, and the heat setting temperature is 95 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example No. three
(1) Uniformly mixing polyamide 56 resin and polyamide 66 resin in a mixing bin according to a mass ratio of 70:30, and drying in a vacuum drum dryer at a drying temperature of 95 ℃ for 16 h;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.8, the relative viscosity of the polyamide 66 resin was 2.7, and the water content of the polyamide resin blend after drying was 600 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 240 ℃; the temperature of the second zone is 260 ℃; the temperature of the three zones is 270 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the fifth zone is 290 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 290 ℃, and the pressure of the spinning assembly is 17.0 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.5 times, and the heat setting temperature is 95 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example No. four
(1) Uniformly mixing polyamide 56 resin and polyamide 66 resin in a mixing bin according to the mass ratio of 50:50, and drying in a vacuum drum dryer at the drying temperature of 90 ℃ for 18 h;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 3.0, the relative viscosity of the polyamide 66 resin was 2.8, and the water content of the polyamide resin blend after drying was 500 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 245 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 290 ℃; the temperature of the fourth zone is 305 ℃; the temperature of the fifth area is 300 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 295 ℃, and the pressure of the spinning assembly is 18.3 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching multiple is 1.4 times, and the heat setting temperature is 88 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example five
(1) Polyamide 56 resin and polyamide 66 resin are uniformly mixed in a mixing bin according to the mass ratio of 35:65, and then are dried in a vacuum drum dryer, wherein the drying temperature is 120 ℃, and the drying time is 11 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 2.7, the relative viscosity of the polyamide 66 resin was 2.7, and the water content of the polyamide resin blend after drying was 700 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 220 ℃; the temperature of the second zone is 240 ℃; the temperature of the three zones is 260 ℃; the temperature of the fourth zone is 270 ℃; the temperature of the fifth zone is 280 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the manifold was 275 ℃ and the pressure of the spinning pack was 12.2 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.6 times, and the heat setting temperature is 80 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example six
(1) Polyamide 6 resin and polyamide 66 resin are uniformly mixed in a mixing bin according to the mass ratio of 65:35, and then are dried in a vacuum drum dryer, wherein the drying temperature is 120 ℃, and the drying time is 10 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 6 resin in the step (1) was 2.7, the relative viscosity of the polyamide 66 resin was 2.7, and the water content of the polyamide resin blend after drying was 700 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 220 ℃; the temperature of the second zone is 240 ℃; the temperature of the three zones is 260 ℃; the temperature of the fourth zone is 270 ℃; the temperature of the fifth zone is 280 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the manifold was 275 ℃ and the pressure of the spinning pack was 12.8 MPa.
In the step (3), the stretching and heat setting are completed on two pairs of hot rollers, the stretching multiple is 1.6 times, and the heat setting temperature is 80 ℃.
The properties of the products obtained are shown in tables 1 and 2.
Comparative example seven
(1) Polyamide 6 resin and polyamide 66 resin are uniformly mixed in a mixing bin according to the mass ratio of 50:50, and then are dried in a vacuum drum dryer, wherein the drying temperature is 90 ℃, and the drying time is 18 hours;
(2) heating the polyamide resin to a molten state to form a polyamide melt, and extruding the polyamide melt through a spinneret to form primary yarns;
(3) and carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber.
The relative viscosity of the polyamide 56 resin in the step (1) was 3.0, the relative viscosity of the polyamide 66 resin was 2.8, and the water content of the polyamide resin blend after drying was 500 ppm.
The heating in the step (2) is carried out in a screw extruder, and the screw extruder is divided into five zones for heating; wherein the temperature of the first zone is 245 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 290 ℃; the temperature of the fourth zone is 305 ℃; the temperature of the fifth area is 300 ℃;
the spinning process in the step (2) comprises the following steps:
spraying the polyamide melt through a spinning nozzle of a spinning box to form the primary yarn; the temperature of the box body is 295 ℃, and the pressure of the spinning assembly is 18.6 MPa.
In the step (3), the stretching and heat setting are finished on two pairs of hot rollers, the stretching multiple is 1.4 times, and the heat setting temperature is 88 ℃.
The properties of the products obtained are shown in tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from tables 1 and 2, examples 1 to 8 have good elastic resilience compared to the comparative example, and thus have excellent lodging resistance, are not easily deformed by soft collapse, have good breaking strength, and have high mechanical strength and are not easily broken.
The polyamide 56/polyamide 6 blended fiber has higher shrinkage performance than the polyamide 56/polyamide 66 blended fiber and the polyamide 6/polyamide 66 blended fiber.
The polyamide 56/polyamide 6 blended fiber has the advantages of large boiling water shrinkage, high shrinkage performance and good softness, and can be used for preparing high-shrinkage fabrics. In addition, the fabric has softness, moderate tension and firmness, good hand feeling and extremely high quality, so that the fabric can be applied to high-grade clothes.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A high-shrinkage polyamide fiber, characterized in that the high-shrinkage polyamide fiber is a blend fiber of polyamide 6 and polyamide 56;
wherein the boiling water shrinkage rate of the high-shrinkage polyamide fiber is 30-60%;
the high-shrinkage polyamide fiber contains 20-80 wt% of polyamide 56 and 80-20 wt% of polyamide 6.
2. The high shrinkage polyamide fiber as claimed in claim 1, wherein the weight ratio of the polyamide 56 to the polyamide 6 is 25:75 to 75: 25; preferably, the weight ratio of the polyamide 56 to the polyamide 6 is 35:65 to 70:30, more preferably 40:60 to 65:35, and particularly preferably 45:55 to 60: 40.
3. The high shrinkage polyamide fiber according to claim 1, wherein the high shrinkage polyamide fiber has an elastic recovery of 96% or more, preferably 96 to 100% under 10% stretch; and/or the presence of a gas in the gas,
the elastic recovery rate of the high-shrinkage polyamide fiber under 20% stretching condition is more than 85.5%, and preferably 86-90%.
4. The high shrinkage polyamide fiber as claimed in claim 1, wherein 1, 5-pentanediamine, which is one of raw materials of the polyamide 56, is prepared from bio-based raw materials through a fermentation process or an enzymatic conversion process.
5. The high shrinkage polyamide fiber as claimed in claim 1,
the modulus of the high-shrinkage polyamide fiber is 20-45 cN/dtex, preferably 25-40 cN/dtex, and more preferably 30-40 cN/dtex; and/or the presence of a gas in the gas,
the high shrinkage polyamide fiber has a breaking strength of 2.5 to 10.0cN/dtex, preferably 3.0 to 8.5cN/dtex, more preferably 3.5 to 6.0cN/dtex, and even more preferably 4.0 to 5.7 cN/dtex.
6. A process for preparing a high shrinkage polyamide fibre as claimed in any one of claims 1 to 5, characterized in that the process comprises the steps of:
(1) polyamide 56 and polyamide 6 resin raw materials are uniformly mixed according to a certain proportion and then dried;
(2) heating the blended polyamide resin obtained by drying in the step (1) to a molten state to form a polyamide melt, and extruding to form a primary yarn;
(3) carrying out stretching and heat setting treatment on the primary yarn to obtain the high-shrinkage polyamide fiber; wherein the stretching heat setting treatment is completed on two pairs of hot rollers, the stretching ratio of the stretching heat setting is 1-2.8 times, preferably, the stretching ratio of the stretching heat setting is 1.2-1.8 times, more preferably 1.3-1.6 times, and even more preferably 1.4-1.6 times.
7. The method of claim 6, wherein in step (3),
the heat setting temperature is 60-150 ℃, preferably 65-95 ℃, more preferably 70-93 ℃, and even more preferably 80-90 ℃.
8. The method of claim 6, wherein in step (1),
the relative viscosity of the polyamide 56 resin raw material is 2.4-3.5, preferably 2.5-3.3, more preferably 2.6-3.2, and further preferably 2.7-3.1; and/or the presence of a gas in the gas,
the relative viscosity of the polyamide 6 resin raw material is 2.2-3.5, preferably 2.3-3.3, more preferably 2.4-3.0, and further preferably 2.5-2.8; and/or the presence of a gas in the gas,
the drying temperature is 60-120 ℃, and the drying time is 8-30 h; and/or the presence of a gas in the gas,
the water content of the dried blended polyamide resin is less than or equal to 1000ppm, preferably 200-900 ppm, more preferably 300-800 ppm, and further preferably 400-600 ppm.
9. A high shrinkage polyamide fiber as claimed in any one of claims 1 to 5 comprising a civilian filament, an industrial filament, a bulked textured yarn, a monofilament and a short fiber.
10. Use of the high-shrinkage polyamide fiber as claimed in any one of claims 1 to 5 for producing high-grade suede-like fabrics, polyester peach-like fabrics, high-density fabrics, silk-like fabrics and/or differential shrinkage mixed fiber fabrics.
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CN113122953A (en) * | 2021-03-16 | 2021-07-16 | 浙江恒澜科技有限公司 | Preparation method of high-shrinkage antistatic polyamide fiber |
CN114228292A (en) * | 2021-12-13 | 2022-03-25 | 厦门长塑实业有限公司 | High-shrinkage biaxial oriented polyamide film and preparation method and application thereof |
CN114293278A (en) * | 2020-09-22 | 2022-04-08 | 上海凯赛生物技术股份有限公司 | Polyamide 5X fully drawn yarn and preparation method and application thereof |
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CN106555250A (en) * | 2015-09-30 | 2017-04-05 | 上海凯赛生物技术研发中心有限公司 | Long Carbon Chain Polyamide fiber and preparation method thereof |
CN109072491A (en) * | 2016-05-26 | 2018-12-21 | 东丽株式会社 | High heat-shrinkable Fypro and the combined yarn and fabric for having used the Fypro |
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WO2016108076A1 (en) * | 2015-06-18 | 2016-07-07 | Rhodia Poliamida E Especialidades Ltda | Polyamide fiber with enhanced dyeing properties, process for obtaining such fiber and polyamide article made therefrom |
CN106555250A (en) * | 2015-09-30 | 2017-04-05 | 上海凯赛生物技术研发中心有限公司 | Long Carbon Chain Polyamide fiber and preparation method thereof |
CN109072491A (en) * | 2016-05-26 | 2018-12-21 | 东丽株式会社 | High heat-shrinkable Fypro and the combined yarn and fabric for having used the Fypro |
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CN114293278A (en) * | 2020-09-22 | 2022-04-08 | 上海凯赛生物技术股份有限公司 | Polyamide 5X fully drawn yarn and preparation method and application thereof |
CN114293278B (en) * | 2020-09-22 | 2024-02-23 | 上海凯赛生物技术股份有限公司 | Polyamide 5X fully drawn yarn and preparation method and application thereof |
CN113122953A (en) * | 2021-03-16 | 2021-07-16 | 浙江恒澜科技有限公司 | Preparation method of high-shrinkage antistatic polyamide fiber |
CN114228292A (en) * | 2021-12-13 | 2022-03-25 | 厦门长塑实业有限公司 | High-shrinkage biaxial oriented polyamide film and preparation method and application thereof |
CN114228292B (en) * | 2021-12-13 | 2022-09-30 | 厦门长塑实业有限公司 | High-shrinkage biaxial oriented polyamide film and preparation method and application thereof |
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