CN114134582B - PET/water-soluble polyester sea-island fiber and preparation method thereof - Google Patents
PET/water-soluble polyester sea-island fiber and preparation method thereof Download PDFInfo
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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
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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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
- D01D10/06—Washing or drying
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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
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
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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
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
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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
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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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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention relates to a PET/water-soluble polyester sea-island fiber and a preparation method thereof, wherein the preparation method comprises the working procedures of spinning, cooling, cluster oiling and dry heat drawing, the raw materials comprise a sea phase material and an island phase material, the sea phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is more than 2.0 wt%, and the island phase material is PET resin; in the cooling process, firstly cooling air blowing at the temperature of less than or equal to 25 ℃ is adopted to solidify the spinning melt to form nascent fiber, and then hot air blowing at the temperature of more than or equal to 70 ℃ is adopted to heat and crystallize the water-soluble polyester in the nascent fiber until the crystallinity is 9.2-9.9%; the dry heat drafting temperature is 80-90 ℃. The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is less than or equal to 12.0 percent, and the tensile breaking strength after heat treatment at 130 ℃ is more than or equal to 3.0 cN/dtex. The method of the invention has simple preparation and the prepared fiber has high tensile breaking strength.
Description
Technical Field
The invention belongs to the technical field of sea-island fibers, and relates to a PET/water-soluble polyester sea-island fiber and a preparation method thereof.
Background
The sea-island fiber is characterized in that the sea component dissolving process of the sea-island fiber is mainly divided into benzene decrement and alkali decrement according to the type of sea-phase materials and the difference of post-processing processes, but the benzene decrement process and the alkali decrement process have respective defects, the problem of generating a little three wastes is still avoided, and certain risks exist in the aspects of toluene residue and smell of a final product. In order to realize environment-friendly and healthy sea-island fibers, many domestic and foreign enterprises have developed research and preparation on a novel water-soluble sea-island fiber, i.e., the sea component in the sea-island fiber can be dissolved by heating and steaming with boiled water without using toluene and alkali solution, so as to obtain the sea-island superfine fiber, wherein the sea component in the sea-island fiber is some water-soluble polymers sold in the market in recent years, such as water-soluble polyester or water-soluble polyvinyl alcohol.
In the preparation of the water-soluble sea-island fiber staple fiber, since the "sea" component is a water-soluble substance, the drawing conditions of the water-soluble sea-island fiber cannot be applied with conventional wet-heat drawing, but dry-heat drawing is required. However, the water-soluble sea-island fiber having PET as an island phase has the following problems in the process of drawing with dry heat:
dry heat drafting, wherein the heating medium is air, and the air has poor heat transfer effect, so that the drafting temperature is required to be high; however, when the dry heat drafting temperature is high (> 70 ℃), the sea component water-soluble polyester in the water-soluble sea-island fiber is easy to be softened and bonded, the fiber is bulked after drafting, and the bonded fibers cannot be carded into an independent single fiber state by a subsequent carding machine, so the dry heat drafting temperature is generally required to be controlled below 70 ℃ when preparing the sea-island fiber containing water-soluble polyester; however, if a sea-island fiber having PET as an island component and a water-soluble polyester as a sea component is prepared, it is difficult to obtain a sea-island fiber having high PET crystallinity by controlling the dry-heat drawing temperature to 70 ℃ or lower, because the PET molecular chain has high rigidity and Tg as high as about 70 ℃ and the PET molecular chain is frozen when the dry-heat drawing temperature is controlled to 70 ℃ or lower, the island component has low crystallinity, and the heat-treated sea-island fiber has low tensile breaking strength.
Disclosure of Invention
The invention aims to solve the problems of the PET/water-soluble polyester sea-island fiber (namely, the sea-island fiber with the island component being PET resin and the sea component being water-soluble polyester) in the dry-heat drafting process in the prior art, and provides the PET/water-soluble polyester sea-island fiber and the preparation method thereof.
The invention aims to solve the problem that the water-soluble polyester in the PET/water-soluble polyester sea-island fiber is not softened and bonded by heating when the PET/water-soluble polyester sea-island fiber is subjected to dry-heat drawing at the temperature of 80-90 ℃ by improving the crystallinity of the water-soluble polyester in the nascent fiber and further improving the high-temperature resistance of the water-soluble polyester in the nascent fiber.
In order to achieve the purpose, the invention adopts the following scheme:
a preparation method of PET/water-soluble polyester sea-island fiber comprises the working procedures of spinning, cooling, cluster oiling and dry heat drawing, wherein the raw materials comprise a sea phase material and an island phase material, the sea phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is more than 2.0 wt% (the graphene cannot play a role when the addition amount of the graphene is too small), and the island phase material is PET resin; in the cooling process, firstly cooling air blowing at the temperature of less than or equal to 25 ℃ is adopted to solidify spinning melt to form nascent fibers, and then hot air blowing at the temperature of more than or equal to 70 ℃ is adopted to heat and crystallize water-soluble polyester in the nascent fibers until the crystallinity is 9.2-9.9% (the fibers are not bundled, and the problem of adhesion does not exist); the dry heat drafting temperature is 80-90 ℃.
Sea phase materials are not heat resistant, while crystallization of island phase materials requires high heat; the cooling process in the conventional sea-island fiber composite spinning process only adopts cooling air blowing, for the fibers, in order to avoid viscous flow deformation caused by overheating of the water-soluble polyester, only a lower drafting temperature (such as 70 ℃) can be used, and the glass transition temperature of the PET is about 70 ℃, which is the main reason for difficult preparation of the PET/water-soluble polyester sea-island fiber, because the PET is wrapped by the water-soluble polyester, the heat energy is concentrated on the surface of the water-soluble polyester during drafting, so that the overheating of the water-soluble polyester on the surface is caused, and the crystallization degree of the PET inside is also caused to be lower;
because the difference of the thermal properties of two polymers (PET and water-soluble polyester) in the special PET/water-soluble polyester sea-island fiber spun by the invention is large, the water-soluble polyester as the sea phase is afraid of being sticky by heating, while the PET as the island phase does need heat energy to improve the oriented crystallization during hot drawing, however, the prior art does not have a proper processing window;
according to the method, the process steps of hot air blowing are added after cooling air blowing, the purpose of hot air blowing is to heat and crystallize the sea component water-soluble polyester in the water-soluble sea-island nascent fiber, the crystallinity of the sea component water-soluble polyester is improved, the sea component water-soluble polyester has certain crystallinity during nascent fiber and before dry heat drafting, and the water-soluble polyester in the fiber is not heated, softened and bonded when the PET/water-soluble polyester sea-island fiber is subjected to dry heat drafting at the temperature of 80-90 ℃; the crystallinity of the finally obtained sea component water-soluble polyester in the nascent fiber is about 9.2-9.9%, and experiments prove that the water-soluble sea-island fiber is not bonded during dry hot drawing although the temperature of the post-spinning dry hot drawing is 80-90 ℃ and is more than 70 ℃;
furthermore, the heat conduction material graphene is added into the sea phase, the graphene has a huge specific surface area, and few graphene is added into the sea phase material, so that the heat energy on the surface of the sea phase can be quickly conducted to the island phase dispersed in the sea-island fiber, and the instability of melt spinning cannot be caused; on one hand, the island phase material absorbing the heat energy can be oriented and crystallized under the action of the drawing stress, the crystallization degree of island component PET is improved, the heat shrinkage performance of the fiber is reduced, the tensile breaking strength of the sea-island fiber after heat treatment is improved, and the problem that the crystallization degree of the PET in the dry heat drawing process of the water-soluble sea-island fiber in the prior art is extremely low is solved; on the other hand, the heat energy on the surface is quickly conducted to the inside by introducing the graphene, so that the continuous heat accumulation on the surface is avoided.
As a preferred technical scheme:
the preparation method of the PET/water-soluble polyester sea-island fiber comprises the steps that the temperature of cooling air blowing is 15-25 ℃, and the temperature of hot air blowing is 70-80 ℃; the blowing modes of the cooling blowing and the hot blowing are both circular blowing and circular suction;
after cooling and blowing, hot blowing is added to ensure that the nascent fiber obtains a certain initial crystallinity, and after hot blowing, the crystallinity of the water-soluble polyester of the sea component in the water-soluble sea-island nascent fiber is improved to 9.2-9.9% from 4-5% without hot blowing;
relatively high and uniform crystallinity of the as-spun fiber is necessary for obtaining high performance sea-island fiber by dry heat drawing, because the developed target is the PET/water-soluble polyester sea-island fiber, when the as-spun silk is spun by using the conventional process, although the PET/water-soluble polyester sea-island fiber as-spun silk can be obtained with higher yield, the as-spun silk can be drawn only by using lower drawing temperature, the PET in the obtained drawn sea-island fiber is difficult to be fully crystallized, so that the thermal shrinkage resistance of the fiber is poor, and the mechanical property of the sea-island fiber after being drawn and heat treated is poor; the relatively high, uniform crystallinity of the as-spun fibers makes it possible to increase the draw temperature of the dry heat draw;
the water-soluble polyester reaches the optimal crystallization temperature under hot air blowing at 70-80 ℃, the water-soluble polyester presents viscoelasticity at the temperature, the movement capacity of a molecular chain is enhanced, the arrangement of chain segments can be rapidly adjusted, the growth of crystal grains is realized, and the air with the corresponding temperature can be uniformly acted on the surface of each fiber by using the circular air blowing and the circular air suction; particularly, during hot blowing, although the fibers are not bundled, the fibers are prevented from being adhered to each other due to fluctuation by selecting a proper blowing mode, and the nascent fibers can obtain uniform and basically consistent crystallization degree;
theoretically, hot air blowing can be used for increasing melt crystallization, and then cooling air blowing is used for solidification, so that high-crystallization nascent fiber can be obtained; however, for the sea-island PET/water-soluble polyester fiber, if hot air blowing is used to increase the crystallinity of the water-soluble polyester, and then cooling air blowing is used to solidify the spinning melt to form the primary fiber, the elongation at break of the finally obtained sea-island PET/water-soluble polyester fiber is greatly increased, the tensile breaking strength of the fiber is not good, and even if the crystallinity of the primary fiber is increased, the mechanical strength of the finished fiber after hot drawing is not improved, so we find that the sea-island material with low thermal property such as water-soluble polyester is more suitable for increasing the crystallinity of the primary fiber by using the cold crystallization after solidification; the PET/water-soluble polyester sea-island fiber of the invention firstly uses cooling air blow to solidify spinning melt to form nascent fiber, and then uses hot air blow to improve the crystallinity of water-soluble polyester, thereby avoiding the problems and finally obtaining the PET/water-soluble polyester sea-island fiber with the dry-heat shrinkage rate of less than or equal to 12.0 percent (after heat treatment at 130 ℃) and the tensile breaking strength of more than or equal to 3.0cN/dtex (after heat treatment at 130 ℃).
The preparation method of the PET/water-soluble polyester sea-island fiber has the advantages that the length of the air channel for cooling and blowing is 15-25 cm, and the air speed is 0.2-0.7 m/s; the length of an air channel of the hot blast is 50-100 cm, and the wind speed is 0.5-1.5 m/s; the length of the air channel determines the processing time at the corresponding air temperature, and when the cooling and blowing time is too short, the fiber enters a hot blowing link after being insufficiently cooled and solidified, and the elongation at break is greatly improved, so that the mechanical property of the final finished fiber is poor; when the hot air blowing time is too short, the crystallinity of the as-spun fiber is insufficient, so that the fiber is easily adhered when the fiber is subjected to stretching orientation at a high temperature.
The preparation method of the PET/water-soluble polyester sea-island fiber is characterized in that the dry heat drafting multiple is 2.8-4.2 times; the mechanical properties of the fiber, such as breaking strength, breaking elongation and fineness, can be directly influenced by the drawing multiple; high draft multiple, high fiber strength, low elongation, small titer, but too high can produce broken filaments and broken ends; if the draft ratio is too low, the draft will be uneven, so the draft ratio should be selected in a proper range, the draft ratio of the invention is 2.8-4.2 times, and the aim is to obtain the PET/water-soluble polyester sea-island fiber with higher strength.
The preparation method of the PET/water-soluble polyester sea-island fiber comprises the following steps of (1) preparing the sea-phase material, wherein the content of graphene in the sea-phase material is 2.0-5.0 wt%; too much graphene (more than 5.0 wt%) is added, which has great influence on the melt flow property of the water-soluble polyester, so that the sea-island fiber spinning process becomes unstable; and if too little graphene (less than 2.0 wt%) is added, the heat conductivity of the sea component water-soluble polyester cannot be improved.
In the preparation method of the PET/water-soluble polyester sea-island fiber, the graphene has an average layer number of 1-3 (AFM statistical value) and a specific surface area of more than 80m 2 Graphene powder per gram; compared with single-component spinning, the spinning of the sea-island fiber has higher requirement on the spinning stability of a melt, and the graphene serving as an excellent heat conduction material cannot cause melt spinning instability in the spinning process when compared with other particle type heat conduction materials; the graphene powder with relatively large specific surface area is selected and added into the sea phase material, so that the heat energy on the surface of the sea phase can be quickly conducted to the island phase dispersed inside, the island phase material absorbing the heat energy can be oriented and crystallized under the action of drafting stress, the crystallization degree of the island component PET resin is improved, and the performance and the dimensional stability of the fiber are further improved.
The preparation method of the PET/water-soluble polyester sea-island fiber comprises the following steps: preparing sea-island fibers by adopting a double-screw sea-island composite spinning method, wherein a sea phase material and an island phase material are converged at a spinneret plate to form a sea-island fiber tow, wherein the melt temperature of the sea phase material at the spinneret plate convergence position is 260-280 ℃, the melt temperature of the island phase material at the spinneret plate convergence position is 275-295 ℃, the mass ratio of the sea phase material to the island phase material is 30: 70-50: 50, and the spinning speed is 300-700 m/min; the spinning speed influences the cooling and solidifying speed of the polymer melt in the sea-island fiber, further influences the crystallization degree obtained by cooling the melt, when the spinning speed is too high, the crystallization degree of the obtained nascent fiber is extremely low, most segments are solidified without being adjusted and rearranged, and the nascent fiber obtained when the spinning speed is too high is difficult to withstand the high-temperature stretching condition.
The preparation method of the PET/water-soluble polyester sea-island fiber is characterized in that the oiling agent used for oiling is an anhydrous spinning oiling agent, and the dynamic viscosity of the oiling agent at 30 ℃ is 3-5 mPa & s; the measurement method of the viscosity is divided into two categories of absolute viscosity and relative viscosity, and the absolute viscosity is divided into two categories of dynamic viscosity and kinematic viscosity; the conventional spinning oil has relatively high dynamic viscosity and needs to be prepared into a water solution with a certain concentration for use, and the sea component in the invention is water-soluble polyester, and the fibers are easy to bond after meeting water, so the invention selects the anhydrous spinning oil with low viscosity, does not prepare the oil solution in the oiling process, directly uses the anhydrous spinning oil to oil the PET/water-soluble polyester sea-island fibers, and simultaneously has good fluidity of the anhydrous spinning oil with low dynamic viscosity, so that the oiling rate of the fibers is small and uniform.
The preparation method of the PET/water-soluble polyester sea-island fiber also comprises a curling process and a drying and shaping process after the dry heat drawing process; the curling process parameters are as follows: the main pressure is 0.10-0.25 MPa, and the back pressure is 0.05-0.15 MPa; the drying and shaping temperature is 30-40 ℃, and the time is 5-10 min.
The invention also provides the PET/water-soluble polyester sea-island fiber prepared by the preparation method of the PET/water-soluble polyester sea-island fiber, wherein the dry heat shrinkage rate (the testing method is basically referred to as FZ/T50004-2011, and is only different from the testing method) of the PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is less than or equal to 12.0 percent, and the tensile breaking strength (namely after testing the dry heat shrinkage rate) of the PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is more than or equal to 3.0 cN/dtex.
The principle of the invention is as follows:
when preparing the PET/water-soluble polyester sea-island fiber, the research is mainly divided into two aspects, on one hand, how to avoid bonding of the water-soluble polyester of the sea component after being softened by heat when the dry heat drafting temperature is high (more than 70 ℃); on the other hand, under the limited dry heat drafting temperature, the crystallinity of island components is improved, the thermal shrinkage of the fiber is reduced, and the tensile breaking strength of the island fiber after heat treatment is improved.
According to the invention, a hot air blowing process step is innovatively added in a spinning melt crystallization stage, before primary fibers are not bundled, sea component water-soluble polyester is heated to crystallize, the finally obtained fiber has certain crystallinity before post-spinning dry hot drawing, the initial crystallization is beneficial to smooth high-temperature drawing, the problem that the water-soluble polyester is easy to bond when being subjected to dry hot drawing at a higher temperature is solved, and the crystallinity of the sea component water-soluble polyester in the primary fibers is about 9.2-9.9%; the excessively high crystallinity has strict requirements on the spinning process and is not easy to realize, and the addition of the nucleating agent has great influence on the dissolution of the water-soluble polyester unless the nucleating agent is added; the too low crystallinity makes the primary fiber basically have amorphous chain segments, and the primary fiber is easy to soften and bond by heating, so that the subsequent processing is difficult.
Furthermore, experiments show that the water-soluble polyester has poor heat conductivity, limited heat cannot be quickly transferred into the island component in a short time, the graphene is used as an excellent heat conduction material, and the graphene is added into the water-soluble polyester as the sea component, so that the heat conductivity of the water-soluble polyester as the sea component can be effectively improved, and the water-soluble polyester as the sea component has certain crystallinity before post-spinning dry-hot drafting by combining the preparation method disclosed by the invention, and experiments prove that although the post-spinning dry-hot drafting temperature is 80-90 ℃ and is more than 70 ℃, the water-soluble sea-island fibers are not bonded after drafting; meanwhile, due to the action of graphene in the sea component, heat is promoted to be rapidly transferred into the island component in the dry heat drafting process, the crystallization degree of the island component is improved, the thermal shrinkage performance of the fiber is reduced, and the tensile breaking strength of the sea-island fiber after heat treatment is improved.
Advantageous effects
The preparation method is simple, the dry heat shrinkage rate of the finally prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is less than or equal to 12.0 percent, and the tensile breaking strength after heat treatment at 130 ℃ is more than or equal to 3.0 cN/dtex.
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 may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples and comparative examples were tested for some of the performance indicators as follows:
(1) degree of crystallinity: the crystallinity of the polymer was determined using X-ray diffraction.
(2) Hydrodynamic viscosity of oil agent: the viscosity of the anhydrous spin finish at 30 ℃ was determined by a method of measuring viscosity and flow properties with a rotary viscometer with reference to GB/T5561-.
(3) Dry heat shrinkage: the fiber samples were randomly sampled at 50 points, and the dry heat shrinkage of the fibers was measured with reference to FZ/T50004-2011, and the heat treatment temperature was set at 130 ℃.
(4) Tensile breaking strength: determining tensile breaking strength of the fiber subjected to the dry heat shrinkage rate test according to GB/T14337-; the fineness of sea-island fibers was measured by GB/T14335, the tensile breaking strength and fineness of 50 fiber samples were obtained by XD-1 fiber fineness meter, respectively, the average tensile breaking strength (abbreviated as "strength") was calculated as Σ breaking strength/Σ fineness, and the average tensile breaking strength was regarded as the tensile breaking strength of the fibers measured.
(5) Bonding condition: the dry and hot drafted fibers are lightly rubbed by hands, and if the fibers are immediately loosened, the fibers are not bonded; if the fibers are not immediately loosened, only a small part of the fibers are adhered, but the adhered part can be torn by hands, and the fibers are slightly adhered; if the fibers are not loose, they remain together and are difficult to separate, i.e., they are strongly bonded.
The PET resin in the following examples and comparative examples adopts China petrochemical characterized chemical fiber FC510, and the relative viscosity is 0.679 +/-0.01; the water-soluble polyester raw material adopts Korean SK water-soluble polyester 7020; the graphene is Xiamen KNG-G2.
The spinning in the following embodiments and comparative examples adopts double screws for composite spinning, the feeding of a metering pump is adjusted according to a preset raw material ratio, a sea phase material and an island phase material are respectively fed into a sea phase screw and an island phase screw for melting, plasticizing and mixing, the screw settings are conventional processes, and a processing window in an ideal mixing state under corresponding ratio can be obtained through limited experiments; in the embodiment, the diameter of the screw used by the marine phase screw is 120mm, and the length-diameter ratio of the screw is 30: 1; the diameter of the island phase screw rod is 120mm, and the length-diameter ratio of the screw rod is 28: 1.
Example 1
A preparation method of PET/water-soluble polyester sea-island fiber comprises the following steps:
(1) spinning: preparing sea-island fibers by a double-screw sea-island composite spinning method, wherein a sea-phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is 2 wt%, an island-phase material is PET (polyethylene terephthalate) resin, the sea-phase material and the island-phase material are converged at a spinneret plate to form a sea-island fiber tow, the melting temperature of a sea-phase screw is 260 ℃, and the rotating speed of the screw is 5.60 rpm; the melting temperature of the island phase screw is 275 ℃, and the rotating speed of the screw is 13.08 rpm; wherein the melt temperature of the sea phase material at the junction of the spinneret plate is 260 ℃, the melt temperature of the island phase material at the junction of the spinneret plate is 275 ℃, the mass ratio of the sea phase material to the island phase material is 30:70, and the spinning speed is 300 m/min;
(2) and (3) cooling: firstly, cooling air blowing at the temperature of 25 ℃ and the air speed of 0.7m/s is used for solidifying spinning melt to form nascent fiber, and then hot air blowing at the temperature of 70 ℃ and the air speed of 1.5m/s is used for heating and crystallizing water-soluble polyester in the nascent fiber until the crystallinity is 9.2 percent; the blowing modes of cooling blowing and hot blowing are both circular blowing and circular suction blowing; the length of the air channel of the cooling air blower is 15cm, and the length of the air channel of the hot air blower is 50 cm;
(3) bundling and oiling: the oil used for oiling is anhydrous spinning oil (Changzhouling 1058);
(4) dry heat drawing: the temperature of dry heat drawing is 80 ℃; the multiple of dry heat drafting is 4.2 times;
(5) curling: the crimping main pressure is 0.1MPa, and the back pressure is 0.05 MPa;
(6) drying and shaping: drying and shaping at 30 deg.C for 5 min;
(7) and (4) cutting the fiber obtained in the step (6) by cutting equipment to obtain the PET/water-soluble polyester sea-island fiber.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 11.4 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 3.09 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Comparative example 1
A method for preparing a PET/water-soluble polyester sea-island fiber, which is substantially the same as example 1, except that the sea-phase material does not contain graphene.
After hot air blowing, the water-soluble polyester in the as-spun fibers was crystallized by heating to a crystallinity of 9%.
The prepared PET/water-soluble polyester sea-island fiber has a dry heat shrinkage of 22.5% after heat treatment at 130 ℃, and a tensile breaking strength of 2.05cN/dtex after heat treatment at 130 ℃; the prepared PET/water-soluble polyester sea-island fiber is slightly bonded.
Compared with example 1, the PET/water-soluble polyester sea-island fiber prepared in comparative example 1 has improved dry heat shrinkage after heat treatment, poor fiber size stability and obviously reduced fiber strength. The reason is that the graphene is not added in the water-soluble polyester in the comparative example 1, and limited heat cannot be rapidly transferred into the island component in a short time in the dry heat drafting process, so that the crystallization degree of the island component PET is low, the thermal shrinkage performance of the fiber is high, the strength of the fiber after heat treatment is low, and meanwhile, the drafting heat is continuously concentrated on the surface of the fiber, so that the surface of the fiber is easily overheated, and a slight adhesion phenomenon is caused.
Comparative example 2
A process for preparing sea-island PET/water-soluble polyester fiber, substantially the same as in example 1, except that no hot air blow is applied in comparative example 2, that is, step (2) is: and (3) solidifying the spinning melt into nascent fiber by using cooling air blowing at the temperature of 25 ℃ and the air speed of 0.7m/s, wherein the air blowing mode of the cooling air blowing is that circular air blowing and circular air suction are used simultaneously, and the length of an air channel of the cooling air blowing is 15 cm.
The as-spun fiber had a crystallinity of 4.8%.
Compared with example 1, comparative example 2 is that because only cooling air blast is used in the process of cooling the nascent fiber, and no hot air blast is used, the crystallinity of the sea component water-soluble polyester in the finally obtained nascent fiber is low, the fiber is seriously bonded in the process of dry heat drafting, the drafting is difficult, and the PET/water-soluble polyester sea-island fiber can not be prepared.
Comparative example 3
A process for preparing a PET/water-soluble polyester sea-island fiber, substantially as in example 1, except that the temperature of dry heat drawing is 70 ℃.
After hot air blowing, the water-soluble polyester in the as-spun fibers was crystallized by heating to a crystallinity of 9.2%.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 25.6 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 1.52 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Comparative example 4
A method for preparing PET/water-soluble polyester sea-island fiber, which is substantially the same as example 1, except that the sea-phase material does not contain graphene, and the dry heat drawing temperature is 70 ℃.
After hot air blowing, the water-soluble polyester in the as-spun fibers was crystallized by heating to a crystallinity of 9%.
The prepared PET/water-soluble polyester sea-island fiber has a dry heat shrinkage rate of 33.4% after heat treatment at 130 ℃, and a tensile breaking strength of 1.47cN/dtex after heat treatment at 130 ℃; the prepared PET/water-soluble polyester sea-island fiber is slightly bonded.
Compared with example 1, comparative examples 3 and 4 both reduce the dry heat drafting temperature to 70 ℃, and although the PET/water-soluble polyester sea-island fiber is prepared, the PET/water-soluble polyester sea-island fiber prepared in comparative examples 3 and 4 has the advantages of remarkably improved dry heat shrinkage rate after heat treatment, poorer fiber dimensional stability and remarkably reduced fiber strength after heat treatment. This is because when the dry heat drawing temperature is low (< 80 ℃), the Tg of PET is high, the molecular chain is basically in a frozen state at 70 ℃, the island component crystallization degree is low, the fiber heat shrinkage performance is high, and the fiber strength after heat treatment is poor. Compared with the comparative example 3 and the comparative example 4, as the graphene is added into the water-soluble polyester of the sea component in the comparative example 3, and the graphene is not added into the water-soluble polyester of the sea component in the comparative example 4, the dry heat shrinkage rate of the fiber in the comparative example 3 is lower than that in the comparative example 4, and the strength of the fiber in the comparative example 3 after heat treatment is higher than that in the comparative example 4, the effect of improving the heat conductivity of the water-soluble polyester is further demonstrated by adding the graphene into the water-soluble polyester of the sea component.
Comparative example 5
A method for preparing a PET/water-soluble polyester sea-island fiber, which is substantially the same as example 1, except that the sequence of the cooling air blowing and the hot air blowing of the step (2) is reversed, that is, the step (2) is: firstly, using hot air blowing at the temperature of 70 ℃ and the air speed of 1.5m/s to heat and crystallize the water-soluble polyester, and then using cooling air blowing at the temperature of 25 ℃ and the air speed of 0.7m/s to solidify spinning melt to form nascent fiber; the blowing modes of cooling blowing and hot blowing are both circular blowing and circular suction blowing; the length of the air channel of the cooling air blower is 15cm, and the length of the air channel of the hot air blower is 50 cm.
After cooling and blowing, the crystallinity of the water-soluble polyester in the as-spun fiber was 9.5%.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 11.6 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 1.89 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Compared with example 1, the dry heat shrinkage rate of comparative example 5 is larger than that of example 1, and the tensile breaking strength is smaller than that of example 1, because the fiber is stretched by a certain winding force during melt cooling, the arrangement of the polymers in the fiber along the drawing direction is increased, the crystallinity of the water-soluble polyester is improved by using hot air blowing, and then the spinning melt is solidified to form the primary fiber by using cooling air blowing, which is equivalent to increasing the time from melting to solidification of the primary fiber, and is higher than the orientation behavior of the primary fiber obtained by heating after melt solidification; the time of melting and cooling is prolonged, the arrangement of the fiber in the drafting direction under the winding force is increased, so that the breaking elongation of the final PET/water-soluble polyester sea-island fiber is greatly improved, the tensile breaking strength among polymers in the fiber is poor due to the loss of molecular chain entanglement force, and the mechanical strength of the finished fiber after hot drafting is not improved even if the crystallinity of the nascent fiber is improved.
Comparative example 6
A method for preparing a PET/water-soluble polyester sea-island fiber, which is substantially the same as example 1, except that the length of the air passage of the cooling air blower is 10 cm.
After hot air blowing, the water-soluble polyester in the as-spun fibers was crystallized by heating to a crystallinity of 9.3%.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 11.9 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 1.8 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Comparative example 6 has a larger dry heat shrinkage than example 1 and a smaller tensile break strength than example 1, compared to example 1, because the as-spun fiber is not completely cured and is heated again, which also presents the same problem as comparative example 5.
Comparative example 7
A method for preparing a PET/water-soluble polyester sea-island fiber, which is substantially the same as example 1, except that the length of the hot-air blowing duct is 30 cm.
After hot air blowing, the water-soluble polyester in the as-spun fibers was crystallized by heating to a crystallinity of 7.5%.
In comparison with example 1, comparative example 7 produced fibers in which the adhesion was severe and fibers could not be produced because the air passage of the hot blast was too short to increase the crystallinity of the as-spun fibers significantly, and the fibers were found to be seriously adhered under the subsequent high temperature drawing at 80 ℃, and finally a fiber product could not be produced.
Example 2
A preparation method of PET/water-soluble polyester sea-island fiber comprises the following steps:
(1) spinning: preparing sea-island fibers by a double-screw sea-island composite spinning method, wherein a sea-phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is 5 wt%, an island-phase material is PET (polyethylene terephthalate) resin, and the sea-phase material and the island-phase material are converged at a spinneret plate to form sea-island fiber tows; the melting temperature of the sea phase screw is 280 ℃, and the rotating speed of the screw is 15.02 rpm; the melting temperature of the island phase screw is 295 ℃, and the rotating speed of the screw is 15.02 rpm; wherein the melt temperature of the sea phase material at the junction of the spinneret plate is 280 ℃, the melt temperature of the island phase material at the junction of the spinneret plate is 295 ℃, the mass ratio of the sea phase material to the island phase material is 50:50, and the spinning speed is 700 m/min;
(2) and (3) cooling: firstly, cooling air blowing at the temperature of 15 ℃ and the air speed of 0.2m/s is used for solidifying the spinning melt to form nascent fiber, and then hot air blowing at the temperature of 80 ℃ and the air speed of 0.5m/s is used for heating and crystallizing the water-soluble polyester in the nascent fiber until the crystallinity is 9.9%; the blowing modes of cooling blowing and hot blowing are both circular blowing and circular suction blowing; the length of the air channel of the cooling air blower is 25cm, and the length of the air channel of the hot air blower is 100 cm;
(3) bundling and oiling: the oil used for oiling is anhydrous spinning oil (Changzhouling 4058);
(4) dry heat drawing: the temperature of dry heat drawing is 90 ℃; the multiple of dry heat drafting is 2.8 times;
(5) curling: the crimping main pressure is 0.25MPa, and the back pressure is 0.15 MPa;
(6) drying and shaping: drying and shaping at 40 deg.C for 10 min;
(7) and (4) cutting the fiber obtained in the step (6) by cutting equipment to obtain the PET/water-soluble polyester sea-island fiber.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 10.4 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 3.26 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Example 3
A preparation method of PET/water-soluble polyester sea-island fiber comprises the following steps:
(1) spinning: preparing sea-island fibers by a double-screw sea-island composite spinning method, wherein a sea-phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is 3 wt%, an island-phase material is PET (polyethylene terephthalate) resin, and the sea-phase material and the island-phase material are converged at a spinneret plate to form sea-island fiber tows; the melting temperature of the marine phase screw is 270 ℃, and the rotating speed of the screw is 9.93 rpm; the melting temperature of the island phase screw is 285 ℃, and the rotating speed of the screw is 14.98 rpm; wherein the melt temperature of the sea phase material at the junction of the spinneret plate is 270 ℃, the melt temperature of the island phase material at the junction of the spinneret plate is 285 ℃, the mass ratio of the sea phase material to the island phase material is 40:60, and the spinning speed is 500 m/min;
(2) and (3) cooling: firstly, cooling air blowing at the temperature of 20 ℃ and the air speed of 0.4m/s is used for solidifying spinning melt to form nascent fiber, and then hot air blowing at the temperature of 75 ℃ and the air speed of 0.8m/s is used for heating and crystallizing water-soluble polyester in the nascent fiber until the crystallinity is 9.5%; the blowing modes of cooling blowing and hot blowing are both circular blowing and circular suction blowing; the length of the air channel of the cooling air blower is 20cm, and the length of the air channel of the hot air blower is 80 cm;
(3) bundling and oiling: the oil used for oiling is anhydrous spinning oil (Changzhouling 1058);
(4) dry heat drawing: the temperature of dry heat drawing is 85 ℃; the multiple of dry heat drafting is 3.4 times;
(5) curling: the crimping main pressure is 0.15MPa, and the back pressure is 0.1 MPa;
(6) drying and shaping: drying and shaping at 30 deg.C for 10 min;
(7) and (4) cutting the fiber obtained in the step (6) by cutting equipment to obtain the PET/water-soluble polyester sea-island fiber.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 10.9 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 3.14 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Example 4
A preparation method of PET/water-soluble polyester sea-island fiber comprises the following steps:
(1) spinning: preparing sea-island fibers by a double-screw sea-island composite spinning method, wherein a sea-phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is 4 wt%, an island-phase material is PET (polyethylene terephthalate) resin, and the sea-phase material and the island-phase material are converged at a spinneret plate to form sea-island fiber tows; the melting temperature of the sea phase screw is 275 ℃, and the rotating speed of the screw is 15.35 rpm; the melting temperature of the island phase screw is 290 ℃, and the rotating speed of the screw is 6.60 rpm; wherein the melt temperature of the sea phase material at the junction of the spinneret plate is 275 ℃, the melt temperature of the island phase material at the junction of the spinneret plate is 290 ℃, the mass ratio of the sea phase material to the island phase material is 30:70, and the spinning speed is 400 m/min;
(2) and (3) cooling: firstly, cooling air blowing at the temperature of 15 ℃ and the air speed of 0.5m/s is used for solidifying the spinning melt to form nascent fiber, and then hot air blowing at the temperature of 80 ℃ and the air speed of 1m/s is used for heating and crystallizing the water-soluble polyester in the nascent fiber to the crystallinity of 9.8 percent; the blowing modes of cooling blowing and hot blowing are both circular blowing and circular suction blowing; the length of the air channel of the cooling air blower is 20cm, and the length of the air channel of the hot air blower is 80 cm;
(3) bundling and oiling: the oil used for oiling is anhydrous spinning oil (Changzhouling 1058);
(4) dry heat drawing: the temperature of dry heat drawing is 90 ℃; the multiple of dry heat drafting is 3.6 times;
(5) curling: the crimping main pressure is 0.1MPa, and the back pressure is 0.15 MPa;
(6) drying and shaping: drying and shaping at 40 deg.C for 5 min;
(7) and (4) cutting the fiber obtained in the step (6) by cutting equipment to obtain the PET/water-soluble polyester sea-island fiber.
The dry heat shrinkage rate of the prepared PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is 10.1 percent, and the tensile breaking strength after heat treatment at 130 ℃ is 3.35 cN/dtex; the prepared PET/water-soluble polyester sea-island fiber is not bonded.
Claims (10)
1. A preparation method of PET/water-soluble polyester sea-island fiber comprises the working procedures of spinning, cooling, cluster oiling and dry heat drawing, and raw materials comprise a sea phase material and an island phase material, and is characterized in that the sea phase material is a mixture of graphene and water-soluble polyester, the content of the graphene is more than 2.0 wt%, and the island phase material is PET resin; in the cooling process, firstly cooling air blowing at the temperature of less than or equal to 25 ℃ is adopted to solidify the spinning melt to form nascent fiber, and then hot air blowing at the temperature of more than or equal to 70 ℃ is adopted to heat and crystallize the water-soluble polyester in the nascent fiber until the crystallinity is 9.2-9.9%; the dry heat drafting temperature is 80-90 ℃.
2. The method for preparing PET/water-soluble polyester sea-island fiber according to claim 1, wherein the temperature of the cooling air blowing is 15-25 ℃, and the temperature of the hot air blowing is 70-80 ℃; the blowing modes of the cooling blowing and the hot blowing are both circular blowing and circular suction blowing.
3. The method for preparing the PET/water-soluble polyester sea-island fiber according to claim 2, wherein the length of the cooling air-blowing duct is 15-25 cm, and the air speed is 0.2-0.7 m/s; the length of the hot blast air channel is 50-100 cm, and the air speed is 0.5-1.5 m/s.
4. The method of claim 1, wherein the dry heat draft is 2.8 to 4.2 times.
5. The method for preparing PET/water-soluble polyester sea-island fiber according to claim 1, wherein the graphene content in the sea-phase material is 2.0-5.0 wt%.
6. The method for preparing PET/water-soluble polyester sea-island fiber according to claim 5, wherein the graphene has an average number of layers of 1-3 and a specific surface area of more than 80m 2 Graphene powder per gram.
7. The method for preparing the PET/water-soluble polyester sea-island fiber according to claim 1, wherein the spinning process comprises: the sea-island fiber is prepared by adopting a double-screw sea-island composite spinning method, and sea-island materials and island materials are converged at a spinneret plate to form a sea-island fiber tow, wherein the melt temperature of the sea-island materials at the spinneret plate convergence position is 260-280 ℃, the melt temperature of the island materials at the spinneret plate convergence position is 275-295 ℃, the mass ratio of the sea-island materials to the island materials is 30: 70-50: 50, and the spinning speed is 300-700 m/min.
8. The method for preparing PET/water-soluble polyester sea-island fiber according to claim 1, wherein the finish used for oiling is an anhydrous spinning finish with dynamic viscosity of 3-5 mPa s at 30 ℃.
9. The method of claim 1, further comprising a crimping step and a drying and setting step after the dry heat drawing step; the curling process parameters are as follows: the main pressure is 0.10-0.25 MPa, and the back pressure is 0.05-0.15 MPa; the drying and shaping temperature is 30-40 ℃, and the time is 5-10 min.
10. The PET/water-soluble polyester sea-island fiber prepared by the method for preparing the PET/water-soluble polyester sea-island fiber according to any one of claims 1 to 9, wherein the dry heat shrinkage rate of the PET/water-soluble polyester sea-island fiber after heat treatment at 130 ℃ is less than or equal to 12.0%, and the tensile breaking strength after heat treatment at 130 ℃ is more than or equal to 3.0 cN/dtex.
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| CN1621582A (en) * | 2003-11-27 | 2005-06-01 | 厦门翔鹭化纤股份有限公司 | Processing method for producing full dull island fiber FDY/POY based on general island fiber production apparatus |
| CN103122502A (en) * | 2011-11-18 | 2013-05-29 | 东丽纤维研究所（中国）有限公司 | Sea-island composite fiber and superfine fiber fabric |
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| KR20190022045A (en) * | 2017-08-25 | 2019-03-06 | 국방과학연구소 | Method for manufacturing sea-island typed organic nano composite fiber, sea-island typed organic nano composite fiber manufactured by the method and composite material having the fiber |
| CN109706546A (en) * | 2018-11-12 | 2019-05-03 | 上海德福伦化纤有限公司 | A kind of graphene sea-island fibre and its manufacturing method |
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| CN1621582A (en) * | 2003-11-27 | 2005-06-01 | 厦门翔鹭化纤股份有限公司 | Processing method for producing full dull island fiber FDY/POY based on general island fiber production apparatus |
| CN103122502A (en) * | 2011-11-18 | 2013-05-29 | 东丽纤维研究所（中国）有限公司 | Sea-island composite fiber and superfine fiber fabric |
| KR20190022045A (en) * | 2017-08-25 | 2019-03-06 | 국방과학연구소 | Method for manufacturing sea-island typed organic nano composite fiber, sea-island typed organic nano composite fiber manufactured by the method and composite material having the fiber |
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