CN113106562A - Preparation method of antimony-free DTY polyester fiber - Google Patents
Preparation method of antimony-free DTY polyester fiber Download PDFInfo
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- CN113106562A CN113106562A CN202110292780.1A CN202110292780A CN113106562A CN 113106562 A CN113106562 A CN 113106562A CN 202110292780 A CN202110292780 A CN 202110292780A CN 113106562 A CN113106562 A CN 113106562A
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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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
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01H—SPINNING OR TWISTING
- D01H13/00—Other common constructional features, details or accessories
- D01H13/04—Guides for slivers, rovings, or yarns; Smoothing dies
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/20—Combinations of two or more of the above-mentioned operations or devices; After-treatments for fixing crimp or curl
Abstract
The invention discloses a preparation method of antimony-free DTY polyester fiber, which relates to the field of polyester fiber and comprises the following preparation steps: 1) preparing a polyester melt from terephthalic acid, ethylene glycol, a cocatalyst and a titanium catalyst through esterification reaction, pre-polycondensation and final polycondensation; 2) carrying out spinning on the polyester melt to form nascent fiber; 3) cooling and solidifying the nascent fiber, bundling and oiling, and winding and forming; 4) texturing the formed fiber, namely performing low-friction yarn guide, one roller, one hot box, twister, two hot boxes, oiling and winding to prepare the antimony-free DTY polyester fiber; the invention reduces the friction generated during the movement of fine denier silk strips by arranging the low-friction silk guide when fibers are subjected to texturing, thereby reducing the problem of broken silk, preventing the phenomena of broken ends, generating flocks on porcelain pieces of texturing machines, low dyeing M% rate and the like.
Description
Technical Field
The invention relates to the field of polyester fibers, in particular to a preparation method of antimony-free DTY polyester fibers.
Background
Polyethylene terephthalate (PET) fiber or polyester fiber has a series of excellent performances such as high elastic modulus and breaking strength, moderate rebound resilience, excellent heat setting, good heat and light resistance, acid and alkali resistance, corrosion resistance and the like since the coming out, and the fabric has the advantages of crease resistance, easy ironing, good stiffness and the like, and is widely applied to the fields of clothing, home textiles, medical products and the like.
At present, most of domestic polyester fibers adopt one or more of antimony acetate, antimony trioxide and ethylene glycol antimony as catalysts. Antimony is used as a heavy metal element, coexists with virulent arsenic in nature, and can cause serious threat to human health if contacting beverage bottles and non-food packaging materials prepared from antimony-containing polyester chips for a long time. In addition, in the printing and dyeing process of the polyester fiber prepared by adopting the antimony catalyst, antimony can be separated out from the polyester fiber at high temperature, so that the pollution of process water is caused, and the final antimony content in the circulating process water exceeds the relevant national standard. The titanium catalyst is the best choice for replacing antimony catalyst due to its high catalytic activity, relatively moderate price, environmental friendliness and no harm to human body.
In the prior patent publications, there are many related patents for preparing titanium catalysts for polyester polycondensation and technologies for preparing polyester chips and polyester staple fibers by using the titanium catalysts, and a method for preparing antimony-free polyester DTY fibers by using the titanium catalysts is rarely reported.
In the previous method for preparing polyester by adopting titanium catalyst, the stability of titanium compound is widely studied, wherein the diol compound of titanium has been accepted by various large research institutions at home and abroad due to the stable annular chelating structure, but the catalyst causes more side reactions due to too high activity, so that molecular chains are broken, the viscosity of the prepared polyester slice is not ideal, especially when antimony-free polyester is used for texturing porous fine denier filaments, the problems of filament evenness and uneven wool are easy to occur, wool is generated on porcelain pieces of texturing machines, the rate of M% dyeing is not high, the problems of easy end breakage and wool are caused compared with the conventional porous fine denier filaments with the same specification, and meanwhile, the texturing speed is low, so that the production efficiency is low.
Disclosure of Invention
The invention provides a preparation method of antimony-free DTY (draw textured yarn) polyester fiber, aiming at overcoming the problems of unsatisfactory spinning condition and the like when the polyester fine-denier porous filament is subjected to texturing by using a titanium catalyst at present.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) preparing a polyester melt from terephthalic acid, ethylene glycol, a cocatalyst and a titanium catalyst through esterification reaction, pre-polycondensation and final polycondensation;
(2) carrying out spinning on the polyester melt to form nascent fiber;
(3) cooling and solidifying the nascent fiber, bundling and oiling, and winding and forming;
(4) and (3) performing texturing on the formed fiber, wherein the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a second hot box, oiling and winding to prepare the antimony-free DTY polyester fiber.
According to the invention, the low-friction yarn guide is arranged when the fibers are subjected to texturing, so that the friction generated during the motion of fine denier yarn is reduced, the problem of broken yarns is reduced, the phenomenon of broken ends is not easy to occur, and the phenomena of generation of flocks on porcelain pieces of texturing machines, low dyeing M% rate and the like are prevented.
Preferably, the mass ratio of the terephthalic acid to the ethylene glycol in the step (1) is 1: 0.41-0.55.
Preferably, the cocatalyst in the step (1) comprises one or more of magnesium acetate, zinc acetate and cobalt acetate, and the dosage is 30-50 ppm.
Preferably, the titanium catalyst in the step (1) comprises one or more of ethylene glycol titanium, titanate and nano titanium dioxide, and the dosage is 7-15 ppm.
Preferably, the esterification reaction temperature in the step (1) is 260-270 ℃, and the pressure is 300-700 Kpa; the pre-polycondensation is carried out for 2-3h at 265 ℃ and 272 ℃ and 200 ℃ and 550 Pa; the final polycondensation is carried out at the temperature of 273-.
Preferably, the polyester melt in the step (2) is pressurized by a melt booster pump and then is conveyed to a spinning manifold through a melt cooler to form the nascent fiber after being extruded by a spinneret plate, wherein the post-pumping pressure of the booster pump is 145-160bar, and the temperature of the melt cooler is 280-288 ℃.
Preferably, the cooling wind temperature during cooling solidification in the step (3) is 20-25 ℃, and the winding speed during winding is 2600-.
Preferably, the oil used in the texturing in the step (4) is an SSS oil.
Preferably, the low-friction wire guide in the step (4) comprises a wire guide body (1), a wire hole (2) penetrates through the wire guide body (1), the wire hole presents an hourglass-shaped structure with a small middle part and large two ends in the thickness direction of the wire guide body, and the wire hole (2) is communicated with the side wall of the wire guide body (1) through a wire guide channel (3).
The low-friction yarn guide adopts the yarn hole (2) with the hourglass-shaped structure and is communicated with the side wall of the yarn guide body (1) through the yarn guide channel (3), so that the yarn opening is positioned on the side wall of the yarn guide, the problems that the yarn opening in the existing flat yarn guide can shear fine denier yarns and the yarns are easy to rub against irregular yarn openings during strand silk movement are solved, the problems of broken yarns and broken yarns are reduced, and the dyeing rate is increased by M%.
Preferably, the texturing time in the step (4) is 650-750m/s, the draft ratio is 1.73-1.75%, the speed ratio is 1.45-1.55%, the temperature of the first hot box is 175-185 ℃, and the temperature of the second hot box is 165-170 ℃.
In the invention, the low-friction yarn guide is adopted, so that the speed of the vehicle can be improved compared with the conventional process, the production efficiency is greatly improved, meanwhile, the yarn path is smoother after the low-friction yarn guide is adopted, and the draft ratio and the speed ratio are required to be adjusted, wherein the draft ratio is improved to increase the strength of the yarn, but the phenomenon of broken yarn or even broken ends is easy to occur due to the overhigh draft specific volume, and the speed ratio is reduced, the tension is increased, the speed ratio is increased, and the tension is reduced; compared with the conventional process, the invention reduces the draft ratio, is beneficial to the phenomena of reduction of the resistance and the tension of a yarn channel, reduces the speed ratio and increases the tension, thereby obtaining the antimony-free DTY polyester fiber with higher breaking strength, higher breaking elongation, less broken yarn and higher dyeing M% rate. Compared with the conventional process, the internal stress of the yarn after texturing is lower due to the reduction of the yarn path resistance, so that the temperature in the second heating box is lower than that in the conventional process.
In this regard, the present inventors intend to emphasize that the present invention does not merely make simple and routine adjustments of process parameters, and in order to obtain antimony-free DTY polyester fibers with better performance, it is necessary to strictly define the vehicle speed, the draft ratio, the speed ratio, the temperature of the first hot box and the temperature of the second hot box based on the use of the low friction yarn guide, and each parameter has an important influence on the fiber performance, so that the antimony-free DTY polyester fibers with higher breaking strength, higher breaking elongation, less yarn breakage, higher dyed M% ratio and better overall performance can be obtained only by strictly defining the process parameters within the range defined by the present invention based on the use of the low friction yarn guide of the present invention, and it is very difficult for a person skilled in the art to balance the various properties.
Therefore, the invention has the following beneficial effects: the invention reduces the friction generated during the movement of fine denier silk strips by arranging the low-friction silk guide when fibers are subjected to texturing, thereby reducing the problem of broken silk, preventing the phenomena of broken ends, generating flocks on porcelain pieces of texturing machines, low dyeing M% rate and the like.
Drawings
FIG. 1 is a schematic cross-sectional view of the low friction guidewire device of the present invention.
FIG. 2 is a side cross-sectional view of the low friction guidewire device of the present invention.
In the figure: the thread guide device body 1 is penetrated with a thread hole 2 and a thread guide channel 3.
Detailed Description
The invention is further described with reference to specific embodiments.
General example:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.41-0.55, then adding 30-50ppm of cocatalyst and 7-15ppm of titanium catalyst, and preparing a polyester melt after carrying out esterification reaction at 270 ℃ and 700Kpa of 260-plus, carrying out pre-polycondensation reaction for 2-3h at 272 ℃ and 550pa of 265-plus, and carrying out final polycondensation reaction for 2-3h at 282 ℃ and 360pa of 200-plus;
the cocatalyst comprises one or more of magnesium acetate, zinc acetate and cobalt acetate;
the titanium catalyst comprises one or more of ethylene glycol titanium, titanate and nano titanium dioxide;
(2) the polyester melt is pressurized by a melt booster pump and then is conveyed to a spinning manifold through a melt cooler, and is extruded by a spinneret plate to form nascent fiber, wherein the post-pump pressure of the booster pump is 145-160bar, and the temperature of the melt cooler is 280-288 ℃;
(3) cooling and solidifying the nascent fiber at the cooling air temperature of 20-25 ℃, bundling and oiling, and then winding and forming at the winding speed of 2600-;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed is 650-750m/s, the draft ratio is 1.73-1.75%, the speed ratio is 1.45-1.55%, the temperature of the first hot box is 175-185 ℃, and the temperature of the second hot box is 165-170 ℃.
Example 1:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Example 2:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw-texturing machine is 680m/s, the draw ratio is 1.73%, the speed ratio is 1.55%, the temperature of the first hot box is 183 ℃, and the temperature of the second hot box is 168 ℃.
Example 3:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.48%, the temperature of the first hot box is 175 ℃, and the temperature of the second hot box is 165 ℃.
Example 4:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw-texturing machine is 750m/s, the draw ratio is 1.75%, the speed ratio is 1.45%, the temperature of the first hot box is 185 ℃, and the temperature of the second hot box is 170 ℃.
Example 5:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw ratio is 1.75%, the speed ratio is 1.52%, the temperature of the first hot box is 178 ℃, and the temperature of the second hot box is 172 ℃.
Example 6:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.41, then adding 30ppm of zinc acetate as a cocatalyst and 7ppm of titanium ethylene glycol titanium as a titanium catalyst, and preparing a polyester melt by carrying out esterification reaction at 260 ℃ and 300Kpa, pre-polycondensation reaction for 2h at 265 ℃ and 200pa, and final polycondensation reaction for 2h at 273 ℃ and 200 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 145bar, and the temperature of the melt cooler is 280 ℃;
(3) cooling and solidifying the nascent fiber at the cooling air temperature of 20 ℃, bundling and oiling, and then winding and forming at the winding speed of 2600 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Example 7:
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.55, then adding 50ppm of co-catalyst cobalt acetate and 15ppm of titanium catalyst nano titanium dioxide, and preparing a polyester melt after carrying out esterification reaction at 270 ℃, 700Kpa, pre-polycondensation reaction for 3 hours at 272 ℃, 550pa and final polycondensation reaction for 3 hours at 282 ℃, 360 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 160bar, and the temperature of the melt cooler is 288 ℃;
(3) cooling and solidifying the nascent fiber at the cooling air temperature of 25 ℃, bundling and oiling, and then winding and forming at the winding speed of 2900 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
as shown in fig. 1-2, the low-friction thread guide comprises a thread guide body 1, a thread hole 2 penetrates through the thread guide body, the thread hole presents an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the thread guide body, and the thread hole is communicated with the side wall of the thread guide body through a thread guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Comparative example 1: the difference from the embodiment 1 is that a low-friction yarn guide is not adopted, and a conventional texturing process is adopted;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the speed of the draw-texturing machine is 500m/s, the draw ratio is 1.76%, the speed ratio is 1.6%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 175 ℃.
Comparative example 2: the difference from example 1 is that no low friction guide is used;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a conventional yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the speed of the draw ratio is 1.74%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Comparative example 3: the difference from the example 1 is that the conventional elasticizing process is adopted;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the low-friction wire guide comprises a wire guide body 1, a wire hole 2 penetrates through the wire guide body, the wire hole is of an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the wire guide body, and the wire hole is communicated with the side wall of the wire guide body through a wire guide channel 3;
the speed of the draw-texturing machine is 500m/s, the draw ratio is 1.76%, the speed ratio is 1.6%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 175 ℃.
Comparative example 4: the difference from the embodiment 1 is that a low-friction yarn guide is not adopted, and a conventional texturing process is adopted;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the low-friction wire guide comprises a wire guide body 1, a wire hole 2 penetrates through the wire guide body, the wire hole is of an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the wire guide body, and the wire hole is communicated with the side wall of the wire guide body through a wire guide channel 3;
the speed of the draw-texturing machine is 700m/s, the draw ratio is 1.76%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Comparative example 5: the difference from the embodiment 1 is that a low-friction yarn guide is not adopted, and a conventional texturing process is adopted;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the low-friction wire guide comprises a wire guide body 1, a wire hole 2 penetrates through the wire guide body, the wire hole is of an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the wire guide body, and the wire hole is communicated with the side wall of the wire guide body through a wire guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.57%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 170 ℃.
Comparative example 6: the difference from the embodiment 1 is that a low-friction yarn guide is not adopted, and a conventional texturing process is adopted;
a preparation method of antimony-free DTY polyester fibers comprises the following preparation steps:
(1) mixing terephthalic acid and ethylene glycol in a mass ratio of 1:0.48, then adding 40ppm of co-catalyst magnesium acetate and 8ppm of titanium catalyst titanate, and preparing a polyester melt after esterification reaction at 265 ℃ and 500Kpa, pre-polycondensation reaction for 2.5h at 270 ℃ and 350pa and final polycondensation reaction for 2.5h at 278 ℃ and 280 pa;
(2) pressurizing the polyester melt by a melt booster pump, conveying the polyester melt to a spinning manifold by a melt cooler, and extruding the polyester melt by a spinneret plate to form nascent fiber, wherein the post-pumping pressure of the booster pump is 150bar, and the temperature of the melt cooler is 284 ℃;
(3) cooling and solidifying the nascent fiber at a cooling air temperature of 22 ℃, bundling and oiling, and then winding and forming at a winding speed of 2700 m/min;
(4) the formed fiber is subjected to texturing by adopting SSS as an oiling agent, and the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a hot box, oiling and winding, so that the antimony-free DTY polyester fiber is prepared;
the low-friction wire guide comprises a wire guide body 1, a wire hole 2 penetrates through the wire guide body, the wire hole is of an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the wire guide body, and the wire hole is communicated with the side wall of the wire guide body through a wire guide channel 3;
the speed of the draw ratio is 1.74%, the speed ratio is 1.50%, the temperature of the first hot box is 180 ℃, and the temperature of the second hot box is 175 ℃.
The antimony-free DTY polyester fibers prepared in the examples and comparative examples were subjected to spinning property characterization, and the results are shown in the following table.
The data show that the antimony-free DTY polyester fiber prepared by the method has high breaking strength, large breaking elongation, less broken yarn and high dyeing M% rate; comparative examples 1-3, which did not use a low friction guide or used a conventional process, were inferior in each performance, while comparative examples 4-6, which used the low friction guide of the present invention, were inferior in overall performance because the process parameters exceeded the defined ranges.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the antimony-free DTY polyester fiber is characterized by comprising the following preparation steps:
(1) preparing a polyester melt from terephthalic acid, ethylene glycol, a cocatalyst and a titanium catalyst through esterification reaction, pre-polycondensation and final polycondensation;
(2) carrying out spinning on the polyester melt to form nascent fiber;
(3) cooling and solidifying the nascent fiber, bundling and oiling, and winding and forming;
(4) and (3) performing texturing on the formed fiber, wherein the texturing comprises a low-friction yarn guide, a roller, a hot box, a twister, a second hot box, oiling and winding to prepare the antimony-free DTY polyester fiber.
2. The method of preparing antimony-free DTY polyester fiber as claimed in claim 1, wherein the mass ratio of terephthalic acid and ethylene glycol in step (1) is 1: 0.41-0.55.
3. The method for preparing antimony-free DTY polyester fiber as claimed in claim 1, wherein the cocatalyst in step (1) comprises one or more of magnesium acetate, zinc acetate and cobalt acetate in an amount of 30-50 ppm.
4. The method for preparing the antimony-free DTY polyester fiber as claimed in claim 1, wherein the titanium catalyst in step (1) comprises one or more of ethylene glycol titanium, titanate and nano titanium dioxide, and the amount of the titanium catalyst is 7-15 ppm.
5. The method for preparing the antimony-free DTY polyester fiber as claimed in claim 1, wherein the esterification reaction temperature in step (1) is 260-270 ℃, and the pressure is 300-700 Kpa; the pre-polycondensation is carried out for 2-3h at 265 ℃ and 272 ℃ and 200 ℃ and 550 Pa; the final polycondensation is carried out at the temperature of 273-.
6. The method as claimed in claim 1, wherein the polyester melt in step (2) is pressurized by a melt booster pump, then is transported to a spinning beam through a melt cooler, and is extruded by a spinneret plate to form a nascent fiber, wherein the post-pumping pressure of the booster pump is 145-160bar, and the temperature of the melt cooler is 280-288 ℃.
7. The method for preparing antimony-free DTY polyester fiber as claimed in claim 1, wherein the cooling wind temperature during cooling solidification in step (3) is 20-25 ℃, winding speed during winding is 2600-.
8. The method for preparing antimony-free DTY polyester fiber as claimed in claim 1, wherein the oiling agent used in the texturing in step (4) is SSS oiling agent.
9. The preparation method of the antimony-free DTY polyester fiber as claimed in claim 1, wherein the low-friction yarn guide in the step (4) comprises a yarn guide body (1), the yarn guide body (1) is penetrated with yarn holes (2), the yarn holes are in an hourglass-shaped structure with a small middle part and large two ends towards the thickness direction of the yarn guide body, and the yarn holes (2) are communicated with the side wall of the yarn guide body (1) through yarn guide channels (3).
10. The method as claimed in claim 1, wherein the texturing step in step (4) is carried out at a speed of 650-750m/s, a draw ratio of 1.73-1.75%, a speed ratio of 1.45-1.55%, a temperature of the first hot box of 175-185 ℃ and a temperature of the second hot box of 165-170 ℃.
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