CN107574502B - Preparation method of superfine denier polyester FDY (fully drawn yarn) for high-density fabric - Google Patents
Preparation method of superfine denier polyester FDY (fully drawn yarn) for high-density fabric Download PDFInfo
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Abstract
The invention relates to a preparation method of superfine denier polyester FDY (fully drawn yarn) for high-density fabrics, which comprises the steps of mixing dimethyl isophthalate-5-sodium benzenesulfonate, ethylene glycol and a catalyst, carrying out ester exchange reaction, adding the ethylene glycol, sodium glycol and sulfuric acid after the reaction is finished, mixing the terephthalic acid, the ethylene glycol, the catalyst and a stabilizer, carrying out esterification reaction, adding a product obtained after the ester exchange reaction into a reaction system reaching the end point of the esterification reaction, carrying out polycondensation reaction to obtain a spinning melt, and finally carrying out metering, extruding, cooling, oiling, stretching, heat setting and winding on the spinning melt to obtain the superfine denier polyester FDY for the high-density fabrics. The method reduces the generation of impurities in the production process of the polyester FDY yarns, thereby reducing the pressure rise of a spinning assembly and a filter, prolonging the service cycle of the spinning assembly and the filter, ensuring the continuity and safety of the whole production process and having good economic value and popularization value.
Description
Technical Field
The invention belongs to the field of polyester spinning, and relates to a preparation method of superfine denier polyester FDY yarns for high-density fabrics.
Background
The high-density fabric refers to a fabric with low number of warp and weft yarn raw materials and high warp and weft density during fabric production. The density of the fabric is divided into warp density and weft density, the finer the yarn count is, the higher the density is possible, so the high-density fabric is usually based on high count, and the cotton fabric has fine and dense lines, thin and comfortable hand feeling and is not permeable, and belongs to the category of high-grade fabrics. When defining fabrics according to the production practice and the application of chemical fiber filament fabrics, the fabrics with the fineness of below 50D (55.5dtex) and the warp density and weft density of 1200 pieces/10 cm and above are conventionally regarded as high-count (low-denier) high-density fabrics.
The raw material commonly used for spinning the high-count and high-density fabric is terylene, which has a series of excellent performances such as high breaking strength and elastic modulus, moderate rebound resilience, excellent heat setting, good heat and light resistance, good acid, alkali and corrosion resistance and the like, and in addition, the fabric also has the advantages of crease resistance, material free, good stiffness and the like, so the high-density fabric is widely applied to the fields of clothing, home textiles and the like. However, because the polyester fiber has the characteristics of high crystallinity, high orientation degree, high glass transition temperature and the like, the dye is difficult to diffuse into PET molecules under the condition of no carrier under normal pressure, and the dyeing is difficult, so the dyeing of the PET fiber needs to be carried out under the conditions of high temperature and high pressure or the presence of a carrier, and the high-density superfine denier fabric is difficult to dye due to high warp and weft density, high tightness and fine yarn count, and wrinkles, laps and stains which are difficult to eliminate easily appear, and the product quality is seriously influenced due to the fact that the polyester fiber is usually subjected to cutting treatment in finished product inspection to generate more short code drop and the like.
Cationic Dyeable PET (CDP) is a copolymer formed by introducing a third component into a macromolecular chain of PET and leading the third component to be formed with the macromolecular chain of the PET, overcomes the defect that terylene is not easy to dye, and is an important PET variety after a large bright and semi-dull PET slice at present, wherein the third component generally contains a strong acid sodium sulfonate group-SO3Na and sodium sulfonate groups can perform chemical reaction with cationic dye, and have affinity to the cationic dye, so that the dye is easy to fix on fibers, and dyed fabrics have the advantages of bright color, complete chromatogram, high dye-uptake rate, difficult fading and fading after washing and the like, and can fully meet the requirement of modern life diversification, therefore, the cationic dye dyeable PET is rapidly developed in recent years.
However, due to the addition of the third component in the CDP melt, the apparent viscosity is high, impurities generated in the production process are increased correspondingly, the pressure of part of spinning components and the pressure difference rising speed of the filter are caused to be high, and meanwhile, carbonized cokes are generated on the inner wall of the pipeline and adhered to the inner wall of the pipeline, so that the pipeline system is easy to block and is difficult to remove, and the pipeline dredging work is very difficult.
Therefore, a method for preparing the ultra-fine denier polyester FDY for high-density fabrics, which can effectively reduce the generation of impurities in the production process, is needed to be researched.
Disclosure of Invention
In the production process of superfine denier polyester FDY yarns for high-density fabrics, sulfonic-SO-containing yarns are often added for improving the dye uptake of the polyester FDY yarns3 -A third component of (a), sulfonic acid group-SO3 -The structural characteristics of (A) are as follows: 1) sulfonic acid-SO3 -The group has three oxygen atoms, can be connected with metal ions from different directions to form a complex with higher structure dimension, and can also be used as a hydrogen bond acceptor to simultaneously accept three hydrogen bonds in different directions to form a divergent hydrogen bond; 2) the sulfonic group has strong electron-withdrawing ability, can reduce pi electron density on a benzene ring, can strengthen the electrical functional property of a metal complex of the metal complex, and is easy to form a porous complex; 3) the coordination degree of the sulfonic acid group is adjustable. Sulfonic acid group-SO3 -There are over ten different coordination modes with metal ions, and coordination with metals and transition metals can be performed.
Sb catalysts (ethylene glycol antimony or antimony oxide) are usually added into the polymerization stage of the superfine denier polyester FDY yarns for the high-density fabrics, the addition amount is generally ten-thousandth of terephthalic acid, the content of Sb in cokes is very high, obviously, the Sb is completely sourced from the catalysts, and the enrichment of metal Sb is realized because antimony ions in the Sb catalysts are easy to be combined with sulfonic acid-SO in a third component and/or polymer3 -By formation of coordination compounds by means of coordinative bonds, once antimony ions have been bound to sulfonic acid groups-SO3 -The enrichment in a matching action mode can cause the increase of impurities in the spinning melt, carbonized coke is generated on the inner wall of a melt pipeline, and the blockage of a pipeline system is caused, the difficulty of the pipeline dredging work is greatly brought by the indissolvability of the carbonized coke, meanwhile, the rising speed of partial component pressure and the filter differential pressure is high, the service cycle of the filter and certain components is seriously influenced, the service cycle of the filter is only one week, and the service cycle of the components is only about 10 days. Increase in the number of cleaning and frequency of replacement of componentsOnly the running cost is increased, and the continuity and safety of the whole production process are affected. The superfine denier polyester FDY yarn for the high-density fabric has small linear density and often has the total titer of less than 10dtex, so the spinning difficulty is high, the requirement on a spinning melt is high, the impurity amount in the melt is reduced, and the spinnability of the melt is improved, so the reduction of the impurity is very important, and the key point of the spinning of the superfine denier polyester FDY yarn for the high-density fabric is realized.
The invention aims to overcome the problems in the prior art and provide a preparation method of superfine denier polyester FDY yarns for high-density fabrics, which can effectively reduce the generation of impurities in the production process.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) mixing dimethyl isophthalate-5-sodium benzenesulfonate, glycol and a catalyst, then carrying out ester exchange reaction, and adding glycol, sodium glycol and sulfuric acid after the reaction is finished for modulation;
the purpose of adding ethylene glycol after the ester exchange reaction is to adjust the percentage concentration of the dihydroxy ethyl isophthalate-5-sodium Sulfonate (SIPE) in the ethylene glycol solution, because when the concentration of the dihydroxy ethyl isophthalate-5-sodium Sulfonate (SIPE) is more than 40 wt%, precipitation can occur, which is not beneficial to the subsequent reaction; in the prior art, the catalyst used in the polymerization stage of the superfine denier terylene FDY yarn for the high-density fabric is generally ethylene glycol antimony or antimony oxide, antimony ions in the catalyst and sulfonic acid groups in a third component introduced into a PET slice often undergo a coordination chemical reaction to form a complex, the complex further undergoes a self-polymerization reaction along with the third component to generate a coke which is deposited on the surface of a pipeline and a spinneret plate to form a blockage, and the ethylene glycol sodium can provide a certain amount of coexisting ions which have a competitive relationship with the antimony ions to influence and weaken the coordination effect of the antimony ions and the sulfonic acid groups, so that the complex formed by the coordination of the sulfonic acid groups and the catalyst is effectively reduced, namely the complex in a spinning melt is reducedThe good flow property of the polyester is kept, so that the spinnability of the superfine denier polyester FDY for the high-density fabric is ensured; h in sulfuric acid+Can react with sulfonic acid groups to influence the formation of complexes due to H+The presence of (A) reduces the ability of the sulfonic acid group to undergo a complexation reaction, which may be referred to as an acid effect, H+The greater the concentration of (A), the more pronounced the effect of the acid, a certain amount of acid reduces the formation of the complex, but an excessive amount affects the thermal stability of the polyester. The addition of a certain amount of sulfuric acid can reduce the generation of the complex, so that the polyester flows more stably.
(2) Mixing terephthalic acid, ethylene glycol, a catalyst and a stabilizer, and then carrying out esterification reaction;
the addition of the stabilizer can effectively reduce the side reaction in the esterification reaction process of the polyester;
(3) adding the product of (1) into (2) to carry out polycondensation reaction to obtain a spinning melt;
b) spinning;
and (3) metering, extruding, cooling, oiling, stretching, heat setting and winding the spinning melt to obtain the superfine denier polyester FDY yarn for the high-density fabric.
As a preferred technical scheme:
the preparation method of the superfine denier polyester FDY yarn for the high-density fabric comprises the following specific steps of:
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol into a preparation kettle, and adding a catalyst Zn (Ac)2Then carrying out ester exchange reaction at 175-185 ℃ until the distilled amount of water reaches more than 90% of a theoretical value, obtaining sodium dihydroxy ethyl isophthalate-5-sulfonate, adding ethylene glycol, sodium ethylene glycol and sulfuric acid, and modulating to obtain an ethylene glycol solution containing 30-35 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol into slurry, adding a catalyst and a stabilizer, uniformly mixing, and then carrying out esterification reaction to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out in a nitrogen atmosphere under a pressure of normal pressure to 0.3MPa at a temperature of 250-260 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches more than 90% of the theoretical value;
(3) preparing spinning melt through polycondensation;
and (3) adding the product in the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the reaction temperature is 260-270 ℃, the reaction time is 30-50 min, then, continuing to carry out polycondensation reaction in a high vacuum stage by vacuumizing, and reducing the reaction pressure to below 100Pa absolute, the reaction temperature is 275-285 ℃, and the reaction time is 50-90 min, thus obtaining the spinning melt.
In the preparation method of the superfine denier polyester FDY yarn for the high-density fabric, in the step (1), when the ester exchange reaction is started, the molar ratio of dimethyl isophthalate-5-sodium benzenesulfonate to ethylene glycol is 10-12: 1, and a catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.2-0.5 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate;
during preparation, the addition amount of the sodium ethylene glycol is 1.5-6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 40-60%, and the addition amount of the sulfuric acid is 1.5-6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate.
In the step (2), when the esterification reaction is started, the molar ratio of the terephthalic acid to the ethylene glycol is 1.10-1.30: 1, the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate, the adding amount of the catalyst is 0.01-0.05 wt% of the adding amount of the terephthalic acid, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, and the adding amount of the stabilizer is 0.01-0.05 wt% of the adding amount of the terephthalic acid.
According to the preparation method of the superfine denier polyester FDY yarn for the high-density fabric, in the step (3), when the polycondensation reaction starts, the molar ratio of the m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate to the terephthalic acid glycol ester is 1-3: 100.
In order to adapt to the influence of the addition of the stabilizer, the glycol, the sulfuric acid, the sodium glycol and other substances on the final spinning process in the preparation process, the method for preparing the superfine denier polyester FDY yarns for the high-density fabric needs to adjust the spinning process parameters of the superfine denier polyester FDY yarns for the high-density fabric, and the adjusted spinning process parameters are as follows:
spinning temperature: 285-295 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20 to 0.30 MPa;
a roll speed: 1000-1500 m/min;
first roll temperature: 86-95 ℃;
two roll speed: 3820-4200 m/min;
temperature of the two rolls: 117-130 ℃;
winding speed: 3800-4100 m/min.
According to the preparation method of the superfine denier polyester FDY yarn for the high-density fabric, in the spinning process, the pressure rise delta P of the spinning assembly is less than or equal to 0.8 bar/day, the pressure rise delta P of the filter is less than or equal to 2.9 bar/day, the service cycle of the spinning assembly is 36-38 days, and the service cycle of the filter is 25-27 days.
According to the preparation method of the superfine denier polyester FDY for the high-density fabric, the linear density of the superfine denier polyester FDY for the high-density fabric is 7-8D, the filament number of the superfine denier polyester FDY is 0.5-0.7 dtex, the breaking strength is more than or equal to 3.80cN/dtex, and the dye uptake is more than 95%.
The preparation method of the superfine denier polyester FDY yarns for the high-density fabric has the advantages that the breaking elongation of the superfine denier polyester FDY yarns for the high-density fabric is 40.0 +/-5.0%, the linear density deviation rate is less than or equal to 0.8%, the breaking strength CV value is less than or equal to 5.0%, the breaking elongation CV value is less than or equal to 10.0%, and the yarn evenness CV value is less than or equal to 1.5%.
Has the advantages that:
(1) according to the preparation method of the superfine denier polyester FDY yarn for the high-density fabric, impurities generated in the production process are reduced, so that the pressure rise of a spinning assembly and a filter is reduced, the service cycle of the spinning assembly and the filter is prolonged, the production cost is reduced, the continuity and the safety of the whole production process are further ensured, and the preparation method has good economic value and popularization value;
(2) according to the preparation method of the superfine denier polyester FDY yarn for the high-density fabric, the sodium ethylene glycol and the sulfuric acid are added, so that the formation of a complex in the production process is reduced, impurities in a spinning melt are reduced, the good flow property of polyester is maintained, and the spinnability of the superfine denier polyester FDY yarn for the high-density fabric is further ensured;
(3) the preparation method of the superfine denier polyester FDY yarns for the high-density fabric reduces the generation of impurities in the melt conveying process, and solves the problems that the high-density fabric is easy to have the phenomena of uneven evenness, poor cloth cover, unclear weave patterns, multiple defects, unstable quality and the like due to too high yarn count density and high production difficulty.
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.
Example 1
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 10:1 into a preparation kettle, and adding a catalyst Zn (Ac)2Performing ester exchange reaction at 175 deg.C until water distillate reaches 90% of theoretical value to obtain sodium dihydroxy ethyl isophthalate-5-sulfonate, adding ethylene glycol, sodium ethylene glycol and sulfuric acid, and concocting to obtain ethylene glycol containing 30 wt% sodium dihydroxy ethyl isophthalate-5-sulfonateAlcoholic solution of catalyst Zn (Ac)2The adding amount of the sodium ethylene glycol is 0.2 wt% of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate, during preparation, the adding amount of the sodium ethylene glycol is 1.5 wt% of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 40%, and the adding amount of the sulfuric acid is 1.5 wt% of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.10:1 into slurry, adding antimony trioxide and triphenyl phosphate, uniformly mixing, and performing esterification reaction at 250 ℃ to obtain ethylene glycol terephthalate, wherein the esterification reaction is performed under a nitrogen atmosphere and under a normal pressure, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 90% of a theoretical value, wherein the adding amount of the antimony trioxide is 0.01 wt% of the adding amount of the terephthalic acid, and the adding amount of the triphenyl phosphate is 0.05 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
adding the product of the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to an absolute pressure of 500Pa, the reaction temperature is 260 ℃, the reaction time is 30min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, reducing the reaction pressure to an absolute pressure of 99.5Pa, the reaction temperature is 275 ℃, and the reaction time is 50min, and preparing a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the sodium m-hydroxyethyl phthalate-5-sulfonate to the ethylene glycol terephthalate is 1: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 285 ℃;
cooling temperature: 20 ℃;
network pressure: 0.20 MPa;
a roll speed: 1500 m/min;
first roll temperature: 86 ℃;
two roll speed: 3820 m/min;
temperature of the two rolls: 130 ℃;
winding speed: 3900 m/min;
in the spinning process, due to the preparation of ethylene glycol, sodium ethylene glycol and sulfuric acid, the amount of impurities in the melt is greatly reduced, and the pressure rise of a spinning assembly and a filter is effectively reduced, wherein the pressure rise delta P of the spinning assembly is 0.7 bar/day, the pressure rise delta P of the filter is 2.7 bar/day, the service cycle of the spinning assembly is 38 days, and the service cycle of the filter is 25 days.
The superfine denier polyester FDY for the high-density fabric obtained by the steps has the linear density of 8D, the filament number of 0.6dtex, the breaking strength of 3.90cN/dtex, the dye uptake of 98 percent, the elongation at break of 40.0 percent, the linear density deviation rate of 0.6 percent, the CV value of the breaking strength of 5.0 percent, the CV value of the elongation at break of 9.5 percent and the CV value of the yarn evenness rate of 1.4 percent.
Comparative example 1
In the prior art, the steps of the superfine denier polyester FDY fiber for high-density fabrics are performed under the conditions of high temperature and high pressure, which is basically the same as the example 1, except that in the step (1), glycol, sodium glycol and sulfuric acid are not used for modulation after the ester exchange reaction. The pressure rise delta P of the spinning assembly in the spinning process is 4.3 bar/day, the pressure rise delta P of the filter is 8.7 bar/day, the service cycle of the spinning assembly is 7 days, and the service cycle of the filter is 10 days. Compared with the example 1, the single filament number of the prepared cationic dyeable polyester fiber is 6.3dtex, the breaking strength is 2.87cN/dtex, the dye uptake is 93.2%, the elongation at break is 34.6%, the linear density deviation rate is 0.45%, the breaking strength CV value is 3.75%, the elongation at break CV value is 7.87%, and the evenness unevenness CV value is 1.94%.
Example 2
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 11:1 into a preparation kettle, and adding a catalyst Zn (Ac)2After the reaction product and an ether inhibitor NaAc are subjected to ester exchange reaction at 178 ℃ until the distilled amount of water reaches 92% of a theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then glycol, sodium glycol and sulfuric acid are added for modulation, and a glycol solution containing 31 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.3 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is 0.13 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the addition amount of the sodium ethylene glycol is 2 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 45%, and the addition amount of the sulfuric acid is 3.5 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.15:1 into slurry, adding ethylene glycol antimony and trimethyl phosphate, uniformly mixing, carrying out esterification reaction at 253 ℃ to obtain ethylene glycol terephthalate, carrying out pressure reaction in a nitrogen atmosphere at a pressure of 0.1MPa, and taking the esterification reaction as an end point when the distilled water amount in the esterification reaction reaches 91% of a theoretical value, wherein the adding amount of the ethylene glycol antimony is 0.02 wt% of the adding amount of the terephthalic acid, and the adding amount of the trimethyl phosphate is 0.04 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
performing polycondensation reaction in a low vacuum stage in the product (2) of the step (1) under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 490Pa, the reaction temperature is 262 ℃, the reaction time is 35min, then continuously vacuumizing to perform polycondensation reaction in a high vacuum stage, the reaction pressure is reduced to absolute pressure of 98Pa, the reaction temperature is 277 ℃, the reaction time is 60min, and preparing a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the dihydroxy ethyl isophthalate-5-sodium sulfonate to the ethylene terephthalate is 1.3: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 287 deg.C;
cooling temperature: 21 ℃;
network pressure: 0.22 MPa;
a roll speed: 1400 m/min;
first roll temperature: 88 ℃;
two roll speed: 3870 m/min;
temperature of the two rolls: 124 ℃;
winding speed: 3870 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.8 bar/day, the pressure rise delta P of the filter is 2.9 bar/day, the service cycle of the spinning assembly is 37 days, and the service cycle of the filter is 25 days.
The superfine denier polyester FDY yarn for the high-density fabric obtained in the step has the linear density of 7.2D, the filament number of 0.7dtex, the breaking strength of 3.84cN/dtex, the dye uptake of 96.5%, the elongation at break of 35.0%, the linear density deviation rate of 0.7%, the breaking strength CV value of 4.5%, the elongation at break CV value of 8.8% and the yarn evenness CV value of 1.3%.
Example 3
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 12:1 into a preparation kettle, and adding a catalyst Zn (Ac)2After being mixed with an ether inhibitor NaAc, the reaction is carried out at 179 DEG CThe ester exchange reaction is finished until the distilled amount of water reaches 91 percent of a theoretical value to obtain the dihydroxy ethyl isophthalate-5-sodium sulfonate, then the glycol, the sodium glycol and the sulfuric acid are added to prepare the glycol solution containing 32 weight percent of dihydroxy ethyl isophthalate-5-sodium sulfonate, wherein the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.25 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is 0.15 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the addition amount of the sodium ethylene glycol is 2.5 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 50%, and the addition amount of the sulfuric acid is 4 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.20:1 into slurry, adding antimony acetate and trimethyl phosphite, uniformly mixing, performing esterification reaction at 255 ℃ to obtain ethylene glycol terephthalate, performing pressure reaction in a nitrogen atmosphere at a pressure of 0.15MPa, and determining an esterification reaction endpoint when the distilled water amount in the esterification reaction reaches 92% of a theoretical value, wherein the adding amount of the antimony acetate is 0.03 wt% of the adding amount of the terephthalic acid, and the adding amount of the trimethyl phosphite is 0.03 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
adding the product of the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is steadily pumped from normal pressure to absolute pressure of 480Pa, the reaction temperature is 264 ℃, the reaction time is 40min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, so that the reaction pressure is reduced to absolute pressure of 98Pa, the reaction temperature is 279 ℃, the reaction time is 70min, and preparing a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the m-hydroxyethyl phthalate-5-sodium sulfonate to the ethylene glycol terephthalate is 1.7: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 289 deg.C;
cooling temperature: 22 ℃;
network pressure: 0.24 MPa;
a roll speed: 1300 m/min;
first roll temperature: 89 ℃;
two roll speed: 3900 m/min;
temperature of the two rolls: 122 ℃;
winding speed: 4100 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.7 bar/day, the pressure rise delta P of the filter is 2.9 bar/day, the service cycle of the spinning assembly is 38 days, and the service cycle of the filter is 26 days.
The superfine denier polyester FDY yarn for the high-density fabric obtained in the step has the linear density of 7.3D, the filament number of 0.57dtex, the breaking strength of 3.80cN/dtex, the dye uptake of 95.8%, the elongation at break of 35.0%, the linear density deviation rate of 0.8%, the breaking strength CV value of 4.1%, the elongation at break CV value of 9.0% and the yarn evenness CV value of 1.5%.
Example 4
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 10.5:1 into a preparation kettle, and adding a catalyst Zn (Ac)2After the reaction product and an ether inhibitor NaAc are subjected to ester exchange reaction at 180 ℃ until the distilled amount of water reaches 93% of a theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then glycol, sodium glycol and sulfuric acid are added for modulation, and a glycol solution containing 33 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.35 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is the addition amount of the dimethyl isophthalate-5-benzene0.2 wt% of the addition amount of sodium sulfonate; during preparation, the addition amount of the sodium ethylene glycol is 5 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 55%, and the addition amount of the sulfuric acid is 4.5 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.25:1 into slurry, adding antimony trioxide and trimethyl phosphate, uniformly mixing, performing esterification reaction at 257 ℃ to obtain ethylene glycol terephthalate, performing pressure reaction in a nitrogen atmosphere at a pressure of 0.2MPa, and determining an esterification reaction endpoint when the distilled water amount in the esterification reaction reaches 93% of a theoretical value, wherein the adding amount of the antimony trioxide is 0.04 wt% of the adding amount of the terephthalic acid, and the adding amount of the trimethyl phosphate is 0.02 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
adding the product of the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 470Pa, the reaction temperature is 265 ℃, the reaction time is 40min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, reducing the reaction pressure to absolute pressure of 96Pa, the reaction temperature is 280 ℃, and the reaction time is 70min, thus obtaining a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the m-hydroxyethyl phthalate-5-sodium sulfonate to the ethylene glycol terephthalate is 2: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 293 ℃;
cooling temperature: 21.5 ℃;
network pressure: 0.26 MPa;
a roll speed: 1200 m/min;
first roll temperature: 90 ℃;
two roll speed: 4000 m/min;
temperature of the two rolls: 130 ℃;
winding speed: 3800 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.6 bar/day, the pressure rise delta P of the filter is 2.2 bar/day, the service cycle of the spinning assembly is 36 days, and the service cycle of the filter is 27 days.
The superfine denier polyester FDY yarn for the high-density fabric obtained in the step has the linear density of 8D, the filament number of 0.52dtex, the breaking strength of 3.91cN/dtex, the dye uptake of 95.1%, the elongation at break of 45.0%, the linear density deviation rate of 0.77%, the breaking strength CV value of 4.8%, the elongation at break CV value of 10.0% and the yarn evenness CV value of 1.2%.
Example 5
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 11.5:1 into a preparation kettle, and adding a catalyst Zn (Ac)2After the reaction product and an ether inhibitor NaAc are subjected to ester exchange reaction at 182 ℃ until the distilled amount of water reaches 96% of a theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then glycol, sodium glycol and sulfuric acid are added for modulation, and a glycol solution containing 34 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.4 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is 0.13 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the addition amount of sodium ethylene glycol is 4 wt% of the addition amount of dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 45%, and the addition amount of the sulfuric acid is 5 wt% of the addition amount of dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.30:1 into slurry, adding ethylene glycol antimony and trimethyl phosphite, uniformly mixing, carrying out esterification reaction at 252 ℃ to obtain ethylene glycol terephthalate, carrying out pressure reaction in a nitrogen atmosphere at a pressure of 0.25MPa, and setting the end point of the esterification reaction when the distilled water amount in the esterification reaction reaches 94% of a theoretical value, wherein the adding amount of the ethylene glycol antimony is 0.04 wt% of the adding amount of the terephthalic acid, and the adding amount of the trimethyl phosphite is 0.01 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
adding the product of the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is steadily pumped from normal pressure to below 500Pa absolute, the reaction temperature is 268 ℃, the reaction time is 45min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, so that the reaction pressure is reduced to 95Pa absolute, the reaction temperature is 282 ℃, the reaction time is 80min, and preparing a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the m-hydroxyethyl phthalate-5-sodium sulfonate to the ethylene glycol terephthalate is 2.5: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 295 ℃;
cooling temperature: 23 ℃;
network pressure: 0.25 MPa;
a roll speed: 1100 m/min;
first roll temperature: 93 ℃;
two roll speed: 4200 m/min;
temperature of the two rolls: 123 ℃;
winding speed: 4050 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.8 bar/day, the pressure rise delta P of the filter is 2.9 bar/day, the service cycle of the spinning assembly is 36 days, and the service cycle of the filter is 25 days.
The superfine denier polyester FDY yarn for the high-density fabric obtained by the steps has the linear density of 7D, the filament number of 0.55dtex, the breaking strength of 3.80cN/dtex, the dye uptake of 96 percent, the elongation at break of 40.0 percent, the linear density deviation rate of 0.75 percent, the CV value of the breaking strength of 4.9 percent, the CV value of the elongation at break of 10.0 percent and the CV value of the yarn evenness rate of 1.5 percent.
Example 6
A preparation method of superfine denier polyester FDY yarns for high-density fabrics comprises the following steps:
a) preparing a spinning melt;
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
firstly, adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol in a molar ratio of 12:1 into a preparation kettle, and adding a catalyst Zn (Ac)2After the reaction product is subjected to ester exchange reaction with an ether inhibitor NaAc at 185 ℃ until the distilled amount of water reaches 94% of a theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then glycol, sodium glycol and sulfuric acid are added for modulation, and a glycol solution containing 35 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.5 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is 0.2 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the addition amount of the sodium ethylene glycol is 6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 60%, and the addition amount of the sulfuric acid is 6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.25:1 into slurry, adding antimony acetate and triphenyl phosphate, uniformly mixing, and then carrying out esterification reaction at 260 ℃ to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out under a pressure of 0.3MPa in a nitrogen atmosphere, and the end point of the esterification reaction is when the distilled amount of water in the esterification reaction reaches 90% of a theoretical value, wherein the adding amount of the antimony acetate is 0.05 wt% of the adding amount of the terephthalic acid, and the adding amount of the triphenyl phosphate is 0.35 wt% of the adding amount of the terephthalic acid;
(3) preparing spinning melt through polycondensation;
adding the product of the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to an absolute pressure of 500Pa, the reaction temperature is 270 ℃, the reaction time is 50min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, reducing the reaction pressure to an absolute pressure of 94Pa, the reaction temperature is 285 ℃, and the reaction time is 90min, thus obtaining a spinning melt, wherein when the polycondensation reaction starts, the molar ratio of the m-hydroxyethyl phthalate-5-sodium sulfonate to the ethylene glycol terephthalate is 3: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric; the spinning process parameters are as follows:
spinning temperature: 291 deg.C;
cooling temperature: 25 ℃;
network pressure: 0.30 MPa;
a roll speed: 1000 m/min;
first roll temperature: 95 ℃;
two roll speed: 4160 m/min;
temperature of the two rolls: 117 ℃;
winding speed: 3900 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.7 bar/day, the pressure rise delta P of the filter is 2.85 bar/day, the service cycle of the spinning assembly is 36 days, and the service cycle of the filter is 26 days.
The superfine denier polyester FDY yarn for the high-density fabric obtained in the step has the linear density of 7.8D, the filament number of 0.5dtex, the breaking strength of 3.83cN/dtex, the dye uptake of 95.6%, the elongation at break of 35.0%, the linear density deviation rate of 0.8%, the breaking strength CV value of 5.0%, the elongation at break CV value of 9.2% and the yarn evenness CV value of 1.3%.
Claims (8)
1. A preparation method of superfine denier polyester FDY yarns for high-density fabrics is characterized by comprising the following steps:
a) preparing a spinning melt;
(1) mixing dimethyl isophthalate-5-sodium benzenesulfonate, glycol and a catalyst, then carrying out ester exchange reaction, and adding glycol, sodium glycol and sulfuric acid after the reaction is finished for modulation;
(2) mixing terephthalic acid, ethylene glycol, a catalyst and a stabilizer, and then carrying out esterification reaction; the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate;
(3) adding the product of (1) into (2) to carry out polycondensation reaction to obtain a spinning melt;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the superfine denier polyester FDY yarn for the high-density fabric;
in the spinning process, the pressure rise delta P of the spinning assembly is less than or equal to 0.8 bar/day, the pressure rise delta P of the filter is less than or equal to 2.9 bar/day, the service cycle of the spinning assembly is 36-38 days, and the service cycle of the filter is 25-27 days.
2. The preparation method of the superfine denier polyester FDY yarn for the high-density fabric according to claim 1, wherein the specific steps of preparing the spinning melt are as follows:
(1) preparing m-phthalic acid dihydroxy ethyl ester-5-sodium sulfonate by ester exchange reaction;
adding dimethyl isophthalate-5-sodium benzenesulfonate and ethylene glycol into a preparation kettle, and adding a catalyst Zn (Ac)2Then carrying out ester exchange reaction at 175-185 ℃ until the distilled amount of water reaches more than 90% of a theoretical value, obtaining sodium dihydroxy ethyl isophthalate-5-sulfonate, adding ethylene glycol, sodium ethylene glycol and sulfuric acid, and modulating to obtain an ethylene glycol solution containing 30-35 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
preparing terephthalic acid and ethylene glycol into slurry, adding a catalyst and a stabilizer, uniformly mixing, and then carrying out esterification reaction to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out in a nitrogen atmosphere under a pressure of normal pressure to 0.3MPa at a temperature of 250-260 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches more than 90% of the theoretical value;
(3) preparing spinning melt through polycondensation;
and (3) adding the product in the step (1) into the step (2), firstly, carrying out polycondensation reaction in a low vacuum stage under a negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the reaction temperature is 260-270 ℃, the reaction time is 30-50 min, then, continuing to carry out polycondensation reaction in a high vacuum stage by vacuumizing, and reducing the reaction pressure to below 100Pa absolute, the reaction temperature is 275-285 ℃, and the reaction time is 50-90 min, thus obtaining the spinning melt.
3. The method for preparing the superfine denier polyester FDY yarn for the high-density fabric according to claim 2, wherein in the step (1), the molar ratio of dimethyl isophthalate-5-sodium benzenesulfonate to ethylene glycol is 10-12: 1 at the beginning of the ester exchange reaction, and the catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.2-0.5 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate;
during preparation, the addition amount of the sodium ethylene glycol is 1.5-6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate, the mass concentration of the added sulfuric acid is 40-60%, and the addition amount of the sulfuric acid is 1.5-6 wt% of the addition amount of the dimethyl isophthalate-5-sodium benzenesulfonate.
4. The method for preparing the ultra-fine denier polyester FDY yarn for the high-density fabric as claimed in claim 2, wherein in the step (2), the molar ratio of terephthalic acid to ethylene glycol is 1.10-1.30: 1 at the beginning of the esterification reaction, the addition amount of the catalyst is 0.01-0.05 wt% of the addition amount of the terephthalic acid, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, and the addition amount of the stabilizer is 0.01-0.05 wt% of the addition amount of the terephthalic acid.
5. The preparation method of the ultra-fine denier polyester FDY yarn for the high-density fabric as claimed in claim 2, wherein in the step (3), the molar ratio of the sodium bis-hydroxyethyl isophthalate-5-sulfonate to the ethylene terephthalate is 1-3: 100 at the beginning of the polycondensation reaction.
6. The preparation method of the superfine denier polyester FDY yarn for the high-density fabric according to claim 1, wherein the spinning process parameters are as follows:
spinning temperature: 285-295 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20 to 0.30 MPa;
a roll speed: 1000-1500 m/min;
first roll temperature: 86-95 ℃;
two roll speed: 3820-4200 m/min;
temperature of the two rolls: 117-130 ℃;
winding speed: 3800-4100 m/min.
7. The preparation method of the superfine denier polyester FDY yarn for the high-density fabric, as claimed in claim 1, is characterized in that the linear density of the superfine denier polyester FDY yarn for the high-density fabric is 7-8D, the filament number is 0.5-0.7 dtex, the breaking strength is not less than 3.80cN/dtex, and the dye uptake is more than 95%.
8. The method for preparing the superfine denier polyester FDY yarns for the high-density fabric as claimed in claim 7, wherein the superfine denier polyester FDY yarns for the high-density fabric have an elongation at break of 40.0 +/-5.0%, a linear density deviation rate of less than or equal to 0.8%, a breaking strength CV value of less than or equal to 5.0%, an elongation at break CV value of less than or equal to 10.0%, and a yarn unevenness CV value of less than or equal to 1.5%.
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