CN107604464B - Preparation method of double-special-shaped-section moisture-absorbing and sweat-releasing fiber - Google Patents
Preparation method of double-special-shaped-section moisture-absorbing and sweat-releasing fiber Download PDFInfo
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Abstract
The invention relates to a preparation method of double-irregular-section moisture-absorbing and sweat-releasing fiber, which comprises the steps of mixing dimethyl isophthalate-5-sodium benzenesulfonate, ethylene glycol, a catalyst and an ether inhibitor, then carrying out ester exchange reaction, adding the ethylene glycol and phosphoric acid for modulation after the reaction is finished, then mixing the terephthalic acid, the ethylene glycol, the catalyst, a stabilizer and a flatting agent, carrying out esterification reaction, then adding a product prepared after the ester exchange reaction into a reaction system reaching the end point of the esterification reaction for polycondensation reaction to prepare spinning melt, and finally carrying out metering, extruding, cooling, oiling, stretching, heat setting and winding on the spinning melt to prepare the double-irregular-section moisture-absorbing and sweat-releasing fiber. The method reduces the generation of impurities in the fiber production process, thereby reducing the pressure rise of the spinning assembly and the filter, prolonging the service cycle of the spinning assembly and the filter, ensuring the continuity and safety of the whole production flow and having good economic value and popularization value.
Description
Technical Field
The invention belongs to the field of polyester spinning, and particularly relates to a preparation method of double-special-shaped-section moisture-absorbing and sweat-releasing fibers.
Background
The brand-new production concept oriented to the functions has rewritten the traditional market positioning of the textile industry and led the textile industry to enter the new era of the high-tech field. Starting from water, heat, air, skin feel and safety and comfort, it has been the aim of the textile industry to create fabrics with health-promoting and refreshing comfort properties. In recent years, the proportion of functional fabrics on the market is increased year by year, and high-tech intelligent textiles with health and functional characteristics such as antibiosis, deodorization, ultraviolet resistance, fire prevention, warm keeping, perspiration, moisture permeability and water resistance become mainstream products in the future market.
However, synthetic fiber fabrics often have the defect of uneasy moisture absorption and sweat release, and in order to overcome the defect, fiber and textile researchers at home and abroad have conducted a great deal of research, and various moisture absorption and sweat release fibers and fabrics have been developed. The product is developed, firstly, the outer layer of the fabric is coated with the modified auxiliary agent; secondly, carrying out post-treatment on the fabric by using a hydrophilic treatment agent; thirdly, various differential fibers with moisture permeability and special-shaped cross sections, such as Coolmax, Sweatsenor, Tricactor, Hydropore and the like, of fine denier or superfine denier are adopted.
The profiled fiber is generally prepared by a specially designed and manufactured profiled spinneret plate through a special spinning process, and the method is the most commonly used method for producing profiled fibers at home and abroad. The producer can produce the profiled fiber with any section shape by improving and optimizing the processing technology of the guide holes and the micropores of the spinneret plate and the spinning technology. Common special-shaped fibers have various shapes such as triangle, trilobal, multilobal, cross and hollow fibers. The double-profile fiber is a profile fiber prepared by spinning two profile holes on the same spinneret plate at the same time. The double-special-shaped-section moisture-absorbing and sweat-releasing fiber has good moisture-absorbing and sweat-releasing performance, can keep the inside of clothes dry and comfortable, reduces the friction between the clothes and the skin, brings comfortable wearing experience to people, and is more and more concerned by people. The moisture-absorbing and sweat-releasing fiber with double special-shaped cross sections is developed on the existing melt direct spinning circular blowing equipment, and the national guidelines for promoting differentiation of chemical fiber industrial products are met.
However, since PET fibers have characteristics such as high crystallinity, high degree of orientation, and high glass transition temperature, it is difficult to disperse dyes into PET molecules in the absence of carriers under normal pressure, and thus dyeing of PET fibers is difficult. 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, have affinity to the cationic dye, ensure that the dye is easy to fix on fibers, and the dyed fabric has the advantages of bright color, complete chromatogram, high dye uptake, difficult fading and fading after washing and the like, and can fully and fully reactMeets the diversified requirements of modern life, so that 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 preparation method of the moisture-absorbing and sweat-releasing fiber with the double irregular cross sections, which can effectively reduce the generation of impurities in the fiber production process, needs to be researched.
Disclosure of Invention
In the production process of the moisture-absorbing and sweat-releasing fiber with the double special-shaped cross section, sulfonic acid group-SO is often added to improve the dyeing rate of the fiber3 -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-series catalyst (ethylene glycol) is often added in the polymerization stage of the double-irregular-section moisture-absorbing and sweat-releasing type fiber polyesterAntimony or antimony oxide) is generally added in parts per million of terephthalic acid, while the content of Sb in the coke is very high, obviously, the Sb should be completely sourced from the catalyst, and the enrichment of metal Sb is because the antimony ions in the Sb-based catalyst are easy to react with the sulfonic acid group-SO in the 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. The increased number of cleaning and component replacement frequency not only increases the running cost, but also affects the continuity and safety of the whole production process. Therefore, the reduction of the generation of the impurities becomes the key point for producing the double-profiled-section moisture absorption and sweat releasing type fiber spinning.
The invention aims to overcome the problems in the prior art and provide a preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber, which can effectively reduce the generation of impurities in the fiber production process.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of double-special-shaped section moisture absorption and sweat releasing fiber comprises the following steps:
a) preparing a spinning melt;
(1) mixing dimethyl isophthalate-5-sodium benzenesulfonate, glycol, a catalyst and an ether inhibitor, and then carrying out ester exchange reaction, and adding glycol and phosphoric acid for modulation after the reaction is finished;
the addition of the ether inhibitor in the ester exchange reaction process can effectively reduce the generation of diglycol in the ester exchange reaction and improve the quality of the prepared polyester; the purpose of adding ethylene glycol after the ester exchange reaction is to adjust isophthalic acid bisThe percentage concentration of the hydroxyethyl-5-Sulfonate (SIPE) in the glycol solution is not favorable for the subsequent reaction because the precipitation can occur when the concentration of the dihydroxy ethyl isophthalate-5-Sulfonate (SIPE) is more than 40 wt%; in the prior art, the catalyst used in the polymerization stage of the double-irregular-section moisture-absorbing and sweat-releasing fiber polyester 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 can 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 blockage, and H in phosphoric 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 phosphoric acid can reduce the generation of the complex, so that the polyester flows more stably.
(2) Mixing terephthalic acid, ethylene glycol, a catalyst, a stabilizer and a delustering agent, and then carrying out esterification reaction; the flatting agent is titanium dioxide particles coated by calcium oxide;
the addition of the stabilizer can effectively reduce the side reaction in the esterification reaction process of the polyester; the addition of the flatting agent can change the polyester from the original large bright state to the later semi-dull (semi-transparent) state, which is beneficial to the subsequent reaction, and the metal calcium ions and the sulfonic acid groups can only form weak coordination, and the metal titanium ions and the sulfonic acid groups can form strong coordination, and the titanium dioxide particles coated by the calcium oxide further reduce the coordination of the titanium ions and the sulfonic acid groups, and simultaneously, the flatting effect of the titanium dioxide particles is not influenced.
(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 double-different-surface moisture-absorbing and sweat-releasing fiber, wherein a spinneret plate with the same plate and multiple shapes is adopted as a spinneret plate in the spinning process, and two different spinneret holes with special-shaped cross sections are formed in the spinneret plate.
As a preferred technical scheme:
the preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber 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)2Carrying out ester exchange reaction with an ether inhibitor NaAc at 175-185 ℃ until the distilled amount of water reaches more than 90% of a theoretical value to obtain sodium dihydroxy ethyl isophthalate-5-sulfonate, and adding ethylene glycol and phosphoric acid to modulate 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, a stabilizer and a flatting agent, 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 the pressure of normal pressure to 0.3MPa at the 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 double-irregular-section moisture-absorbing and sweat-releasing fiber, in the step (1), when the ester exchange reaction is started, the molar ratio of the dimethyl isophthalate-5-sodium benzenesulfonate to the ethylene glycol is10 to 12:1, 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, and the addition amount of the ether inhibitor NaAc is 0.1-0.2 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate;
during preparation, the mass concentration of the added phosphoric acid is 40-60%, and the adding amount of the phosphoric acid is 1.5-6 wt% of the adding 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 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, the addition amount of the stabilizer is 0.01-0.05 wt% of the addition amount of the terephthalic acid, and the addition amount of the matting agent is 0.05-0.2 wt% of the addition amount of the terephthalic acid.
According to the preparation method of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber, 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 ethylene terephthalate is 1-3: 100.
According to the preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber, the content of calcium oxide in the flatting agent is 1-5% of the mass of titanium dioxide, and the BET specific surface area is 50-200 m2/g；
The preparation method of the flatting agent comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of 5-10%, adding calcium salt to react at the reaction temperature of 60-80 ℃ for 2-3 h, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at the temperature of 400-800 ℃ for 2-5 h to prepare calcium oxide coated titanium dioxide particles;
wherein the calcium salt is calcium chloride or calcium sulfate, the molar ratio of calcium ions to titanium ions is 1-5: 100 at the beginning of the reaction, and the pH value of the reaction system is 10-14;
the special-shaped cross section comprises a trilobal shape, a c shape, a strip shape, a Y shape, a V shape and a pentalobal shape. The shape of the profiled cross-section includes, but is not limited to, only some preferred cross-sectional shapes are listed here.
In order to adapt to the influence of the addition of substances such as an ether inhibitor, ethylene glycol, phosphoric acid, a stabilizer, a delustering agent and the like on the final spinning processing in the preparation process, the preparation method of the double-profiled-section moisture-absorbing and sweat-releasing fiber needs to adjust the spinning process parameters of the double-profiled-section moisture-absorbing and sweat-releasing fiber, and the adjusted spinning process parameters are as follows:
spinning temperature: 285-300 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.30-0.40 MPa;
a roll speed: 2200-2600 m/min;
first roll temperature: 70-80 ℃;
two roll speed: 4200-4500 m/min;
temperature of the two rolls: 125-135 ℃;
winding speed: 4100 to 4400 m/min.
According to the preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber, in the spinning process, the pressure rise delta P of the spinning assembly is less than or equal to 0.75 bar/day, the pressure rise delta P of the filter is less than or equal to 2.6 bar/day, the service cycle of the spinning assembly is 38-40 days, and the service cycle of the filter is 27-30 days.
According to the preparation method of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber, the double-special-shaped-section moisture-absorbing and sweat-releasing fiber simultaneously has two different special-shaped sections, the filament number of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is 0.5-1.5 dtex, the breaking strength is not less than 4.00cN/dtex, the dye uptake is greater than 95%, and the comprehensive index of liquid water dynamic transmission of a fabric prepared from the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is greater than 0.65. The moisture absorption performance of the double-profiled-section moisture absorption and sweat release type fiber fabric is tested according to GB/T21655.2-2009.
According to the preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber, the degree of irregularity of the double-irregular-section moisture-absorbing and sweat-releasing fiber is 70-78%, the elongation at break is 40.0 +/-5.0%, the linear density deviation rate is less than or equal to 0.5%, the breaking strength CV value is less than or equal to 5.0%, the elongation at break CV value is less than or equal to 10.0%, and the yarn evenness CV value is less than or equal to 1.8%. Has the advantages that:
(1) according to the preparation method of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber, 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 double-special-shaped-section moisture-absorbing and sweat-releasing fiber has good economic value and popularization value;
(2) according to the preparation method of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber, the formation of a complex in the production process of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is reduced due to the addition of phosphoric acid, so that impurities in a spinning melt are reduced, the good flowing property of polyester is maintained, and the spinnability of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is further ensured;
(3) according to the preparation method of the moisture-absorbing and sweat-releasing fiber with the double special-shaped cross sections, the flatting agent is titanium dioxide particles coated with calcium oxide, so that the coordination effect of titanium ions and sulfonic acid groups is further reduced, and the flatting effect of the fiber is not influenced.
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 double-special-shaped section moisture absorption and sweat releasing fiber 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, m-phthalic acid dimethyl ester-5-benzene sulfonic acid with the molar ratio of 10:1Adding sodium and ethylene glycol into a preparation kettle, adding a catalyst Zn (Ac)2After the reaction product and an ether inhibitor NaAc are subjected to ester exchange reaction at 175 ℃ until the distilled amount of water reaches 90% of a theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then glycol and phosphoric acid are added for modulation, and a glycol solution containing 30 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein a catalyst Zn (Ac)2The addition amount of the sodium sulfoisophthalate is 0.2 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate, and the addition amount of the ether inhibitor NaAc is 0.1 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 40 percent, and the adding amount of the phosphoric acid is 1.5 percent by weight of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of the titanium dioxide of 5%, adding calcium chloride for reaction, wherein the molar ratio of calcium ions to titanium ions is 1:100 at the beginning of the reaction, the reaction temperature is 60 ℃, the reaction time is 2 hours, the pH of a reaction system is 10, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 400 ℃ for 2 hours to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol into slurry with the molar ratio of 1.10:1, adding antimony trioxide, triphenyl phosphate and calcium oxide-coated titanium dioxide particles, uniformly mixing, carrying out esterification reaction at 250 ℃ to obtain the ethylene glycol terephthalate, carrying out the esterification reaction in a nitrogen atmosphere, wherein the esterification reaction is carried out under normal pressure, the pressure is the end point of the esterification reaction when the distilled amount of water in the esterification reaction reaches 90% of the theoretical value, the adding amount of the antimony trioxide is 0.01 wt% of the adding amount of the terephthalic acid, the adding amount of the triphenyl phosphate is 0.01 wt% of the adding amount of the terephthalic acid, the adding amount of the calcium oxide-coated titanium dioxide particles is 0.05 wt% of the adding amount of the terephthalic acid, the content of calcium oxide in the calcium oxide-coated titanium dioxide particles is 1% of the mass of the titanium dioxide, and the BET specific surface area is 50m2/g；
(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 double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a same-plate multi-shape spinneret plate is adopted as a spinneret plate in the spinning process, and the cross section of spinneret holes on the spinneret plate is trilobal and strip-shaped; the spinning process parameters are as follows:
spinning temperature: 300 ℃;
cooling temperature: 20 ℃;
network pressure: 0.31 MPa;
a roll speed: 2350 m/min;
first roll temperature: 75 ℃;
two roll speed: 4500 m/min;
temperature of the two rolls: 125 ℃;
winding speed: 4400 m/min;
in the spinning process, due to the modulation of ethylene glycol and phosphoric acid, the quantity 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 0.63 bar/day, the pressure rise delta P of the filter is 2.8 bar/day, the service cycle of the spinning assembly is 38 days, and the service cycle of the filter is 28 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained in the step is 1.5dtex, the breaking strength is 4.00cN/dtex, the dye uptake is 97%, and the comprehensive index of liquid water dynamic transfer of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is 0.75. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 77%, the elongation at break is 40.0%, the linear density deviation rate is 0.5%, the CV value of the breaking strength is 4.5%, the CV value of the elongation at break is 9.0%, and the CV value of the evenness unevenness is 1.7%.
Comparative example 1
In the prior art, the dyeing of PET fiber needs to be carried out under high temperature and high pressure or in the presence of a carrier, the preparation steps are basically the same as those of the example 1, except that in the step (1), no ethylene glycol and phosphoric acid are used for modulation after the ester exchange reaction, the pressure rise delta P of a spinning assembly is 1.8 bar/day, the pressure rise delta P of a filter is 4.2 bar/day, the service cycle of the spinning assembly is 7 days, and the service cycle of the filter is 10 days. The single filament number measured by the prepared double-irregular-section moisture-absorbing and sweat-releasing type fiber is 0.18dtex, the breaking strength is 3.57cN/dtex, the dye uptake is 92.3%, the comprehensive index of liquid water dynamic transfer of a fabric made of the double-irregular-section moisture-absorbing and sweat-releasing type fiber is 0.54, the irregularity is 52%, the elongation at break is 32.7%, the linear density deviation rate is 0.60%, the CV value of the breaking strength is 6.18%, the CV value of the elongation at break is 10.15%, and the CV value of yarn evenness unevenness is 2.54%.
Example 2
A preparation method of double-special-shaped section moisture absorption and sweat releasing fiber 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)2Performing ester exchange reaction with ether inhibitor NaAc at 178 deg.C until water distillate reaches 92% of theoretical value to obtain sodium dihydroxy ethyl isophthalate-5-sulfonate, adding ethylene glycol andpreparing phosphoric acid to obtain ethylene glycol solution containing 31 wt% of sodium bis (hydroxyethyl) isophthalate-5-sulfonate, 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 0.2 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 45 percent, and the adding amount of the phosphoric acid is 2 weight percent of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of titanium dioxide of 6%, adding calcium sulfate to react, wherein the molar ratio of calcium ions to titanium ions is 2:100 at the beginning of the reaction, the reaction temperature is 65 ℃, the reaction time is 2.2h, the pH of a reaction system is 11, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 500 ℃ for 2.5h to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol into slurry with the molar ratio of 1.15:1, adding ethylene glycol antimony, trimethyl phosphate and titanium dioxide particles coated with calcium oxide, uniformly mixing, and performing esterification reaction at 253 ℃ to obtain the ethylene glycol terephthalate, wherein the esterification reaction is performed under the pressure of 0.1MPa in a nitrogen atmosphere, the end point of the esterification reaction is determined when the distilled water amount in the esterification reaction reaches 91% of the theoretical value, the adding amount of the ethylene glycol antimony is 0.02 wt% of the adding amount of the terephthalic acid, the adding amount of the trimethyl phosphate is 0.02 wt% of the adding amount of the terephthalic acid, the adding amount of the titanium dioxide particles coated with calcium oxide is 0.08 wt% of the adding amount of the terephthalic acid, the content of the calcium oxide in the titanium dioxide particles coated with the calcium oxide is 2% of the mass of the titanium dioxide, and the BET specific surface area is 70m2/g；
(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 490Pa, the reaction temperature is 262 ℃, the reaction time is 35min, 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 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 glycol 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 double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a same-plate multi-shape spinneret plate is adopted as a spinneret plate in the spinning process, and the cross section of spinneret holes on the spinneret plate is Y-shaped or five-leaf-shaped; the spinning process parameters are as follows:
spinning temperature: 287 deg.C;
cooling temperature: 21 ℃;
network pressure: 0.37 MPa;
a roll speed: 2600 m/min;
first roll temperature: 70 ℃;
two roll speed: 4500 m/min;
temperature of the two rolls: 128 ℃;
winding speed: 4300 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.75 bar/day, the pressure rise delta P of the filter is 2.59 bar/day, the service cycle of the spinning assembly is 40 days, and the service cycle of the filter is 27 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained in the step is 1.2dtex, the breaking strength is 5.00cN/dtex, the dye uptake is 96%, and the comprehensive index of liquid water dynamic transfer of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is 0.75. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 7%, the elongation at break is 35.0%, the linear density deviation rate is 0.5%, the CV value of the breaking strength is 5.0%, the CV value of the elongation at break is 10.0%, and the CV value of the evenness unevenness is 1.55%.
Example 3
A preparation method of double-special-shaped section moisture absorption and sweat releasing fiber 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 179 ℃ until the distilled amount of water reaches 91% of the theoretical value, sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, then ethylene glycol and phosphoric acid are added for modulation, and an ethylene glycol solution containing 32 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, 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 0.17 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 50 percent, and the adding amount of the phosphoric acid is 3 weight percent of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of 7 percent, adding calcium chloride for reaction, wherein the molar ratio of calcium ions to titanium ions is 3:100 at the beginning of the reaction, the reaction temperature is 70 ℃, the reaction time is 2.3h, the pH of a reaction system is 12, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 600 ℃ for 3h to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.20:1 into slurry, adding antimony acetate, trimethyl phosphite and calcium oxide coated titanium dioxide particles, uniformly mixing, and carrying out esterification reaction at 255 ℃ to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out under a nitrogen atmosphere with a pressure of 0.15MPa, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 92% of a theoretical value; wherein the addition amount of the antimony acetate is 0.03 wt% of that of the terephthalic acid, and the addition amount of the trimethyl phosphite is that of the terephthalic acid0.03 wt% of the added amount, 0.11 wt% of the added amount of terephthalic acid, 3 wt% of the calcium oxide content in the calcium oxide-coated titanium dioxide particles, and a BET specific surface area of 100m2/g；
(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 double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a spinneret plate with the same plate and multiple shapes is adopted as a spinneret plate in the spinning process, and the cross section of spinneret holes on the spinneret plate is in a strip shape or a five-leaf shape; the spinning process parameters are as follows:
spinning temperature: 290 ℃;
cooling temperature: 20 ℃;
network pressure: 0.35 MPa;
a roll speed: 2200 m/min;
first roll temperature: 79 ℃;
two roll speed: 4200 m/min;
temperature of the two rolls: 130 ℃;
winding speed: 4200 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.70 bar/day, the pressure rise delta P of the filter is 2.6 bar/day, the service cycle of the spinning assembly is 40 days, and the service cycle of the filter is 27 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained in the step is 0.5dtex, the breaking strength is 4.00cN/dtex, the dye uptake is 96.5%, and the comprehensive index of liquid water dynamic transmission of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is 0.68. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 78%, the elongation at break is 45.0%, the linear density deviation rate is 0.4%, the CV value of the breaking strength is 4.7%, the CV value of the elongation at break is 9.3%, and the CV value of the evenness unevenness is 1.8%.
Example 4
A preparation method of double-special-shaped section moisture absorption and sweat releasing fiber 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 and phosphoric acid are added for modulation, and a glycol solution containing 33 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein a 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 0.15 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 55 percent, and the adding amount of the phosphoric acid is 4 weight percent of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of titanium dioxide of 8%, adding calcium sulfate to react, wherein the molar ratio of calcium ions to titanium ions is 4:100 at the beginning of the reaction, the reaction temperature is 75 ℃, the reaction time is 2.5h, the pH of a reaction system is 13, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 650 ℃ for 3.5h to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol into slurry with the molar ratio of 1.25:1, adding antimony trioxide, triphenyl phosphate and calcium oxide coated titanium dioxide particles, uniformly mixing, performing esterification reaction at 257 ℃ to obtain ethylene glycol terephthalate, performing pressure reaction in a nitrogen atmosphere at the pressure of 0.2MPa, and determining the end point of the esterification reaction when the distilled amount of water 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, the adding amount of the triphenyl phosphate is 0.04 wt% of the adding amount of the terephthalic acid, the adding amount of the calcium oxide coated titanium dioxide particles is 0.13 wt% of the adding amount of the terephthalic acid, the content of calcium oxide in the calcium oxide coated titanium dioxide particles is 4% of the mass of the titanium dioxide, and the BET specific surface area is 120m2/g；
(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 double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a spinneret plate with the same plate and multiple shapes is adopted as a spinneret plate in the spinning process, and the cross section of spinneret holes on the spinneret plate is in a c shape and a Y shape; the spinning process parameters are as follows:
spinning temperature: 295 ℃;
cooling temperature: 23 ℃;
network pressure: 0.30 MPa;
a roll speed: 2550 m/min;
first roll temperature: 80 ℃;
two roll speed: 4300 m/min;
temperature of the two rolls: 135 deg.C;
winding speed: 4100 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.60 bar/day, the pressure rise delta P of the filter is 2.55 bar/day, the service cycle of the spinning assembly is 40 days, and the service cycle of the filter is 30 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained in the step is 1.5dtex, the breaking strength is 5.20cN/dtex, the dye uptake is 98.5%, and the comprehensive index of liquid water dynamic transfer of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is 0.69. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 76%, the elongation at break is 35.0%, the linear density deviation rate is 0.5%, the CV value of the breaking strength is 4.0%, the CV value of the elongation at break is 8.9%, and the CV value of the evenness unevenness is 1.66%.
Example 5
A preparation method of double-special-shaped section moisture absorption and sweat releasing fiber 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 and phosphoric acid are added for modulation, a glycol solution containing 34 wt% of sodium dihydroxy ethyl isophthalate-5-sulfonate is obtained, wherein a 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 0.12 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 60 percent, and the adding amount of the phosphoric acid is 5 weight percent of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate.
(2) Preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of titanium dioxide of 9%, adding calcium sulfate to react, wherein the molar ratio of calcium ions to titanium ions is 5:100 at the beginning of the reaction, the reaction temperature is 72 ℃, the reaction time is 2.7h, the pH of a reaction system is 10, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 700 ℃ for 4h to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.30:1 into slurry, adding ethylene glycol antimony, trimethyl phosphate and calcium oxide coated titanium dioxide particles, uniformly mixing, and carrying out esterification reaction at 252 ℃ to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out in a nitrogen atmosphere under a pressure of 0.25MPa, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 94% of a theoretical value; wherein the addition amount of ethylene glycol antimony is 0.04 wt% of the addition amount of terephthalic acid, the addition amount of trimethyl phosphate is 0.05 wt% of the addition amount of terephthalic acid, the addition amount of calcium oxide-coated titanium dioxide particles is 0.17 wt% of the addition amount of terephthalic acid, the content of calcium oxide in the calcium oxide-coated titanium dioxide particles is 4% of the mass of titanium dioxide, and the BET specific surface area is 150m2/g；
(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 268 ℃, the reaction time is 45min, then, continuously carrying out the polycondensation reaction in a high vacuum stage by vacuumizing, reducing the reaction pressure to an absolute pressure of 95Pa, the reaction temperature is 282 ℃, and the reaction time is 80min, 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 2.5: 100;
b) spinning;
the spinning melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare the double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a same-plate multi-shape spinneret plate is adopted as a spinneret plate in the spinning process, and the cross section of a spinneret hole on the spinneret plate is in a trilobal shape and a V shape; the spinning process parameters are as follows:
spinning temperature: 292 deg.C;
cooling temperature: 21 ℃;
network pressure: 0.40 MPa;
a roll speed: 2200 m/min;
first roll temperature: 70 ℃;
two roll speed: 4500 m/min;
temperature of the two rolls: 129 ℃;
winding speed: 4350 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.55 bar/day, the pressure rise delta P of the filter is 2.45 bar/day, the service cycle of the spinning assembly is 38 days, and the service cycle of the filter is 30 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained by the steps is 1.5dtex, the breaking strength is 4.00cN/dtex, the dye uptake is more than 95%, and the comprehensive index of liquid water dynamic transfer of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is more than 0.65. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 70%, the elongation at break is 40.0%, the linear density deviation rate is 0.5%, the CV value of the breaking strength is 5.0%, the CV value of the elongation at break is 8.0%, and the CV value of the evenness unevenness is 1.5%.
Example 6
A preparation method of double-special-shaped section moisture absorption and sweat releasing fiber 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)2Performing ester exchange reaction with ether inhibitor NaAc at 185 deg.C until water distillate reaches 94% of theoretical value to obtain sodium dihydroxy ethyl isophthalate-5-sulfonate, adding ethylene glycol and phosphoric acid, and concocting to obtain final product containing 35 wt% of m-xyleneA solution of bishydroxyethyl-5-sulfonate in ethylene glycol, in which 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 0.1% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate; during preparation, the mass concentration of the added phosphoric acid is 60 percent, and the adding amount of the phosphoric acid is 6 weight percent of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate;
(2) preparing ethylene terephthalate through esterification reaction;
the preparation method of the calcium oxide coated titanium dioxide particles comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of 10 percent, adding calcium chloride for reaction, wherein the molar ratio of calcium ions to titanium ions is 2:100 at the beginning of the reaction, the reaction temperature is 80 ℃, the reaction time is 3 hours, the pH of a reaction system is 14, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at 800 ℃ for 5 hours to prepare titanium dioxide particles coated with calcium oxide;
preparing terephthalic acid and ethylene glycol with a molar ratio of 1.25:1 into slurry, adding antimony acetate, trimethyl phosphite and calcium oxide coated titanium dioxide particles, uniformly mixing, and carrying out esterification reaction at 260 ℃ to obtain ethylene glycol terephthalate, wherein the esterification reaction is carried out under a nitrogen atmosphere with a pressure of 0.3MPa, 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 addition amount of antimony acetate is 0.05 wt% of the addition amount of terephthalic acid, the addition amount of trimethyl phosphite is 0.03 wt% of the addition amount of terephthalic acid, the addition amount of calcium oxide-coated titanium dioxide particles is 0.2 wt% of the addition amount of terephthalic acid, the content of calcium oxide in the calcium oxide-coated titanium dioxide particles is 5% of the mass of titanium dioxide, and the BET specific surface area is 200m2/g；
(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 495Pa, 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 absolute pressure 99Pa, 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 double-profile cross-section moisture-absorbing and sweat-releasing fiber, wherein a same-plate multi-shape spinneret plate is adopted as a spinneret plate in the spinning process, and the cross section of a spinneret hole on the spinneret plate is in a trilobal shape or a pentalobal shape; the spinning process parameters are as follows:
spinning temperature: 285 ℃;
cooling temperature: 20 ℃;
network pressure: 0.35 MPa;
a roll speed: 2300 m/min;
first roll temperature: 71 ℃;
two roll speed: 4250 m/min;
temperature of the two rolls: 125 ℃;
winding speed: 4200 m/min;
in the spinning process, the pressure rise delta P of the spinning assembly is 0.72 bar/day, the pressure rise delta P of the filter is 2.58 bar/day, the service cycle of the spinning assembly is 40 days, and the service cycle of the filter is 28 days.
The filament number of the double-special-shaped cross section moisture absorption and sweat release type fiber obtained in the step is 1.5dtex, the breaking strength is 4.00cN/dtex, the dye uptake is 95.7%, and the comprehensive index of liquid water dynamic transfer of the fabric made of the double-special-shaped cross section moisture absorption and sweat release type fiber is 0.75. The moisture-absorbing and sweat-releasing fiber with the special-shaped section has the advantages that the special-shaped degree is 75%, the elongation at break is 45.0%, the linear density deviation rate is 0.3%, the CV value of the breaking strength is 5.0%, the CV value of the elongation at break is 10.0%, and the CV value of the evenness unevenness is 1.62%.
Claims (9)
1. A preparation method of double-special-shaped-section moisture-absorbing and sweat-releasing fibers is characterized by comprising the following steps:
a) preparing a spinning melt;
(1) mixing dimethyl isophthalate-5-sodium benzenesulfonate, glycol, a catalyst and an ether inhibitor, and then carrying out ester exchange reaction, and adding glycol and phosphoric acid for modulation after the reaction is finished;
(2) mixing terephthalic acid, ethylene glycol, a catalyst, a stabilizer and a delustering agent, and then carrying out esterification reaction; the flatting agent is titanium dioxide particles coated by calcium oxide; 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 double-different-surface moisture-absorbing and sweat-releasing fiber, wherein a spinneret plate with the same plate and multiple shapes is adopted as a spinneret plate in the spinning process, and spinneret plates are provided with two different spinneret holes with special-shaped cross sections;
in the spinning process, the pressure rise delta P of the spinning assembly is less than or equal to 0.75 bar/day, the pressure rise delta P of the filter is less than or equal to 2.6 bar/day, the service cycle of the spinning assembly is 38-40 days, and the service cycle of the filter is 27-30 days.
2. The method for preparing the double-profiled-section moisture-absorbing and sweat-releasing fiber according to claim 1, wherein the specific steps for 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)2Carrying out ester exchange reaction with an ether inhibitor NaAc at 175-185 ℃ until the distilled amount of water reaches more than 90% of a theoretical value to obtain sodium dihydroxy ethyl isophthalate-5-sulfonate, and adding ethylene glycol and phosphoric acid to modulate 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, a stabilizer and a flatting agent, 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 the pressure of normal pressure to 0.3MPa at the 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 double-profiled-section moisture-absorbing and sweat-releasing fiber according to claim 2, wherein 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, and the addition amount of the ether inhibitor NaAc is 0.1-0.2 wt% of the addition amount of the dimethyl isophthalate-5-benzene sulfonate;
during preparation, the mass concentration of the added phosphoric acid is 40-60%, and the adding amount of the phosphoric acid is 1.5-6 wt% of the adding amount of the dimethyl isophthalate-5-sodium benzenesulfonate.
4. The method for preparing the moisture-absorbing and sweat-releasing fiber with the double-shaped cross section as claimed in claim 2, wherein 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 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, the addition amount of the stabilizer is 0.01-0.05 wt% of the addition amount of the terephthalic acid, and the addition amount of the flatting agent is 0.05-0.2 wt% of the addition amount of the terephthalic acid.
5. The method for preparing the double-profiled-section moisture-absorbing and sweat-releasing fiber according to claim 2, wherein in the step (3), when the polycondensation reaction is started, the molar ratio of the sodium bis (hydroxyethyl) isophthalate-5-sulfonate to the ethylene terephthalate is 1-3: 100.
6. The preparation method of the double-irregular-section moisture-absorbing and sweat-releasing fiber according to claim 1 or 2, wherein the content of calcium oxide in the matting agent is 1-5% of the mass of titanium dioxide, and the BET specific surface area is 50-200 m2/g；
The preparation method of the flatting agent comprises the following steps: mixing titanium dioxide with the average particle size of 0.3 mu m and deionized water, stirring, performing ultrasonic dispersion to prepare titanium dioxide suspension with the solid content of 5-10%, adding calcium salt to react at the reaction temperature of 60-80 ℃ for 2-3 h, and after the reaction is finished, centrifuging, washing, drying and performing high-temperature treatment at the temperature of 400-800 ℃ for 2-5 h to prepare calcium oxide coated titanium dioxide particles;
wherein the calcium salt is calcium chloride or calcium sulfate, the molar ratio of calcium ions to titanium ions is 1-5: 100 at the beginning of the reaction, and the pH value of the reaction system is 10-14;
the special-shaped cross section comprises a trilobal shape, a c shape, a strip shape, a Y shape, a V shape and a pentalobal shape.
7. The method for preparing the double-profiled-section moisture-absorbing and sweat-releasing fiber according to claim 1, wherein the spinning process parameters are as follows:
spinning temperature: 285-300 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.30-0.40 MPa;
a roll speed: 2200-2600 m/min;
first roll temperature: 70-80 ℃;
two roll speed: 4200-4500 m/min;
temperature of the two rolls: 125-135 ℃;
winding speed: 4100 to 4400 m/min.
8. The method for preparing the double-special-shaped-section moisture-absorbing and sweat-releasing fiber according to claim 1, wherein the double-special-shaped-section moisture-absorbing and sweat-releasing fiber has two different special-shaped sections, the single-filament titer of the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is 0.5-1.5 dtex, the breaking strength is not less than 4.00cN/dtex, the dye uptake is more than 95%, and the comprehensive index of liquid water dynamic transmission of the fabric prepared from the double-special-shaped-section moisture-absorbing and sweat-releasing fiber is more than 0.65.
9. The method for preparing the double-profiled-section moisture-absorbing and sweat-releasing fiber according to claim 8, wherein the degree of profile of the double-profiled-section moisture-absorbing and sweat-releasing fiber is 70-78%, the elongation at break is 40.0 +/-5.0%, the linear density deviation rate is less than or equal to 0.5%, the breaking strength CV value is less than or equal to 5.0%, the elongation at break CV value is less than or equal to 10.0%, and the yarn evenness CV value is less than or equal to 1.8%.
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| CN109505026B (en) * | 2018-12-27 | 2020-10-16 | 江苏恒力化纤股份有限公司 | Moisture-absorbing sweat-releasing polyester fiber and preparation method thereof |
| CN112725932B (en) * | 2020-12-29 | 2022-10-04 | 浙江恒逸石化有限公司 | Preparation method of antimony-free polyester POY (polyester pre-oriented yarn) filament with high moisture absorption and sweat releasing performance |
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| CN101314637A (en) * | 2007-05-31 | 2008-12-03 | 中国科学院化学研究所 | Poly-p-benzene dicarboxylic acid 1,2-propylene glycol ester and copolyester, and preparation thereof |
| CN101570596B (en) * | 2009-04-30 | 2013-07-17 | 江苏江南高纤股份有限公司 | Method for preparing cationic-dyeable copolyester |
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| CN106811821B (en) * | 2016-12-29 | 2020-06-05 | 江苏恒科新材料有限公司 | Multi-blade special-shaped polyester fiber FDY (fully drawn yarn) and preparation method thereof |
| CN107557902B (en) * | 2017-09-07 | 2020-10-02 | 江苏恒科新材料有限公司 | Preparation method of cationic dyeable polyester POY (polyester pre-oriented yarn) |
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