CN111206299A - Parallel composite elastic fiber and preparation method thereof - Google Patents
Parallel composite elastic fiber and preparation method thereof Download PDFInfo
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- CN111206299A CN111206299A CN201811402191.9A CN201811402191A CN111206299A CN 111206299 A CN111206299 A CN 111206299A CN 201811402191 A CN201811402191 A CN 201811402191A CN 111206299 A CN111206299 A CN 111206299A
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- naphthalenedicarboxylic acid
- addition amount
- esterification
- copolymerization modified
- ptt
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- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 210000004177 elastic tissue Anatomy 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 28
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 235000017060 Arachis glabrata Nutrition 0.000 claims abstract 2
- 241001553178 Arachis glabrata Species 0.000 claims abstract 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims abstract 2
- 235000018262 Arachis monticola Nutrition 0.000 claims abstract 2
- 235000020232 peanut Nutrition 0.000 claims abstract 2
- 238000005886 esterification reaction Methods 0.000 claims description 56
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- 230000032050 esterification Effects 0.000 claims description 44
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000009987 spinning Methods 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000003054 catalyst Substances 0.000 claims description 22
- 239000008187 granular material Substances 0.000 claims description 20
- 239000004408 titanium dioxide Substances 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 15
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 13
- 238000006068 polycondensation reaction Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims description 8
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 8
- 229940035437 1,3-propanediol Drugs 0.000 claims description 8
- KLDXJTOLSGUMSJ-JGWLITMVSA-N Isosorbide Chemical compound O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 KLDXJTOLSGUMSJ-JGWLITMVSA-N 0.000 claims description 8
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 8
- 229960002479 isosorbide Drugs 0.000 claims description 8
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 8
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005453 pelletization Methods 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004804 winding Methods 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- KRXBVZUTZPDWQI-UHFFFAOYSA-N ethane-1,2-diol;titanium Chemical compound [Ti].OCCO KRXBVZUTZPDWQI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 16
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000004744 fabric Substances 0.000 abstract description 5
- 210000002268 wool Anatomy 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229920006306 polyurethane fiber Polymers 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920006309 Invista Polymers 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
- D02G1/0206—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
- D02G1/0286—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist characterised by the use of certain filaments, fibres or yarns
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Polyesters Or Polycarbonates (AREA)
- Multicomponent Fibers (AREA)
Abstract
The invention discloses a parallel composite elastic fiber and a preparation method thereof, wherein the cross section of the fiber is of a peanut type parallel structure, and the fiber is prepared by extruding 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT respectively according to the mass ratio of 45-55: 55-45 and then compounding. The side-by-side composite elastic fiber prepared by the invention has excellent elasticity and elastic recovery, the breaking strength is more than or equal to 3.5cN/dtex, the elongation at break is 22-35%, the fiber has high crimpability and fluffiness similar to wool, the crimp rate is 40-45%, the elastic elongation of the fabric is more than or equal to 28%, and the elastic recovery is more than or equal to 95%.
Description
Technical Field
The invention belongs to the technical field of composite fibers and processing thereof, and particularly relates to a parallel composite elastic fiber and a preparation method thereof.
Background
Currently, the most well-known spandex belongs to the polyurethane fiber of DuPont, and is highly favored because of its excellent elasticity and elastic recovery. However, polyurethane fibers also have some defects, which have promoted the development of polyester elastic fibers, such as T400 of Invista corporation, which are superior to polyurethane elastic fibers in elastic stability, dyeability, high temperature resistance, alkali resistance and chlorine bleaching resistance.
The bicomponent side-by-side elastic fiber is made of polymers with different shrinkage characteristics, shrinkage heat treatment is carried out after the fiber is formed, the shrinkage difference enables the fiber to generate a permanent three-dimensional spiral three-dimensional curled structure, compared with the conventional fiber, the bicomponent side-by-side elastic fiber has excellent elasticity, the bicomponent side-by-side elastic fiber also has excellent fluffiness and soft hand feeling, and the bicomponent side-by-side elastic fiber is a supplement or even a substitute of polyurethane fiber in many aspects and is rapidly developed in recent years. The currently researched bicomponent elastic fibers mainly comprise the following components: (1) PET/PTT composite fibers such as CN105274637A, CN101974802, CN1280462C and the like; (2) PET/PBT and high-low IV PBT/PBT conjugate fibers, such as CN101851812 and CN 101654814A; (3) high and low IV PET/PET and modified PET/PET, such as CN104141178, CN201420425923, CN103882538B, CN204676206U, CN104831417A, CN101718008A, CN854355A and the like.
However, the elastic fiber prepared by the prior art has the defects that the PTT or PBT component is seriously thermally degraded in the fiber preparation process, the component period is short, the spinneret surface is easy to generate a white powder phenomenon, the spinnability is poor, the breaking strength of a processed fiber product is low, and the fiber elasticity and the elastic resilience are insufficient, so that the application range of the product is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a side-by-side composite elastic fiber.
Another object of the present invention is to provide a method for producing the above side-by-side conjugate elastic fiber.
The technical scheme of the invention is as follows:
a side-by-side composite elastic fiber is of a peanut-shaped side-by-side structure in cross section and is formed by extruding 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT respectively according to a mass ratio of 45-55: 55-45 and then compounding;
the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET has the intrinsic viscosity of 0.53-0.65 dl/g, the terminal carboxyl group content of 20-30 mol/t, the melting point of 255-265 ℃ and the chroma b value of 3-6;
the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT has the intrinsic viscosity of 1.05-1.25 dl/g, the terminal carboxyl group content of 10-20 mol/t, the melting point of 224-230 ℃ and the chroma b value of 9-11.
In a preferred embodiment of the present invention, the method for preparing the 2, 6-naphthalenedicarboxylic acid copolymerized modified PET comprises: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol in an acid-alcohol molar ratio of 1: 1.2-1.4 according to the mass calculation of the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET theoretically produced, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 245-260 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, and the esterification rate reaches more than 96% to complete esterification, so as to obtain a first esterified substance; sequentially adding isosorbide, trimethyl phosphate, an antioxidant 1010, titanium dioxide and a catalyst titanium glycol into the first esterified substance, heating and vacuumizing to enable the esterified substance to carry out polycondensation reaction under the vacuum condition, stopping the reaction when the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the 2, 6-naphthalenedicarboxylic acid copolymerized modified PET.
More preferably, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 1-8%, the addition amount of isosorbide is 0.1-0.8%, the addition amount of trimethyl phosphate is 50-200 ppm, the addition amount of the catalyst ethylene glycol titanium is 30-70 ppm, the addition amount of the antioxidant 1010 is 1000-2000 ppm, and the addition amount of the titanium dioxide is 0.28-0.31% by mass of the theoretically-produced 2, 6-naphthalenedicarboxylic acid copolymerized modified PET.
In a preferred embodiment of the present invention, the process for preparing the 2, 6-naphthalenedicarboxylic acid copolymerized modified PTT comprises: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and tetrabutyl titanate serving as a catalyst in an acid-alcohol molar ratio of 1: 1.25-1.55 according to the mass of the theoretically-produced 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid, the 1, 3-propanediol and the tetrabutyl titanate serving as the catalyst into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 225-250 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, and the esterification rate reaches more than 99% to complete esterification so as to obtain a second esterified substance; adding an antioxidant 1076 and titanium dioxide into the second esterified product, heating and vacuumizing to enable the esterified product to carry out polycondensation reaction under the vacuum condition, stopping the reaction when the stirring current and the online viscosity value reach preset values, extruding and granulating, and then conveying to a vacuum rotary drum for solid-phase tackifying to obtain the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT.
More preferably, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 0.5 to 1.5%, the addition amount of tetrabutyl titanate as a catalyst is 25 to 60ppm, the addition amount of the antioxidant 1076 is 1000 to 2000ppm, and the addition amount of titanium dioxide is 0.28 to 0.31% by mass of the 2, 6-naphthalenedicarboxylic acid copolymerization-modified PTT produced theoretically.
A preparation method of the side-by-side composite elastic fiber comprises the following steps:
and respectively carrying out melt extrusion on the dried 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT granules with the water content of below 50ppm by using respective screw extruders, feeding the extruded granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers.
In a preferred embodiment of the invention, the temperature of the spinning manifold corresponding to the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET in the composite spinning component is 260-280 ℃, the temperature of the spinning manifold corresponding to the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT in the composite spinning component is 250-270 ℃, and the spinning speeds are 2400-3000 m/min.
In a preferred embodiment of the present invention, the temperature of the first heat box for false twisting is 160 to 175 ℃, the draft ratio is 1.7 to 1.85, and the processing speed is 500-800 m/min.
The invention has the beneficial effects that:
1. the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT prepared by the method have excellent spinnability, thermal stability and thermo-oxidative stability.
2. The side-by-side composite elastic fiber prepared by the invention has excellent elasticity and elastic recovery, the breaking strength is more than or equal to 3.5cN/dtex, the elongation at break is 22-35%, the fiber has high crimpability and fluffiness similar to wool, the crimp rate is 40-45%, the elastic elongation of the fabric is more than or equal to 28%, and the elastic recovery is more than or equal to 95%.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
In the following examples, the modified PET means the 2, 6-naphthalenedicarboxylic acid copolymer modified PET of the present invention, and the modified PTT means the 2, 6-naphthalenedicarboxylic acid copolymer modified PTT of the present invention.
Example 1
(1) Preparing modified PET granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification according to the mass calculation of the modified PET theoretically produced, wherein the molar ratio of an acid component to an alcohol component is 1: 1.25, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 3.0%, the esterification temperature is 250 ℃, the esterification pressure is micro-positive pressure of 0.02MPa, the esterification rate reaches over 96%, finishing esterification, adding 0.5% of isosorbide into the esterified product, sequentially adding 100ppm of trimethyl phosphate, 1700ppm of antioxidant 1010 and 0.3% of titanium dioxide, finally adding 50ppm of catalyst titanium glycol, heating to 284 ℃, maintaining the vacuum below 80Pa for polycondensation reaction, stopping the reaction after the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the modified PET.
(2) Preparing modified PTT granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and catalyst tetrabutyl titanate, mixing and adding into a reaction kettle for esterification according to the mass calculation of the modified PTT produced theoretically, wherein the molar ratio of an acid component to an alcohol component is 1: 1.5, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 0.5%, the addition amount of the catalyst tetrabutyl titanate is 35ppm, the esterification temperature is 230 ℃, the esterification rate reaches more than 99% after esterification, adding 1500ppm of antioxidant 1076 and 0.3% of titanium dioxide, heating to 265 ℃, maintaining the vacuum below 80Pa for polycondensation, stopping the reaction after the stirring current and the online viscosity value reach preset values, extruding and granulating, and conveying to a vacuum drum for solid phase tackifying to obtain the high-viscosity modified PTT.
(3) Preparing the parallel composite elastic fiber: and respectively carrying out melt extrusion on the dried modified PET and modified PTT granules with the water content of below 50ppm by respective screw extruders, feeding the granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers. The mass ratio of the modified PET to the modified PTT is 50: 50, the temperature of a modified PET spinning box body is 268 ℃, the temperature of the modified PTT spinning box body is 260 ℃, and the spinning speed is 2700 m/min. The temperature of the first heat box for false twisting is 165 ℃, the drafting ratio is 1.78, and the processing speed is 600 m/min.
Example 2
(1) Preparing modified PET granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification according to the mass calculation of the modified PET theoretically produced, wherein the molar ratio of an acid component to an alcohol component is 1: 1.3, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 3.5%, the esterification temperature is 252 ℃, the esterification pressure is micro-positive pressure of 0.02MPa, the esterification rate reaches over 96%, the esterification is completed, adding 0.5% of isosorbide into the esterified product, then sequentially adding 100ppm of trimethyl phosphate, 1700ppm of antioxidant 1010 and 0.3% of titanium dioxide, finally adding 50ppm of catalyst titanium glycol, heating to 284 ℃, maintaining the vacuum below 80Pa for polycondensation reaction, stopping the reaction after the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the modified PET.
(2) Preparing modified PTT granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and catalyst tetrabutyl titanate, mixing and adding into a reaction kettle for esterification according to the mass calculation of the modified PTT produced theoretically, wherein the molar ratio of an acid component to an alcohol component is 1: 1.45, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 0.5%, the addition amount of the catalyst tetrabutyl titanate is 35ppm, the esterification temperature is 230 ℃, the esterification rate reaches over 99% after esterification is completed, 1500ppm of antioxidant 1076 and 0.3% of titanium dioxide are added, the temperature is increased to 260 ℃ and the vacuum is maintained below 80Pa for polycondensation reaction, the reaction is stopped after the stirring current and the online viscosity value reach preset values, and the high-viscosity modified PTT is obtained after solid-phase tackifying in a vacuum rotary drum after extrusion and granulation.
(3) Preparing the parallel composite elastic fiber: and respectively carrying out melt extrusion on the dried modified PET and modified PTT granules with the water content of below 50ppm by respective screw extruders, feeding the granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers. The mass ratio of the modified PET to the modified PTT is 45: 55, the temperature of the modified PET spinning box is 270 ℃, the temperature of the modified PTT spinning box is 260 ℃, and the spinning speed is 2700 m/min. The temperature of the first heat box for false twisting is 165 ℃, the drafting ratio is 1.78, and the processing speed is 650 m/min.
Example 3
(1) Preparing modified PET granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification according to the mass calculation of the modified PET theoretically produced, wherein the molar ratio of an acid component to an alcohol component is 1: 1.25, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 5.0%, the esterification temperature is 255 ℃, the esterification pressure is micro-positive pressure of 0.02MPa, the esterification rate reaches over 96%, the esterification is completed, adding 0.5% of isosorbide into the esterified product, then sequentially adding 100ppm of trimethyl phosphate, 1700ppm of antioxidant 1010 and 0.3% of titanium dioxide, finally adding 50ppm of catalyst titanium glycol, heating to 284 ℃, maintaining the vacuum below 80Pa for polycondensation reaction, stopping the reaction after the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the modified PET.
(2) Preparing modified PTT granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and catalyst tetrabutyl titanate, mixing and adding into a reaction kettle for esterification according to the mass calculation of the modified PTT produced theoretically, wherein the molar ratio of an acid component to an alcohol component is 1: 1.4, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 0.7%, the addition amount of the catalyst tetrabutyl titanate is 50ppm, the esterification temperature is 232 ℃, the esterification rate reaches more than 99% after esterification, 1100ppm of antioxidant 1076 and 0.3% of titanium dioxide are added, heating is carried out to 260 ℃ and vacuum is maintained below 80Pa for polycondensation reaction, the reaction is stopped after the stirring current and the online viscosity value reach preset values, and the high-viscosity modified PTT is obtained after solid-phase tackifying in a vacuum rotary drum after extrusion and granulation.
(3) Preparing the parallel composite elastic fiber: and respectively carrying out melt extrusion on the dried modified PET and modified PTT granules with the water content of below 50ppm by respective screw extruders, feeding the granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers. The mass ratio of the modified PET to the modified PTT is 55: 45, the temperature of the modified PET spinning box body is 272 ℃, the temperature of the modified PTT spinning box body is 262 ℃, and the spinning speed is 2850 m/min. The temperature of the first heat box for false twisting is 165 ℃, the drafting ratio is 1.78, and the processing speed is 650 m/min.
Example 4
(1) Preparing modified PET granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification according to the mass calculation of the modified PET theoretically produced, wherein the molar ratio of an acid component to an alcohol component is 1: 1.25, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 7.0%, the esterification temperature is 255 ℃, the esterification pressure is micro-positive pressure of 0.02MPa, the esterification rate reaches more than 96%, the esterification is completed, adding 0.3% of isosorbide into the esterified product, sequentially adding 70ppm of trimethyl phosphate, 1500ppm of antioxidant 1010 and 0.3% of titanium dioxide, finally adding 70ppm of catalyst titanium glycol, heating to 284 ℃, maintaining the vacuum below 80Pa for polycondensation reaction, stopping the reaction after the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the modified PET.
(2) Preparing modified PTT granules: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and catalyst tetrabutyl titanate, mixing and adding into a reaction kettle for esterification according to the mass calculation of the modified PTT produced theoretically, wherein the molar ratio of an acid component to an alcohol component is 1: 1.45, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 1.5%, the addition amount of the catalyst tetrabutyl titanate is 50ppm, the esterification temperature is 235 ℃, the esterification rate reaches more than 99% after the esterification is completed, 1100ppm of antioxidant 1076 and 0.3% of titanium dioxide are added, the temperature is raised to 263 ℃ and kept under vacuum of 80Pa for polycondensation, the reaction is stopped after the stirring current and the online viscosity value reach preset values, and the modified PTT is obtained after solid-phase tackifying in a vacuum drum after extrusion and granulation.
(3) Preparing the parallel composite elastic fiber: and respectively carrying out melt extrusion on the dried modified PET and modified PTT granules with the water content of below 50ppm by respective screw extruders, feeding the granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers. The mass ratio of the modified PET to the modified PTT is 52: 48, the temperature of the modified PET spinning manifold is 275 ℃, the temperature of the modified PTT spinning manifold is 263 ℃, and the spinning speed is 2800 m/min. The temperature of the first heat box for false twisting is 168 ℃, the drafting multiplying power is 1.78, and the processing speed is 600 m/min.
The detection method of the modified PET, PTT cut grain, parallel composite elastic fiber and fabric thereof in the above embodiment is described as follows:
1. the intrinsic viscosity, melting point, carboxyl end group and chromaticity of the modified PET and PTT particles are tested according to the national standard GB/T14190-2008.
2. The fineness test of the elastic composite fiber is carried out according to the national standard GB/T14343-2008, and the breaking strength and breaking elongation test is carried out according to the standard GB/T14344-2008.
3. The crimp rate test of the elastic composite fiber is carried out according to the standard GB/T6506-2001.
4. Elastic elongation and elastic recovery testing of elastic composite fiber fabrics is performed according to the standard ASTM D3107.
The main performance test indexes of the modified PET and modified PTT pellets prepared in examples 1 to 4 are shown in Table 1, and the main performance test indexes of the prepared parallel composite elastic fiber and the fabric thereof are shown in Table 2.
TABLE 1 Performance index of modified PET and PTT pellets from examples 1-4
TABLE 2 Performance index of the side-by-side conjugate elastic fiber obtained in examples 1 to 4
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (8)
1. A side-by-side conjugate elastic fiber characterized by: the cross section of the composite material is of a peanut type parallel structure, and the composite material is formed by respectively extruding 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT according to the mass ratio of 45-55: 55-45 and then compounding;
the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET has the intrinsic viscosity of 0.53-0.65 d1/g, the terminal carboxyl group content of 20-30 mol/t, the melting point of 255-265 ℃, and the chroma b value of 3-6;
the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT has an intrinsic viscosity of 1.05-1.25 d1/g, a carboxyl end group content of 10-20 mol/t, a melting point of 224-230 ℃ and a chroma b value of 9-11.
2. A side-by-side conjugate elastic fiber as defined in claim 1, wherein: the preparation method of the 2, 6-naphthalenedicarboxylic acid copolymerized and modified PET comprises the following steps: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid and ethylene glycol in an acid-alcohol molar ratio of 1: 1.2-1.4 according to the mass calculation of the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET theoretically produced, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid and the ethylene glycol into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 245-260 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, and the esterification rate reaches more than 96% to complete esterification, so as to obtain a first esterified substance; sequentially adding isosorbide, trimethyl phosphate, an antioxidant 1010, titanium dioxide and a catalyst titanium glycol into the first esterified substance, heating and vacuumizing to enable the esterified substance to carry out polycondensation reaction under the vacuum condition, stopping the reaction when the stirring current and the online viscosity value reach preset values, and extruding and pelletizing to obtain the 2, 6-naphthalenedicarboxylic acid copolymerized modified PET.
3. A side-by-side conjugate elastic fiber as defined in claim 2, wherein: calculated according to the mass of the 2, 6-naphthalenedicarboxylic acid copolymerized and modified PET theoretically produced, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 1-8%, the addition amount of isosorbide is 0.1-0.8%, the addition amount of trimethyl phosphate is 50-200 ppm, the addition amount of the catalyst ethylene glycol titanium is 30-70 ppm, the addition amount of the antioxidant 1010 is 1000-2000 ppm, and the addition amount of the titanium dioxide is 0.28-0.31%.
4. A side-by-side conjugate elastic fiber as defined in claim 1, wherein: the preparation method of the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT comprises the following steps: weighing terephthalic acid, 2, 6-naphthalenedicarboxylic acid, 1, 3-propanediol and tetrabutyl titanate serving as a catalyst in an acid-alcohol molar ratio of 1: 1.25-1.55 according to the mass of the theoretically-produced 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT, adding the terephthalic acid, the 2, 6-naphthalenedicarboxylic acid, the 1, 3-propanediol and the tetrabutyl titanate serving as the catalyst into a reaction kettle for esterification reaction, wherein the temperature of the esterification reaction is 225-250 ℃, the pressure of the esterification reaction is micro-positive pressure of 0.02MPa, and the esterification rate reaches more than 99% to complete esterification so as to obtain a second esterified substance; adding an antioxidant 1076 and titanium dioxide into the second esterified product, heating and vacuumizing to enable the esterified product to carry out polycondensation reaction under the vacuum condition, stopping the reaction when the stirring current and the online viscosity value reach preset values, extruding and granulating, and then conveying to a vacuum rotary drum for solid-phase tackifying to obtain the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT.
5. A side-by-side conjugate elastic fiber as defined in claim 4, wherein: calculated by the mass of the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT produced theoretically, the addition amount of the 2, 6-naphthalenedicarboxylic acid is 0.5-1.5%, the addition amount of tetrabutyl titanate serving as a catalyst is 25-60 ppm, the addition amount of an antioxidant 1076 is 1000-2000 ppm, and the addition amount of titanium dioxide is 0.28-0.31%.
6. A method for producing a side-by-side conjugate elastic fiber as set forth in any one of claims 1 to 5, characterized in that: the method comprises the following steps:
and respectively carrying out melt extrusion on the dried 2, 6-naphthalenedicarboxylic acid copolymerization modified PET and 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT granules with the water content of below 50ppm by using respective screw extruders, feeding the extruded granules into a composite spinning assembly through respective melt pipelines, carrying out composite extrusion at a spinneret plate, carrying out air blowing cooling, oiling and winding to obtain parallel composite pre-oriented yarns, and carrying out false twisting processing to obtain the parallel composite elastic fibers.
7. The method of claim 6, wherein: the temperature of a spinning manifold corresponding to the 2, 6-naphthalenedicarboxylic acid copolymerization modified PET in the composite spinning component is 260-280 ℃, the temperature of a spinning manifold corresponding to the 2, 6-naphthalenedicarboxylic acid copolymerization modified PTT in the composite spinning component is 250-270 ℃, and the spinning speed is 2400-3000 m/min.
8. The method of claim 6, wherein: the temperature of the first heat box for false twisting is 160-175 ℃, the drafting ratio is 1.7-1.85, and the processing speed is 500-800 m/min.
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