CN115491789B - Functional parallel composite elastic fiber and preparation method thereof - Google Patents
Functional parallel composite elastic fiber and preparation method thereof Download PDFInfo
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- CN115491789B CN115491789B CN202210768412.4A CN202210768412A CN115491789B CN 115491789 B CN115491789 B CN 115491789B CN 202210768412 A CN202210768412 A CN 202210768412A CN 115491789 B CN115491789 B CN 115491789B
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 210000004177 elastic tissue Anatomy 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 140
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 121
- 239000011787 zinc oxide Substances 0.000 claims abstract description 70
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 60
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 36
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 22
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 22
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 claims abstract description 9
- 238000006068 polycondensation reaction Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- GRTOGORTSDXSFK-XJTZBENFSA-N ajmalicine Chemical compound C1=CC=C2C(CCN3C[C@@H]4[C@H](C)OC=C([C@H]4C[C@H]33)C(=O)OC)=C3NC2=C1 GRTOGORTSDXSFK-XJTZBENFSA-N 0.000 claims description 15
- 238000005809 transesterification reaction Methods 0.000 claims description 15
- 238000004537 pulping Methods 0.000 claims description 13
- 238000009987 spinning Methods 0.000 claims description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- GBQYMXVQHATSCC-UHFFFAOYSA-N 3-triethoxysilylpropanenitrile Chemical compound CCO[Si](OCC)(OCC)CCC#N GBQYMXVQHATSCC-UHFFFAOYSA-N 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000002074 melt spinning Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000004224 protection Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 abstract description 10
- 230000006750 UV protection Effects 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000975 dye Substances 0.000 description 11
- 238000001354 calcination Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 6
- 125000002091 cationic group Chemical group 0.000 description 6
- 230000032050 esterification Effects 0.000 description 6
- 238000005886 esterification reaction Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000004115 Sodium Silicate Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 229910052911 sodium silicate Inorganic materials 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920002334 Spandex Polymers 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical group [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 description 2
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 description 2
- 239000000986 disperse dye Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- IYVLHQRADFNKAU-UHFFFAOYSA-N oxygen(2-);titanium(4+);hydrate Chemical compound O.[O-2].[O-2].[Ti+4] IYVLHQRADFNKAU-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000004759 spandex Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 dihydroxyethyl Chemical group 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004383 yellowing Methods 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- 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
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Multicomponent Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the field of composite fibers, and provides a functional parallel composite elastic fiber and a preparation method thereof, aiming at the problems that the composite fiber has high elasticity, dyeing property and ultraviolet resistance, wherein the fiber is a parallel double-component composite fiber consisting of PTT and modified PET, the molecular chain of the modified PET contains polyethylene glycol molecular chain segments and sulfonate groups, and the PTT and the modified PET molecular chain are dispersed with silica coated nano zinc oxide; the cross section of the fiber is arranged in a double-blade shape, and grooves are formed in the surface of the double-blade shape. The invention hopes to be by PTT and modified PET make up side by side double-component composite fiber, contain polyethylene glycol molecule chain segment, sulfonate group on the molecular chain of modified PET, also disperse the nanometer zinc oxide coated with silicon dioxide; the groove double-blade section matched with the fiber has excellent elasticity, low-temperature dyeing property and ultraviolet resistance.
Description
Technical Field
The invention relates to the field of composite fibers, in particular to a functional parallel composite elastic fiber and a preparation method thereof.
Background
Since the 21 st century, parallel composite fibers have been rapidly developed, and parallel composite elastic fibers represented by PTT/PET, PBT/PET, high-viscosity PET/low-viscosity PET and the like are appeared on the market, and the fibers have high bulkiness, good elasticity and good hand feeling, wherein the parallel composite elastic fibers represented by PTT/PET have the best elastic performance and are widely applied to elastic underwear, swimwear, knitwear, webbing and socks.
Although PTT/PET parallel composite elastic fiber has very good shape retention and curl elasticity, the elasticity is still quite different from spandex elasticity, and a small amount of spandex is still required to be added to improve the elasticity in actual use, and because of lack of fiber functionality, the PTT/PET parallel composite elastic fiber is often required to be blended or woven with other fibers; in addition, due to the existence of PET components, the disperse dye can enter a molecular structure to realize dyeing under the condition of high temperature and high pressure, so that the bright color and the wide range of the color spectrum after dyeing are greatly limited, and the further application of the disperse dye is limited by high-temperature dyeing.
Chinese patent No. 108138379A of Dongli discloses a parallel type composite fiber, which realizes that PBT and cationic polyester form a bi-component elastic fiber with moderate elasticity and good elastic recovery rate in parallel by improving the viscosity of PBT, and can realize cationic dyeing effect, but can not achieve high-elasticity effect due to the limitation of the molecular structure of PBT. Moreover, with the extension of fiber application, more functional requirements are put on the fiber, such as ultraviolet resistance when used in swimwear. There is a need for an ideal solution.
Disclosure of Invention
The invention provides a functional parallel composite elastic fiber, which is a parallel double-component composite fiber composed of PTT and modified PET, wherein the molecular chain of the modified PET contains polyethylene glycol molecular chain segments, sulfonate groups and silica coated nano zinc oxide; the groove double-blade section matched with the fiber has excellent elasticity, low-temperature dyeing property and ultraviolet resistance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a functional parallel composite elastic fiber is a parallel double-component composite fiber composed of PTT and modified PET, wherein the molecular chain of the modified PET contains polyethylene glycol molecular chain segments and sulfonate groups, and the PTT and the modified PET molecular chain are dispersed with silica coated nano zinc oxide; the cross section of the fiber is arranged in a double-blade shape, and grooves are formed in the surface of the double-blade shape.
Preferably, the preparation method of the silica coated nano zinc oxide comprises the following steps: fully mixing zinc nitrate, sodium silicate and deionized water, dropwise adding ammonia water, regulating the pH of a system to 8-11, reacting for 0.5-6 h to obtain a coprecipitation product, and washing, drying, grinding and calcining to obtain the silica coated nano zinc oxide; the drying is that the drying is carried out for 6 to 18 hours at the temperature of 80 to 100 ℃ under the vacuum condition; the calcination is that the low temperature is 300-500 ℃ for 1-3 hours, and the high temperature is 500-800 ℃ for 0.5-4 hours. Zinc oxide has very excellent anti-ultraviolet function, and the grooves combined with the surface of the fiber can reflect ultraviolet light. The uncoated nano ZnO has strong electron-withdrawing effect, so that zinc has positive electricity, can be complexed with the intermediate product BHET of polyester, and has very strong catalytic reaction activity, so that the reaction speed is increased, the molecular weight distribution is poor, the color is seriously yellow, and the activity of the zinc is inhibited by coating silicon dioxide, so that the normal operation of the reaction is ensured. And the silica coated nano zinc oxide is more uniformly dispersed in the modified PET, so that agglomeration is not easy to occur.
Preferably, the mass ratio of zinc nitrate to sodium silicate is 1 (1-1.6).
Preferably, the average particle diameter D90 of the silica-coated nano zinc oxide is 100 to 500nm.
Preferably, the surface of the nano zinc oxide coated by the silicon dioxide is modified, and the steps are as follows: dispersing the nano zinc oxide coated with silicon dioxide in ethanol, heating to 40-50 ℃, adding 2-cyanoethyl triethoxysilane, wherein the mass ratio of the nano zinc oxide coated with silicon dioxide to the 2-cyanoethyl triethoxysilane is (2-4): 1, and carrying out reflux reaction for 3-5h under the protection of nitrogen to obtain the modified nano zinc oxide coated with silicon dioxide. The nano zinc oxide coated by the silicon dioxide is dispersed in ethanol solution, hydroxyl groups are carried on the surface, 2-cyanoethyl triethoxysilane reacts with the hydroxyl groups, and the surface of the nano zinc oxide is adsorbed and aggregated, so that C=C double bonds are carried on the surface of the nano zinc oxide coated by the silicon dioxide, the nano zinc oxide can participate in polymerization reaction in the later period, and the dispersibility and the stability of the nano zinc oxide coated by the silicon dioxide in fibers are improved.
Preferably, the preparation method of the modified PET comprises the following steps:
(1) Mixing terephthalic acid and ethylene glycol in a molar ratio of 1 (1.1-1.4), pulping, and esterifying the slurry to obtain an esterified substance I;
(2) Mixing the esterified substance I, a catalyst, polyethylene glycol, SIPE and silicon dioxide coated nano zinc oxide, and performing transesterification reaction to obtain an esterified substance II;
(3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PET; the temperature of the polycondensation is 260-280 ℃, the time is 3-5h, and the pressure is 200-400 Pa.
Wherein, the pulping temperature in the step (1) is 50-70 ℃ and the pulping time is 0.5-2.0 h; the esterification temperature is 240-260 ℃, the pressure is 60-65 kPa, and the time is 0.5-2 h;
the temperature of the transesterification reaction in the step (2) is 235-255 ℃, the pressure is 10-15 kPa, and the time is 0.5-2 h; the catalyst is selected from ethylene glycol antimony, antimony acetate or antimony trioxide, and the addition amount of the catalyst takes antimony as a unit and is 100-300 ppm of the total mass of the mixture; the weight average molecular weight of the polyethylene glycol is 1000-4000 g/mol.
As a further preferable mode, the polyethylene glycol addition amount in the step (2) is 1-5% of the total mass of the mixture, the SIPE addition amount is 4-10% of the total mass of the mixture, and the silica coated nano zinc oxide addition amount is 0.1-2% of the total mass of the mixture.
The preparation method of the PTT comprises the following steps: 1) Mixing terephthalic acid and propylene glycol in a molar ratio of 1 (1.05-2.5), pulping, and esterifying the slurry to obtain an esterified substance I;
2) Mixing the esterified substance I, the nano zinc oxide coated by silicon dioxide and a titanium catalyst, wherein the addition amount of the nano zinc oxide coated by silicon dioxide is 0.1-2% of the total mass of the mixture, and performing transesterification reaction to obtain the esterified substance II;
3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PTT; the temperature of the polycondensation is 220-250 ℃, the time is 1.0-3.0 h, and the pressure is 0-500 Pa.
Wherein, the pulping temperature in the step 1) is 50-70 ℃ and the pulping time is 0.5-2.0 h; the esterification temperature is 230-250 ℃, the pressure is 40-45 kPa, and the time is 1.0-2.5 h;
step 2), the temperature of the transesterification reaction is 235-255 ℃, the pressure is 10-15 kPa, and the time is 0.5-2 h; the catalyst is selected from tetrabutyl titanate, isopropyl titanate or titanium dioxide hydrate, and the adding amount of the catalyst takes titanium as a unit and is 20-100 ppm of the total mass of the mixture;
the invention also provides a preparation method of the functional parallel composite elastic fiber, wherein the melt spinning adopts a double screw, a double melt pipeline, a double spinning box body and a double-channel parallel spinning component, and the temperature balance of the PTT and the modified PET is realized in the double box body; the mass ratio of PTT to modified PET is 1 (0.5-1.2).
Therefore, the invention has the beneficial effects that: (1) According to the invention, polyethylene glycol and SIPE are uniformly distributed in the modified PET, and soft and hard segments are simultaneously present in the chain segments after polymerization of the PET, the polyethylene glycol and the SIPE, so that the elasticity of the fiber can be improved. Polyethylene glycol has hydrophilicity, can reduce the polymerization glass transition temperature, increases the free volume in a polymer system, combines with a parallel fiber double-blade-shaped section to have a large number of groove structures (the existence of silica coated nano zinc oxide can form a groove structure on a molecular level), so that micromolecular dye can enter the interior of the molecule more easily, and sulfonate groups of SIPE are firmly combined with cationic dye through chemical bonds, thereby realizing a low-temperature cationic dyeing function; (2) The nano zinc oxide coated by the silicon dioxide is dispersed in ethanol solution, hydroxyl groups are carried on the surface, 2-cyanoethyl triethoxysilane reacts with the hydroxyl groups, and the surface of the nano zinc oxide is adsorbed and aggregated, so that C=C double bonds are carried on the surface of the nano zinc oxide coated by the silicon dioxide, the nano zinc oxide can participate in polymerization reaction in the later period, and the dispersibility and the stability of the nano zinc oxide coated by the silicon dioxide in fibers are improved.
Drawings
FIG. 1 is a schematic illustration of a spinneret plate used in the present invention;
FIG. 2 is a cross-sectional view A-A of FIG. 1;
FIG. 3 is a cross-sectional view of the B-direction spinneret orifice of FIG. 2;
FIG. 4 is a cross-sectional view of a spun formed composite fiber of example 1;
FIG. 5 is a cross-sectional view of a conjugate fiber formed by ordinary spinning in comparative example 1.
Detailed Description
The technical scheme of the invention is further described through specific embodiments.
In the present invention, unless otherwise specified, the materials and equipment used are commercially available or are commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
General examples
A functional parallel composite elastic fiber is a parallel double-component composite fiber composed of PTT and modified PET, wherein the molecular chain of the modified PET contains polyethylene glycol molecular chain segments and sulfonate groups, and the PTT and the modified PET molecular chain are dispersed with silica coated nano zinc oxide; the cross section of the fiber is arranged in a double-blade shape, and grooves are formed in the surface of the double-blade shape.
The preparation method of the functional parallel composite elastic fiber comprises the following steps:
A. preparation of silica coated nano zinc oxide
Zinc nitrate and sodium silicate are mixed and dispersed in deionized water according to the mass ratio of 1 (1-1.6), ammonia water is added dropwise to adjust the pH value of the system to 8-11, the reaction is carried out for 0.5-6 hours, a coprecipitation product is obtained, and the nano zinc oxide coated with silicon dioxide is obtained through washing, drying, grinding and calcining; the drying is that the drying is carried out for 6 to 18 hours at the temperature of 80 to 100 ℃ under the vacuum condition; the calcination is that the low temperature is 300-500 ℃ for 1-3 hours, and the high temperature is 500-800 ℃ for 0.5-4 hours; the average particle diameter D90 of the silica coated nano zinc oxide is 100-500 nm.
B. Preparation of modified PET
(1) Mixing terephthalic acid and ethylene glycol according to a molar ratio of 1 (1.1-1.4), pulping at 50-70 ℃ for 0.5-2.0 h; esterifying the slurry to obtain an esterified substance I, wherein the esterification temperature is 240-260 ℃, the pressure is 60-65 kPa, and the time is 0.5-2 h;
(2) Mixing an esterified substance I, a catalyst, polyethylene glycol, SIPE (dihydroxyethyl isophthalate-5-sodium sulfonate) and silicon dioxide coated nano zinc oxide, wherein the weight average molecular weight of the polyethylene glycol is 1000-4000 g/mol, the adding amount of the polyethylene glycol is 1-5% of the total mass of the mixture, the adding amount of the SIPE is 4-10% of the total mass of the mixture, the adding amount of the silicon dioxide coated nano zinc oxide is 0.1-2% of the total mass of the mixture, the catalyst is selected from ethylene glycol antimony, antimony acetate or antimony trioxide, and the adding amount of the catalyst takes antimony as 100-300 ppm of the total mass of the mixture; performing transesterification reaction to obtain an esterified substance II, wherein the temperature of the transesterification reaction is 235-255 ℃, the pressure is 10-15 kPa, and the time is 0.5-2 h;
(3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PET; the temperature of the polycondensation is 260-280 ℃, the time is 3-5h, and the pressure is 200-400 Pa.
C. Preparation of PTT
1) Mixing terephthalic acid and propylene glycol in a molar ratio of 1 (1.05-2.5), pulping at 50-70 ℃ for 0.5-2.0 h; esterifying the slurry to obtain an esterified substance I, wherein the esterification temperature is 230-250 ℃, the pressure is 40-45 kPa, and the time is 1.0-2.5 h;
2) Mixing the esterified substance I, the nano zinc oxide coated by the silicon dioxide and a titanium catalyst, wherein the addition amount of the nano zinc oxide coated by the silicon dioxide is 0.1-2% of the total mass of the mixture, the catalyst is selected from tetrabutyl titanate, isopropyl titanate or titanium dioxide hydrate, and the addition amount of the catalyst takes titanium as a unit and is 20-100 ppm of the total mass of the mixture; performing transesterification reaction to obtain an esterified substance II, wherein the temperature of the transesterification reaction is 235-255 ℃, the pressure is 10-15 kPa, and the time is 0.5-2 h;
3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PTT; the temperature of the polycondensation is 220-250 ℃, the time is 1.0-3.0 h, and the pressure is 0-500 Pa.
D. The melt spinning takes modified PET as a component A, PTT as a component B, and the mass ratio of the component A to the component B is 1 (0.5-1.2), and the functional parallel composite elastic fiber is prepared by adopting double-screw melt extrusion, melt filtration, spinning by a spinneret plate, drafting and shaping, wherein the cross section is arranged in a double-fan blade shape, and grooves are formed on the surface of the double-fan blade shape. The temperature balance of the two components is realized in the double-box body by adopting double screws, double melt pipelines, double spinning box bodies and double-channel parallel spinning components.
During melt spinning, the temperature of a screw corresponding to the modified PTT is 240-270 ℃, the temperature of a spinning box corresponding to the modified PTT is 245-260 ℃, the temperature of a modified PET screw is 260-285 ℃, the temperature of a spinning box corresponding to the modified PET is 265-280 ℃, the lateral blowing temperature is 15-30 ℃, and the wind speed is 0.35-0.65 m/s;
the temperature of GR1 is 60-80 ℃, the speed of GR1 is 1280-2560 m/min, and the number of turns of GR1 is 6-7; the temperature of GR2 is 105-140 ℃, the speed of GR2 is 4000-6000 m/min, and the number of turns of GR2 is 6-8; the winding speed is 3800-5800 m/min.
Example 1
A functional parallel composite elastic fiber is a parallel double-component composite fiber composed of PTT and modified PET, wherein the molecular chain of the modified PET contains polyethylene glycol molecular chain segments and sulfonate groups, and the PTT and the modified PET molecular chain are dispersed with silica coated nano zinc oxide; the cross section of the fiber is arranged in a double-blade shape, and grooves are formed in the surface of the double-blade shape.
The preparation method of the functional parallel composite elastic fiber comprises the following steps:
A. preparation of silica coated nano zinc oxide
Zinc nitrate and sodium silicate are mixed and dispersed in deionized water according to the mass ratio of 1:1.5, ammonia water is added dropwise to adjust the pH value of the system to 9, the reaction is carried out for 3 hours, a coprecipitation product is obtained, and the nano zinc oxide coated with silicon dioxide is obtained through washing, drying, grinding and calcining; the drying is carried out for 10 hours at 90 ℃ under vacuum condition; the calcination is that the low temperature is 400 ℃ for 2 hours, and then the high temperature is 600 ℃ for 2 hours; the average particle diameter D90 of the silica coated nano zinc oxide is 100-500 nm.
B. Preparation of modified PET
(1) Mixing terephthalic acid and ethylene glycol in a molar ratio of 1:1.3, and pulping at 60 ℃ for 1.0h; esterifying the slurry to obtain an esterified substance I, wherein the esterification temperature is 250 ℃, the pressure is 60kPa, and the time is 1.0h;
(2) Mixing an esterified substance I, a catalyst, polyethylene glycol, SIPE and silicon dioxide coated nano zinc oxide, wherein the weight average molecular weight of the polyethylene glycol is 2000g/mol, the adding amount of the polyethylene glycol is 3% of the total mass of the mixture, the adding amount of the SIPE is 4% of the total mass of the mixture, the adding amount of the silicon dioxide coated nano zinc oxide is 1% of the total mass of the mixture, the catalyst is antimony trioxide, and the adding amount of the catalyst is 200ppm of the total mass of the mixture by taking antimony as a unit; carrying out transesterification reaction to obtain an esterified substance II, wherein the temperature of the transesterification reaction is 250 ℃, the pressure is 13kPa, and the time is 1h;
(3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PET; the temperature of the polycondensation was 270℃for 4 hours and the pressure was 300Pa.
C. Preparation of PTT
1) Mixing terephthalic acid and propylene glycol in a molar ratio of 1:2.0, and pulping at 60 ℃ for 1.0h; esterifying the slurry to obtain an esterified substance I, wherein the esterification temperature is 240 ℃, the pressure is 45kPa, and the time is 1.0h;
2) Mixing an esterified substance I, silicon dioxide coated nano zinc oxide and a titanium catalyst, wherein the addition amount of the silicon dioxide coated nano zinc oxide is 1% of the total mass of the mixture, the catalyst is tetrabutyl titanate, and the addition amount of the catalyst takes titanium as a unit to be 60ppm of the total mass of the mixture; carrying out transesterification reaction to obtain an esterified substance II, wherein the temperature of the transesterification reaction is 245 ℃, the pressure is 10kPa, and the time is 2 hours;
3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PTT; the temperature of the polycondensation was 240℃for 2.0h and the pressure was 300Pa.
D. The melt spinning takes modified PET as a component A, PTT as a component B, the mass ratio of the component A to the component B is 1 (0.5-1.2), twin-screw melt extrusion is adopted, melt filtration is carried out, spinning is carried out through a spinneret plate shown in the figures 1-3, the functional parallel composite elastic fiber is obtained after drafting and shaping, the cross section is shown in the figure 4, the fiber is in a double-blade shape arrangement, and grooves are formed on the surfaces of the double-blade shape.
During melt spinning, the temperature of a screw corresponding to the modified PTT is 250 ℃, the temperature of a spinning box corresponding to the modified PTT is 250 ℃, the temperature of a modified PET screw is 285 ℃, the temperature of a spinning box corresponding to the modified PET is 270 ℃, the lateral blowing temperature is 20 ℃, and the wind speed is 0.45m/s;
the temperature of GR1 is 70 ℃, the speed of GR1 is 2000m/min, and the number of turns of GR1 is 6; the temperature of GR2 is 130 ℃, the speed of GR2 is 5000m/min, and the number of turns of GR2 is 7; the winding speed was 4800m/min.
Example 2
The difference from example 1 is that the surface of the nano zinc oxide coated with silicon dioxide in the step A is modified, and the steps are as follows: dispersing the silicon dioxide coated nano zinc oxide in ethanol, heating to 50 ℃, adding 2-cyanoethyl triethoxysilane, wherein the mass ratio of the silicon dioxide coated nano zinc oxide to the 2-cyanoethyl triethoxysilane is 3:1, and carrying out reflux reaction for 4 hours under the protection of nitrogen to obtain the modified silicon dioxide coated nano zinc oxide.
Example 3
The difference from example 1 is that the silica coated nano zinc oxide in step a is calcined at 600 ℃ for 4 hours.
Example 4
The difference from example 1 is that the amount of silica-coated nano zinc oxide added in step (2) of step B is 3% of the total mass of the mixture.
Comparative example 1
The difference from example 1 is that the spinneret used in step D is a conventional spinneret and the cross-section of the resulting fiber is shown in fig. 5.
Comparative example 2
The difference from example 1 is that no SIPE was added in step (2).
Comparative example 3
The difference from example 1 is that the nano zinc oxide in step a is not coated.
Performance testing
The functional side-by-side composite elastic fibers prepared in the above examples and comparative examples were subjected to performance tests, and the results are shown in the following table.
And (3) taking the medium black PV as a dye, wherein the dye consumption is 5%, and the dye uptake of the dye is measured by heat preservation for 30min at 80 ℃.
| Sequence number | Elastic recovery% | Breaking strength cN/dtex | Dye uptake% | UPF |
| Example 1 | 91 | 4.3 | 87 | 32 |
| Example 2 | 88 | 4.4 | 90 | 35 |
| Example 3 | 89 | 4.2 | 86 | 30 |
| Example 4 | 86 | 4.1 | 87 | 33 |
| Comparative example 1 | 88 | 4.5 | 82 | 29 |
| Comparative example 2 | 85 | 4.4 | 35 | 32 |
| Comparative example 3 | 80 | 4.2 | 79 | 24 |
As can be seen from the table, the functional parallel composite elastic fiber prepared by the embodiments of the invention has better elasticity and has low-temperature dyeing property and ultraviolet resistance. Compared with the embodiment 1, the embodiment 2 carries out modification treatment on the surface of the nano zinc oxide coated by the silicon dioxide to ensure that the nano zinc oxide has double bonds and can participate in polymerization, so that the dispersibility and the stability of the nano zinc oxide coated by the silicon dioxide in the fiber are improved, and the dye uptake and the ultraviolet resistance are further improved; example 3 calcination of silica-coated nano zinc oxide does not adopt stepwise progressive calcination, and the stepwise calcination has the advantages that volatile matters are gradually volatilized from the outer layer to the inner layer, the adhesion between the inner layer and the outer layer is not obviously reduced after the drying is completed, the separation is not easy, and the stability is good. Example 4 silica coated nano zinc oxide was added in an excessive amount, which adversely affects the fiber properties, because too much silica coated nano zinc oxide increases the fiber roughness and reduces its elasticity.
Compared with example 1, the comparative example 1 adopts a common spinneret plate, and the surface of the fiber is not provided with grooves, so that the dye uptake is reduced, and the ultraviolet resistance is also adversely affected; the dye uptake is obviously reduced without adding SIPE when the PET is modified in comparative example 2, because the sulfonate group of SIPE is firmly combined with the cationic dye through a chemical bond, the low-temperature cationic dyeing function is realized; the nano zinc oxide of comparative example 3 was not coated, and the nano zinc oxide was complexed with BHET, an intermediate product of polyester, and had poor molecular weight distribution and severe yellowing of color, and was easily agglomerated, and had an influence on each property.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalent changes and variations in the above-mentioned embodiments can be made by those skilled in the art without departing from the scope of the present invention.
Claims (5)
1. A functional parallel composite elastic fiber is characterized by comprising a PTT and a modified PET, wherein the molecular chain of the modified PET contains polyethylene glycol molecular chain segments and sulfonate groups, and the PTT and the modified PET molecular chain are dispersed with silica coated nano zinc oxide; the cross section of the fiber is arranged in a double-blade shape, and grooves are formed in the surface of the double-blade shape;
the preparation method of the modified PET comprises the following steps: mixing terephthalic acid and ethylene glycol, pulping to obtain an esterified substance I, mixing the esterified substance I with a catalyst, polyethylene glycol, SIPE and silica coated nano zinc oxide, performing transesterification reaction to obtain an esterified substance II, and sequentially performing pre-polycondensation and final polycondensation to obtain modified PET;
the preparation method of the PTT comprises the following steps: mixing terephthalic acid and propylene glycol, pulping to obtain an esterified substance III, mixing the esterified substance III with nano zinc oxide coated with silicon dioxide, performing transesterification reaction to obtain an esterified substance IV, and sequentially performing pre-polycondensation and final polycondensation to obtain PTT;
the surface of the nano zinc oxide coated by the silicon dioxide is modified, and the steps are as follows: dispersing the nano zinc oxide coated with silicon dioxide in ethanol, heating to 40-50 ℃, adding 2-cyanoethyl triethoxysilane, wherein the mass ratio of the nano zinc oxide coated with silicon dioxide to the 2-cyanoethyl triethoxysilane is (2-4): 1, and carrying out reflux reaction under the protection of nitrogen for 3-5h to obtain the modified nano zinc oxide coated with silicon dioxide.
2. A functional side-by-side composite elastic fiber according to claim 1, characterized in that the average particle diameter D90 of the silica-coated nano zinc oxide is 100 to 500nm.
3. The functional side-by-side composite elastic fiber according to claim 1, wherein the modified PET is prepared by the following steps:
(1) Mixing terephthalic acid and ethylene glycol in a molar ratio of 1 (1.1-1.4), pulping, and esterifying the slurry to obtain an esterified substance I;
(2) Mixing the esterified substance I, a catalyst, polyethylene glycol, SIPE and silicon dioxide coated nano zinc oxide to obtain a mixture, and performing transesterification reaction to obtain an esterified substance II;
(3) Sequentially performing pre-polycondensation and final polycondensation on the esterified substance II to obtain modified PET; the temperature of polycondensation is 260-280 ℃, the time is 3-5h, and the pressure is 200-400 Pa.
4. The functional parallel composite elastic fiber according to claim 3, wherein the polyethylene glycol addition amount in the step (2) is 1-5% of the total mass of the mixture, the SIPE addition amount is 4-10% of the total mass of the mixture, and the silica coated nano zinc oxide addition amount is 0.1-2% of the total mass of the mixture.
5. The method for preparing the functional parallel composite elastic fiber as claimed in claim 1, wherein the melt spinning adopts a double screw, a double melt pipeline, a double spinning box and a double-channel parallel spinning component, and the mass ratio of PTT and modified PET is 1 (0.5-1.2).
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