CN115233334B - High-brightness composite noctilucent fiber and preparation method thereof - Google Patents
High-brightness composite noctilucent fiber and preparation method thereof Download PDFInfo
- Publication number
- CN115233334B CN115233334B CN202210917638.6A CN202210917638A CN115233334B CN 115233334 B CN115233334 B CN 115233334B CN 202210917638 A CN202210917638 A CN 202210917638A CN 115233334 B CN115233334 B CN 115233334B
- Authority
- CN
- China
- Prior art keywords
- fiber
- composite
- powder
- core layer
- noctilucent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 104
- 239000002131 composite material Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 79
- 238000009987 spinning Methods 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 58
- 239000012792 core layer Substances 0.000 claims abstract description 54
- 239000000155 melt Substances 0.000 claims abstract description 37
- 239000010410 layer Substances 0.000 claims abstract description 35
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920001634 Copolyester Polymers 0.000 claims description 45
- 239000008188 pellet Substances 0.000 claims description 41
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 238000002844 melting Methods 0.000 claims description 28
- 230000008018 melting Effects 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 27
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 24
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 24
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 21
- 238000004804 winding Methods 0.000 claims description 20
- -1 rare earth aluminate Chemical class 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- 235000019441 ethanol Nutrition 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000005086 pumping Methods 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000005886 esterification reaction Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical compound [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 10
- 238000006068 polycondensation reaction Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 8
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910003668 SrAl Inorganic materials 0.000 claims description 4
- 150000001263 acyl chlorides Chemical class 0.000 claims description 4
- 230000032050 esterification Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000013538 functional additive Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- HVECYHMPWPDALU-UHFFFAOYSA-N 2,6-ditert-butylphenol;propanoic acid Chemical compound CCC(O)=O.CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O HVECYHMPWPDALU-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 abstract description 13
- 239000004594 Masterbatch (MB) Substances 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000007380 fibre production Methods 0.000 abstract description 3
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000001125 extrusion Methods 0.000 abstract description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 16
- 239000005020 polyethylene terephthalate Substances 0.000 description 16
- 229920001707 polybutylene terephthalate Polymers 0.000 description 15
- 230000008569 process Effects 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 8
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010128 melt processing Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 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 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance 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
-
- 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
-
- 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
- D01D5/34—Core-skin 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Multicomponent Fibers (AREA)
Abstract
The invention discloses a high-brightness composite noctilucent fiber and a preparation method thereof, wherein the composite noctilucent fiber is of a sheath-core composite structure, the middle skin layer of the fiber section is round, and the core layer is in a hexadecimal star shape; the core layer is made of PBT powder with good fluidity, bottle-grade PET powder is taken as a carrier, and the core layer is made of a section of fiber forming processing technology under the action of a functional auxiliary agent with efficient coupling, antioxidation and good water repellency, the luminous powder can be uniformly dispersed under the operation of a double-screw extruder with vacuumizing function and is spun through direct melt extrusion, so that the master batch granulating section is reduced, the melt residence time is shortened, the melt temperature is lower, the obtained melt has good fluidity, the degradation of polyester materials is low, the spinning performance is good, and the fiber strength is higher, and the core layer is suitable for being popularized in the existing polyester fiber production enterprises.
Description
Technical Field
The invention belongs to the technical field of chemical fiber processing, and particularly relates to a high-brightness composite noctilucent fiber and a preparation method thereof.
Background
The luminous fiber is a functional fiber capable of emitting light with certain color for long time under dark condition after absorbing energy under light irradiation with fixed wavelength, and is widely applied in clothing and shoes material, home textile, transportation, building decoration, fire emergency, night work, anti-fake field, recreational and other fields. The basic performance of the luminous fiber not only can meet the requirements of all quality indexes of fiber manufacturing process, textile processing and end application products, but also has good luminous performance, and besides the requirements of few application places such as anti-counterfeiting field and the like on luminous brightness and afterglow length are not high, most application fields need to stop illumination of the luminous fiber, and the emitted luminous brightness is still as high as possible and the afterglow time is as long as possible.
The luminescent base material used by the luminous fiber is mostly alkaline earth luminescent material which takes rare earth ions as an activator, and rare earth aluminate is one of the most commercial luminous materials at present. The rare earth aluminate has the advantages of long afterglow time, high brightness, stable performance, reusability, no radioactivity and the like, but the alkaline earth aluminate has the problem of easy hydrolysis when meeting water, and the rest of the glow performance is reduced or even eliminated. Meanwhile, the larger the particle size of the rare earth aluminate is, the higher the content of the rare earth aluminate in the noctilucent fiber is, and the higher the luminescence brightness is; however, the larger the particle size, the higher the content, the more difficult the fiber production, and the greater the influence on the properties of the fiber itself.
The luminous fiber is produced through the process of melting spinning, including heating and melting high molecular polymer, spraying out the polymer from the spinning hole, cooling and solidifying in air to form fiber, and has the advantages of simple operation, easy preparation, stable luminous performance, high strength and long service life.
In addition, the luminance of the presently disclosed luminescent fibers is low, especially in the fields of clothing and shoe materials requiring finer fineness. Chinese patent CN 1374415a discloses a single-component polyester DTY fiber modified by rare earth noctilucent material, which is manufactured by preparing high-concentration noctilucent master batch, mixing the master batch with large luminous slice, melt spinning, and processing into DTY fiber in two stages. The product has the defects of large friction force on the surface of the fiber, large damage to equipment, serious degradation of materials after twice melt processing, low fiber strength, poor spinnability, low efficiency due to a two-stage processing mode, low practical application value and the like. Chinese patent CN 103882556a discloses a composite noctilucent fiber with skin-core structure and its manufacturing method, the rare earth noctilucent master batch made of the composite noctilucent fiber is used for the skin layer, the core layer is made of common fiber material, the strength performance of the fiber is improved by melt extrusion, but the product still has the disadvantages of large friction force on the surface of the fiber, large damage to equipment, low efficiency by two-section fiber processing mode, and the like, the two materials of the skin and the core do not consider the flow performance of the two materials, and the problems of poor spinning, easy broken filaments, easy eccentric formation of the fiber structure, and even non-formation of the skin-core structure can occur in the actual spinning process. Chinese patent CN106480525a discloses a noctilucent fiber with sheath-core structure, wherein the sheath is nylon resin, the core is made of rare earth luminescent material and nylon resin, the problem of friction force on the surface of the fiber is solved, the fiber has higher brightness, but the particle size of the noctilucent material is small (less than 1 μm), the adding amount of the noctilucent material is large (up to 30%), and the two-time melting and two-stage fiber processing mode is adopted, so that the defects of high cost, poor spinnability and the like are overcome. Chinese patent CN 110952164a discloses a high-brightness light-accumulating polyester fiber, the aluminate is doped with trace rare earth elements for the noctilucent material, the fiber structure is a core-sheath structure, the core is a light-accumulating master batch, the sheath is polyester, the problem of friction force on the surface of the fiber is solved, the sheath-core ratio is more than 40:60, higher fiber strength can be obtained, but the brightness is also affected, the light-accumulating powder needs to be modified in a complex way, and an organic solvent such as isopropanol is used, so that the process is not environment-friendly and the cost is high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-brightness composite noctilucent fiber and a preparation method thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a high-brightness composite noctilucent fiber is of a sheath-core composite structure, wherein a middle sheath layer of the fiber section is round, and a core layer is in a hexadecimal star shape; the core layer accounts for 75-88% and the skin layer accounts for 12-25% in percentage by mass, and the sum of the core layer and the skin layer is 100%;
wherein the core layer is prepared from the following raw materials in parts by weight:
60-76 parts by weight of polybutylene terephthalate (PBT) powder;
15-31 parts by weight of polyethylene terephthalate (PET) powder;
4-9 parts of noctilucent powder;
0.2-0.8 parts by weight of functional auxiliary agent;
the cortex is prepared by using dibasic acid and dihydric alcohol as raw materials and granulating bright copolyester obtained by esterification and copolymerization.
Further, the PBT powder is fiber-grade semi-extinction type, the Intrinsic Viscosity (IV) is 1.0+/-0.012 dl/g, and the titanium dioxide content is 1.0%.
Further, the PET powder is bottle grade, and the Intrinsic Viscosity (IV) is 0.60+/-0.010 dl/g.
Further, the particle sizes of the PBT powder and the PET powder are less than or equal to 38 microns.
Further, the noctilucent powder is SrAl 2 O 4 :Eu 2+ ,Dy 3+ The average grain diameter of the rare earth aluminate luminescent material is 2-7 microns, and the highest grain diameter is 10 microns.
Further, the dibasic acid is a mixture of terephthalic acid and isophthalic acid, and the weight ratio of the terephthalic acid to the isophthalic acid is 60:40-80:20; the dihydric alcohol is a mixture of ethylene glycol and 1, 4-butanediol, and the weight ratio of the ethylene glycol to the 1, 4-butanediol is 70:30-85:15.
Further, the melting point of the bright copolyester pellets is 225-240 ℃.
Further, the single fiber fineness of the composite noctilucent fiber is 1 dtex-7 dtex, the fiber strength is more than or equal to 3.3 cN/dtex, and the initial brightness value is more than or equal to 650 mcd/m 2 。
The preparation method of the high-brightness composite noctilucent fiber comprises the following steps:
(1) Preparation of core layer material: simultaneously adding PBT powder, PET powder, noctilucent powder and functional additives in a metering ratio into a double-screw extruder on line, melting, mixing and homogenizing to fully mix, extruding by a melt pump, and metering and pumping into a composite spinning component by the melt;
(2) Preparation of the skin layer material: preparing binary acid and dihydric alcohol into uniform slurry according to the acid/alcohol molar ratio of 1:1.15, and then carrying out esterification and polycondensation reaction by using ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain the bright copolyester granules.
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, then sending the bright copolyester pellets into a single screw extruder, sending the single screw extruder into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component together with the core layer material in the step (1), and then cooling, oiling, hot roller drafting and winding the obtained fiber filaments into FDY.
Further, the melting section and the exhaust port of the kneading section of the twin-screw extruder used in the step (1) are connected with a vacuum-pumping device to control the vacuum degree to be 300Pa or less.
Further, the outlet temperature of the melt pump of the twin-screw extruder used in the step (1) is 270-275 ℃.
Further, the screw outlet temperature of the single screw extruder used in the step (3) is 272-278 ℃.
Further, the spinning temperature of the composite spinning component in the step (3) is 275-280 ℃, and the spinning winding speed is 4000-4800 m/min.
The beneficial effects of the invention are as follows:
1. according to the invention, rare earth noctilucent powder is added into a core layer, PBT powder with good fluidity is used as a carrier, bottle-grade PET powder is used as a carrier, and the functions of high-efficiency coupling, antioxidation and good water repellency are combined, so that not only can the thermo-oxidative stability of polyester be improved, but also the unexpected effect of enhancing the dispersion uniformity of the polyester is obtained, meanwhile, the noctilucent powder is prepared by adopting a double-screw extruder with a vacuumizing function, so that the noctilucent powder is fully and uniformly dispersed, and is directly melt extruded for spinning, the master batch granulating section is reduced, the melt residence time is shortened, the melting temperature is lower, the obtained melt has good fluidity, the polyester material is low in degradation, good spinning performance is realized, high fiber strength is maintained, the product specification of the noctilucent powder can meet the requirements of fine denier fibers of clothes, and the application of most textiles can be met.
2. The leather layer material used in the invention adopts the common glossy copolyester obtained by the reaction of the dibasic acid and the dibasic alcohol to cut particles, the crystallization rate of the fiber prepared by the glossy copolyester is greatly reduced, the light transmittance is improved, the luminous brightness is increased, the melting point of the modified polyester is reduced, the spinning temperature is reduced, the melt flow property is similar to the flow property of the core layer, the fiber structure symmetry can be maintained during composite spinning, and the broken filaments are prevented.
3. The cross section of the core layer of the composite noctilucent fiber is in a sixteen-star shape, and the proportion of the core layer is high, so that the core layer has larger specific surface area, more noctilucent materials are contained, the luminous brightness of the fiber is greatly improved, and the problem of high friction force on the surface of the fiber is solved.
4. The invention adopts a section of fiber forming processing technology, is similar to the common FDY processing technology, has high efficiency, only needs to carry out a small amount of modification and process adjustment on the existing polymerization and spinning equipment for polyester production, and is suitable for popularization in the existing polyester fiber production enterprises.
Drawings
FIG. 1 is a schematic cross-sectional view of a high brightness composite luminescent fiber prepared according to the invention.
Detailed Description
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, wherein a middle sheath layer of the fiber section is round, and a core layer is in a hexadecimal star shape; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (60-76 parts by weight), PET powder (15-31 parts by weight), srAl 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (4-9 parts by weight) and the functional auxiliary agent (0.2-0.8 parts by weight) into a double-screw extruder simultaneously on line, melting, mixing and homogenizing to fully mix, extruding by a melt pump, and pumping into a composite spinning component by melt metering; the melting section and the mixing section of the twin-screw extruder are connected with a vacuum pumping device to control the vacuum degree to be below 300PaThe outlet temperature of the melt pump is 270-275 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid with the weight ratio of 60:40-80:20 into a mixed solution of ethylene glycol and 1, 4-butanediol with the weight ratio of 70:30-85:15 according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245-255 ℃ and polycondensation reaction at 280-285 ℃ by taking ethylene glycol antimony as a catalyst until the viscosity value of the polymer reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets (the melting point is 225-240 ℃);
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, then feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 272-278 ℃) and feeding the bright copolyester pellets into a composite spinning assembly through a melt metering pump, wherein the bright copolyester pellets and the core layer material in the step (1) are subjected to composite spinning assembly (the processing temperature of the spinning assembly is 275-280 ℃) to form fiber filaments with a sheath-core structure according to the mass percentage ratio of (12-25) of the sheath layer to the core layer (75-88), and then cooling, oiling, hot roller drafting and winding the obtained fiber filaments into FDY (the spinning winding speed is 4000-4800 m/min).
The single fiber fineness of the obtained composite noctilucent fiber is 1 dtex-7 dtex, the fiber strength is more than or equal to 3.3 cN/dtex, and the initial brightness value is more than or equal to 650 mcd/m 2 。
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
The PBT powder is fiber-grade semi-degerming, the Intrinsic Viscosity (IV) is 1.0+/-0.012 dl/g, the titanium dioxide content is 1.0%, and the particle size is less than or equal to 38 microns.
The PET powder is bottle grade, the Intrinsic Viscosity (IV) is 0.60+/-0.010 dl/g, and the grain diameter is less than or equal to 38 microns.
The noctilucent powder is SrAl 2 O 4 :Eu 2+ ,Dy 3+ Rare earth aluminate luminescent materials.
The preparation method of the functional auxiliary agent comprises the following steps:
(1) Taking 4g of vacuum dried nano silicon dioxide, adding 200mL of anhydrous toluene, carrying out ultrasonic treatment for 30min, then adding 1.8mL of N-2-aminoethyl-3-aminopropyl triethoxysilane (NSCA), and reacting at 60 ℃ for 24h; filtering after the reaction is finished, washing a filter cake with anhydrous toluene and absolute ethanol for a plurality of times, vacuum drying the filter cake to constant weight at 80 ℃, and grinding the filter cake into powder to obtain the SiO modified by the surface silane 2 ；
(2) Accurately weighing 4g of 3, 5-di-tert-butyl-4-hydroxy benzene propionic acid, dissolving in 200mL of anhydrous dichloromethane, slowly dropwise adding 2.6mL of distilled thionyl chloride and 0.1mL of N, N-dimethylformamide by using a constant pressure dropping funnel, and stirring and refluxing for 4 hours at 30 ℃ under the protection of nitrogen; removing solvent dichloromethane and unreacted thionyl chloride from the obtained reaction liquid by rotary evaporation to obtain solid acyl chloride;
(3) Taking 4g of the surface silane modified SiO prepared in the step (1) 2 Dissolving in 200mL of anhydrous toluene, carrying out ultrasonic treatment for 30 minutes, then dissolving the solid acyl chloride prepared in the step 3) in 200mL of anhydrous toluene, slowly dripping 4.00mL of triethylamine, and reacting for 20 hours at 60 ℃ under the protection of nitrogen; and after the reaction is finished, carrying out suction filtration, washing a filter cake for a plurality of times by using anhydrous toluene and absolute ethyl alcohol, and finally, drying the product in a vacuum drying oven (80 ℃) to constant weight to obtain the functional auxiliary agent.
The composite spinning component mainly comprises a distributing plate, a guide plate and a spinneret plate, wherein the outlet hole of a core layer channel on the guide plate is in a sixteen-star shape, the outlet hole of a skin layer channel is in a round shape, the micropore of the spinneret plate is in a round shape, two melts respectively flow through the distributing plate and the guide plate after being extruded, and finally are sprayed out of the spinneret plate together, so that the obtained fiber yarn forms a unique section.
The main index test method is as follows:
intrinsic viscosity of the polyester pellets: according to the national standard GB/T14190-2008.
Spin pack cycle: when the spin pack pressure was 3Mpa higher than the pressure at the time of new exchange of the pack, the exchange was performed for 1 cycle, time in hours.
Spinning breaking rate: converted to a single spinning position with 10 spindle filaments, the number of filament breaks in 1 assembly period was measured (excluding equipment factors leading to the number of filament breaks).
Fiber fineness and strength: according to the national standard GB/T8960-2015.
The initial luminance value test method adopts PR-305 type long afterglow fluorescent powder tester, adopts D65 standard light source, puts the sample into dark environment for more than 24 hours, excites illuminance 1000 lx, excites time 15min, and records afterglow luminance for 10 seconds after the light source is removed.
Example 1
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is circular, and the section of a core layer is hexadecimal star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (62.5 parts by weight), PET powder (31 parts by weight), srAl having an average particle diameter of 2 μm 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (6 parts by weight) and the functional auxiliary agent (0.5 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device, the vacuum degree is controlled below 300Pa, and the outlet temperature of the melt pump is 275 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 65:35) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 80:20) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245 ℃ and polycondensation reaction at 280 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, then feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 278 ℃) and feeding the bright copolyester pellets into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure by the composite spinning component (the processing temperature of the spinning component is 280 ℃) together with the core layer material in the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 20:80, cooling, oiling, hot roller drafting and winding the obtained fiber into FDY (the spinning winding speed is 4500 m/min), wherein the specification is 83dtex/72F, and the composite luminous fiber with the specification is suitable for being applied to the application fields of clothing and the like with relatively thin fiber properties and relatively high flexibility.
Example 2
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is circular, and the section of a core layer is hexadecimal star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (67.8 parts by weight), PET powder (28 parts by weight), srAl having an average particle diameter of 5 μm 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (4 parts by weight) and the functional auxiliary agent (0.2 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 273 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 80:20) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 75:25) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245 ℃ and polycondensation reaction at 280 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 275 ℃) and feeding the bright copolyester pellets into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component together with the core layer material in the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 12:88 (the processing temperature of the spinning component is 277 ℃), cooling, oiling, hot roller drafting and winding the obtained fiber filaments into FDY (the spinning winding speed is 4800 m/min), wherein the specification is 83dtex/36F.
Example 3
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is circular, and the section of a core layer is hexadecimal star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (69.4 parts by weight), PET powder (23 parts by weight), srAl having an average particle size of 5 μm 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (8 parts by weight) and the functional auxiliary agent (0.6 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 272 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 60:40) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 85:15) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245 ℃ and polycondensation reaction at 280 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 274 ℃) and feeding the bright copolyester pellets into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component (the processing temperature of the spinning component is 276 ℃) together with the core layer material in the step (1) according to the mass percentage ratio of 25:75 of the sheath layer to the core layer, cooling, oiling, hot roller drafting and winding the fiber filaments into FDY (the spinning winding speed is 4450 m/min), wherein the specification is 165dtex/48F.
Example 4
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is circular, and the section of a core layer is hexadecimal star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (75.2 parts by weight), PET powder (15 parts by weight), srAl having an average particle diameter of 7 μm 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (9 parts by weight) and the functional auxiliary agent (0.8 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 270 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 70:30) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 78:22) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245 ℃ and polycondensation reaction at 280 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 272 ℃), feeding the bright copolyester pellets into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component (the processing temperature of the spinning component is 274 ℃) together with the core layer material of the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 20:80, cooling, oiling, drawing by a hot roller, and winding into FDY (the spinning winding speed is 4000 meters/min), wherein the specification is 83dtex/12F.
Example 5
A high-brightness composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is circular, and the section of a core layer is hexadecimal star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (67.4 parts by weight), PET powder (25 parts by weight), srAl having an average particle diameter of 6 μm 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (7 parts by weight) and the functional auxiliary agent (0.6 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 271 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 75:25) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 80:20) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 255 ℃ and polycondensation reaction at 285 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 273 ℃), feeding the bright copolyester pellets into a composite spinning assembly through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning assembly (the processing temperature of the spinning assembly is 275 ℃) together with the core layer material of the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 19:81, cooling, oiling, drawing by a hot roller, and winding the fiber filaments into FDY (the spinning winding speed is 4600 meters/min), wherein the specification is 83dtex/24F.
Comparative example 1
The composite noctilucent fiber is of a sheath-core composite structure, the section of the composite noctilucent fiber is concentric circles, and the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (67.4 parts by weight), PET powder (25 parts by weight), and a mixture of a PET powder and a polyester powder having an average particle diameter of6 micron SrAl 2 O 4 :Eu 2+ ,Dy 3+ Adding the rare earth aluminate luminescent material (7 parts by weight) and the functional additive (0.6 parts by weight) into a double-screw extruder simultaneously on line, fully mixing the materials through the processes of melting, mixing, homogenizing and the like, pressurizing and extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 271 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 75:25) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 80:20) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 255 ℃ and polycondensation reaction at 285 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 273 ℃), feeding the bright copolyester pellets into a composite spinning assembly through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning assembly (the processing temperature of the spinning assembly is 275 ℃) together with the core layer material of the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 19:81, cooling, oiling, drawing by a hot roller, and winding the fiber filaments into FDY (the spinning winding speed is 4600 meters/min), wherein the specification is 83dtex/24F.
Comparative example 2
A composite noctilucent fiber is of a sheath-core composite structure, the section of a sheath layer is round, and the section of a core layer is sixteen-star-shaped; the preparation method comprises the following steps:
(1) Preparation of core layer material: PBT powder (62.5 parts by weight), PET powder (31 parts by weight), srAl having an average particle diameter of 2 μm 2 O 4 :Eu 2+ ,Dy 3+ Rare earth aluminate luminescent material (6 weight parts) and antioxidant 1010 (0.5 weight parts) are simultaneously added on line into a double screwIn an extruder, after fully mixing the materials through the processes of melting, mixing, homogenizing and the like, extruding the materials through a melt pump, and pumping the materials into a composite spinning component through melt metering; the exhaust ports of the melting section and the mixing section of the double-screw extruder are connected with a vacuumizing device to control the vacuum degree to be below 300Pa, and the outlet temperature of the melt pump is 275 ℃;
(2) Preparation of the skin layer material: adding a mixture of terephthalic acid and isophthalic acid (the weight ratio is 65:35) into a mixed solution of ethylene glycol and 1, 4-butanediol (the weight ratio is 80:20) according to the mol ratio of acid to alcohol of 1:1.15 to prepare uniform slurry, and then carrying out esterification reaction at 245 ℃ and polycondensation reaction at 280 ℃ by taking ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, feeding the bright copolyester pellets into a single screw extruder (the screw outlet temperature is 278 ℃), feeding the bright copolyester pellets into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component (the processing temperature of the spinning component is 280 ℃) together with the core layer material in the step (1) according to the mass percentage ratio of the sheath layer to the core layer of 20:80, cooling, oiling, drawing by a hot roller, and winding the fiber filaments into FDY (the spinning winding speed is 4500 m/min), wherein the specification is 83dtex/72F.
Table 1 shows the results of comparison of the properties of the composite fibers prepared in examples and comparative examples.
TABLE 1
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the invention.
Claims (8)
1. A high-brightness composite noctilucent fiber is characterized in that: the composite noctilucent fiber is of a sheath-core composite structure, wherein a middle skin layer of the fiber section is round, and a core layer is in a sixteen-pointed star shape; the core layer accounts for 75-88% and the skin layer accounts for 12-25% in percentage by mass, and the sum of the core layer and the skin layer is 100%;
wherein the core layer is prepared from the following raw materials in parts by weight:
60-76 parts by weight of PBT powder;
15-31 parts of PET powder;
4-9 parts of noctilucent powder;
0.2-0.8 parts by weight of functional auxiliary agent;
the cortex is prepared by using dibasic acid and dihydric alcohol as raw materials and granulating bright copolyester obtained by esterification and copolymerization;
the noctilucent powder is SrAl 2 O 4 :Eu 2+ ,Dy 3+ The rare earth aluminate luminescent material has an average particle size of 2-7 microns and a highest particle size of 10 microns;
the preparation method of the functional auxiliary agent comprises the following steps:
(1) Taking 4g of vacuum dried nano silicon dioxide, adding 200mL of anhydrous toluene, carrying out ultrasonic treatment for 30min, then adding 1.8mL of N-2-aminoethyl-3-aminopropyl triethoxysilane, and reacting at 60 ℃ for 24h; filtering after the reaction is finished, washing a filter cake with anhydrous toluene and absolute ethanol for a plurality of times, vacuum drying the filter cake to constant weight at 80 ℃, and grinding the filter cake into powder to obtain the SiO modified by the surface silane 2 ；
(2) Accurately weighing 4g of 3, 5-di-tert-butyl-4-hydroxy benzene propionic acid, dissolving in 200mL of anhydrous dichloromethane, slowly dropwise adding 2.6mL of distilled thionyl chloride and 0.1mL of N, N-dimethylformamide by using a constant pressure dropping funnel, and stirring and refluxing for 4 hours at 30 ℃ under the protection of nitrogen; removing solvent dichloromethane and unreacted thionyl chloride from the obtained reaction liquid by rotary evaporation to obtain solid acyl chloride;
(3) Taking 4g of the surface silane modified SiO prepared in the step (1) 2 Dissolving in 200mL of anhydrous toluene, performing ultrasonic treatment for 30 minutes, slowly dripping the solid acyl chloride prepared in the step 3) after dissolving in 200mL of anhydrous toluene, slowly dripping 4.00mL of triethylamine, and reacting at 60 ℃ under the protection of nitrogen20h; and after the reaction is finished, carrying out suction filtration, washing a filter cake for a plurality of times by using anhydrous toluene and absolute ethyl alcohol, and finally, drying the product in a vacuum drying oven at 80 ℃ to constant weight to obtain the functional auxiliary agent.
2. The high brightness composite luminescent fiber of claim 1, wherein: the PBT powder is fiber-grade semi-degerming type, the intrinsic viscosity of the PBT powder is 1.0+/-0.012 dl/g, and the titanium dioxide content is 1.0%; the PET powder is bottle grade, and the intrinsic viscosity of the PET powder is 0.60+/-0.010 dl/g; the particle sizes of the PBT powder and the PET powder are less than or equal to 38 microns.
3. The high brightness composite luminescent fiber of claim 1, wherein: the dibasic acid is a mixture of terephthalic acid and isophthalic acid, and the weight ratio of the terephthalic acid to the isophthalic acid is 60:40-80:20; the dihydric alcohol is a mixture of ethylene glycol and 1, 4-butanediol, and the weight ratio of the ethylene glycol to the 1, 4-butanediol is 70:30-85:15.
4. A high brightness composite luminescent fiber as claimed in claim 1, wherein: the melting point of the bright copolyester pellets is 225-240 ℃.
5. A high brightness composite luminescent fiber as claimed in claim 1, wherein: the single fiber fineness of the composite noctilucent fiber is 1 dtex-7 dtex, the fiber strength is more than or equal to 3.3 cN/dtex, and the initial brightness value is more than or equal to 650 mcd/m 2 。
6. A method for preparing the high-brightness composite luminous fiber as claimed in claim 1, wherein: the method comprises the following steps:
(1) Preparation of core layer material: simultaneously adding PBT powder, PET powder, noctilucent powder and functional additives in a metering ratio into a double-screw extruder on line, melting, mixing and homogenizing to fully mix, extruding by a melt pump, and metering and pumping into a composite spinning component by the melt;
(2) Preparation of the skin layer material: preparing binary acid and dihydric alcohol into uniform slurry according to the acid/alcohol molar ratio of 1:1.15, and then carrying out esterification and polycondensation reaction by using ethylene glycol antimony as a catalyst until the polymer viscosity value reaches 0.68dl/g, and discharging under vacuum to obtain bright copolyester pellets;
(3) Spinning: drying the obtained bright copolyester pellets until the water content is below 30ppm, then sending the bright copolyester pellets into a single screw extruder, sending the single screw extruder into a composite spinning component through a melt metering pump, forming fiber filaments with a sheath-core structure through the composite spinning component together with the core layer material in the step (1), and then cooling, oiling, hot roller drafting and winding the obtained fiber filaments into FDY.
7. The method for preparing the high-brightness composite luminous fiber as claimed in claim 6, wherein the method comprises the following steps: and (2) connecting the melting section and the exhaust port of the mixing section of the double-screw extruder used in the step (1) with a vacuum pumping device so as to control the vacuum degree to be below 300Pa, wherein the outlet temperature of a melt pump of the double-screw extruder is 270-275 ℃.
8. The method for preparing the high-brightness composite luminous fiber as claimed in claim 6, wherein the method comprises the following steps: the screw outlet temperature of the single screw extruder used in the step (3) is 272-278 ℃, the spinning temperature of the composite spinning component is 275-280 ℃, and the spinning winding speed is 4000-4800 m/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210917638.6A CN115233334B (en) | 2022-08-01 | 2022-08-01 | High-brightness composite noctilucent fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210917638.6A CN115233334B (en) | 2022-08-01 | 2022-08-01 | High-brightness composite noctilucent fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115233334A CN115233334A (en) | 2022-10-25 |
| CN115233334B true CN115233334B (en) | 2024-02-23 |
Family
ID=83677148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210917638.6A Active CN115233334B (en) | 2022-08-01 | 2022-08-01 | High-brightness composite noctilucent fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115233334B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349007A (en) * | 2000-10-13 | 2002-05-15 | 三菱丽阳株式会社 | High luminosity luminous fiber, its prepn. method, and the braided fabric therewith |
| CN103882556A (en) * | 2014-03-18 | 2014-06-25 | 闽江学院 | Composite noctilucent fiber with skin-core structure and preparation method of composite noctilucent fiber |
| CN106480525A (en) * | 2016-10-14 | 2017-03-08 | 河南工程学院 | A kind of rare earth aluminic acid strontium long afterglow luminescent fibre of skin-core structure and preparation method thereof |
| CN108530688A (en) * | 2018-03-21 | 2018-09-14 | 浙江大学 | A kind of immobilized Hinered phenols antioxidant of nano-titanium dioxide and its application |
-
2022
- 2022-08-01 CN CN202210917638.6A patent/CN115233334B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349007A (en) * | 2000-10-13 | 2002-05-15 | 三菱丽阳株式会社 | High luminosity luminous fiber, its prepn. method, and the braided fabric therewith |
| CN103882556A (en) * | 2014-03-18 | 2014-06-25 | 闽江学院 | Composite noctilucent fiber with skin-core structure and preparation method of composite noctilucent fiber |
| CN106480525A (en) * | 2016-10-14 | 2017-03-08 | 河南工程学院 | A kind of rare earth aluminic acid strontium long afterglow luminescent fibre of skin-core structure and preparation method thereof |
| CN108530688A (en) * | 2018-03-21 | 2018-09-14 | 浙江大学 | A kind of immobilized Hinered phenols antioxidant of nano-titanium dioxide and its application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115233334A (en) | 2022-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101597816B (en) | Method for preparing colorized fire-retardant delustering hollow polyester filament | |
| CN101238817B (en) | Bacteriostat, far-infrared ray emitting agent, mother particle, fiber and manufacturing method thereof | |
| CN102251308B (en) | Method for preparing colored light-extinction polyester filament | |
| CN106676664B (en) | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre | |
| CN100350084C (en) | High-speed blended fiber-spinning process of nano composite antibacterial dacron POY | |
| CN105908283A (en) | Semidull POY polyester fiber and processing method thereof | |
| CN110938881B (en) | Production process of recyclable degradable fiber | |
| CN111155196A (en) | Luminescent fiber based on recycled polyester material and preparation method thereof | |
| CN102330188A (en) | Method for preparing nano silicon dioxide modified polyester fibers | |
| CN115233334B (en) | High-brightness composite noctilucent fiber and preparation method thereof | |
| CN115028968A (en) | Antibacterial functional master batch, preparation method thereof, antibacterial polyester fiber and fabric | |
| CN1027982C (en) | Preparing process of fine denier and ultra-fine denier polypropylene fibre P | |
| CN102345179A (en) | Preparation method of nano zinc oxide modified polyester fiber | |
| CN1328177A (en) | Ultraviolet fluorescent fibre | |
| CN104451936B (en) | Optical obscurations hydrophilic fibers and preparation method thereof | |
| CN1053714C (en) | Far infrared fiber with good spinning property and its manufacture | |
| CN102797069A (en) | Method for preparing nano titanium dioxide modified polyester fibers | |
| CN110952155B (en) | Production process of cyclic regeneration antistatic fiber | |
| CN1164803C (en) | High luminosity luminous fiber, its prepn. method, and the braided fabric therewith | |
| CN111041585A (en) | Water-repellent polyester functional master batch and preparation method thereof | |
| CN1570226A (en) | Core-skin light storage fabric, method for manufacturing same and use thereof | |
| CN102330189A (en) | Preparation method of nano-tin dioxide modified polyester fiber | |
| CN115262030B (en) | Flame-retardant noctilucent fiber and preparation method thereof | |
| CN104264241B (en) | A kind of method of high degree of profile glossy polyester polyster fibre | |
| CN102345181A (en) | Preparation method of adipic acid modified polyester fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |