CN111364122A - Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof - Google Patents

Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof Download PDF

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Publication number
CN111364122A
CN111364122A CN202010192840.8A CN202010192840A CN111364122A CN 111364122 A CN111364122 A CN 111364122A CN 202010192840 A CN202010192840 A CN 202010192840A CN 111364122 A CN111364122 A CN 111364122A
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pbt
modified
silicon dioxide
nano silicon
parts
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毛佳枫
周克含
蒋进生
李永军
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Zhejiang Hengyuan Chemical Fiber Group Co ltd
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Zhejiang Hengyuan Chemical Fiber Group Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06Washing or drying
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/096Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a porous PBT fiber POY (polyester Pre-oriented yarn) and a preparation method thereof, wherein the porous PBT fiber POY is made of modified PBT polyester, and the modified PBT polyester comprises the following raw materials in parts by weight: 15-20 parts of PBT resin, 5-8 parts of PTFE resin, 0.3-0.8 part of compatibilizer and 3-6 parts of modified nano silicon dioxide, wherein the preparation method of the modified nano silicon dioxide comprises the following steps: 1) dispersing 10 parts of nano silicon dioxide in 40-50 parts of solvent according to the mass parts to obtain nano silicon dioxide dispersion liquid; 2) introducing inert gas into the reaction container for 20-30 min, transferring the nano silicon dioxide dispersion liquid into the reaction container, then adding 1-3 parts of modifier, and reacting for 12-24 h at 25-35 ℃; 3) and after the reaction is finished, removing the redundant solvent, taking out the product in the reaction container, washing the product for 3-5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide. The porous PBT fiber POY yarn prepared by the invention has excellent waterproof and breathable performances.

Description

Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof
Technical Field
The invention relates to the technical field of PBT fibers, in particular to a porous PBT fiber POY (polyester pre-oriented yarn) and a preparation method thereof.
Background
Polyethylene terephthalate fiber, PBT fiber for short, is a fiber prepared by melt spinning of linear polymer which is obtained by esterification and polycondensation of high-purity terephthalic acid or dimethyl terephthalate and 1, 4-butanediol, and belongs to one of polyester fibers. The molecular structure of PBT fiber has not only aromatic ring same as polyester, but also longer methine chain segment same as nylon, so it has both the softness and rubbing resistance of nylon and the excellent mechanical performance of terylene, and its colorability and dyeability are superior to nylon and terylene, and it can use disperse dye to directly carry out ordinary pressure boiling dyeing without carrier. The PBT fiber has the greatest characteristic of good rebound resilience and good curling elasticity, so that the PBT fiber is mainly used for processing elastic textiles such as various sports wear, ski shirts, panty-hose, swimwear, medical bandages and the like.
Along with the progress of society, the living standard of people is improved, and the functional demand on the PBT fiber is higher and higher, so the modification of the PBT fiber is more important, and the purpose of the PBT fiber modification is to optimize the performance of the PBT fiber and mainly endow the PBT fiber with some new properties by a modification means, such as: antistatic, antibacterial, waterproof, breathable, flame retardant, and the like.
Because the PBT fiber is mainly used for processing various sports wear, the PBT fiber is required to have excellent waterproof and air-permeable properties to meet the use requirements of consumers.
Disclosure of Invention
Aiming at the defects in the prior art, one of the purposes of the invention is to provide a porous PBT fiber POY yarn which has excellent waterproof and air-permeable performances; the second purpose of the invention is to provide a preparation method of the porous PBT fiber POY, which has simple preparation process, and the prepared POY has uniform fineness and strength.
The above object of the present invention is achieved by the following technical solutions: the porous PBT fiber POY yarn is made of modified PBT polyester, and the modified PBT polyester comprises the following raw materials in parts by weight: 15-20 parts of PBT resin, 5-8 parts of PTFE resin, 0.3-0.8 part of compatibilizer and 3-6 parts of modified nano silicon dioxide, wherein the preparation method of the modified nano silicon dioxide comprises the following steps: 1) dispersing 10 parts of nano silicon dioxide in 40-50 parts of solvent according to the mass parts to obtain nano silicon dioxide dispersion liquid; 2) continuously introducing inert gas into the reaction container for 20-30 min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of the inert gas, then adding 1-3 parts of a modifier, and reacting for 12-24 h at 25-35 ℃, wherein the modifier is one of perfluorooctyltrichlorosilane, perfluorooctyltrimethoxysilane and perfluorooctyltriethoxysilane; 3) and after the reaction is finished, removing the redundant solvent, taking out the product in the reaction container, washing the product for 3-5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
By adopting the technical scheme, the molecular structure of the PTFE resin is a layered crystal structure formed by combining Van der Waals force, the molecules are easy to release and slide, and meanwhile, the PTFE resin has lower cohesive force and low adhesion force, so that the PTFE resin has good self-lubricating property and is beneficial to modified PBT polyester spinning; in addition, the PTFE resin has low surface energy and good water resistance.
A large number of silicon hydroxyl groups which belong to hydrophilic groups exist on the surface of the silicon dioxide, and a monomolecular layer of fluoroalkyl is formed on the surface of the silicon dioxide after the silicon dioxide is modified by a modifier, so that the surface of the silicon dioxide is changed from hydrophilicity to hydrophobicity; in addition, the fluorine-containing chain segment is introduced into the surface of the modified nano silicon dioxide, so that the surface tension of the modified nano silicon dioxide can be reduced, and the roughness of the surface of the modified nano silicon dioxide can be increased, thereby increasing the waterproof performance. The PBT fiber POY yarn obtained after the modified PBT polyester spinning has a porous structure, and the porous structure can increase the air permeability and the moisture permeability of the fiber, so that the fabric prepared by using the porous PBT fiber POY yarn has excellent waterproof performance and air permeability and moisture permeability, and is suitable for being processed into sports wear.
The present invention in a preferred example may be further configured to: the preparation method of the modified PBT polyester comprises the following steps: 1) melting and blending PBT resin and PTFE resin at 235-250 ℃ to obtain molten liquid; 2) adding the modified nano-silica into the molten liquid, and stirring for 10-30 min to uniformly disperse the modified nano-silica in the molten liquid to obtain a blended liquid; 3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
By adopting the technical scheme, the surface of the modified nano silicon dioxide is changed from hydrophilicity to hydrophobicity, and the modified nano silicon dioxide can be uniformly dispersed in molten liquid of PBT resin and PTFE resin, so that the waterproof performance of the modified PBT polyester is improved.
The present invention in a preferred example may be further configured to: the compatibilizer is EVA-g-MAH.
By adopting the technical scheme, the ethylene-vinyl acetate grafted maleic anhydride is used as the compatibilizer, so that the acting force between two phase interfaces can be reduced, the compatibility between the PBT resin and the PTFE resin is improved, and the performance of the porous PBT fiber POY is uniform.
The present invention in a preferred example may be further configured to: the solvent is absolute ethyl alcohol or toluene.
By adopting the technical scheme, the modifier is easy to decompose when meeting water, and the modifier can be prevented from contacting water in the reaction process by using absolute ethyl alcohol or toluene, so that the modification effect of the nano silicon dioxide is not influenced.
The present invention in a preferred example may be further configured to: the inert gas is nitrogen.
By adopting the technical scheme, the nitrogen is low in price, and the nitrogen is used as the protective gas, so that the air in the reaction container can be removed, and the modification effect of the nano silicon dioxide is improved.
The present invention in a preferred example may be further configured to: the modified PBT polyester also comprises 1-3 parts of graphene.
By adopting the technical scheme, the graphene is stable in chemical property, the surface of the graphene contains rich oxygen-containing functional groups, the hydrophilicity is good, and the porosity of the porous PBT fiber POY can be increased by adding the graphene, so that the moisture permeability of the porous PBT fiber POY is increased, and the comfort of the fabric prepared from the porous PBT fiber POY is improved.
The present invention in a preferred example may be further configured to: the preparation method of the modified PBT polyester comprises the following steps: 1) melting and blending PBT resin and PTFE resin at 235-250 ℃ to obtain molten liquid; 2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 10-30 min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid; 3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
By adopting the technical scheme, after the graphene is added, the prepared modified PBT polyester is spun, and the prepared porous PBT fiber POY has more excellent moisture permeability.
The second aim of the invention is realized by the following technical scheme: a preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 100-120 ℃ for 3-5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at the spinning temperature of 265-280 ℃ at the spinning speed of 2800-3000 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 20-25 ℃, and the air speed is 0.4-0.7 m/s;
step 4, bundling and oiling: the oiling rate is 0.4wt% -1.2 wt%;
step 5, winding and forming: the winding speed is 2800-3000 m/min;
and 6, checking and warehousing.
By adopting the technical scheme, the modified PBT polyester is dried, so that the moisture content of the modified PBT polyester is reduced, and the spinnability is improved; the spinning speed is controlled to be 2800-3000 m/min, because more methylene exists in the PBT macromolecular structure, intermolecular force is weakened, crystallization is easy to occur, and the spinning speed is too high, so that the internal stress of the PBT fiber is increased, the elasticity is reduced, and the elasticity of the fabric made of the PBT fiber is influenced; spinning speeds below 2800m/min result in low efficiency; the porous PBT fiber POY yarn obtained after spinning can be rapidly shaped after cooling, and oiling aims to improve the antistatic and friction-resistant performances of the fiber surface, so that the requirements of production and post-processing are met.
In summary, the invention includes at least one of the following beneficial technical effects:
1. a large number of silicon hydroxyl groups which belong to hydrophilic groups exist on the surface of the silicon dioxide, and a monomolecular layer of fluoroalkyl is formed on the surface of the silicon dioxide after the silicon dioxide is modified by a modifier, so that the surface of the silicon dioxide is changed from hydrophilicity to hydrophobicity; in addition, the fluorine-containing chain segment is introduced into the surface of the modified nano silicon dioxide, so that the surface tension of the modified nano silicon dioxide can be reduced, and the roughness of the surface of the modified nano silicon dioxide can be increased, thereby increasing the waterproof performance. The PBT fiber POY yarn obtained after the modified PBT polyester spinning has a porous structure, and the porous structure can increase the air permeability and the moisture permeability of the fiber, so that the fabric prepared by using the porous PBT fiber POY yarn has excellent waterproof performance and air permeability and moisture permeability, and is suitable for being processed into sportswear;
2. the graphene is stable in chemical property, contains rich oxygen-containing functional groups on the surface, is good in hydrophilic property, and can increase the porosity of the porous PBT fiber POY, so that the moisture permeability of the porous PBT fiber POY is increased, and the comfort of a fabric prepared from the porous PBT fiber POY is improved;
3. the modified PBT polyester is dried, so that the moisture content of the modified PBT polyester is reduced, and the spinnability is improved; the spinning speed is controlled to be 2800-3000 m/min, because more methylene exists in the PBT macromolecular structure, intermolecular force is weakened, crystallization is easy to occur, and the spinning speed is too high, so that the internal stress of the PBT fiber is increased, the elasticity is reduced, and the elasticity of the fabric made of the PBT fiber is influenced; spinning speeds below 2800m/min result in low efficiency; the porous PBT fiber POY yarn obtained after spinning can be rapidly shaped after cooling, and oiling aims to improve the antistatic and friction-resistant performances of the fiber surface, so that the requirements of production and post-processing are met.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
The porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 15kg of PBT resin, 5kg of PTFE resin, 0.3kg of EVA-g-MAH and 3kg of modified nano silicon dioxide.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 40kg of toluene to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction vessel for 20min, transferring the nano silicon dioxide dispersion liquid into the reaction vessel under the protection of nitrogen atmosphere, then adding 1kg of perfluorooctyl trichlorosilane, and reacting for 24h at 25 ℃;
3) and after the reaction is finished, removing redundant toluene, taking out a product in the reaction container, washing for 3 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 235 ℃ to obtain molten liquid;
2) adding the modified nano-silica into the molten liquid, and stirring for 30min to uniformly disperse the modified nano-silica in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 100 ℃ for 5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at the spinning temperature of 265 ℃ at the spinning speed of 3000 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 25 ℃, and the air speed is 0.4 m/s;
step 4, bundling and oiling: the oiling rate is 0.4 wt%;
step 5, winding and forming: the winding speed is 3000 m/min;
and 6, checking and warehousing.
Example 2
A porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 18kg of PBT resin, 6kg of PTFE resin, 0.6kg of EVA-g-MAH and 4kg of modified nano silicon dioxide.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 40kg of absolute ethyl alcohol to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction container for 30min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of nitrogen atmosphere, then adding 1kg of perfluorooctyl trimethoxysilane, and reacting for 24h at 25 ℃;
3) and after the reaction is finished, removing redundant absolute ethyl alcohol, taking out a product in the reaction container, washing the product for 4 times by using the absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 240 ℃ to obtain molten liquid;
2) adding the modified nano-silica into the molten liquid, and stirring for 20min to uniformly disperse the modified nano-silica in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 120 ℃ for 3 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 280 ℃ and 3000 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 20 ℃, and the air speed is 0.5 m/s;
step 4, bundling and oiling: the oiling rate is 0.5 wt%;
step 5, winding and forming: the winding speed is 3000 m/min;
and 6, checking and warehousing.
Example 3
A porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 20kg of PBT resin, 7kg of PTFE resin, 0.8kg of EVA-g-MAH and 5kg of modified nano silicon dioxide.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 50kg of toluene to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction container for 30min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of nitrogen atmosphere, then adding 1kg of perfluorooctyl triethoxysilane, and reacting for 12h at 35 ℃;
3) and after the reaction is finished, removing redundant toluene, taking out a product in the reaction container, washing the product for 5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 250 ℃ to obtain molten liquid;
2) adding the modified nano-silica into the molten liquid, and stirring for 20min to uniformly disperse the modified nano-silica in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 120 ℃ for 5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 275 ℃ and 2800 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 23 ℃, and the air speed is 0.7 m/s;
step 4, bundling and oiling: the oiling rate is 1.2 wt%;
step 5, winding and forming: the winding rate is 2800 m/min;
and 6, checking and warehousing.
Example 4
The porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 17kg of PBT resin, 8kg of PTFE resin, 0.4kg of EVA-g-MAH, 6kg of modified nano silicon dioxide and 1kg of graphene.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 50kg of absolute ethyl alcohol to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction vessel for 25min, transferring the nano silicon dioxide dispersion liquid into the reaction vessel under the protection of nitrogen atmosphere, then adding 2kg of perfluorooctyl trichlorosilane, and reacting for 24h at 30 ℃;
3) and after the reaction is finished, removing redundant absolute ethyl alcohol, taking out a product in the reaction container, washing for 5 times by using the absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 250 ℃ to obtain molten liquid;
2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 20min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 100-120 ℃ for 3-5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 275 ℃ and 2900 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 20 ℃, and the air speed is 0.6 m/s;
step 4, bundling and oiling: the oiling rate is 0.8 wt%;
step 5, winding and forming: the winding speed was 2900 m/min;
and 6, checking and warehousing.
Example 5
The porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 16kg of PBT resin, 5.5kg of PTFE resin, 0.5kg of EVA-g-MAH, 3.5kg of modified nano silicon dioxide and 2kg of graphene.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 45kg of toluene to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction container for 25min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of nitrogen atmosphere, then adding 2kg of perfluorooctyl trimethoxysilane, and reacting for 12h at 30 ℃;
3) and after the reaction is finished, removing redundant toluene, taking out a product in the reaction container, washing the product for 4 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 245 ℃ to obtain molten liquid;
2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 30min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 110 ℃ for 4 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 270 ℃ at a spinning speed of 2850 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 22 ℃, and the air speed is 0.4/s;
step 4, bundling and oiling: the oiling rate is 1 wt%;
step 5, winding and forming: the winding speed is 2850 m/min;
and 6, checking and warehousing.
Example 6
A porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 17kg of PBT resin, 7.5kg of PTFE resin, 0.7kg of EVA-g-MAH, 5.5kg of modified nano silicon dioxide and 3kg of graphene.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 50kg of toluene to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction container for 30min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of a nitrogen atmosphere, then adding 3kg of perfluorooctyl trichlorosilane, and reacting for 12h at 25 ℃;
3) and after the reaction is finished, removing redundant toluene, taking out a product in the reaction container, washing the product for 5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 240 ℃ to obtain molten liquid;
2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 25min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 115 ℃ for 4 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 275 ℃ and at 2950 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 25 ℃, and the air speed is 0.4 m/s;
step 4, bundling and oiling: the oiling rate is 0.6 wt%;
step 5, winding and forming: the winding speed is 2950 m/min;
and 6, checking and warehousing.
Example 7
A porous PBT fiber POY yarn is made of modified PBT polyester, wherein the modified PBT polyester comprises 17.8kg of PBT resin, 6.5kg of PTFE resin, 0.6kg of EVA-g-MAH, 4.8kg of modified nano silicon dioxide and 2.1kg of graphene.
The preparation method of the modified nano silicon dioxide comprises the following steps:
1) dispersing 10kg of nano silicon dioxide in 50kg of toluene to obtain nano silicon dioxide dispersion liquid;
2) continuously introducing nitrogen into the reaction vessel for 30min, transferring the nano silicon dioxide dispersion liquid into the reaction vessel under the protection of nitrogen atmosphere, then adding 2.2kg of perfluorooctyltriethoxysilane, and reacting for 20h at 30 ℃;
3) and after the reaction is finished, removing redundant toluene, taking out a product in the reaction container, washing the product for 5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
The preparation method of the modified PBT polyester comprises the following steps:
1) PBT resin and PTFE resin are melted and blended at 245 ℃ to obtain molten liquid;
2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 20min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid;
3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
A preparation method of porous PBT fiber POY yarns specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 110 ℃ for 3.5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at 270 ℃ and 2900 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 22 ℃, and the air speed is 0.5 m/s;
step 4, bundling and oiling: the oiling rate is 0.55 wt%;
step 5, winding and forming: the winding speed was 2900 m/min;
and 6, checking and warehousing.
Example 8
A porous PBT fiber POY yarn is different from the yarn in example 7 in that the modified nano-silica is 4.5kg, and the yarn is the same as that in example 7.
Example 9
The porous PBT fiber POY yarn is different from the example 7 in that the modified nano-silica is 5.5kg, and the rest is the same as the example 7.
Comparative example 1
A porous PBT fiber POY filament, which differs from example 7 in that the modified nano-silica is replaced with nano-silica.
Comparative example 2
A porous PBT fiber POY yarn is different from the yarn in example 7 in that modified nano silica is not added.
Comparative example 3
A porous PBT fiber POY yarn is different from the yarn in example 7 in that no compatibilizer EVA-g-MAH is added.
Performance detection
The porous PBT fiber POY yarns prepared in examples 1 to 9 and comparative examples 1 to 3 were spun into yarns and then woven into grey cloth, and the following performance tests were performed:
contact angle test: an optical contact angle measuring instrument is used for testing the interface wetting performance of grey cloth of the examples and the comparative examples, distilled water is used as a liquid medium, the volume of dropwise added liquid drops is 5 mu L, and the static contact angle of the grey cloth is tested;
and (3) testing hydrostatic pressure: the hydrostatic pressure of the grey cloth is tested according to AATCC127-2003 hydrostatic test for water resistance, the pressure increasing rate is 6Kpa/min, and the test area is 100cm2
Air permeability: according to GB/T5453-1997 determination of textile fabric air permeability, an air permeability tester is used for determining the air permeability of the grey cloth, the test area is 20cm2, and the pressure drop is 100 Pa;
moisture permeability: with reference to GB/T12704.1-2009 section 1 of textile fabric moisture permeability test method: wet absorption method "tests the moisture permeability of the sample.
Table 1 shows the results of the performance tests
Figure BDA0002416541960000101
The performance test results of the embodiments 7 to 9 show that the waterproof property and the air and moisture permeability are improved with the increase of the modified nano-silica, but the improvement of the performances gradually becomes gentle with the continuous increase of the addition amount of the modified nano-silica. According to the embodiment 7 and the comparative examples 1 and 2, the modified nano-silica can increase the waterproof, air-permeable and moisture-permeable performances of the porous PBT fiber POY, and the unmodified nano-silica has poor waterproof, air-permeable and moisture-permeable performances due to the hydrophilic surface and agglomeration in the polyester melt mixed solution. The compatibilizer is added, so that the interfacial compatibility of the PBT resin and the PTFE resin can be further improved, and the performance of the modified PBT polyester is improved.
The present embodiment is only for explaining the present invention, and not for limiting the present invention, and those skilled in the art can make modifications without inventive contribution to the present embodiment as needed after reading the present specification, but all of which are protected by patent law within the scope of the claims of the present invention.

Claims (8)

1. A porous PBT fiber POY yarn is characterized in that: the porous PBT fiber POY yarn is made of modified PBT polyester, and the modified PBT polyester comprises the following raw materials in parts by weight: 15-20 parts of PBT resin, 5-8 parts of PTFE resin, 0.3-0.8 part of compatibilizer and 3-6 parts of modified nano silicon dioxide, wherein the preparation method of the modified nano silicon dioxide comprises the following steps: 1) dispersing 10 parts of nano silicon dioxide in 40-50 parts of solvent according to the mass parts to obtain nano silicon dioxide dispersion liquid; 2) continuously introducing inert gas into the reaction container for 20-30 min, transferring the nano silicon dioxide dispersion liquid into the reaction container under the protection of the inert gas, then adding 1-3 parts of a modifier, and reacting for 12-24 h at 25-35 ℃, wherein the modifier is one of perfluorooctyltrichlorosilane, perfluorooctyltrimethoxysilane and perfluorooctyltriethoxysilane; 3) and after the reaction is finished, removing the redundant solvent, taking out the product in the reaction container, washing the product for 3-5 times by using absolute ethyl alcohol, and drying to obtain the modified nano silicon dioxide.
2. The porous PBT fiber POY yarn of claim 1, wherein: the preparation method of the modified PBT polyester comprises the following steps: 1) melting and blending PBT resin and PTFE resin at 235-250 ℃ to obtain molten liquid; 2) adding the modified nano-silica into the molten liquid, and stirring for 10-30 min to uniformly disperse the modified nano-silica in the molten liquid to obtain a blended liquid; 3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
3. The porous PBT fiber POY yarn of claim 1, wherein: the compatibilizer is EVA-g-MAH.
4. The porous PBT fiber POY yarn of claim 1, wherein: the solvent is absolute ethyl alcohol or toluene.
5. The porous PBT fiber POY yarn of claim 1, wherein: the inert gas is nitrogen.
6. The porous PBT fiber POY yarn according to claim 2, wherein: the modified PBT polyester also comprises 1-3 parts of graphene.
7. The porous PBT fiber POY yarn according to claim 6, wherein: the preparation method of the modified PBT polyester comprises the following steps: 1) melting and blending PBT resin and PTFE resin at 235-250 ℃ to obtain molten liquid; 2) adding the modified nano-silica and the graphene into the molten liquid, and stirring for 10-30 min to uniformly disperse the modified nano-silica and the graphene in the molten liquid to obtain a blended liquid; 3) and extruding and slicing the blending liquid to obtain the modified PBT polyester.
8. The preparation method of the porous PBT fiber POY yarn according to any one of claims 1 to 7, wherein the preparation method comprises the following steps: the method specifically comprises the following steps:
step 1, drying: drying the modified PBT polyester at 100-120 ℃ for 3-5 h;
step 2, melt spinning: adding the dried modified PBT polyester into a screw extruder for melting, and then spinning at the spinning temperature of 265-280 ℃ at the spinning speed of 2800-3000 m/min;
and 3, cooling: cooling after spinning, wherein the cooling air temperature is 20-25 ℃, and the air speed is 0.4-0.7 m/s;
step 4, bundling and oiling: the oiling rate is 0.4wt% -1.2 wt%;
step 5, winding and forming: the winding speed is 2800-3000 m/min;
and 6, checking and warehousing.
CN202010192840.8A 2020-03-18 2020-03-18 Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof Pending CN111364122A (en)

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