CN111945248A - Anti-ultraviolet composite DTY fiber and preparation method thereof - Google Patents
Anti-ultraviolet composite DTY fiber and preparation method thereof Download PDFInfo
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- 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
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- 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
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
- C08G63/54—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation the acids or hydroxy compounds containing carbocyclic rings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
- C08G63/6854—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6856—Dicarboxylic acids and dihydroxy compounds
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- 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
- D01D5/08—Melt spinning methods
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- 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
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- 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
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- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
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- 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
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/352—Heterocyclic compounds having five-membered heterocyclic rings
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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Abstract
The application relates to the technical field of chemical fibers, and particularly discloses an anti-ultraviolet composite DTY fiber and a preparation method thereof, wherein the anti-ultraviolet composite DTY fiber comprises 10-12 parts by weight of polyester component, 5-8 parts by weight of polyacrylonitrile component and 0.5-1.5 parts by weight of anti-ultraviolet surface treating agent; the polyester component is prepared from 7-10 parts of terephthalic acid, 2-3 parts of vinyl terephthalic acid, 10-15 parts of ethylene glycol, 1-2 parts of ultraviolet resistant copolymerization additive and 0.5-1.3 parts of ultraviolet resistant particles; the uvioresistant particles are at least one of titanium dioxide and zinc oxide. When the uvioresistant composite DTY fiber is prepared, the vinyl terephthalic acid and the terephthalic acid are mixed in ethylene glycol to prepare uniform slurry, the uniform slurry is mixed with the uvioresistant copolymerization additive and the uvioresistant particles and heated to obtain a polyester component, the polyester component and the polyacrylonitrile component are prepared into composite fibers, the uvioresistant surface treating agent is attached to the surfaces of the composite fibers, and finally the uvioresistant composite DTY fiber is obtained through loading, hot stretching and stress relief. The uvioresistant composite DTY fiber has better uvioresistant performance.
Description
Technical Field
The application relates to the technical field of chemical fibers, in particular to an ultraviolet-resistant composite DTY fiber and a preparation method thereof.
Background
DTY fiber is widely used in textile production as a fiber material, and has the advantages of high bulkiness, good heat insulation, high breaking strength, high elastic modulus and the like. The conventional DTY fiber is generally prepared by stretching PET fiber on an elasticizer continuously or simultaneously and then performing texturing processing on the PET fiber by a false twister. The fabric made of the DTY fibers has the characteristics of good elasticity, difficult deformation, stiffness, smoothness and the like after shaping. In order to expand the application range of the DTY fiber, the anti-ultraviolet DTY fiber appears on the market, and has the advantages of good DTY elasticity and difficult deformation while resisting ultraviolet.
An uvioresistant polyester fiber and its production are disclosed in the Chinese patent application with publication number CN101377024, the polyester fiber contains uvioresistant nano particles which specifically include TiO2、ZnO、CeO2、SiO2、Al2O3、Fe2O3、CaCO3One or more of PbO, kaolin, talcum powder and pottery clay nano particles, wherein the content of the uvioresistant nano particles is 0.1 to 30 weight percent, and the titer of the fiber is 0.7 to 10 dtex. The uvioresistant polyester fiberThe production method comprises the following steps: adding the uvioresistant nano particles into polyester through extrusion blending or copolymerization to prepare uvioresistant polyester chips, then obtaining nascent fiber through spinning winding, and obtaining DTY through false twisting or stretching the obtained nascent fiber.
Because the polymerization unit of the DTY fiber has weak ultraviolet resistance, the ultraviolet resistance improved by adding the ultraviolet resistant particles is always limited on the premise of ensuring the performance of the fiber, thereby influencing the ultraviolet resistance of the DTY fiber.
Disclosure of Invention
Aiming at the problem of limited ultraviolet resistance in the prior art, the first object of the present application is to provide an ultraviolet resistant composite DTY fiber, which has a fiber structure with good ultraviolet resistance in addition to being capable of being better combined with ultraviolet resistant particles.
A second object of the present application is to provide a method for preparing an anti-ultraviolet composite DTY fiber, by which a polyester component in the fiber has a higher degree of polymerization, and a product has better quality, better and stable wear resistance and elasticity.
In order to achieve the first object, the following technical solutions are provided in the present application:
an anti-ultraviolet composite DTY fiber is mainly prepared from 10-12 parts of polyester component, 5-8 parts of polyacrylonitrile component and 0.5-1.5 parts of anti-ultraviolet surface treating agent by weight;
the polyester component is prepared from 7-10 parts of terephthalic acid, 2-3 parts of vinyl terephthalic acid, 10-15 parts of ethylene glycol, 1-2 parts of anti-ultraviolet copolymerization additive and 0.5-1.3 parts of anti-ultraviolet particles;
the ultraviolet resistant particles comprise at least one of titanium dioxide and zinc oxide.
By adopting the technical scheme, the composite fiber is composed of the polyester component and the polyacrylonitrile component, and the polyacrylonitrile has the cyano group, and the carbon-nitrogen triple bond in the cyano group has a strong ultraviolet absorption effect, so that the prepared polyester fiber has the advantages of good elasticity, wear resistance and the like of the polyester fiber, and also has better ultraviolet resistance. Besides, the product also uses uvioresistant copolymerization additive, uvioresistant particles and uvioresistant surface treatment agent, and the raw materials can absorb or refract ultraviolet rays through copolymerization, blending or external treatment and fiber combination, thereby further improving the uvioresistant capability.
The polyester fiber is copolymerized by terephthalic acid, vinyl terephthalic acid and ethylene glycol, as vinyl belongs to a chromophore group, the vinyl has larger absorption capacity in an ultraviolet region, and the vinyl is connected with a benzene ring, a carbon-carbon double bond of the vinyl and a large pi bond on the benzene ring can generate a conjugation effect, so that the absorption capacity of the polyester fiber on ultraviolet light is enhanced, and the obtained ultraviolet resistance is possessed by the fiber, so that the ultraviolet resistance of the fiber is more durable.
And after condensation, the vinyl group positioned on the side chain can increase the gaps among polymer molecules, so that the polymer molecules can be better and more stably combined with the ultraviolet resistant particles, more ultraviolet resistant particles can be blended, and better ultraviolet resistance is achieved.
The present application may be further configured in a preferred example to: the ultraviolet-resistant copolymerization additive comprises at least one of 3, 6-dihydroxy phthalonitrile and 4, 4' -dihydroxy benzophenone.
By adopting the technical scheme, the carbon-nitrogen triple bond in the 3, 6-dihydroxy phthalonitrile and the conjugated pi bond in the 4, 4' -dihydroxy benzophenone both have good ultraviolet absorption capacity, and hydroxyl is introduced into benzene rings of the two species and is used as a color-assisting cluster, so that the ultraviolet absorption capacity of a chromophore can be improved, and the chromophore has better ultraviolet resistance.
And when the 3, 6-dihydroxy phthalonitrile and the 4, 4 '-dihydroxy benzophenone are simultaneously added, hydrogen bonds are formed between the two, so that the binding capacity of the fiber is improved, the 3, 6-dihydroxy phthalonitrile and the 4, 4' -dihydroxy benzophenone are more stable, and the ultraviolet resistance effect of the fiber is improved.
The present application may be further configured in a preferred example to: the uvioresistant surface treating agent is 5-aminobenzotriazole.
By adopting the technical scheme, in the 5-aminobenzotriazole, pi bonds on benzene rings and nitrogen-nitrogen double bonds are conjugated, and nitrogen atoms in the nitrogen rings and amino groups on the benzene rings can also generate n-pi conjugation with the benzene rings, so that the compound has the function of a chromogenic group, and further improves the ultraviolet absorption capacity of the compound.
The present application may be further configured in a preferred example to: the uvioresistant composite DTY fiber also comprises 0.3-0.5 part of hydroquinone in parts by weight.
By adopting the technical scheme, in the copolymerization process of the polyester component, the vinyl groups are polymerized to a certain degree, so that the content of the vinyl groups is reduced, the ultraviolet resistance is influenced to a certain degree, and the hydroquinone is used as a double-bond polymerization inhibitor to prevent the polymerization of the vinyl groups.
The present application may be further configured in a preferred example to: the fiber structure of the uvioresistant composite DTY fiber is a sheath-core structure, the sheath-core structure comprises a core layer and a skin layer, the core layer is made of a polyacrylonitrile component, and the skin layer is made of a polyester component.
Through adopting above-mentioned technical scheme, the composite fiber of skin-core structure has the advantage that structural strength is even, makes composite fiber have better wholeness to the polyester component is as the cortex, can furthest remain polyester fiber wear-resisting, advantage such as high-elastic, and polyacrylonitrile component is as the sandwich layer, but the ultraviolet ray through the polyester layer is fully absorbed, makes ultraviolet absorption also more even.
In order to achieve the second objective, the present application provides the following technical solutions:
a preparation process of an anti-ultraviolet composite DTY fiber comprises the following steps:
s1: weighing the vinyl terephthalic acid, the terephthalic acid and the ethylene glycol in parts by weight, and mixing the vinyl terephthalic acid and the terephthalic acid in the ethylene glycol to prepare uniform slurry;
s2: nitrogen is used as protective gas, and the nitrogen is 2.5 to 4Kg/cm2Under the pressure of (1), the slurry is heated at the temperature of 200-220 DEG CHeating for 0.5-1 h, weighing the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles in parts by weight, mixing with the slurry, and continuously heating for 1-1.5 h at the temperature of 260-280 ℃ to obtain a polyester component;
s3: respectively putting the prepared polyester component and the polyacrylonitrile component in parts by weight into two screw extruders for heating and melting, and performing extrusion molding on melts in the two screw extruders through a composite spinneret plate to obtain nascent composite fibers;
s4: after the primary composite fiber is cooled, oiling, hot stretching and stress relieving are sequentially carried out, then the anti-ultraviolet surface treating agent is attached to the surface of the fiber, and finally the anti-ultraviolet composite DTY fiber is obtained through false twist deformation.
By adopting the technical scheme, the polyester component adopts a direct esterification method, the vinyl terephthalic acid and the terephthalic acid are mixed in the ethylene glycol, the conditions are controlled, and the direct esterification is carried out, so that the high polymer with the terephthalic acid and the vinyl terephthalic acid intermittently alternated can be prepared, and the vinyl is uniformly distributed on the long chain of the polymer. The direct polymerization method can avoid other impurities from being brought in and enables the product to have higher polymerization degree.
During copolymerization, the polyester is polymerized initially at a lower temperature to form an oligomer, then the ultraviolet-resistant copolymerization additive and the ultraviolet-resistant particles are added and are fully polymerized at a higher temperature, so that the polymerization degree of the polyester can be effectively improved by distributed polymerization, and the fiber has better elasticity and wear resistance. And the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles are added after the preliminary polymerization is finished, so that the raw materials can keep enough concentration during the preliminary polymerization, the raw materials can form oligomer more smoothly, and the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles can be fully wrapped and contacted after the oligomer is formed, so that the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles can be better matched.
The present application may be further configured in a preferred example to: hydroquinone was added to the slurry of S1 with mixing.
By adopting the technical scheme, hydroquinone is added into the slurry of S1, so that the polymerization between vinyl groups can be prevented from occurring from the initial polymerization step, and unnecessary side reactions are reduced.
The present application may be further configured in a preferred example to: in S4, the surface of the nascent fiber is attached with the uvioresistant surface treatment agent through impregnation, and the nascent fiber is subjected to ultrasonic treatment in the impregnation process, wherein the frequency of ultrasonic wave is controlled to be 20-23kHz, and the power is controlled to be 250-300W.
By adopting the technical scheme, the ultraviolet-resistant surface treating agent can be more uniformly attached to the surface of the fiber by the dipping method, and the ultrasonic treatment is adopted in the dipping process, so that the ultrasonic wave can generate fine broomed fibers on the surface of the fiber, the attachment between the ultraviolet-resistant surface treating agent and the fiber is more sufficient, and the service life of the finished product of the ultraviolet-resistant surface treating agent is prolonged.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the polymerized unit of vinyl terephthalic acid in the polyester component has uvioresistant performance, so that the polymerized fiber has uvioresistant performance. And the polyester component and the polyacrylonitrile component are adopted to prepare the composite fiber, so that the fiber has the advantages of high strength, wear resistance and the like, and simultaneously has better ultraviolet resistance.
2. In the application, 3, 6-dihydroxy phthalonitrile and 4, 4' -dihydroxy benzophenone are used as the ultraviolet-resistant copolymerization additive, 5-aminobenzotriazole is used as the ultraviolet-resistant surface treating agent, and the ultraviolet-resistant additive and the ultraviolet-resistant surface treating agent are matched with each other, so that the obtained fiber has a better ultraviolet absorption effect.
3. The skin-core structure is preferably adopted in the application, so that the fiber has better integrity, the respective advantages of the polyester component and the polyacrylonitrile component are better represented, and the fiber has uvioresistant performance and better elasticity and wear resistance.
4. The method adopts a step-by-step polymerization method, and the adding time of the ultraviolet-resistant copolymerization additive, the ultraviolet-resistant particles and the ultraviolet-resistant surface treating agent is different, so that the polyester has higher polymerization degree, various additives can be better combined, and the prepared product has better ultraviolet-resistant effect.
5. The raw materials of the fiber also contain hydroquinone, and the hydroquinone can effectively reduce side reaction polymerization generated between vinyl groups and improve polymerization degree, thereby improving the elasticity and wear resistance of the fiber.
6. The ultraviolet-resistant surface treatment agent is preferably attached by adopting an impregnation method, and ultrasonic treatment is adopted in the impregnation process, so that the ultraviolet-resistant surface treatment agent and the fibers are better combined.
Detailed Description
Examples
Example 1: an anti-ultraviolet composite DTY fiber is prepared from the raw materials with corresponding mass shown in Table 1;
wherein the polyacrylonitrile component is polyacrylonitrile master batch slices;
the uvioresistant particles are mixed particles formed by mixing 0.5kg of titanium dioxide and 0.5kg of zinc oxide;
the ultraviolet resistant copolymerization additive is specifically benzophenone, and the ultraviolet resistant surface treating agent is specifically benzotriazole.
The uvioresistant composite DTY fiber is prepared by the following process:
s1: weighing terephthalic acid, vinyl terephthalic acid and ethylene glycol according to the mass, and mixing the vinyl terephthalic acid and the terephthalic acid in the ethylene glycol to prepare uniform slurry;
s2: nitrogen is used as protective gas and is at 3Kg/cm2Heating the slurry at 200 ℃ for 0.5 hour under the air pressure of (1), then weighing the benzophenone (anti-ultraviolet copolymerization additive), the titanium dioxide and the zinc oxide (anti-ultraviolet particles) in parts by weight, mixing the benzophenone, the titanium dioxide and the zinc oxide with the slurry, and continuously heating the mixture for 1.5 hours at 260 ℃ to obtain a polyester component;
s3: weighing the polyacrylonitrile master batch slices in parts by weight and the prepared polyester, respectively heating and melting in two screw extruders, and then extruding and molding melts in the two screw extruders through a split type composite spinneret plate to obtain nascent composite fibers;
s4: after the nascent composite fiber is cooled, oiling, hot stretching and stress relieving are sequentially carried out, then benzotriazole (anti-ultraviolet surface treating agent) is sprayed on the surface of the nascent composite fiber, and finally the anti-ultraviolet composite DTY fiber is obtained through false twist deformation. Wherein the oiling rate during oiling accounts for 2% of the total weight of the fiber, the rotating speed of the oil tanker is 0.5rpm, and the oil agent adopts ATY common oil agent. The hot stretching is carried out in two steps, the first step of stretching temperature is controlled to be 190 ℃, the second step of stretching temperature is controlled to be 150 ℃, the stretching and winding speed is 600m/min, the false twisting stretching multiple is 1.6, and the linear density of the prepared DTY fiber is 20 tex.
Examples 6 to 7: an uvioresistant composite DTY fiber,
the difference from example 1 is that 4, 4' -dihydroxybenzophenone is used instead of benzophenone as the uv-resistant copolymerization additive, and the specific amounts are shown in table 1 below.
Examples 8 to 9: an uvioresistant composite DTY fiber,
the difference from example 1 is that 3, 6-dihydroxyphthalonitrile was used as an anti-uv copolymerization additive instead of benzophenone, and the specific amounts are shown in table 1 below.
Examples 10 to 11: an uvioresistant composite DTY fiber,
the difference from example 1 is that 3, 6-dihydroxyphthalonitrile and 4, 4' -dihydroxybenzophenone were used instead of benzophenone as the uv-resistant copolymerization additive in the specific amounts shown in table 1 below.
Examples 12 to 14: an uvioresistant composite DTY fiber,
the difference from example 1 is that 5-aminobenzotriazole is used as the anti-ultraviolet surface treating agent instead of benzotriazole, and the specific amount is shown in the following table 1.
The specific amounts of the components of examples 2-14 are shown in Table 1 below.
Table 1 examples 1-16 components and tables of amounts thereof
(Note: the units of the data in the table are kg, "-" indicates that the substance was not added.)
Example 15: an uvioresistant composite DTY fiber,
the difference from example 1 is that hydroquinone was used in the feed, and the specific amounts of hydroquinone used are shown in table 1. The difference from the preparation process of example 1 is that after the slurry is prepared in S1, hydroquinone in the above-mentioned mass is weighed and added to the slurry, and the subsequent process steps are the same.
Example 16: an uvioresistant composite DTY fiber,
the difference from example 14 is that hydroquinone was used in the feed, and the specific amounts of hydroquinone used are shown in table 1. The difference from the preparation process of example 1 is that after the slurry is prepared in S1, hydroquinone in the above-mentioned mass is weighed and added to the slurry, and the subsequent process steps are the same.
Example 17: an uvioresistant composite DTY fiber,
the difference from example 1 is that a sheath-core type composite spinneret was used in S3 to perform extrusion molding, thereby obtaining a sheath-core structured nascent composite fiber having polyacrylonitrile as a core layer and polyester as a sheath layer.
Example 18: an uvioresistant composite DTY fiber,
the difference from example 1 is that in S4, the ultraviolet resistant surface treatment agent was attached by the dipping method, and the as-spun fiber was subjected to ultrasonic treatment during the dipping, the frequency of the ultrasonic wave was controlled to 22kHz, and the power was controlled to 270W.
Comparative example
Comparative example 1: an uvioresistant DTY fiber is provided,
the compound is prepared from the following raw materials in mass: 9kg of PET master batch slices, 10kg of ethylene glycol and 1kg of ultraviolet resistant particles, wherein the ultraviolet resistant particles are nano titanium dioxide particles;
the uvioresistant DTY fiber is prepared by the following process:
s1: weighing the PET master batch slices and the uvioresistant particles in parts by weight, mixing the PET master batch slices and the uvioresistant particles, heating and melting the mixture in a screw extruder, and then extruding and molding the mixture through a spinneret plate to obtain uvioresistant PET fibers;
s2: carrying out upper, hot stretching and destressing on the uvioresistant PET fiber, and then carrying out false twist deformation to obtain the uvioresistant composite DTY fiber. Wherein the total weight proportion of the fibers of the oiling station during oiling is 2 percent, the rotating speed of the oil tanker is 0.5rpm, and the oil agent adopts ATY common oil agent. The hot stretching is carried out in two steps, the first step of stretching temperature is controlled to be 190 ℃, the second step of stretching temperature is controlled to be 150 ℃, the stretching and winding speed is 600m/min, the false twisting stretching multiple is 1.6, and the linear density of the prepared DTY fiber is 20 tex.
Comparative example 2: a DTY fiber is provided, which comprises a DTY fiber,
the difference from the example 1 is that the raw material does not contain polyacrylonitrile component, in the preparation process S3, a single screw extruder is used to heat, melt and extrude the polyester, and the polyester is extruded and molded by a common spinneret plate to prepare single-component common nascent fiber;
s4, cooling the common nascent fiber, coating the surface of the nascent fiber with an ultraviolet-resistant surface treating agent, then sequentially oiling, thermally stretching and destressing, and then performing false twist texturing to obtain the DTY fiber.
Comparative example 3: a composite DTY fiber is provided,
the difference from example 1 is that the raw material does not contain vinyl terephthalic acid, and a single terephthalic acid is dissolved in ethylene glycol and made into a single slurry in step S1, and the subsequent process is performed using the single slurry.
Comparative example 4: a composite DTY fiber is provided,
the difference from example 1 is that benzophenone is not contained in the raw material, and only titanium dioxide and zinc oxide are added to the slurry in S2.
Comparative example 5: a composite DTY fiber is provided,
the difference from example 1 is that benzotriazole is not included in the raw material, and the as-spun fiber is cooled in S4, then subjected to oiling, hot drawing, and destressing directly, and then subjected to false twist texturing to obtain a composite DTY fiber.
Comparative example 6: a composite DTY fiber is provided,
the difference from example 1 is that benzophenone, titanium dioxide and zinc oxide were directly added to the slurry in S2, the slurry was heated at a temperature of 200 c for 0.5 hour and further heated at a temperature of 260 c for 1.5 hours without changing other conditions, and polyester was obtained.
Comparative example 7: a composite DTY fiber is provided,
the difference from example 1 is that benzophenone, titanium dioxide and zinc oxide were directly added to the slurry in S2, and the slurry was directly heated at a temperature of 260 c for 2 hours without changing other conditions to obtain polyester.
Performance test
Since the main purpose and examination criteria of the fibers obtained in the examples and comparative examples of the present application are the uv resistance of the fibers, which are obtained from different raw materials and by using different processes, and the physical properties of the fibers obtained from the respective groups are different, the following analysis and test will be mainly performed around these two aspects.
The fibers of examples 1 to 18 and comparative examples 1 to 7 were made into a number of sample cloths having a density of 128 × 68, and four tests described below were performed using the sample cloths.
Test 1: ultraviolet resistance test
The sample cloths of examples 1 to 18 and comparative examples 1 to 7 were sampled according to the Chinese test standard GB/T18830-2002, and the UPF values of the samples were measured under the environmental conditions specified by the test standard, and the test results are shown in Table 2 below.
TABLE 2 UPF values of sample cloths obtained in examples 1 to 18 and comparative examples 1 to 7
Comparing the UPF values of example 1 and comparative example 1, it can be seen that the value of example 1 is significantly higher than that of comparative example 1, indicating that example 1 has significantly better uv resistance than DTY fiber made of ordinary PET with directly added uv resistant microparticles.
Comparing the UPF values of the example 1 and the comparative example 2, the UPF value of the example 1 is obviously higher than that of the comparative example 2, which shows that the single-component polyester fiber has greatly reduced ultraviolet resistance, and the polyacrylonitrile plays a great role in the ultraviolet resistance of the composite fiber.
Comparing the UPF values of example 1 and comparative example 3, it can be seen that the value of example 1 is significantly higher than that of comparative example 3, indicating that the anti-UV capability of the vinyl terephthalic acid-containing polyester is far better than that of the common polyester, because the vinyl group is a chromophore, has a larger absorbing capability in the UV region, and the vinyl group is connected with the benzene ring, the carbon-carbon double bond of the vinyl group and the large pi bond on the benzene ring generate a conjugation effect and red shift, so that the absorbing capability of the polyester on UV light is enhanced, and the polyester itself can have a better anti-UV capability. And after condensation, the vinyl positioned on the side chain can increase the gaps among polymer molecules, so that the polymer molecules can be better and more stably combined with the ultraviolet-resistant particles, more ultraviolet-resistant particles can be blended, and the ultraviolet resistance is further improved.
The UPF values of the groups are found to be similar in comparison with examples 1-5, which indicates that similar UV resistance can be achieved using the amounts of the raw materials in the groups.
Comparing example 1, examples 6-11 and comparative example 4, it can be seen that examples 6-11 have UPF values higher than example 1, examples 10-11 also have UPF values higher than examples 6-9, and example 1 is higher than comparative example 4. This can indicate that benzophenone has an effect of improving the ultraviolet resistance of the fiber and has a better ultraviolet resistance effect than benzophenone, 3, 6-dihydroxyphthalonitrile and 4, 4' -dihydroxybenzophenone, and when both are added simultaneously, the ultraviolet resistance effect can be further improved. The reason is that the conjugated pi-bonds have good ultraviolet absorption capacity, and hydroxyl groups are introduced to benzene rings of two species and serve as color-aiding clusters, so that the ultraviolet absorption capacity of the chromophore can be improved. And when the 3, 6-dihydroxy phthalonitrile and the 4, 4 '-dihydroxy benzophenone are simultaneously added, hydrogen bonds are formed between the two, so that the binding capacity of the 3, 6-dihydroxy phthalonitrile and the 4, 4' -dihydroxy benzophenone in the fiber is improved, and the fiber is more stable.
Comparing the UPF values of example 1, example 10, examples 12-14 and comparative example 5, it can be seen that examples 12-13 are higher than example 1, example 14 is higher than example 10, and example 1 is comparative example 5, which shows that benzotriazole has the effect of improving the ultraviolet resistance, and that the preferred 5-aminobenzotriazole has a better ultraviolet resistance. The reason is that in the 5-aminobenzotriazole, pi bonds on benzene rings and nitrogen-nitrogen double bonds are conjugated, and nitrogen atoms in the nitrogen rings and amino groups on the benzene rings can also generate n-pi conjugation with the benzene rings to play a role of a chromophore, so that the ultraviolet resistance is improved. Furthermore, the ultraviolet resistance effects of the 5-aminobenzotriazole, the 3, 6-dihydroxyphthalonitrile and the 4, 4' -dihydroxybenzophenone can be superposed and can be matched for use to achieve a more optimal effect.
Comparing the UPF values of example 1 and examples 14-16, it can be seen that examples 14-16 are higher than example 1, and that example 16 has the highest value, indicating that hydroquinone has an accelerating effect on the UV resistance. The reason is that vinyl groups have ultraviolet absorption capacity as chromophoric groups, while vinyl groups are polymerized to a certain extent in the copolymerization process of the polyester component, so that the content of the vinyl groups is reduced, and the ultraviolet resistance is influenced to a certain extent, and hydroquinone is used as a double-bond polymerization inhibitor, so that the free radical chain reaction between the vinyl groups can be prevented, and the polymerization of the vinyl groups is prevented, so that more vinyl groups can be remained in the polymer, and the polymer has better ultraviolet resistance effect.
Comparing the UPF values of example 1 and example 17, it can be seen that the value of example 17 is higher than that of example 1, which indicates that the composite fiber with sheath-core structure is preferable in the present application because the sheath-core structure fiber with polyacrylonitrile as the core layer has more uniform structure and better ultraviolet absorption.
Comparing the UPF values of example 1 and example 18, it can be seen that the value of example 18 is higher than example 1, which can illustrate that the uv resistance of the fiber can be improved by the dipping method and by the ultrasonic treatment of the fiber, because the ultrasonic wave can generate fine broomed fibers on the surface of the fiber, and thus the adhesion between the uv resistant surface treatment agent and the fiber can be made more sufficient.
Comparing the UPF values of example 1 and comparative example 6, it can be seen that the value of example 1 is higher than that of comparative example 6, indicating that the UV resistance of the fiber prepared in comparative example 6 is reduced because if the UV resistant copolymerization additive is added before the first polymerization is carried out, the effective concentrations of terephthalic acid and vinylterephthalic acid in ethylene glycol are affected, thereby affecting the initial polymerization, and the polymerization degree of the product is reduced, thereby affecting the binding ability of the polyester to the UV resistant copolymerization additive.
Comparing the UPF values of example 1 and comparative example 7, it can be seen that the value of example 1 is higher than that of comparative example 7, which effectively illustrates that the uv resistance of the fiber is greatly affected if a single polymerization is directly performed, because the polyester cannot reach a high degree of polymerization and cannot be well combined with the uv-resistant copolymerization additive if a single polymerization is performed, thereby resulting in poor uv resistance.
Test 2: durability test of ultraviolet resistance
The UPF values of the sample cloths of the examples 1, 14-18 and 2-7 are detected and recorded according to the Chinese detection standard GB/T18830-2002, then the sample cloths of each group are exposed and placed in the same outdoor environment, the UPF value of each sample cloth is measured again by the same method after 90 days, the measured values of the front side and the rear side of the same cloth are respectively marked as UPF-1 and UPF-2, the fading rate is calculated, and the test results are shown in the following table 3.
TABLE 3 comparative tables for UPF value changes in examples 1, 14 to 18 and 2 to 7
| Example 1 | Example 14 | Example 15 | Example 16 | Example 17 | Example 18 | |
| UPF-1 | 39.1 | 51.2 | 40.4 | 51.9 | 40.2 | 42.6 |
| UPF-2 | 36.0 | 47.1 | 37.9 | 48.8 | 38.6 | 41.3 |
| Rate of decline (%) | 0.11 | 0.08 | 0.06 | 0.06 | 0.04 | 0.03 |
| Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
| UPF-1 | 29.8 | 32.3 | 27.2 | 28.6 | 37.1 | 35.3 |
| UPF-2 | 24.7 | 23.9 | 23.4 | 24.0 | 29.3 | 27.2 |
| Rate of decline (%) | 0.17 | 0.26 | 0.14 | 0.16 | 0.21 | 0.24 |
Comparing the deterioration rates of example 1 and example 14, it can be shown that when 3, 6-dihydroxyphthalonitrile, 4' -dihydroxybenzophenone and 5-aminobenzotriazole are used as raw materials, the deterioration rate of the ultraviolet resistance of the fiber is reduced, and the ultraviolet resistance is maintained for a longer time. In combination with test 1, it can be shown that 3, 6-dihydroxyphthalonitrile, 4' -dihydroxybenzophenone and 5-aminobenzotriazole have better UV resistance lifetime in addition to rigid UV resistance.
Comparing the deterioration rates of examples 1 and 15, and 14 and 16, it can be shown that the deterioration rate can be reduced after adding hydroquinone, because the polyester has more branched chains inside after the polymerization of vinyl is prevented, thereby increasing the binding ability of the polyester to the uv copolymerization additive and the uv surface treatment agent, and improving the binding stability.
Comparing the deterioration rates of example 1 and examples 17 to 18 shows that the composite fiber of the sheath-core structure and the fiber treated by the dipping method and the ultrasonic treatment have better ultraviolet resistance life because the composite fiber of the sheath-core structure has a more uniform structure, and the absorption and refraction of ultraviolet rays are more uniform, and the excessive consumption of local regions in the fiber can be avoided, thereby having higher ultraviolet resistance life. The impregnation method and the ultrasonic treatment can improve the adsorption of the fiber to the ultraviolet-resistant surface treatment agent, so that the fiber has better ultraviolet-resistant service life.
Comparing the deterioration rates of example 1 and comparative examples 2 to 3, it can be shown that the composite fiber has a better ultraviolet life than the monocomponent fiber. Compared with common fibers, the fibers using the vinyl terephthalic acid in the raw materials have better ultraviolet resistance service life, so that the ultraviolet resistance capability is improved, and the ultraviolet resistance service life of the vinyl in the polyacrylonitrile and the polyester can be improved.
Comparing the deterioration rates of example 1, example 14 and comparative examples 4 to 5, and the analysis results of test 1, it can be shown that 3, 6-dihydroxyphthalonitrile and 4, 4' -dihydroxybenzophenone and 5-aminobenzotriazole can improve the life of the ultraviolet resistance of the fiber in addition to the ultraviolet resistance of the fiber.
Comparing the deterioration rates of example 1 and comparative examples 6 to 7, it can be seen from the analysis results of test 1 that the higher the degree of polymerization of the fiber, the better the bonding with the uv-resistant substance, the better the uv-resistant life.
Test 3: physical property test of fiber
Taking the sample cloths of the example 1, the examples 14 to 18 and the comparative examples 2 to 7, testing the wear resistance of the cloth samples by a test method ASTM D4966 (Martindale method), wherein standard wear-resistant cloth and standard wool felt are used in the test, and when a hole appears at the test endpoint of the test; the plastic deformation rate of the fabric was then measured according to the industry standard FZT 70006-.
TABLE 4 comparative tables of number of times of abrasion resistance and plastic deformation ratio in examples 1, 14 to 18 and 2 to 7
Comparing the data in example 1, example 14 and comparative examples 4-5, it can be seen that the use of benzophenone, 3, 6-dihydroxyphthalonitrile and 4, 4' -dihydroxybenzophenone in the fiber, and the use of benzotriazole and 5-aminobenzotriazole do not adversely affect the abrasion resistance and elasticity of the fiber.
Comparing the data in example 1 and examples 14-16, it is seen that the degree of polymerization of the polyester in the fibers is increased and the abrasion resistance and also the elasticity of the fibers are improved after the addition of hydroquinone.
Comparing the data of example 1 and example 17, and combining the analysis conclusion of test 1, it can be seen that the composite fiber of the sheath-core structure has better abrasion resistance and elasticity.
Comparing the data in example 1 and example 18, and in conjunction with the analysis of test 1, it was concluded that the broomed fibers on the surface of the fibers after ultrasonication did not have an effect on the abrasion resistance and elasticity of the fibers.
Comparing the data in example 1 and comparative example 2, it can be seen that the composite fiber in the present application has better abrasion resistance and elasticity than the monocomponent fiber.
Comparing the data in example 1 and comparative example 3, it can be shown that the composite fiber made of the polyester with vinyl group has better elasticity.
Comparing the data of example 1 and comparative examples 6 to 7, and the results of the analysis of test 1, it can be seen that elasticity, which improves the abrasion resistance of the fiber after adding hydroquinone and increasing the degree of polymerization of the polyester using the stepwise esterification method, is improved.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. An uvioresistant composite DTY fiber is characterized in that: the coating is mainly prepared from 10-12 parts by weight of polyester component, 5-8 parts by weight of polyacrylonitrile component and 0.5-1.5 parts by weight of anti-ultraviolet surface treating agent;
the polyester component is prepared from 7-10 parts of terephthalic acid, 2-3 parts of vinyl terephthalic acid, 10-15 parts of ethylene glycol, 1-2 parts of anti-ultraviolet copolymerization additive and 0.5-1.3 parts of anti-ultraviolet particles;
the ultraviolet resistant particles comprise at least one of titanium dioxide and zinc oxide.
2. The ultraviolet-resistant composite DTY fiber as claimed in claim 1, wherein: the ultraviolet-resistant copolymerization additive comprises at least one of 3, 6-dihydroxy phthalonitrile and 4, 4' -dihydroxy benzophenone.
3. The ultraviolet-resistant composite DTY fiber as claimed in claim 1, wherein: the uvioresistant surface treating agent is 5-aminobenzotriazole.
4. The ultraviolet-resistant composite DTY fiber as claimed in claim 1, wherein: the uvioresistant composite DTY fiber also comprises 0.3-0.5 part of hydroquinone in parts by weight.
5. The ultraviolet-resistant composite DTY fiber as claimed in claim 1, wherein: the fiber structure of the uvioresistant composite DTY fiber is a sheath-core structure, the sheath-core structure comprises a core layer and a skin layer, the core layer is made of a polyacrylonitrile component, and the skin layer is made of a polyester component.
6. The preparation process of the anti-ultraviolet composite DTY fiber according to any one of claims 1 to 5, which is characterized in that: the method comprises the following steps:
s1: weighing the vinyl terephthalic acid, the terephthalic acid and the ethylene glycol in parts by weight, and mixing the vinyl terephthalic acid and the terephthalic acid in the ethylene glycol to prepare uniform slurry;
s2: nitrogen is used as protective gas, and the nitrogen is 2.5 to 4Kg/cm2Heating the slurry at the temperature of 200-220 ℃ for 0.5-1 hour under the air pressure, weighing the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles in parts by weight, mixing the anti-ultraviolet copolymerization additive and the anti-ultraviolet particles with the slurry, and continuously heating the mixture at the temperature of 260-280 ℃ for 1-1.5 hours to obtain a polyester component;
s3: respectively putting the prepared polyester component and the polyacrylonitrile component in parts by weight into two screw extruders for heating and melting, and performing extrusion molding on melts in the two screw extruders through a composite spinneret plate to obtain nascent composite fibers;
s4: after the primary composite fiber is cooled, oiling, hot stretching and stress relieving are sequentially carried out, then the anti-ultraviolet surface treating agent is attached to the surface of the fiber, and finally the anti-ultraviolet composite DTY fiber is obtained through false twist deformation.
7. The preparation process of the anti-ultraviolet composite DTY fiber according to claim 6, wherein the preparation process comprises the following steps: hydroquinone was added to the slurry of S1 with mixing.
8. The preparation process of the anti-ultraviolet composite DTY fiber according to claim 6, wherein the preparation process comprises the following steps: in S4, the surface of the nascent fiber is attached with the uvioresistant surface treatment agent through impregnation, and the nascent fiber is subjected to ultrasonic treatment in the impregnation process, wherein the frequency of ultrasonic wave is controlled to be 20-23kHz, and the power is controlled to be 250-300W.
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