KR101734893B1 - Black dope-dyed para-aramid fiber and method of manufacturing the same - Google Patents

Black dope-dyed para-aramid fiber and method of manufacturing the same Download PDF

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Publication number
KR101734893B1
KR101734893B1 KR1020160011865A KR20160011865A KR101734893B1 KR 101734893 B1 KR101734893 B1 KR 101734893B1 KR 1020160011865 A KR1020160011865 A KR 1020160011865A KR 20160011865 A KR20160011865 A KR 20160011865A KR 101734893 B1 KR101734893 B1 KR 101734893B1
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KR
South Korea
Prior art keywords
black
aramid
para
pigments
less
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KR1020160011865A
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Korean (ko)
Inventor
김성수
이기환
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주식회사 효성
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Publication of KR101734893B1 publication Critical patent/KR101734893B1/en

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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
    • D01F1/04—Pigments
    • 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
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/06—Feeding liquid to the spinning head
    • D01D1/065—Addition and mixing of substances to the spinning solution or to the melt; Homogenising
    • 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
    • D01D5/06—Wet spinning methods
    • 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
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D02G3/047—Blended or other yarns or threads containing components made from different materials including aramid fibres
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
    • D02G3/34—Yarns or threads having slubs, knops, spirals, loops, tufts, or other irregular or decorative effects, i.e. effect yarns
    • D02G3/346—Yarns or threads having slubs, knops, spirals, loops, tufts, or other irregular or decorative effects, i.e. effect yarns with coloured effects, i.e. by differential dyeing process
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
    • D10B2331/021—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides aromatic polyamides, e.g. aramides
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/22—Physical properties protective against sunlight or UV radiation
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2501/00—Wearing apparel
    • D10B2501/04—Outerwear; Protective garments
    • D10B2501/041—Gloves

Abstract

The present invention relates to a black para-aramid dope-dyed yarn unit which has primary particles with average particle size of 600 nm or less, includes three organic pigments-red, blue, and yellow, includes a black inorganic pigment having primary particles with average particle size of 90 nm or less, and has the filament strength of 18 g/d or higher. An L value representing a lightness factor of the black para-aramid dope-dyed yarn unit is 35 or less while the value of chromacity a is in the range of -5 to 3 and the value of chromacity b is in the range of -3 to 5. 1 to 6 wt% of the organic pigment is included with respect to the entire weight of the dope-dyed yarn unit while 1 wt% or less of the black inorganic pigment is included therein. According to the present invention, a fabric woven with the black para-aramid dope-dyed yarn unit prevents discoloration, so it is suitable for an exterior material requiring high durability without becoming colorless while having less degradation of strength compared to a conventional black aramid dope-dyed fabric only using inorganic carbon black pigments having limitations on achieving deep colors only with the blending of organic pigments, thereby enhancing strength.

Description

[0001] The present invention relates to a para-aramid black dye and a method for producing the same,

More particularly, the present invention relates to a para-aramid black coloring agent, and more particularly, to a coloring agent for a para-aramid black coloring agent, which comprises at least three kinds of organic pigments and a black inorganic pigment And a method for producing the para-aramid black dye.

The aramid fiber includes para-aramid fibers having a structure in which benzene rings are linearly connected through an amide group (CONH) and meta-based aramid fibers not having a structure. Para-aramid fiber is a thin thread with a thickness of about 5mm, and has a strength enough to lift a 2-tonne automobile. It is used not only for bulletproof but also for various applications in high-tech industries in aerospace industry.

The aramid fiber has a skin-core structure having a higher elastic modulus of the surface layer than the elastic modulus of the core layer, and stress is mainly concentrated on the surface layer when stress is applied to the aramid fiber. Therefore, the physical properties of the surface layer of the aramid fiber are important factors in determining the strength of the aramid fiber. However, conventionally, no consideration has been given to the management factor for the surface layer of the aramid fiber, and there has been a limitation in increasing the strength of the aramid fiber. In addition, the aramid fiber has a distinctive yellow color, which not only deteriorates the aesthetics but also causes a significant browning phenomenon during long-term contact with the light source, and also has a problem that the cut resistance is significantly lowered. As a result, the aramid fiber is used as a jacket material .

In order to overcome these drawbacks, other fibers have adopted a method of using an ultraviolet screening agent as an additive in a spinning solution. However, since the aramid spinning solution uses concentrated sulfuric acid in the production, no additional additives can be used. Therefore, there is a demand for the development of an aramid fiber which exhibits excellent light resistance and light reflectivity and is less susceptible to browning even after irradiation with ultraviolet rays without lowering the mechanical strength.

Korean Patent Publication No. 10-2015-0079425

Conventional aramid fibers are weak to ultraviolet rays, and therefore, they are severely discolored when exposed to the sun for a long time, making it difficult to use the aramid fibers as a jacket material such as gloves and protective clothing. The black colored aramid fiber according to the present invention is suitable for use as an outer skin material which requires no durability because of no discoloration and has a limitation in producing a heart color only by the organic pigment blend, Strength strength is lower than that of aramid fiber.

In order to achieve the above-mentioned object, the present invention includes a black inorganic pigment which contains red, blue and yellow pigments having an average particle size of primary particles of 600 nm or less and three organic pigments, which are organic, and has a primary particle diameter of 90 nm or less And a filament strength of 18 g / d or more.

The para-aramid black original yarn has a lightness factor L value of 35 or less, a chromaticity a of -5 to 3 and b is -3 to 5, and the organic pigment has a lightness factor of 1 By weight to 6% by weight, and the black inorganic pigment is not more than 1% by weight based on the total weight of the coating composition.

 Further, there is also provided a method for producing a radiation dope comprising the steps of dissolving an aromatic polyamide polymer in a solvent containing at least three kinds of black inorganic pigments, sulfuric acid and organic pigments to prepare a radial dope and then spinning the radial dope by a wet spinning method, And 1 to 6% by weight based on 100% by weight of the whole of the raw material.

At this time, when the encapsulated yarn is produced under the conditions out of the above-mentioned numerical range, there arises a problem in using a sheathing material which is discolored weakly by ultraviolet rays.

Conventional aramid fibers are weak to ultraviolet rays, and therefore, they are severely discolored when exposed to the sun for a long time, making it difficult to use the aramid fibers as a jacket material such as gloves and protective clothing. The black colored aramid fiber according to the present invention is suitable for use as an outer skin material which requires no durability because of no discoloration and has a limitation in producing a heart color only by the organic pigment blend, Strength strength is lower than that of aramid fiber.

Hereinafter, the present invention will be described.

The present invention is characterized in that it comprises a black inorganic pigment containing at least three organic pigments having a filament strength of 18 g / d or more, completely organic, an average particle size of primary particles of 600 nm or less, and a primary particle size of 90 nm or less Lt; RTI ID = 0.0 > aramid < / RTI >

Herein, the organic pigment includes at least one of yellow, blue, and red pigments, respectively.

The yellow pigment may be C.I. Pigment Yellow 1, 3, 12, 13, 16, 17, 42, 53, 73, 74, 81, 83, 97, 120, 139, 150, 151, 154, 155, 175, 180, 181, 184, 191, 194, 213, 216, and 219, but is not limited thereto.

The above-mentioned blue pigment is a mixture of C.I. But is not limited to, at least one selected from the group consisting of Pigment Blue 15: 1, 15: 2, 15: 3, 15: 4 and 28.

Also, the red pigment is preferably a colorant selected from the group consisting of C.I. Pigment Red 4, 5, 9, 12, 14, 48, 53, 57, 101, 112, 122, 144, 146, 149, 168, 170, 179, 185, 187, 188, 209, 242, 254, and 257, but is not limited thereto.

The para-aramid black primary yarn according to the present invention has three or more types of organic pigments in terms of a lightness factor L value of 35 or less and a chromaticity index a (+ a * is red, -a * is green) is -5 to 3, b (+ b is yellow and -b * is blue) represents -3 to 5.

In addition, the para-aramid black original yarn includes at least 3 kinds of organic pigments in an amount of 1 to 6% by weight based on 100% by weight of the whole fiber, and the black inorganic pigment is 1% And a para-aramid black circle.

Further, the method includes dissolving the aromatic polyamide polymer in a solvent containing sulfuric acid and at least three organic pigments to prepare a radial dope, and then spinning the radial dope by a wet spinning method.

Hereinafter, a method for producing an aramid black original yarn according to the present invention will be described.

The method for producing an aramid black original yarn of the present invention comprises dissolving an aromatic polyamide polymer in a solvent containing sulfuric acid and three organic pigments to prepare a spinning dope and then spinning the spinning dope by wet spinning.

The method for producing the aramid black cordyer according to the present invention will be described in detail as follows.

First, a spinning dope is prepared by dissolving an aromatic polyamide polymer in a solvent.

At this time, the aromatic polyamide polymer may be prepared by adding an aromatic salt to an aromatic diamine and an aromatic dicarboxylic acid halide in a mixed solvent prepared by adding an inorganic salt to an amide-based solvent and then dissolving.

Non-limiting examples of the amide solvent include N-methyl-2-pyrrolidone (NMP), N, Ndimethylformamide (DMF), N, N-dimethylacetamide (DMAc) , Dimethyl sulfoxide (DMSO), hexamethylphosphoramide (HMPA), N, N, N ', N'-tetramethylurea And they may be used alone or in a mixture thereof.

As the inorganic salt, calcium chloride, lithium chloride, potassium chloride or the like can be used, and it is most preferable to use calcium chloride in view of the stability and cost of the solvent. The amount to be used is preferably 13 to 15% by weight, more preferably 14% by weight, based on the amide-based solvent. When the inorganic salt is used in an amount of less than 13% by weight, the aromatic dicarboxylic acid halide and the aromatic diamine do not act as a sufficient salt to react, while when it is used in an amount exceeding 15% by weight, And precipitation occurs.

The aromatic diamine is preferably at least one compound selected from the group consisting of paraphenylenediamine, 4,4'-diaminobiphenyl, 2-methyl-paraphenylenediamine, 2-chloropaphenylenediamine, 2,6- Naphthalene diamine, 4,4'-diaminobenzanilide, and the like, but the present invention is not limited thereto.

Specific examples of the aromatic dicarboxylic acid halide include terephthaloyl chloride (TPC), 4,4'-benzoyl chloride, 2-chloroterephthaloyl chloride, 2,5-dichloroterephthaloyl chloride, 2- Terephthaloyl chloride, 2,6-naphthalenecarboxylic acid chloride, 1,5-naphthalenedicarboxylic acid chloride, and the like, but are not limited thereto.

On the other hand, the solvent preferably contains at least three kinds of sulfuric acid and organic pigments.

Herein, the organic pigment includes at least one of yellow, blue, and red pigments, respectively.

The yellow pigment may be C.I. Pigment Yellow 1, 3, 12, 13, 16, 17, 42, 53, 73, 74, 81, 83, 97, 120, 139, 150, 151, 154, 155, 175, 180, 181, 184, 191, 194, 213, 216, and 219, but is not limited thereto.

The above-mentioned blue pigment is a mixture of C.I. But is not limited to, at least one selected from the group consisting of Pigment Blue 15: 1, 15: 2, 15: 3, 15: 4 and 28.

Also, the red pigment is preferably a colorant selected from the group consisting of C.I. Pigment Red 4, 5, 9, 12, 14, 48, 53, 57, 101, 112, 122, 144, 146, 149, 168, 170, 179, 185, 187, 188, 209, 242, 254, and 257, but is not limited thereto.

The organic pigment is preferably 1 to 6% by weight based on 100% by weight of the entirety of the encapsulant. When the content of the organic pigment is less than 1% by weight, the desired blackness effect can not be obtained. When the content exceeds 6% by weight, the production process becomes expensive and the production becomes difficult and it is difficult to ensure uniform dispersibility . The inorganic pigment is preferably 1% by weight or less of the total weight of the encapsulant, and when it is 1% by weight or less, the strength drop ratio is lower than that of the black original aramid fiber using only conventional inorganic pigments.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.

Hereinafter, the present invention will be described in detail with reference to examples. However, these examples are for illustrating the present invention specifically, and the scope of the present invention is not limited to these examples.

Example 1

Blue, and Red pigments having an average primary particle size of 500 nm were added to 100 wt% concentrated sulfuric acid in an amount of 2 wt% based on the weight of the fiber. A carbon black inorganic pigment having a primary particle diameter of 50 nm was added in an amount of 1 wt% And mixed for a certain period of time.

Example 2

Blue, and Red pigments having an average particle size of 500 nm of primary particles were added to 100 wt% sulfuric acid and 3 wt% based on the weight of the fibers. A carbon black inorganic pigment having a primary particle diameter of 50 nm was added in an amount of 1 wt% And mixed for a certain period of time.

Example 3

Blue, and Red pigments having an average primary particle size of 500 nm were added to 100 wt% concentrated sulfuric acid in an amount of 4 wt% based on the weight of the fiber. A carbon black inorganic pigment having a primary particle diameter of 50 nm was added in an amount of 1 wt% And mixed for a certain period of time.

Example 4

Blue, and Red pigments having an average particle size of 500 nm of primary particles in 100 wt% sulfuric acid were added in an amount of 4 wt% based on the weight of the fibers. A carbon black inorganic pigment having a primary particle size of 50 nm was added in an amount of 0.5 wt% For a certain period of time.

Comparative Example 1

Aramid fiber (1500 Da) not containing pigments prepared through conventional aramid fiber manufacturing process.

Comparative Example 2

Carbon black having a primary particle average particle size of 50 nm is added to 100 wt% sulfuric acid and 2 wt% of the carbon black is mixed with sulfuric acid for a predetermined time using a high-speed stirrer.

division Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Pigment content 500 nm Red (wt%) 0.8 1.6 2 2 - - 500 nm Blue (wt%) 0.4 0.5 0.8 0.8 - - 500 nm Yellow (wt%) 0.8 0.9 1.2 1.2 - - 50nm Carbon Black One One One 0.5 - 2 Total (wt%) 3 4 5 4.5 0 2 Properties Strength (g / d) 21.3 20.8 20.5 21.8 23.2 15.5 Truncation 3.4 3.3 3.4 3.4 3.6 2.7 color L * 33.5 32.5 30.2 30.7 84.7 31.3 a *
(Red Green) -3.5 -1.6 -0.7 0.2 -7.2 1.2 b *
(Yellow Blue) 3.6 -0.4 -1.7 -2.8 40.4 -3.8

The physical property was measured by the CIE Lab system CIELAB chromaticity coordinates, and the L value was expressed by lightness. The value of a was red when it was positive, and red when it was negative. The green, b value indicates yellow if positive, and blue if negative. The color is a value measured with a color difference meter (CR-400, light source D65, manufactured by Minolta).

While the present invention has been described in connection with specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined in the appended claims. It will be easy to see.

Claims (4)

In a para-aramid black colored raw material containing a black inorganic pigment having a primary particle size of not more than 600 nm and a primary particle diameter of not more than 90 nm, including red, blue and yellow pigments of three organic pigments,
The black inorganic pigment is used in an amount of 0.5 to 1 wt% based on 100 wt%
The para-aramid black original yarn has a strength of 18 g / d or more, a lightness factor L value of 30.2 to 33.5, a chromaticity a of -3.5 to 0.2, and b of -2.8 to 3.6 Of para-aramid black circle.
delete The method according to claim 1,
Wherein the organic pigment comprises from 1 to 6% by weight of the total weight of the encasement.
Comprising dissolving an aromatic polyamide polymer in a solvent containing at least three kinds of black inorganic pigments, sulfuric acid and organic pigments to prepare a radial dope and then spinning the radial dope by a wet spinning method, 1 to 6% by weight based on 100% by weight of the total of the black inorganic pigments, 0.5 to 1% by weight based on 100%
Wherein the base yarn has a strength of 18 g / d or more, a lightness factor L value of 30.2 to 33.5, a chromaticity a of -3.5 to 0.2, and a bismuth of -2.8 to 3.6. Lt; / RTI >
KR1020160011865A 2016-01-29 2016-01-29 Black dope-dyed para-aramid fiber and method of manufacturing the same KR101734893B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217801A (en) 2006-02-14 2007-08-30 Teijin Techno Products Ltd Para-type aramid fiber adjusted with infrared reflection, and clothing by using the same
JP2008138335A (en) 2006-12-05 2008-06-19 Teijin Techno Products Ltd Spun-dyed aramid fiber

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217801A (en) 2006-02-14 2007-08-30 Teijin Techno Products Ltd Para-type aramid fiber adjusted with infrared reflection, and clothing by using the same
JP2008138335A (en) 2006-12-05 2008-06-19 Teijin Techno Products Ltd Spun-dyed aramid fiber

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