CN115803484A - Polyamide multifilament yarn and process for producing the same - Google Patents
Polyamide multifilament yarn and process for producing the same Download PDFInfo
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- CN115803484A CN115803484A CN202180049017.4A CN202180049017A CN115803484A CN 115803484 A CN115803484 A CN 115803484A CN 202180049017 A CN202180049017 A CN 202180049017A CN 115803484 A CN115803484 A CN 115803484A
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- 229920002647 polyamide Polymers 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims description 28
- 230000008569 process Effects 0.000 title claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 34
- 229920006122 polyamide resin Polymers 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 36
- 229920000642 polymer Polymers 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 16
- 239000004744 fabric Substances 0.000 description 15
- 239000012770 industrial material Substances 0.000 description 12
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- 238000004804 winding Methods 0.000 description 6
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- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
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- 239000000203 mixture Substances 0.000 description 2
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- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229920000299 Nylon 12 Polymers 0.000 description 1
- 229920003189 Nylon 4,6 Polymers 0.000 description 1
- 229920000305 Nylon 6,10 Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
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- 239000010949 copper Substances 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 210000003127 knee Anatomy 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 1
- 229920006118 nylon 56 Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- 230000001629 suppression Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
- 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
-
- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D10B2401/06—Load-responsive characteristics
- D10B2401/061—Load-responsive characteristics elastic
-
- 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
- D10B2401/06—Load-responsive characteristics
- D10B2401/063—Load-responsive characteristics high strength
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention addresses the problem of providing a polyamide multifilament having a fine fineness, high strength and good pile quality, and aims to solve the problem by providing a polyamide multifilament characterized by comprising a polyamide resin and having a total fineness of 30 to 150dtex, a strength of 7.5 to 10.0cN/dtex and an elongation of 15.0 to 35.0%.
Description
Technical Field
The present invention relates to a polyamide multifilament yarn.
Background
Multifilament of polyamide 6 (also known as "polycaprolactam") or polyamide 66 (also known as "polyhexamethylene adipamide") has higher elongation strength and more excellent pile quality than general-purpose multifilament of polyester, polypropylene, or the like, and therefore is used in various fields of industrial applications such as airbags, sportsbook strings, ropes, fishing nets, shoelaces, and the like.
Here, an airbag may be given as an example. In a safety device required for protecting an occupant in a vehicle collision, an airbag whose installation rate rapidly increases has its mounting portion continuously expanded, and has been introduced in an initial stage, that is, for protecting a driver and a passenger in a front passenger seat, for protecting a knee, for protecting a chest incorporated in a seat, for protecting a head mounted in a ceiling above a window, and the like. With the increase in the number of mounting locations and the demand for lower fuel consumption, which has been increasing year by year, and the tendency toward an increase in the space within a vehicle in recent years, various studies have been made on a base fabric for an airbag to reduce the weight and size of the base fabric.
The total fineness of the polyamide 66 base yarn used for the base fabric for an airbag has conventionally been generally 940dtex, but in recent years, 470dtex, and even low-fineness base yarn of 235dtex or less, has been mainly used.
This is because, when a multifilament having a small total fineness is obtained, the influence of the retention of the molten state before the polyamide chips are melted and spun, and the influence of defects such as air bubbles remaining in the fibers during spinning become large. That is, a general facility for producing a fiber for high-strength industrial materials such as a base yarn for an airbag is constituted by a direct drawing machine composed of a spinning section for discharging a high total fineness of about 235 to 2000dtex and a multi-stage hot drawing machine for developing high strength, but the problem occurring when a multifilament having a fineness of 100dtex or less is produced using such a device is not considered. More specifically, when the fineness is reduced to 100dtex or less by a general facility for producing fibers for industrial materials, as described in patent documents 3 (paragraphs [0005] to [0008 ]), and 4 (paragraph [0013 ]), thickening, thermal deterioration, and gelation caused by long-term retention of the polymer generate fine foreign matter, and the foreign matter is mixed into the yarn to cause a yarn-making failure, and a polyamide fiber having high strength and good pile quality cannot be obtained. Thus, it is extremely difficult to produce a polyamide fiber having high strength and good pile quality despite being a fine denier multifilament.
On the other hand, in the field of high-strength polyamide multifilaments for clothing, in recent years, due to demands for further high-grade processed products for clothing use, such as higher strength, thinner thickness, and smaller size, higher strength of raw yarns and smaller fineness thereof have been demanded.
In order to meet the demand for higher strength of such polyamide fibers for clothing, patent document 5 proposes: and a means for temporarily winding the yarn into a package by drawing and heat-fixing or heat-drawing, and further bringing the yarn into contact with a hot plate heated to 170 to 205 ℃ to heat-draw the yarn by 1.15 times or more. However, this method is a method in which the steps are divided into 2 steps of a spinning step and a drawing step, and not only the steps become complicated, but also the winding speed is about 1000m/min, the production speed is slow, and there is a risk of increasing the cost. In addition, in patent document 6, only polyamide multifilament having a strength of up to 7.3cN/dtex can be obtained in most of products obtained by a commercialized process, and the strength is insufficient on the premise of improving the durability of fibers for industrial materials such as airbags and fabrics for clothing.
Documents of the prior art
[ patent document ]
Patent document 1: japanese patent laid-open publication No. 2017-222939
Patent document 2: japanese patent laid-open publication No. 2003-20566
Patent document 3: japanese patent laid-open No. 2007-254945
Patent document 4: japanese patent laid-open No. 2008-133566
Patent document 5: japanese patent laid-open publication No. 11-247022
Patent document 6: japanese patent laid-open publication No. 2002-88577
Disclosure of Invention
Problems to be solved by the invention
An object of the present invention is to solve the above problems, and to provide a polyamide multifilament having a fine fineness, a high strength, and excellent toughness and a good pile quality, and to provide a polyamide multifilament capable of achieving a reduction in weight of industrial materials such as the above-mentioned airbag and an improvement in durability of a cloth for clothing. Further, according to the present invention, a polyamide multifilament having good production efficiency can be obtained.
[ means for solving the problems ]
The present invention has been made to solve the above problems, and mainly includes the following aspects.
(1) A polyamide multifilament comprising a polyamide, having a total fineness of 30 to 150dtex, a strength of 7.5 to 10.0cN/dtex, and an elongation of 15.0 to 35.0%.
(2) A polyamide multifilament comprises a polyamide, has a total fineness of 50 to 120dtex, a strength of 8.0 to 9.7cN/dtex, an elongation of 17.0 to 30.0%, and a coefficient of variation in elongation under a load of 3cN/dtex of 1.00% or less.
(3) The polyamide multifilament according to the above (1) or (2), which has a fuzz number of 0 to 3 pieces/km.
(4) The multifilament polyamide yarn according to any one of (1) to (3) above, wherein the number of bubbles contained in the polyamide filaments constituting the multifilament polyamide yarn is 50/cm or less.
(5) A method for producing a polyamide multifilament according to the above (1) or (2), which comprises the steps of preparing a polyamide scrap and producing a yarn by a direct spin-draw method, wherein | η a- η b | < 0.3 where η a is the relative viscosity of sulfuric acid in the polyamide scrap and η b is the relative viscosity of sulfuric acid in the polyamide multifilament produced by the production of a yarn.
Effects of the invention
According to the present invention, a polyamide multifilament having excellent pile quality, high strength and excellent toughness can be provided in spite of its fine fineness, and weight reduction of industrial materials and improvement of durability of clothes can be achieved.
Drawings
Fig. 1 is a schematic view for explaining an example of a step of producing a polyamide multifilament yarn of the present invention.
Detailed Description
The present invention will be described below by way of examples. However, the present invention is not limited to the specific examples explained below.
Examples of the raw material for the polyamide multifilament yarn of the present invention include nylon 6, nylon 66, nylon 12, nylon 46, nylon 56, nylon 610, a copolymerized polyamide of nylon 6 and nylon 66, a copolymerized polyamide obtained by copolymerizing nylon 6 with polyalkylene glycol, dicarboxylic acid, diamine, and the like, and a polymer in which repeating units are linked via amide bonds is known. The polyamide is not particularly limited as long as it is a polyamide, but among them, polyamide 66 excellent in impact resistance and heat resistance is preferably used. The polyamide multifilament of the present invention may optionally contain components other than polyamide, and examples of such components include a terminal blocking agent such as monocarboxylic acid, a delustering agent such as titanium oxide, a polymerization catalyst or heat resistant agent such as a phosphorus compound, and an antioxidant or heat resistant stabilizer such as a copper compound and a halide of an alkali metal or an alkaline earth metal. The content ratio of the polyamide contained in the polyamide multifilament is preferably 95% by weight or more, and more preferably 97% by weight or more. When the content of the polyamide is less than 95% by weight, the heat resistance is lowered.
The polyamide multifilament of the present invention has a total fineness of 30 to 150dtex, preferably 50 to 120 dtex. When the total fineness is less than 30dtex, it is difficult to secure a sufficient value as the total strength of the multifilament, and when the multifilament is drawn at a high magnification in order to obtain high strength, monofilament breakage is likely to occur, and the possibility of generation of fuzz increases. When the total fineness is more than 150dtex, the weight reduction of industrial materials and the improvement of durability of clothes and fabrics cannot be attained.
The polyamide multifilament yarn of the invention has a strength of 7.5 to 10.0cN/dtex, preferably 8.0 to 9.7cN/dtex. When the strength is within this range, the polyamide fiber is suitable for industrial materials such as airbags and the like, and a cloth for clothing having excellent durability. If the strength is less than 7.5cN/dtex, the durability of fibers for industrial materials such as airbags and fabrics for clothing is not sufficiently improved. In the case of a polyamide fiber having a strength of more than 10.0cN/dtex, it is necessary to perform mechanical stretching at a high magnification, and therefore, monofilament breakage is likely to occur and the pile quality is deteriorated. The polyamide multifilament is not suitable for fibers for industrial materials such as airbags and the like requiring quality.
The polyamide multifilament of the present invention has an elongation of 15.0 to 35.0%, preferably 17.0 to 30.0%. The higher the elongation is, the more preferable the elongation is, and the elongation is actually 35.0% or less in order to obtain a predetermined strength with polyamide. By setting the range, the toughness and the breaking work of the polyamide multifilament can be increased and excellent durability can be maintained.
Although depending on the total fineness and the single-fiber fineness, the elongation-strength product is preferably 38cN/dtex (% 1/2 ) Above, more preferably 40cN/dtex (% 1/2 ) The above. Since the product of strength and elongation is high, generation of fuzz, breakage and the like can be suppressed, and a polyamide multifilament having extremely high quality even with high strength can be obtained. The strength (cN/dtex) and the elongation (%) are values measured under the constant-speed elongation conditions shown in the standard test of JIS L1013 (1999) 8.5.1, and the product of strength and elongation is [ strength × √ (elongation) ]]The calculated value. The upper limit is not particularly limited, but is practically 50.0cN/dtex (% 1/2 ) The following.
The yarn unevenness (U%) of the polyamide multifilament of the present invention is preferably 1.2% or less, more preferably 1.0% or less, and particularly preferably 0.8% or less. When the U% is 1.2% or less, uneven dyeing and streaks do not occur when the fabric is dyed as a cloth for clothing, and the fabric has good appearance and excellent product quality. The lower limit is not particularly limited, but is practically 0.3% or more.
The polyamide multifilament of the present invention preferably has a coefficient of variation in elongation under a load of 3cN/dtex of 1.00% or less, more preferably 0.80%, and particularly preferably 0.50% or less. Since the coefficient of variation is 1.00% or less, when an industrial fabric such as an airbag is subjected to a constant load, the elongation of the multifilament is made uniform, which is advantageous in suppressing the displacement of the meshes. Further, since the coefficient of variation is caused by variation in crystal structure, suppression of uneven dyeing is involved in the case of a cloth for clothing. As a means for suppressing the coefficient of variation in elongation under a load of 3cN/dtex to 1.00% or less, it is relatively simple to control the difference between the relative viscosity of sulfuric acid of the used polyamide chips and the relative viscosity of sulfuric acid of the obtained polyamide multifilament. When the difference in viscosity is large, local thickening or hydrolysis due to thermal crosslinking occurs before the raw material chips are converted into yarns. In the thickening, a local increase in the crystal orientation occurs in the fiber longitudinal direction, while in the hydrolysis, a local decrease in the crystal orientation occurs in the fiber longitudinal direction, and thus the elongation tends to vary. The coefficient of variation of the elongation under a load of 3cN/dtex can be determined by the method described in the section of the examples.
The polyamide multifilament of the present invention has a fuzz number of preferably 0 to 3 pieces/kilometer or less, particularly preferably 0 to 2 pieces/kilometer, and more preferably 0 to 1 piece/kilometer. Since the number of piles is small, applications such as airbags, which require excellent pile quality, can be developed. The number of piles is a value obtained by measuring the total number of piles at a filament length of 10 km or more while unwinding at a speed of 150 m/min, and converting the number of piles to 1 km.
The polyamide multifilament of the present invention has preferably 50 or less/cm, that is, 0 to 50/cm, particularly preferably 0 to 30/cm, and more preferably 0.2 to 20/cm, of the number of cells contained in the polyamide filaments constituting the polyamide multifilament. When the number of cells contained in the polyamide filament is more than 50/cm, the strength of the filament containing cells is lowered. This means that air bubbles in the filaments hinder the drawing. In addition, the polymer in the melt excessively absorbs moisture in the air, which causes hydrolysis to occur, and the viscosity of the polyamide to decrease, resulting in insufficient crystal orientation and consequently a decrease in strength. Further, the pile quality is also deteriorated. On the other hand, when the number of the fibers is 0.2 or more, the raw yarn having good pile quality can be obtained by sucking moisture in the air into the molten polymer. As a method for reducing the bubbles, for example, a method in which the pressure of an extruder at the time of extruding the polyamide is set to 20.0 to 80.0kPa can be mentioned.
FIG. 1 is a schematic view of a direct spinning drawing apparatus preferably used in the present invention.
Hereinafter, a method for producing a polyamide multifilament yarn of the present invention will be described with reference to fig. 1 as an example.
First, raw material chips of polyamide, which are raw materials of the polyamide multifilament yarn of the present invention, are prepared. The polymerization method of the polyamide may use a well-known polymerization method.
The sulfuric acid relative viscosity (hereinafter, also simply referred to as "viscosity") of the polyamide raw material scraps used in the polyamide multifilament of the present invention is preferably 2.8 to 3.9, and more preferably 3.3 to 3.9. If the viscosity of the crushed aggregates is 4.0 or more, when the total fineness is within the range defined in the present invention, thickening, thermal deterioration, and gelation due to long-term retention of the polymer result in formation of fine foreign matter, and the fluff quality is deteriorated. When the viscosity of the crushed aggregates is less than 2.8, it is difficult to obtain the polyamide multifilament having the strength specified in the present invention. The relative viscosity of sulfuric acid is a value measured at 25 ℃ with an austenite viscometer using a solution prepared by dissolving 1g of crushed material in 100ml of 98% sulfuric acid and 98% sulfuric acid of undissolved crushed material. The details of the measurement are as described in the items of examples.
When the polyamide multifilament of the present invention is produced by a direct spinning and drawing method, it is preferable that the relative viscosity of sulfuric acid of the polyamide chips used as a raw material is represented by η a and the relative viscosity of sulfuric acid of the polyamide multifilament obtained by spinning is represented by η b | η a- η b | < 0.3. The | η a- η b | is more preferably less than 0.2. For example, polyamide multifilament produced by | η a- η b | < 0.3 can provide polyamide multifilament having excellent pile quality, high tenacity and little variation in elongation at 3% elongation. Although not specifically shown, it is considered that the composition can suppress thickening or thermal deterioration due to long-term retention of the polymer or hydrolysis of the polyamide by satisfying | η a- η b | < 0.3. Further, if the productivity is acceptable, the screening may be performed in an inspection step after the production of the polyamide multifilament.
Next, an example of a production method satisfying the requirement of | η a- η b | < 0.3 is described, in which polyamide chips having the relative viscosity of sulfuric acid are prepared, dried, supplied to an extruder-type spinning machine, and distributed to a spinning spinneret by a metering pump to perform melt spinning. In this case, the pressure in the supply section of the extruder is preferably 20.0 to 80.0kPa, more preferably 40.0 to 60.0kPa, not vacuum (pressure 0.0 kPa), in order to suppress thickening, thermal deterioration, or gelation of the polymer. When the pressure in the supply part of the extruder is less than 20.0kPa, the fluff quality may be deteriorated due to thickening, thermal deterioration, and gelation of the polymer, and a high-strength yarn may not be obtained. When the pressure in the supply part of the extruder is 80.0kPa or more, the number of bubbles contained in the polyamide filaments increases, and a high-strength yarn cannot be obtained even when the hydrolysis reaction of the polymer preferentially proceeds.
Referring to fig. 1, the polyamide discharged from the spinneret 1 preferably passes through a heating tube 2 surrounding the spinneret by 5 to 300cm from directly below the spinneret. The temperature in the heating cylinder is preferably-30 to +30 ℃ and more preferably-15 to +15 ℃ relative to the melting point of the polymer polyamide. By gradually cooling the spun yarn in a high-temperature environment surrounded by the heating cylinder without immediately cooling the spun yarn, the orientation of the melt-spun polyamide molecules can be relaxed, and the uniformity of molecular orientation between single fibers can be improved, thereby making it possible to increase the strength of the polyamide multifilament. On the other hand, if the fiber is immediately cooled without passing through a high-temperature environment, the undrawn yarn becomes highly oriented, and the variation in the degree of orientation among the single fibers becomes large. When the undrawn yarn is subjected to hot drawing, high-strength polyamide multifilament yarn may not be obtained.
The undrawn sliver 5 having passed through the high-temperature environment is cooled and solidified by blowing air at 10 to 80 ℃, preferably 10 to 50 ℃ by a cross-flow cooling device 3. When the cooling air temperature is higher than 80 ℃, the filaments are greatly shaken during spinning, and therefore, the filaments collide with each other, which causes deterioration in yarn formability.
Then, the obtained cooled yarn is supplied with a finish by a well-known finish supply device 4, drawn by a drawing roll 6, and drawn and then wound. The finish agent may be any known finish agent, and the amount of the finish agent to be adhered is preferably 0.3 to 1.5% by weight, more preferably 0.5 to 1.0% by weight, in order to suppress the entanglement of filaments on the pulling roll 6.
The spinning speed defined by the rotational speed of the drawing roll 6 is preferably 500 to 1200 m/min, more preferably 600 to 800 m/min. When the spinning speed is 500 m/min or more, the final production speed is sufficient, the productivity is good, and the polyamide multifilament yarn can be produced at low cost. When the average particle diameter is 1200 m/min or less, the occurrence of yarn breakage or fuzz can be suppressed, and the preferred range is. The stretching speed represented by the maximum speed of the stretching roll is preferably 2800 m/min or more, and more preferably 3000 m/min or more.
The spun yarn obtained by these methods can be subjected to stretching, relaxation heat treatment, winding, and the like by a known method. Specifically, in the case of 2-stage drawing, the spun yarn drawn by the drawing roll 6 (1 FR) is wound around a yarn supply roll 7 (2 FR), a 1 st drawing roll 8 (1 DR), a 2 nd drawing roll 9 (2 DR), and a relax roll 10 (RR) in this order, subjected to heat treatment and drawing, and wound on a winder 11.
The pre-drawing stretching is performed between 1FR and 2FR, the 1 st stretching is performed between 2FR and 1DR, and the 2 nd stretching is performed between 1DR and 2 DR. The temperature of 2FR is set to 30-50 ℃ and the temperature of 1DR is set to 100-225 ℃, and the pre-drawing and the 1 st stage drawing are preferably performed by thermal drawing at about the glass transition temperature. The other stretching and heat-setting temperatures are generally preferably carried out at a temperature in the range of 180 to 240 ℃ and more preferably 200 to 220 ℃.
The total draw ratio (hereinafter, also simply referred to as "draw ratio"), that is, the ratio at the time of drawing between the drawing rolls 6 and the 2 nd drawing roll 9, is preferably a high draw ratio in order to obtain a high-strength polyamide multifilament, and if the fineness is within the range of the fineness described in the present invention, the drawing may be carried out at 3.8 to 5.0 times. The winding speed is usually preferably 2000 to 5000 m/min, more preferably 2500 to 4500 m/min. Further, it is preferable to wind the yarn into a flat package by a winding device under a winding tension of 20 to 250 gf.
By using the method described above, thickening, thermal deterioration, gelation, and hydrolysis of the polyamide polymer can be suppressed, and the influence of mechanical properties due to bubbles is small, and even when the total fineness is as small as 150dtex or less, a polyamide multifilament having high strength and high elongation, that is, high toughness and good quality can be obtained.
Examples
The present invention will be described in detail below with reference to examples. However, the present invention is not to be construed as being limited to the embodiments specifically shown in the examples. The definition and measurement of each characteristic in the present invention are as follows.
(1) Relative viscosity of sulfuric acid (. Eta.r): a sample of crushed polymer or raw yarn was dissolved in 0.25g of 98% sulfuric acid (25 ml), and the solution was measured at 25 ℃ using an Ostwald viscometer and determined by the following formula. The measurement values were obtained from the average values of 5 samples.
η r = seconds of flow-down of the sample solution/seconds of flow-down of only sulfuric acid.
(2) Total fineness: measured according to JIS L1090 (1999).
(3) Number of single fibers: it was calculated by the method of JIS L1013 (1999) 8.4.
(4) Single fiber fineness: the total fineness was calculated by dividing the total fineness by the number of single fibers.
(5) Strength, elongation: measured under the conditions of constant-speed elongation as shown in the JIS L1013 (1999) standard 8.5.1 test. A multifilament sample was subjected to a test using a universal Tester (TENSILON) UCT-100 (available from ORIENTEC corporation) at a holding interval of 25cm and a drawing speed of 30 cm/min. The strength was determined from the maximum strength in the S-S curve, the elongation was determined from the elongation at the point in the S-S curve representing the maximum strength, and the strength was determined by dividing the strength by the total fineness. The multifilament sample was sampled at 1m intervals in the longitudinal direction, and the measurement was performed at 5 points, and the average value was obtained from the measurement data.
(6) Uneven yarn (U%): using USTER TESTER IV manufactured by zellweger ster, the sample length: 500m, measurement of yarn speed: the measurement was carried out at 25m/min and 1/2 insert.
(7) Coefficient of variation in elongation under 3cN/dtex load: the SS curve was obtained under the same conditions as in the measurement of strength and elongation in (5) above, and the elongation at the time of application of a load of 3cN/dtex was obtained. In the measurement, the multifilament sample to be measured was sampled at 1m intervals in the fiber length direction, measured at 10 points, and the average value and standard deviation were calculated from the measurement data and obtained by the following formula.
Coefficient of variation = [ standard deviation ]/[ mean ] × 100 (%).
(8) The number of the fluff: the fiber package was unwound at a speed of 150 m/min, and a laser fluff detector "Flytec V" manufactured by HEBERLIN corporation was installed at a distance of 2m from the unwinding sliver to evaluate the total number of fluff detected. The evaluation was performed on multifilaments of 10 km or more and expressed in terms of the number per 1 km.
(9) Number of bubbles: the number of bubbles observed was evaluated by using a lens having a magnification of 1000 times under a microscope "VHX-5000" manufactured by KEYENCE. When a bubble is present in the fiber, a portion that inhibits stretching from the bubble as a starting point is generated, and therefore, the bubble is observed with an optical lens having a magnification of 1000 times, and then the stretch-inhibited portion is confirmed with a polarizing lens, and the bubble is confirmed. A sample was taken in which fibers of the same length were cut out from all the polyamide filaments constituting the polyamide multifilament yarn. However, the sampling was performed so that the total length of the cut fibers became 100cm. The cut-out samples were observed, and the total number of bubbles was expressed in terms of the number per 1 cm. The cut sample does not need to be strictly 100cm as long as the total length to be measured is 100cm.
(example 1)
A 5 wt% aqueous solution of copper acetate was added as an antioxidant to nylon 66 crushed material obtained by liquid phase polymerization, and mixed, and the mixture was adsorbed so that 68ppm of copper was added to the polymer weight. Next, a 50 wt% aqueous solution of potassium iodide and a 20 wt% aqueous solution of potassium bromide were added and adsorbed so that the potassium content became 0.1 wt% with respect to 100 parts by weight of the polymer chips, and the resultant was solid-phase polymerized using a batch type solid-phase polymerization apparatus to obtain nylon 66 pellets having a sulfuric acid relative viscosity of 3.75. The obtained nylon 66 pellets were fed to an extruder having a diameter of 110mm, and melted at a melting temperature of 300 ℃ under an environment of a pressure of 50.0kPa at the feeding part of the extruder. The molten polymer was distributed to a spinning pack by adjusting the discharge amount with a metering pump so that a multifilament yarn having a total fineness of 80dtex could be obtained. Then, the fiber was filtered through a nonwoven metal fabric filter having a roughness of 40 μm in a spinning pack, and then spun through a spinneret having a circular hole and a hole number of 24 using the apparatus having the structure shown in fig. 1. A heating cylinder with a heating cylinder length of 20cm is arranged below the spinneret surface, and the spinneret is heated until the ambient temperature in the cylinder reaches 250 ℃. The ambient temperature in the cylinder here means the air temperature in a portion 1cm away from the inner wall in the center of the heating cylinder length. A cross-flow type smoke jet blowing air from one direction was installed just below the heating cylinder, and a cold air of 18 ℃ was blown to the sliver at a speed of 35 m/min to cool and solidify the sliver, and then a yarn finish was applied thereto.
The undrawn yarn having the finish applied thereto was wound around 1FR rotating at a surface speed of 800 m/min and drawn, and then drawn at a total draw ratio of 4.3. The drawn sliver was continuously drawn at 5% between the drawing roll and 2FR without being temporarily wound, and then the 1 st stage drawing was performed at a rotation speed ratio of 2.80 times, and further the 2 nd stage drawing was performed at a rotation speed ratio of 1.46 times, and the drawn sliver was wound at 3400 m/min. The roll surfaces of 1FR and 2FR were mirror finished, the roll surfaces of 1DR, 2DR and RR were roughened, and the roll temperatures were: 1FR, 2FR, 1DR, 150 deg.C, 2DR, 225 deg.C, and RR, respectively, were unheated, 40 deg.C, 150 deg.C, and 150 deg.C. The melt spinning and drawing were carried out to obtain nylon 66 multifilament. The interlacing process is performed by jetting high-pressure air to the running sliver from a right-angle direction in the interlacing device. Guides for regulating the advancing yarn are provided before and after the entanglement imparting device, and the pressure of the air to be jetted is a fixed value of 0.2 MPa.
(examples 2 to 5)
The same procedure as in example 1 was repeated, except that the total fineness and total draw ratio of the polyamide multifilament were changed to table 1.
(examples 6 to 8)
The same procedure as in example 1 was repeated, except that the number of filaments of the polyamide multifilament yarn was changed to table 1.
(examples 9 to 10)
The same procedure as in example 1 was repeated, except that the total stretching ratio was changed to table 1.
(examples 11 to 12)
The procedure of example 1 was repeated, except that the pressure in the supply part of the extruder and the total draw ratio were changed to those in table 1.
Table 1 shows the results of evaluating the physical properties of the polyamide multifilaments obtained in examples 1 to 12.
As is clear from table 1, the polyamide multifilaments of the present invention have a fine fineness and high strength, but have good pile quality.
The polyamide multifilament yarn of the present invention was produced in examples 1 to 5 with various total fineness. As compared with examples 11 and 12 and comparative examples 1 to 5 described below, thickening can be suppressed by melting the polymer under an environment of a pressure of 50.0kPa at the supply part of the extruder, and the objective polyamide multifilament can be obtained. Further, the total fineness is reduced and the single fiber fineness is reduced, which is more advantageous for cooling, and the tensile strength product of the polyamide multifilament tends to be increased. On the other hand, if the single fiber fineness is too small as in example 8, the uniform cooling by the chimney wind becomes insufficient, and the influence on the yarn unevenness (U%) is exhibited. Examples 11 to 12 were each a yarn made at 25.0kPa and 75.0kPa, respectively, based on the pressure at the supply part of the extruder. The thickening or hydrolysis tendency from the crushed pieces to the multifilament was observed, and the influence of the coefficient of variation on the elongation under a load of 3cN/dtex was observed.
(reference example 1)
The procedure of example 1 was repeated, except that the total fineness of the polyamide multifilament yarn was 175dtex, and the yarn was melted under an environment of 0.0kPa at the feeding part of the extruder.
Comparative examples 1 and 2
The same procedure as in reference example 1 was repeated, except that the total fineness of the polyamide multifilament yarn was changed to 110dtex, and the total draw ratio was changed as shown in Table 2.
Comparative examples 3 to 4
The same procedure as in reference example 1 was repeated, except that the total fineness of the polyamide multifilament yarn was changed to 80dtex, and the total draw ratio was changed to that shown in Table 2.
Comparative example 5
The same procedure as in comparative example 4 was repeated, except that the pressure in the supply part of the extruder and the total draw ratio were changed as shown in Table 2.
(reference example 2)
The physical properties of a polyamide multifilament yarn for general clothing produced as described in example 1 of International publication WO2016/076184 are shown as reference example 2.
Table 2 shows the results of evaluating the physical properties of the polyamide multifilaments obtained in comparative examples 1 to 5 and reference examples 1 and 2.
Reference example 1 produced a polyamide multifilament having a total fineness of 175dtex, and it was found that the polymer was melted under vacuum (under an environment of 0.0kPa of pressure at the feeding part of the extruder), and therefore, the polymer was thickened to some extent. However, since the total fineness is large, the object of the present invention is not sufficient to achieve good production efficiency, weight reduction of industrial materials such as airbags, and improvement of durability of cloth for clothing.
In comparative example 1, although a polyamide multifilament having a total fineness of 110dtex was produced in the same manner as in reference example 1, it was not possible to produce a yarn at this time. In comparative example 2, the same polyamide multifilament as in comparative example 1 was produced at a draw ratio of 3.6, and as a result, a yarn could be produced. However, the obtained polyamide multifilament yarn is thickened, thermally deteriorated, lost in strength due to long-term retention of the polymer, and generates much fluff.
In comparative example 3, a polyamide multifilament having a total fineness of 80dtex was produced under the same yarn-making conditions as in comparative example 2, but in this case, yarn-making was impossible. In comparative example 4, the draw ratio in comparative example 3 was reduced to 3.2 times, and yarn was produced. However, the obtained polyamide multifilament yarn is thickened, deteriorated, and loses strength due to long-term polymer retention, and generates much fluff. It is understood that, as compared with comparative examples 1 and 2, comparative examples 3 and 4 have a smaller fineness, the retention time of the polymer increases, thickening of the polymer becomes more remarkable, and the stretchability of the polymer is lost, so that yarn formation at a high draw ratio cannot be performed.
In comparative example 5, the production was carried out in the same manner as in example 1 except that the polymer was melted under an environment of an extruder supply pressure of 101.3kPa, but the hydrolysis reaction of the polymer became remarkable at this time, and as a result, the viscosity of the multifilament was considerably lower than that of the crushed material. Further, the amount of bubbles in the yarn increases, so that much fluff is generated, and the strength specified in the present invention cannot be achieved.
Reference example 2 is an example of producing a polyamide multifilament yarn in a general facility for producing fibers for clothing according to the description of WO 2016/076184. In this case, it is found that the polymer hardly thickens because the residence time of the polymer is short, as compared with the case of using a general facility for producing fibers for industrial materials. On the other hand, since the number of stretching stages is 1 stage and the stretching is performed at a low magnification, the strength is insufficient, and the crystal structure tends to be easily deviated in the fiber length direction, and the influence of the coefficient of variation with respect to the elongation under a load of 3cN/dtex is greatly exhibited.
Possibility of industrial utilization
The polyamide multifilament of the present invention has a fine fineness, high strength, and good pile quality, and therefore is suitable for mainly reducing the weight of industrial materials such as airbags and improving the durability of clothes.
Description of the figures
1: spinning spinneret
2 heating cylinder
3: cross flow cooling device
4: oil supply device
5, sliver
6: pulling roll (1 FR)
Yarn supply roller (2 FR)
8: 1 st drawing roll (1 DR)
9: 2 nd stretching roll (2 DR)
10 Relaxation Roller (RR)
11: winder
Claims (5)
1. A polyamide multifilament comprises polyamide, has a total fineness of 30 to 150dtex, a strength of 7.5 to 10.0cN/dtex, and an elongation of 15.0 to 35.0%.
2. A multifilament polyamide yarn comprising a polyamide, having a total fineness of 50 to 120dtex, a strength of 8.0 to 9.7cN/dtex, an elongation of 17.0 to 30.0%, and a coefficient of variation in elongation under a load of 3cN/dtex of 1.00% or less.
3. The polyamide multifilament yarn according to claim 1 or 2, having a fluff number of 0 to 3/km.
4. The polyamide multifilament according to any one of claims 1 to 3, wherein the number of air bubbles contained in the polyamide filaments constituting the polyamide multifilament is 50/cm or less.
5. A process for producing a polyamide multifilament according to claim 1 or 2, comprising the steps of preparing polyamide chips and producing a yarn by a direct spin-draw method,
when the relative viscosity of sulfuric acid of the crushed polyamide is defined as eta a and the relative viscosity of sulfuric acid of the multifilament polyamide obtained by filament-making is defined as eta b, | eta a-eta b | < 0.3.
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| JP2020-139838 | 2020-08-21 | ||
| JP2020139838 | 2020-08-21 | ||
| PCT/JP2021/029073 WO2022039033A1 (en) | 2020-08-21 | 2021-08-05 | Polyamide multifilament, and method for manufacturing same |
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| CN115803484A true CN115803484A (en) | 2023-03-14 |
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| CN202180049017.4A Pending CN115803484A (en) | 2020-08-21 | 2021-08-05 | Polyamide multifilament yarn and process for producing the same |
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| Country | Link |
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| US (1) | US20230279586A1 (en) |
| EP (1) | EP4202093A1 (en) |
| JP (1) | JPWO2022039033A1 (en) |
| CN (1) | CN115803484A (en) |
| TW (1) | TW202219342A (en) |
| WO (1) | WO2022039033A1 (en) |
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| US20230279586A1 (en) | 2023-09-07 |
| WO2022039033A1 (en) | 2022-02-24 |
| JPWO2022039033A1 (en) | 2022-02-24 |
| TW202219342A (en) | 2022-05-16 |
| EP4202093A1 (en) | 2023-06-28 |
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