CN103882550B - Coldness sense polyamide fiber - Google Patents

Coldness sense polyamide fiber Download PDF

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Publication number
CN103882550B
CN103882550B CN201210565284.XA CN201210565284A CN103882550B CN 103882550 B CN103882550 B CN 103882550B CN 201210565284 A CN201210565284 A CN 201210565284A CN 103882550 B CN103882550 B CN 103882550B
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fiber
creeping chill
fypro
polyvinylpyrrolidone
coldness
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CN103882550A (en
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黄儒
藤森稔
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Toray Fibers and Textiles Research Laboratories China Co Ltd
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Toray Fibers and Textiles Research Laboratories China Co Ltd
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Abstract

The invention discloses a coldness sense polyamide fiber and its making method. The coldness sense polyamide fiber comprises a polyamide polymer and inorganic metal oxide particles with the average particle size of 0.1-1.0mum, and the inorganic metal oxide particles contain a silicon element, an aluminum element and a potassium element, and the amounts of the silicon element, the aluminum element and the potassium element account for 0.23-2.3wt%, 0.21-2.1wt% and 0.083-0.83wt% of the total weight of the fiber respectively. Preferably, the fiber contains 3.0-10.0wt% of polyvinylpyrrolidone. The fiber has the advantages of coldness sense, good strength and elongation, and excellent moisture absorption performance.

Description

A kind of creeping chill Fypro
Technical field
The present invention relates to a kind of creeping chill Fypro.
Background technology
As terrestrial climate is gradual warmed up, gradually paid attention to by people with functional fabric.Especially hot humid In summer, requirement of the human body to environment temperature is reduced to reach it is desirable to wear the clothing of hydroscopic fast-drying of some nice and cool property.In recent years, As the fabric of summer, have studied using nice and cool sensation is caused when wearing, assign the fibre of the highly cool to touch of refrigerant sense The fabric of dimension, as the method for the fiber that such highly cool to touch is obtained, implement in the past the water imbibition that improves fiber or Method of conductivity of heat of fiber etc. is improved, or the hydrophily such as carboxyl or carboxyl Jede resin fibre can be introduced, can also drawn Enter the fiber containing the resin for being mixed into conductivity of heat filler high or fiber of plating treatment etc. is implemented to surface.However, making With the occasion of such fiber, although can obtain contact coldness in theory really, but actually enter the function experiment of pedestrian When, it is no actually to feel contact coldness substantially with common fiber without anything different.
Chinese patent CN102331581A discloses a kind of manufacture method of super cool health-care polyester fiber, the spy of the technique It is to use inorganic super cool cool feeling master batch to be blended with percentage by weight 8%~15% and polyester slice to levy, through the super nice and cool guarantor of spinning Strong polyester fiber, wherein inorganic super cool cool feeling master batch is that zinc oxide and far-infrared material are in certain proportion by sheet mica After mixing, then master batch is obtained with polyester melt blending.However, containing substantial amounts of porous, inorganic powder particle, its result is to feel Or skin sense of touch produces harmful effect, does not have good comfortableness.
Chinese patent CN201110325475.4 disclose a kind of ice-cold polyester fiber of cross normal atmosphere cation-dyeable and Its manufacture method, the technique is characterized in carry out melt blending spinning using the ice-cold master batch of mica and normal pressure cation dyeable polyester Silk, the content of mica powder is 0.8-1.5%, the cross normal atmosphere cation-dyeable for obtaining is sprayed through cross spinneret ice-cold Polyester fiber.But, although good dyeability has been obtained, but the fiber of reality is no can to feel contact coldness.Simply The theoretic effect that can obtain contact coldness.
The content of the invention
It is an object of the invention to provide a kind of creeping chill and holding good strength and elongation and excellent hygroscopic Fypro.
Creeping chill fiber of the invention at least contains the metal that polyamide polymers and average grain diameter are 0.1~1.0 micron Oxide inorganic particle, contains in the metal oxides inorganic particle and accounts for the silicon unit that total weight of fibers is respectively 0.23~2.3wt% The potassium element of element, the aluminium element of 0.21~2.1 wt% and 0.083~0.83wt%.
What the polyamide polymers can be enumerated has nylon 6, nylon66 fiber and their modified copolymer etc..
In creeping chill Fypro of the invention, preferably also contain relative to the poly- second that total weight of fibers is 3.0~10.0wt% Alkene pyrrolidone;It is preferred that the constitutional repeating unit of polyvinylpyrrolidone is:
,
The K values of the polyvinylpyrrolidone are 20~70.
The creeping chill Fypro of polyvinylpyrrolidone be with the addition of compared to the creeping chill for being not added with polyvinylpyrrolidone Fypro, the hydroscopicity difference parameter value of its fabric improves 2%.With more preferable moisture pick-up properties, the hydroscopicity of its fabric Difference parameter value is 4%~6%.
Creeping chill Fypro of the invention, its form can be preoriented yarn POY or false twist yarn DTY.
Orientation degree Δ n=0.03~0.04 of preoriented yarn POY.
False twist yarn DTY meets following condition:
A. boiling water shrinkage≤10%,
B.20%≤flexible return rate(CR)≤50%.
Creeping chill fiber of the invention, can be manufactured by following method and obtained:Polyamide polymers feeding screw rod is squeezed While press, the master batch of at least containing metal oxide inorganic particulate is fed the import of screw extruder, spinning or further Creeping chill Fypro is obtained after processing.
Preferably:While polyamide polymers are fed into screw extruder, by containing metal oxide inorganic particulate Master batch and polyvinylpyrrolidone master batch feed the import of screw extruder, spinning or obtain creeping chill polyamides after being processed further Amine fiber.
Specifically, creeping chill Fypro of the invention, can be using any known melt spinning method, first spinning Preoriented yarn POY is obtained, also further false twisting processing false twist yarn DTY can be obtained.Spinning speed is 1500-4000m/min, false Elongating temperature is 150~180 degree when twisting with the fingers processing, and extension ratio is 1.20~4.00, and process velocity is 500~1000m/min.
It is described in detail below:
Polyamide polymers section is dried to below moisture 300ppm in drying machine, and puts into feed bin, gold will be contained Belong to the master batch of oxide inorganic particle or the master batch and polyvinylpyrrolidone master batch of containing metal oxide inorganic particulate through small powder Storehouse is melted into screw rod at a temperature of 250~300 DEG C, and its discharge-amount is controlled by measuring pump, and temperature is controlled by by spinning manifold Filament spinning component under the conditions of 250~300 DEG C, spins as-spun fibre, is cooled down under the conditions of 15~40m/min of cross air blasting wind speed solid Chemical conversion type, then make the collection of filaments and reduce friction through fiber uniformly oils to oil nozzle, oil addition is 0.5~1.5%.
The fiber that oil supply boundling is over passes through spinning shaft, into first roller(1GR), then through around the second roller(2GR) Prepared preoriented yarn POY is batched into coiling machine afterwards, the coiling speed of coiling machine is 1500~4000m/min.
Gained preoriented yarn POY further by following methods can be made false twist yarn DTY.
Obtained preoriented yarn POY is processed on false twisting machine, process velocity is 500~1000m/min, elongating temperature is 150~180 DEG C, extension ratio be to carry out false twisting processing under conditions of 1.20~4.00, false twist yarn DTY is obtained.
Hydroscopicity is determined after being made volume thing or fabric with gained false twist yarn DTY poor(ΔMR).The suction of fiber of the invention Wet rate difference can reach 2%~6%, with good moisture pick-up properties.
Due to containing inorganic particulate in creeping chill fiber, there is good heat conductivity.Use the fabric of the creeping chill fibre spinning There is more preferable cold-type yellow (clear) relative to common fabric.Fabric using the fiber weaving can effectively make temperature relative to common fabric Decline 1.5~2.2 degree, and good strength and elongation can be kept.Meanwhile, the manufacture method of the fiber is applicable existing disclosed various Melt spinning method, and without heavy metal, belong to the green fiber being safe from harm to environment, effectively can largely produce.
The method of testing of the parameter being related in the present invention is as follows:
1. absorb-discharge humid parameter, Δ MR(Hydroscopicity is poor):
(1)3 parts of the fabric sample of about 1g weight is chosen, is placed in the measuring cup of known quality, be put into 60 DEG C In drying machine, bottle cap is taken down, after preparation is dried 30 minutes, cover bottle cap and take out measuring cup;
(2)Measuring cup is put into the constant temperature and humidity machine of 20 DEG C × 65%RH environment, bottle cap is taken down, balance is covered after 24 hours Upper bottle cover, takes out measuring cup, is weighed using precision balance, and the quality for claiming subtracts the quality as sample weight W1 of measuring cup;
(3)Measuring cup is put into the constant temperature and humidity machine of 30 DEG C × 90%RH environment, bottle cap is taken down, balance is covered after 24 hours Upper bottle cover, takes out measuring cup, is weighed using precision balance on the same stage, and the quality for claiming subtracts the quality as sample weight of measuring cup W2 ;
(4)Measuring cup is placed in 105 DEG C of drying machine, bottle cap is taken down, after drying 2 hours, bottle cap is covered and is taken out, and In drying basin after normal temperature cooling, weighed using precision balance on the same stage, the quality for claiming subtracts the quality as sample weight of measuring cup Amount W3;
(5)Calculate:
MR1=(W1-W3)/W3
MR2=(W2-W3)/W3
Hydroscopicity difference △ MR(%)=MR2-MR1, as a result takes 3 average values of sample.
2. the constituent content mensure method in fiber:
Tester:ICAP-6500 types(Thermo Scientific are manufactured)
ICS-2000(Dionex is manufactured)
Method of testing:Al, Si element:Alkali fusion after ashing, ICP is tested after acid is extracted;
K element:ICP tests are extracted in acid after ashing.
3. the average particle size of the dispersion of inorganic particulate:
The surface of fiber and section are observed by scanning electron microscope sem or transmission electron microscope TEM, obtain electronic image, The average particle size of the dispersion of inorganic particulate is obtained by winrof software processings again.
4. polyvinylpyrrolidone K values
Polyvinylpyrrolidone is made the aqueous solution that mass concentration is 1%, its relative viscosity is determined, then use Fikentscher calculates its K value,
logZ=C[75K2/ (1+1.5KC)+K],
Wherein K:K value × 103, C:Concentration of aqueous solution(W/V%), Z:Concentration is the relative viscosity of the aqueous solution of C.
5. fabric face reduces the assay method of temperature:
Determining instrument:KES-7, infrared induction temperature camera
Determination step:The heat of setting is stored on 10cm × 10cm areas, the hot plate of certain mass, thermal settings are behaved 33 degree of body skin temperature, area is placed on the surface of hot plate for the test portion of 20cm × 20cm, after the contact of test portion surface, using red Outer sensing temperature camera determines the temperature change on test portion surface.The shooting time of infrared induction temperature camera is 5min, is clapped Take the photograph at intervals of 5sec, final fabric face reduction temperature(MAX)Computing formula:
Fabric face reduction temperature=hot plate design temperature-fabric face minimum temperature.
6. the orientation degree assay method of preoriented yarn POY:
Determining instrument:Petrographic microscope, magnification of ocular 10X 40X
Assay method:The POY for needing to determine is fabricated to test sample using paraffin solution;
(1)The reading of monofilament fineness degree is read in test(d)
(2)Monofilament is adjusted to level, analyzer is moved into light path, load is rotated after the pivoted loop of analyzer is turned into 45 degree of positions Thing platform, and sample is transferred to about 45 degree of direction Rotational analysis mirror pivoted loops(Analyzer), it is set to the striped that 0 degree of checks otch Number(X)
(3)The pivoted loop of analyzer is rotated counterclockwise, the condition line in the middle of yarn forms a black line, record analysis The reading of mirror angle(θ)
(4)Calculated relationship:
Use eyepiece string diameter d and D relations
10 × → D=d × 10
40 × → D=d × 2.5
λ=546nm(Constant)
Calculating formula
Δ n=R/D.
7. boiling water shrinkage and flexible return rate assay method
Use the boiling water shrinkage and flexible return rate of the standard test yarns of JIS L 1013.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
By nylon 6 slice drying to below moisture 300ppm, silica, alundum (Al2O3), the nothing of potassium oxide will be contained Machine particle master batch feeds screw extruder import, and section is melted into screw extruder through feed bin at a temperature of 255 DEG C, by measuring Pump controls its discharge-amount, and filament spinning component of the temperature under the conditions of 255 DEG C is controlled by by spinning manifold, spins as-spun fibre, Shaping is cooled and solidified under the conditions of cross air blasting wind speed 25m/min, then is made the collection of filaments and is reduced through fiber uniformly oils to oil nozzle Friction, oil addition is 0.9%.The fiber that oil supply boundling is over passes through spinning shaft, into first roller(1GR), speed is 1500m/min, then be second roller of 1500m/min through around speed(2GR)Afterwards prepared orientation degree Δ n=is batched into coiling machine 0.03 preoriented yarn POY, the coiling speed of coiling machine is 1500m/min.
Obtained preoriented yarn POY is processed on false twisting machine, and process velocity is 500m/min, elongating temperature is 160 degree, prolongs Multiplying power is stretched to carry out under conditions of 3.55 extending false twisting processing, and false twist yarn DTY is obtained.Test obtains false twist yarn DTY degree of stretching and reaches 32.3%, intensity reaches 4.06dtex/cN, and hydroscopicity difference is 2.0%, and boiling is received as 5.2%, CR is 37.1%.Fiber in the present embodiment In the average particle size of the dispersion of inorganic particulate that contains obtain being 0.5 micron that and silicon content is in fiber by test 0.23wt%, aluminium element content is 0.21wt%, and Determination of Potassium is 0.083wt%.Spinning is used with fiber false twist yarn DTY100% The fabric of system, shoot test to obtain fabric face reduction temperature using infrared induction temperature camera is 1.5 degree.
Embodiment 2
By nylon 6 slice drying to below moisture 300ppm, polyvinylpyrrolidone master batch and contain silica, three oxygen Change two aluminium, the inorganic particulate master batch feeding screw extruder import of potassium oxide, section enters screw extruder at 255 DEG C through feed bin At a temperature of melt, its discharge-amount is controlled by measuring pump, control spinning group of the temperature under the conditions of 255 DEG C by by spinning manifold Part, spins as-spun fibre, under the conditions of cross air blasting wind speed 25m/min cool and solidify shaping, then through to oil nozzle by fiber it is uniform on Oil makes the collection of filaments and reduces friction, and oil addition is 0.9%.The fiber that oil supply boundling is over passes through spinning shaft, into first sieve Draw(1GR), speed is 1500m/min, then is second roller of 1500m/min through around speed(2GR)Batched into coiling machine afterwards The preoriented yarn POY of orientation degree Δ n=0.03 is obtained, the coiling speed of coiling machine is 1500m/min.
Obtained false twist yarn DTY is processed on false twisting machine, and process velocity is 500m/min, elongating temperature is 160 DEG C, extends Multiplying power is to carry out extending false twisting processing under conditions of 3.35, and false twist yarn DTY is obtained.Test false twist yarn DTY obtains degree of stretching and reaches 34.5%, intensity reaches 3.92dtex/cN, and hydroscopicity difference is 4.3%, and boiling is received as 6.3%, CR is 32.3%.Fiber in the present embodiment In the average particle size of the dispersion of inorganic particulate that contains obtain being 0.3 micron by test, and polyvinylpyrrolidone in fiber Content is 5wt%, and silicon content is 0.23wt%, and aluminium element content is 0.21wt%, and Determination of Potassium is 0.083wt%.With this Fiber false twist yarn DTY100% is shot test and is obtained fabric face drop using the fabric of spinning using infrared induction temperature camera Low temperature is 1.5 degree.
Embodiment 3
Spinning is carried out with embodiment 2, carries out extending false twisting processing under conditions of being further 3.15 in extension ratio, be obtained False twist yarn DTY, test obtains degree of stretching and reaches 30.5%, and intensity reaches 3.78dtex/cN, and hydroscopicity difference is 6.0%, and boiling receipts are 7.5%, CR are 38.3%.It is 0.3 that the average particle size of the dispersion of the inorganic particulate contained in fiber in the present embodiment is obtained by test Micron, and polyvinyl pyrrolidone content is 10wt% in fiber, and silicon content is 0.23wt%, and aluminium element content is 0.21wt%, Determination of Potassium is 0.083wt%.With fiber false twist yarn DTY100% using the fabric of spinning, infrared induction is used It is 1.5 degree that temperature camera shoots test and obtains fabric face reduction temperature.
Embodiment 4
Spinning is carried out with embodiment 2, carries out extending false twisting processing under conditions of being further 3.65 in extension ratio, be obtained False twist yarn DTY, test obtains degree of stretching and reaches 34.5%, and intensity reaches 3.66dtex/cN, and hydroscopicity difference is 4.3%, and boiling receipts are 4.7%, CR are 27.4%.It is 0.3 that the average particle size of the dispersion of the inorganic particulate contained in fiber in the present embodiment is obtained by test Micron, and polyvinyl pyrrolidone content 5wt% in fiber, silicon content are 2.3wt%, and aluminium element content is 2.1wt%, Determination of Potassium is 0.83wt%.With fiber false twist yarn DTY100% using the fabric of spinning, imaged using infrared induction temperature It is 2.2 degree that machine shoots test and obtains fabric face reduction temperature.
Comparative example 1
Spinning is carried out with embodiment 2, carries out extending false twisting processing under conditions of being further 3.35 in extension ratio, be obtained False twist yarn DTY, measure obtains degree of stretching and reaches 24.5%, and intensity reaches 3.12dtex/cN, and hydroscopicity difference is 4.3% creeping chill polyester Fiber, the average particle size of the dispersion of the inorganic particulate contained in fiber in the present embodiment obtains being 0.7 micron by test, and fibre Polyvinyl pyrrolidone content is 5wt% in dimension, and silicon content is 4.6wt%, and aluminium element content is 4.2wt%, Determination of Potassium It is 1.66wt%.With fiber false twist yarn DTY100% using the fabric of spinning, shot using infrared induction temperature camera and tested It is 2.4 degree to obtain fabric face reduction temperature.Although the fabric has obvious creeping chill effect, but monofilament strength and elongation occurs It is decreased obviously.
Comparative example 2
Spinning is carried out with embodiment 1, carries out extending false twisting processing under conditions of being further 3.35 in extension ratio, be obtained False twist yarn DTY, test obtains degree of stretching and reaches 41.2%, and intensity reaches 4.15dtex/cN, and hydroscopicity difference is 4.3%, fine in embodiment It is 0.5 micron that the average particle size of the dispersion of the inorganic particulate contained in dimension is obtained by test, and polyvinylpyrrolidine in fiber Ketone content is 5wt%, and silicon content is 0.115wt%, and aluminium element content is 0.105wt%, and Determination of Potassium is 0.0415wt%. With the fiber 100% using the fabric of spinning, shoot test using infrared induction temperature camera and obtain fabric face reduction temperature It is 0.4 degree.The fabric does not have obvious creeping chill effect.

Claims (6)

1. a kind of creeping chill Fypro, it is characterized in that:At least it is containing polyamide polymers and average grain diameter in the fiber 0.1~1.0 micron of metal oxides inorganic particle, the metal oxides inorganic particle is by silica, alundum (Al2O3) With potassium oxide composition, contain in the metal oxides inorganic particle and account for the silicon unit that total weight of fibers is respectively 0.23~2.3wt% The potassium element of element, the aluminium element of 0.21~2.1wt% and 0.083~0.83wt%.
2. creeping chill Fypro according to claim 1, it is characterized in that:The fiber contains The polyvinylpyrrolidone of 3.0~10.0wt%.
3. creeping chill Fypro according to claim 2, it is characterized in that:The repetitive structure of the polyvinylpyrrolidone Unit is:
,
The K values of the polyvinylpyrrolidone are 20-70.
4. creeping chill Fypro according to claim 1 and 2, it is characterized in that:The form of the fiber is preoriented yarn POY or false twist yarn DTY.
5. creeping chill Fypro according to claim 4, it is characterized in that:The orientation degree Δ n=0.03 of preoriented yarn POY ~0.04.
6. creeping chill Fypro according to claim 4, it is characterized in that:False twist yarn DTY meets following condition:
A. boiling water shrinkage≤10%,
B.20%≤flexible return rate≤50%.
CN201210565284.XA 2012-12-24 2012-12-24 Coldness sense polyamide fiber Active CN103882550B (en)

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WO2016108078A1 (en) 2015-09-14 2016-07-07 Rhodia Poliamida E Especialidades Ltda Polyamide fiber with improved comfort management, process thereof and article made therefrom
CN107012529A (en) * 2017-04-25 2017-08-04 福建恒捷实业有限公司 A kind of preparation method of feature nylon-6 fiber
CN110396758B (en) * 2018-04-24 2021-12-17 东丽纤维研究所(中国)有限公司 Cool sense circular knitting surface fabric
CN109778359B (en) * 2018-12-27 2021-07-09 福建鑫森合纤科技有限公司 Production method of nylon stretch textured yarn
CN110129901A (en) * 2019-05-05 2019-08-16 江阴芗菲服饰有限公司 A kind of preparation method of creeping chill fiber
CN113430668B (en) * 2021-06-28 2023-04-11 安踏(中国)有限公司 Ice-feeling quick-drying fiber and preparation method thereof, and ice-feeling quick-drying fabric and preparation method thereof

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JP3804097B2 (en) * 1996-03-29 2006-08-02 東レ株式会社 Support stockings with excellent wearing comfort
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