CN105780188A - Polyester fiber with moisture absorption/desorption performance and preparation method thereof - Google Patents

Polyester fiber with moisture absorption/desorption performance and preparation method thereof Download PDF

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CN105780188A
CN105780188A CN201410821360.8A CN201410821360A CN105780188A CN 105780188 A CN105780188 A CN 105780188A CN 201410821360 A CN201410821360 A CN 201410821360A CN 105780188 A CN105780188 A CN 105780188A
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polyester fiber
polyester
absorb
fiber
poly
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范志恒
吴亚薇
望月克彦
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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 polyester fiber with moisture absorption/desorption performance and a preparation method thereof. The polyester fiber contains polyester with melting point being 200-240 DEG C, poly(N-vinyl lactam), a phosphorous heat stabilizer and a sodium nucleating agent, wherein poly(N-vinyl lactam) accounts for 3-15 wt% of weight of polyester fiber; weighed according to P element, the phosphorous heat stabilizer accounts for 50-500 ppm of weight of polyester fiber; weighed according to Na element, the odium nucleating agent accounts for 10-100 ppm of weight of polyester fiber; and content of antimony element in the polyester fiber is below 5 ppm. By adding a moisture absorption component, the phosphorous heat stabilizer and the sodium nucleating agent into polyester, the moisture-absorption polyester fiber which can be applied to materials for clothing such as underwear, sport suit and the like is obtained.

Description

A kind of absorb-discharge humid polyester fiber and preparation method thereof
Technical field
The present invention relates to a kind of moisture absorption type polyester fiber and preparation method thereof.Specifically, by adding moisture absorbing component, phosphorus system heat stabilizer and sodium nucleator in the polyester, obtain can apply to the moisture absorption type polyester fiber of the dress material material such as underwear, sweat shirt.
Background technology
Polyester fiber is typical thermoplastic synthetic fiber, since being born, excellent due to its mechanical strength, resistance to chemical reagents, thermostability etc., is widely used in terms of dress material and industry.
But, the absorb-discharge humid of polyester fiber is extremely low, it is impossible to discharge sweat in time, when directly contact skin or skin-proximal are worn, has tacky sensation, therefore limits polyester fiber development in interior clothing dress material purposes.
Improving the hygroscopic method of polyester fiber has copolymerization in the polyester to enter moisture absorbing component or interpolation has hygroscopic compound.Such as, during pet reaction, with on side chain there is the glycol copolymerization of hydroxy alkylidene glycol, or with the dicarboxylic acids copolymerization etc. containing metal organic sulfonate.But, there is intensity and the low problem of weatherability in the moisture absorption type polyester fiber that combined polymerization obtains.
Except above by give fibrous raw material polyester with hygroscopicity, make fiber have hygroscopic method in addition to, it is also possible to make hygroscopic compound be attached on polyester fiber by chemical method.Such as during post-treatment, the polyester fiber in fabric is carried out acrylic or methacrylic acid grafting, then replaces carboxyl therein with alkali metal, thus improve the hygroscopicity of polyester fiber.But owing to hygroscopic compound adheres on the fiber surface, in use there is the problems such as intensity declines, feel is bad, light resistance is poor.
Japanese Unexamined Patent Publication 2-99612 disclose a kind of using hygroscopicity resin that hydroscopicity is more than 10% as core, conventional polyester as the sheath-core type conjugate fiber in sheath portion.The fiber obtained in this way is when doing the heat treatment such as refine, dyeing, owing to the hygroscopicity resin of core segment is hygroscopic and expand, can form crackle at fiber surface, and owing to hygroscopicity resin is high and flow outwardly to the dissolubility of water so that hygroscopicity declines.
Patent CN201210379074 discloses polyvinylpyrrolidone is added to the technology improving polyester fiber wettability power in the middle of polyester.This technology inhibits the impact that polyester fiber performance is produced by the interpolation of polyvinylpyrrolidone to a certain extent.But for be directed to use low melting point polymer and the percent thermal shrinkage that brings becomes big, the problem using difficulty in actual applications, solution is not proposed.The creating of wet absorption and discharging fibre the most simultaneously meeting absorb-discharge humid and fibrous physical property is always expected to.
Summary of the invention
It is an object of the invention to provide excellent polyester fiber of a kind of hygroscopicity and preparation method thereof,
The technical solution of the present invention is:
A kind of absorb-discharge humid polyester fiber, containing polyester, poly N-ethylene lactams, phosphorus system heat stabilizer and sodium system nucleator in this polyester fiber, wherein poly N-ethylene lactams accounts for the 3~15wt% of polyester fiber weight;The content of phosphorus system heat stabilizer accounts for the 50~500ppm of polyester fiber weight in terms of P element;The content of sodium system nucleator accounts for the 10~100ppm of polyester fiber weight in terms of sodium element;And in this polyester fiber antimony element content at below 5ppm.
The invention also discloses the preparation method of a kind of above-mentioned absorb-discharge humid polyester fiber, by polyester and poly N-ethylene lactams with the weight ratio of 95:5~60:40, the double screw extruder of use screw diameter 40mm~130mm, L/D40~80 carries out melting mixing, obtains poly N-vinyl lactams and averagely disperses footpath at the master batch polymer of below 300nm;Then mixed with the weight ratio of 60:40~10:90 with polyester by gained master batch polymer in device for spinning, melt spinning prepares moisture adsorption and releasing polyester fiber;In terms of P elements, account for the phosphorus system heat stabilizer of polyester fiber weight 50ppm~500ppm in blended stage or the interpolation of melt spinning stage simultaneously;Containing the sodium system nucleator being equivalent to weight polyester 10~120ppm in terms of sodium element in described polyester, the amount of antimony element is at below 5ppm.
The hygroscopicity parameter, Δ MR of absorb-discharge humid polyester fiber of the present invention, more than 1.0%, has the moisture absorption and desorption property of excellence, tone is good and light fastness well, dry-hot shrinkage is low simultaneously, can preferably be applied to the dress material such as underwear, sweat shirt field.
Detailed description of the invention
The present invention is by adding hygroscopic matter poly N-vinyl lactams in the polyester so that it is differential dissipates in the polyester, thus improves the hygroscopicity of polyester fiber.The fiber excellent in order to obtain excellent color tone, light fastness, also added phosphorus system heat stabilizer in this fiber, and in fiber the content of metallic antimony element at below 5ppm.In addition to the dry-hot shrinkage of suppression fiber, this fiber also added sodium nucleator.
In the described polyester fiber of the present invention, relative to the weight of polyester fiber, the content of poly N-vinyl lactams is 3~15wt%.When in polyester fiber, the content of poly N-vinyl lactams is less than 3wt%, fiber does not have enough hygroscopicity, and practical application is poor;When in polyester fiber, the content of poly N-vinyl lactams is more than 15wt%, fiber has viscous sense, very uncomfortable during contact, and fibrous physical property declines.It is 5~12wt% to make polyester fiber obtain more preferably moisture-absorption characteristics, the preferably content of poly N-vinyl lactams.
Heretofore described poly N-vinyl lactams can be the polymer of the N-vinyl lactam classes such as NVP, N-vinyl-2-piperidones, N-caprolactam.From the standpoint of there is less absorption sterically hindered, easy and release hydrone, in the present invention, as described poly N-vinyl lactams, the polymer of NVP, i.e. polyvinylpyrrolidone (PVP) are preferably used.
In the present invention, it is preferred to the polyvinylpyrrolidone using K value to be 15~90, the polyvinylpyrrolidone more preferably using K value to be 20~70.If the K value of polyvinylpyrrolidone is too low, then polyvinylpyrrolidone is not strong with the complexing power of polyester, and in Cooling Process after the extrusion, easy dissolution, causes fiber to can not get good hygroscopicity.And if its K value is too high, then the viscosity of polyester system is greatly increased, and mixing discharge is bad, is difficult to pelletize, causes production efficiency low.
Possibly together with the phosphorus system heat stabilizer being equivalent to polyester fiber weight 50~500ppm in terms of P element in heretofore described polyester fiber.In the present invention, by adding phosphorus system heat stabilizer, can suppress polyester that thermal degradation and hydrolysis occur when being blended with moisture absorbing component, improve the tone of gained polyester fiber, improve its light fastness.
Described phosphorus system heat stabilizer can be phosphoric acid class, phosphorous acids, phosphonic acid based, phosphoric acid ester etc..Specifically can enumerate have phosphoric acid, trimethyl phosphate, triethyl phosphate, tricresyl phosphate phenolic aldehyde, phosphorous acid, NSC 6513, methyl acid phosphate, phenolic aldehyde phosphoric acid, diphenylphosphoric acid, methyl acid phosphate methyl ester, phenolic aldehyde etherophosphoric acid, diphenylphosphoric acid phenolic aldehyde ester, phosphoryl ethyl acetate, distearyl pentaerythritol diphosphate, double (2; 4 6-tri-tert phenyl) pentaerythritol diphosphate, resorcinol-bis-(two (tetramethylolmethane)) phosphate ester, double (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate or double (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate etc..
Described phosphorus system heat stabilizer is preferably the bisphosphate based compound shown in formula 1:
Formula 1
R in formula1、R2It is each independently the aromatic hydrocarbyl with substituent group.Described aromatic hydrocarbyl is preferably the aromatic hydrocarbyl of C6~C10, and described substituent group can be the alkyl of C1~C6, amino, hydroxyl or sulfo group.Described R1And R2Can be phenyl, the phenyl that meta has the alkyl substituent that carbon number is 1~5, the aryl radical that to alkyl phenyl, can be replaced by amino or the aryl radical etc. that can be replaced by sulfo group.In the present invention, R1、R2It is preferably the one in the group of formula 2 as follows~formula 4 independently of one another:
Formula 2,
Formula 3,
Formula 4.
When bisphosphate based compound shown in above-mentioned formula 1 uses as stabilizer, it is more preferable to the improvement effect of polyester fiber tone, thus becomes preferred.
In bisphosphate based compound shown in above-mentioned formula 1 double (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphate or double (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate is when using as stabilizer, it is especially good to the improvement effect of polyester fiber tone, thus most preferably.
Possibly together with the sodium system nucleator of be equivalent to polyester fiber weight in terms of Na element 10~100ppm in heretofore described polyester fiber, preferred content is 20~60ppm.The poly N-vinyl lactams added as hygroscopic agent in the present invention can suppress the crystalline orientation of polyester fiber to a certain extent, so that the dry-hot shrinkage of fiber becomes big, affects its use during post-treatment.Therefore to improve this unfavorable factor present invention to the addition of sodium system nucleator in the polymerization process of polyester to improve the crystallinity of polyester, thus reduce adverse effect that poly N-vinyl lactams brings so as to get the dry-hot shrinkage of polyester fiber reduce.Described sodium system nucleator can be the various organic carboxylic acid sodium salts such as acetic acid, oxalic acid, propanoic acid, butanoic acid, octanoic acid, dodecyl acid, stearic acid, behenic acid, benzoic acid, p-phthalic acid, benzoic acid, salicylic acid, naphthalene-carboxylic acid, hexahydrobenzoid acid, it is also possible to is the various organic sodium sulfonate salt such as benzene methanesulfonic acid, sulfosalicylic acid, ethylacrylic acid and the sodium salt of methacrylic acid copolymer, the sodium salt of styrene anhydrous maleic acid copolymer, benzylidene sorbitol and derivant thereof etc..The sodium system nucleator of the present invention is also not limited to above example, but the sodium system nucleator of preferred organic carboxylic acid sodium salt's class.
To the polyester used in the present invention, can be aliphatic polyester, it is also possible to be aromatic polyester.Generally, mainly it is made up of binary acid repetitive and dihydroxylic alcohols repetitive.
Dihydroxylic alcohols repetitive can be specifically aliphatic diol or aromatic diol, such as ethylene glycol, propylene glycol, butanediol and isomer thereof, pentanediol and isomer thereof, the straight or branched aliphatic diol of C6~C20 and isomer thereof, bisphenol-A and one or more in oxirane addition product, Polyethylene Glycol, polypropylene glycol, polytetramethylene glycol, cyclobutanediol, ring pentanediol, cyclohexanediol, benzene dimethanol, naphthalene dimethanol etc..
C8~the C18 aromatic acids such as binary acid repetitive can be specifically malonic acid, succinic acid, 1,3-propanedicarboxylic acid, adipic acid, the alicyclic diacids of C7~C20 or its isomer, p-phthalic acid or its esterification derivative, M-phthalic acid or its esterification derivative, other binary acid containing phenyl ring, naphthalene diacid or derivatives thereof.
For using polyester in the present invention, its antimony atoms content the following is essential condition at 5ppm.Catalyst during polycondensation of polyester, what in general antimony oxide was employed is more, in this case in polyester, antimony atoms content is more than 100ppm, and the polyester used in the present invention, the content of its antimony atoms must be at below 5ppm, and now the antimony atoms content in absorb-discharge humid polyester fiber is also at below 5ppm.Finding after the present inventor's research, antimony atoms and poly N-vinyl lactams reaction can cause fibre staining, but the coloring of polyester fiber can well be suppressed when the content of antimony atoms is at below 5ppm, and the tone L-value of fiber is more than 85.In order to make the antimony atoms content in polyester control at below 5ppm, it is possible to use the polymerization catalyst (titanium system, stannum system, germanium system etc.) outside antimony system, or by these catalyst and antimony system polymerization catalyst and be used for realizing.
As the fusing point Tm that the melting point polyester used in the present invention is 200 DEG C~the polyester of 240 DEG C, i.e. polyester more than or equal to 200 DEG C less than or equal to 240 DEG C.Poly N-vinyl lactams at high temperature thermostability is poor, with polyester blend after obtained by fiber tone easily turn yellow.Therefore, in order to prepare the polyester fiber of good hygroscopicity and excellent color tone, processing needs to control to carry out at a lower temperature as far as possible.So selecting the polyester of low melting point can reach this effect.
Described fusing point be 200 DEG C~240 DEG C polyester preferred polyethylene terephthalate system polyester, poly terephthalic acid propylene glycol system polyester, polybutylene terephthalate system polyester.
More preferably possibly together with the polyethylene terephthalate system polyester of diol copolymer unit and/or binary acid copolymerization units, poly terephthalic acid propylene glycol system polyester, polybutylene terephthalate system polyester.
The dihydroxylic alcohols repetitive of copolymerization can be aliphatic diol or aromatic diol, preferably propylene glycol, butanediol, bisphenol-A and one or more in ethylene oxide adduct.
The binary acid repetitive of copolymerization can be aliphatic dibasic acid, aromatic acid or their derivant.Derivant can be the methyl ester of above-mentioned binary acid, ethyl ester, propyl ester etc., the preferably methyl ester of binary acid.Aliphatic dibasic acid is preferably in the representative examples of saturated aliphatic binary acid of carbon number 3~20, most preferably malonic acid, succinic acid, 1,3-propanedicarboxylic acid, adipic acid, Azelaic Acid one or more;Aromatic acid is preferably M-phthalic acid or naphthalenedicarboxylic acid.The copolymerization binary acid repetitive of the present invention is most preferably M-phthalic acid or M-phthalic acid sulfonate salt units.
Described polyester can also be containing sulfonate copolymerization units and/or the polyethylene terephthalate system polyester of polyethers copolymerization repetitive, poly terephthalic acid propylene glycol system polyester, polybutylene terephthalate system polyester.
The sulfonate component of copolymerization can be one or more in M-phthalic acid 5-sodium sulfonate, M-phthalic acid 5-Sulfonic Lithium, M-phthalic acid 5-sulfoacid calcium, ethylene isophthalate 5-sodium sulfonate, ethylene isophthalate 5-Sulfonic Lithium, ethylene isophthalate 5-sulfoacid calcium, dimethyl isophthalate 5-sodium sulfonate, dimethyl isophthalate 5-Sulfonic Lithium, dimethyl isophthalate 5-sulfoacid calcium.
The polyether components of copolymerization can be one or more in Polyethylene Glycol, polypropylene glycol, polytetramethylene glycol.
In the case of not affecting effect of the present invention, described polyethylene terephthalate system polyester, poly terephthalic acid propylene glycol system polyester, polybutylene terephthalate system polyester can also comprise the polyfunctional copolymerization repetitives such as benzenetricarboxylic acid, benzene tetracarboxylic acid, glycerol, tetramethylolmethane.
Described polyester can produce with industrial normally used polymerization, first carries out being esterified or ester exchange reaction, after obtaining the petchem of low-molecular-weight, carries out polycondensation reaction the most further, obtain polyester under high temperature fine vacuum.Can add catalyst in esterification or ester exchange stage, described catalyst is the compound containing metallic elements such as sodium, lithium, magnesium, calcium, manganese, titanium, zinc, cobalt or stannum.The present invention with titanium compound as esterification, ester exchange reaction or the dominant catalyst of polycondensation reaction.Titanium compound includes the titanium alkoxide of tetrabutyl titanate, tetraisopropyl titanate, isopropyl titanate, titanium ethylene glycolate etc.;Ethylenediaminetetraacetic acid, hydroxyethyliminodiacetic acid, diethylene-triamine pentaacetic acid, triethylenetetramine six acetic acid, or as the polyvalent carboxylic acid of chelating agen and/or the titanium complex etc. of hydroxy carboxylic acid and/or nitrogenous carboxyl.Described chelating agen is the hydroxy carboxylic acids of phthalic acid, three sour three monooctyl esters, trimesic acid, benzene-1, pyromellitic acid anhydride etc.;Or containing the ethylenediaminetetraacetic acid of nitronic acid, NTP, carboxyl imido oxalic acid, carboxymethyl imido grpup dipropionic acid, diethylene-triamine pentaacetic acid, triethylenetetramine six acetic acid, imines two acetic acid, imido grpup dipropionic acid, 2-ethoxy-imido grpup acetic acid, 2-ethoxy-imido grpup dipropionic acid, 2-methoxy ethyl-imido grpup acetic acid.Catalyst also includes other metal compound as catalyst, specifically refers to the cobalt compounds such as the magnesium compounds such as the calcium compounds such as calcium acetate, calcium chloride, magnesium acetate, magnesium chloride, magnesium carbonate, cobaltous acetate, cobaltous chloride, cobalt oxide.
The cation dyeable polyester of the construction unit that the polyester of the present invention is most preferably formed by the M-phthalic acid or derivatives thereof with sodium group, and by being processed further the sulfur content preferably 0.1~1wt% in the polyester fiber obtained.When in polyester fiber, sulfur content is the least, polyester fiber does not have cation dyeable;When sulfur content is the biggest, polyester fiber physical property declines, and practical application is poor.In order to make polyester fiber obtain more preferably cation-dyeable characteristic, sulfur content more preferably 0.15%~0.5wt% in polyester fiber.
The invention still further relates to the preparation method of a kind of above-mentioned polyester fiber, in the method, first by polyester and poly N-ethylene lactams with the weight ratio of 95:5~60:40, use screw slenderness ratio L/D double screw extruder more than 40 to carry out melting mixing, obtain master batch polymer.
The average dispersion footpath of poly N-vinyl lactams can be with polyester fiber complexation well at the poly N-vinyl lactams of below 500nm, it is thus possible to the dissolution of suppression poly N-vinyl lactams, the hygroscopicity preventing polyester fiber declines, and improves the moisture absorption durability of polyester fiber.The average dispersion footpath of the present invention preferred poly N-vinyl lactams at below 300nm, more preferably below 150nm.
So that the average dispersion footpath of poly N-vinyl lactams is at below 500nm, the screw diameter of double screw extruder used in the present invention is that 40mm~130mm, draw ratio L/D are more than 40.If draw ratio L/D is less than 40, the dispersion footpath of poly N-vinyl lactams is big, there will be the problems such as frequent fracture of wire, fibrous physical property be bad in spinning process later.
When making master batch polymer, polyester and poly N-ethylene lactams are blended with 95:5~60:40.The ratio of poly N-ethylene lactams is at below 5wt%, and obtained master batch hygroscopicity is not enough, it is impossible to carry out actually used;The ratio of poly N-ethylene lactams is at more than 40wt%, and mixing property is bad, is unfavorable for being smoothed out in spinning.The preferably blending ratio of polyester and poly N-ethylene lactams is 90:10~70:30, more preferably 85:15~75:25.
Described poly N-ethylene lactams preferred K value is the polyvinylpyrrolidone of 15~90.K value polyvinylpyrrolidone within the range and polyester are easier to be blended, strong with the complexing power of polyester, are not easy dissolution, it is possible to obtain the polyester fiber that hygroscopicity is good in the Cooling Process after blending extrusion;It addition, the viscosity stabilization of polyester system after being blended with K value polyvinylpyrrolidone within the range, the problem that will not produce that mixing discharge is bad, pelletize is difficult, production efficiency is low etc..The more preferably K value of polyvinylpyrrolidone is 20~70.
After obtaining the master batch polymer containing poly N-vinyl lactams, mixed with the weight ratio of 60:40~10:90 with polyester by master batch polymer, melt spinning prepares moisture adsorption and releasing polyester fiber;In terms of P elements, account for the phosphorus system heat stabilizer of polyester fiber weight 50ppm~500ppm in blended stage or the interpolation of melt spinning stage simultaneously;Containing the sodium system nucleator being equivalent to weight polyester 10~120ppm in terms of sodium element in polyester described in described polyester, the amount of antimony element is at below 5ppm.Sodium system nucleator, the amount of antimony element is at below 5ppm.
Owing to the vitrification point of most poly N-vinyl lactams is near 170 DEG C, mixing and spinning temperature must set above this temperature, allows poly N-vinyl lactams have good mobility.Therefore, in the present invention, it is preferred to using fusing point is 200 DEG C~the polyester of 240 DEG C, it can be blended at a lower temperature with poly N-vinyl lactams, when mixing, control fusing department temperature is in the range of than melting point polyester temperature high 10~20 DEG C, and kneading part temperature is in the range of 180~230 DEG C.It addition, poly N-vinyl lactams the most easily absorbs water tacky, therefore can also go back blending extrusion machine spout and add water cooling plant, the temperature of control spout is below 80 DEG C, so that feeding is smoothed out.
In the present invention, phosphorus system heat stabilizer can add when blended, it is also possible to adding during melt spinning, its addition is 50ppm~500ppm being equivalent to polyester fiber weight in terms of P element.Preferably add phosphorus system heat stabilizer in the blended stage.Add heat stabilizer in the blended stage, by the shear action in being blended, make heat stabilizer dispersed, can farthest play its thermostable effect to matrix.Meanwhile, homodisperse heat stabilizer will not produce impact to melt spinning afterwards.
In the described method of the present invention, melt spinning is carried out the most at a lower temperature, and specifically, it is preferable to spinning temperature is 220 DEG C~270 DEG C, and more preferably 235 DEG C~260 DEG C.Spinning under lower temperature conditions, it is possible to reduce the decomposes of each blend components, thus obtain the fiber of excellent color tone.
In the present invention, it is preferred to the hygroscopicity parameter, Δ MR of described moisture absorption type polyester fiber is more than 1.0%, hue b value is below 5.0, and light fastness is more than 3 grades.This polyester fiber has the mechanical property of satisfied general dress material fiber, and at its 180 DEG C, dry-hot shrinkage is below 12%.Δ MR refers to the running ability to comfortableness after outwardly being released by the dampness in clothes, when being light~middle operation or light~middle motion, and the moisture absorption rate variance of the extraneous humiture that humiture and 20 DEG C × 65%RH are characterized in the clothes that 30 DEG C × 90%RH is characterized.Absorb-discharge humid evaluation criterion in the present invention utilizes Δ MR as absorb-discharge humid parameter, and Δ MR is the biggest, and absorb-discharge humid is the highest, and corresponding comfortableness when wearing is the best.More than Δ MR1.0%, fiber has good moisture absorption and desorption property and comfortableness.Preferably more than Δ MR1.5%, more preferably more than Δ MR2.0%.
In the present invention, obtained polyester fiber is evaluated using the following method.
(1) poly N-vinyl lactams averagely disperse footpath
With length direction vertically cutting fibre, take individual filament cross section section and carry out ruthenium dyeing, observe with transmission electron microscope (TEM) (100,000 times), shoot blended state.Fiber presents with continuous print matrix composition (white portion) as sea component, with the scattered composition (gray component) in the sub-circular ground island structure as island component.Island component is regarded as circle, converses diameter from island component area.Using this diameter as the dispersion footpath of polyvinyl pyrrolidone constituting island component, using the meansigma methods of 20 island components as averagely disperseing footpath.
(2) poly N-vinyl lactams K value
Poly N-vinyl lactams is configured to the aqueous solution that mass concentration is 1%, measures its relative viscosity, then calculate its K value with fikentscher,
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.
(3) strength and elongation of fiber is amassed and intensity
Strength and elongation amasss=intensity × (degree of stretching)0.5,
Stress/the fiber number (cN/dtex) of maximum disrumpent feelings some when intensity is fibre stress-strained tensile, degree of stretching is the strain (%) of the maximum disrumpent feelings point of fiber.
Intensity, degree of stretching are by JIS L1013:2010 standard test.
(4) hygroscopicity parameter, Δ MR
From fiber, remove degreaser, the sample of about 1g is put into the weighing botle that glass weight is W, is placed in drying machine, be dried 2 hours in 110 DEG C.This weighing botle is sealed, is placed in exsiccator cooling 30 minutes.Measure weighing botle weight W equipped with sample1.Then, put into open state and be set in 20 DEG C, the constant temperature and humidity machine of 65%RH, place 24 hours.Subsequently, more in sealed states in exsiccator place 30 minutes.Then, weighing botle weight W is again measured2.Continue to put into open state to be set in 30 DEG C, the constant temperature and humidity machine of 90%RH, places 24 hours, more in sealed states in exsiccator after placement 30 minutes, then measure weighing botle weight W3,
MR1=(W2-W1) * 100%/(W1-W),
MR2=(W3-W1) * 100%/(W1-W),
Δ MR=MR2-MR1
(5) light fastness
Testing according to Japan's JIS L-0842 standard, progression the highest expression color fastness to light is the best.
(6) hygroscopic matter and the mensuration of content thereof in fiber
Hydrogen spectrum according to nuclear magnetic resonance, NMR records characteristic peak positions and the intensity of hygroscopic matter, extrapolates the content of this hygroscopic matter further according to chemical formula.
(7) tenor in polyester
6g polymer being pressed into lamellar, measures its intensity with fluorescent x-ray analysis apparatus (X-Ray Analyzer 3270 type that electric corporation of science manufactures), the detection line made in advance with the sample of known metal content converts.
(8) 180 DEG C of dry shrinkage
It is measured according to JIS L1013 standard.
(9) tone
It is measured according to JIS Z8729 standard.
Below in conjunction with embodiment, the present invention is further described.
[manufacturing example 1] < common PET-A >
Ethylene glycol 784g, p-phthalic acid 1324g are carried out esterification, then carries out polycondensation reaction.First by whole p-phthalic acids, ethylene glycol 533g, butyl titanate 0.88g, add in the reactor with rectifying column, temperature 250 DEG C, vacuum are to proceed by esterification under conditions of 400mmHg, while slowly heating up, add the ethylene glycol of remnants continuously.Next move to batch condensation polymerization reactor, at vacuum condition and temperature 285 DEG C, carry out polyreaction.
[ manufacturing example 2 ]<copolymerization PET-B>
Ethylene glycol 784g p-phthalic acid 993g M-phthalic acid 331g, sodium system nucleator sodium stearate are carried out esterification, then carry out polycondensation reaction and first whole p-phthalic acids and M-phthalic acid, sodium system nucleator ethylene glycol 533g calcium acetate 1.2g butyl titanate 0.88g are added in the reactor with rectifying column, it is warming up to 235 DEG C of reactions from 130 DEG C and next moves to batch condensation polymerization reactor in 3 hours, under vacuo temperature is risen to 285 DEG C of finishing reactions 4 hours from 240 DEG C
[ manufacturing example 3 ] < copolymerization PET-D >
Replacing the butyl titanate catalyst as reaction with antimony oxide (0.9g), other are with manufacturing example 2.
[ manufacturing example 4 ]<copolymerization PET-E>
Ethylene glycol 784g p-phthalic acid 993g phthalic acid 331g and sodium system nucleator sodium stearate are carried out esterification, then carry out polycondensation reaction and first whole p-phthalic acids and phthalic acid, sodium system nucleator ethylene glycol 533g calcium acetate 1.2g butyl titanate 0.88g are added in the reactor with rectifying column, it is warming up to 235 DEG C of reactions from 130 DEG C and next moves to batch condensation polymerization reactor in 3 hours, under vacuo temperature is risen to 285 DEG C of finishing reactions 4 hours from 240 DEG C
[ manufacturing example 5 ]<copolymerization PET-F>
Replacing M-phthalic acid with 630 grams of bisphenol-A glycol ethers to react, other is with manufacturing example 2.
[ manufacturing example 6 ]<copolymerization PET-H>
Ethylene glycol 784g p-phthalic acid 993g M-phthalic acid 331g, M-phthalic acid-5 sodium sulfonate 80g and sodium system nucleator sodium stearate are carried out esterification, then carry out polycondensation reaction and first whole p-phthalic acids and M-phthalic acid, M-phthalic acid-5 sodium sulfonate sodium system nucleator, ethylene glycol 533g calcium acetate 1.2g butyl titanate 0.88g are added in the reactor with rectifying column, it is warming up to 235 DEG C of reactions from 130 DEG C and next moves to batch condensation polymerization reactor in 3 hours, under vacuo temperature is risen to 285 DEG C of finishing reactions 4 hours from 240 DEG C
PET: polyethylene terephthalate, PTT: PTT, PBT: polybutylene terephthalate (PBT).
Embodiment 1
Copolymerization PET-B 150 DEG C, be dried 5 hours under vacuum, control moisture content is 80ppm, then by dried copolymerization PET-B and commercially available PVP K30 with the weight ratio of 70: 30 carry out hands mixed after, upper with double (2 at two axle mixing rolls (equidirectional 2 axles, the diameter of axle 70mm, L/D50), 4,6-tri-tert phenyl) pentaerythritol diphosphate carries out mixing.Set the melting temperature of two axle mixing rolls as 240 DEG C, mixing time axle rotating speed as 150rpm, after head spue, carry out water-cooled, pelletizing, make master batch polymer.
It is directed into after this master batch polymer and this copolyesters PET-B by hopper with the weight ratio of 25: 75 are fed an axle extruder (temperature is 260 DEG C), is carried out measuring by gear pump, spued that built-in filament spinning component (260 DEG C) is interior, spins through spinning spinneret, carry out cooling and solidifying, being oiled by feeding means again.Spinning speed is 2500m/min, obtains as-spun fibre, then by 2.2 times of deep processings, as-spun fibre is obtained polyester fiber.After tested, in gained polyester fiber, the average dispersion footpath of PVP is 100nm, and obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 2
Polyester is changed to combined polymerization PET-E, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 3
Polyester is changed to combined polymerization PET-F, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 4
Polyester is changed to combined polymerization PET-H, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 5
Polyester is changed to combined polymerization PTT-I, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 6
Polyester is changed to combined polymerization PBT-J, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 7
The weight ratio of change master batch polymer and copolymerization PET-B is 35: 65, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 8
The weight ratio of change master batch polymer and copolymerization PET-B is 15: 85, and other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Embodiment 9~13
The ratio of PVP, the addition of phosphorus system heat stabilizer during change master batch polymers manufacturing, and the ratio of master batch during spinning, other are with embodiment 1.Obtained fiber has good fibrous physical property, absorb-discharge humid, tone and dry-hot shrinkage.
Comparative example 1
Common PET-A 150 DEG C, be dried 5 hours under vacuum, control moisture content is 80ppm, then by dried PET-A and commercially available PVP with the weight ratio of 70:30 carry out hands mixed after, two axle mixing rolls (equidirectional 2 axles, the diameter of axle 70mm, L/D50) are carried out mixing.Set the melting temperature of two axle mixing rolls as 280 DEG C, mixing time axle rotating speed as 150rpm, after head spue, carry out water-cooled, pelletizing, make master batch polymer.
It is directed into after this master batch polymer and this PET-A by hopper with the weight ratio of 25: 75 are fed an axle extruder (temperature is 290 DEG C), is carried out measuring by gear pump, spued that built-in filament spinning component (290 DEG C) is interior, spins through spinning spinneret, carry out cooling and solidifying, being oiled by feeding means again.Spinning speed is 2500m/min, obtains as-spun fibre, then by 2.2 times of deep processings, as-spun fibre is obtained polyester fiber.After tested, in gained polyester fiber, the average dispersion footpath of PVP is 120nm, and obtained fiber has good fibrous physical property, absorb-discharge humid, dry-hot shrinkage, but the tone of fiber is undesirable.
Comparative example 2
Copolymerization PET-C 150 DEG C, be dried 5 hours under vacuum, control moisture content is 80ppm, then by dried PET-C and commercially available polyvinylpyrrolidone with the weight ratio of 70:30 carry out hands mixed after, two axle mixing rolls (equidirectional 2 axles, the diameter of axle 70mm, L/D50) are carried out mixing.Set the melting temperature of two axle mixing rolls as 280 DEG C, mixing time axle rotating speed as 150rpm, after head spue, carry out water-cooled, pelletizing, make master batch polymer.
It is directed in built-in filament spinning component (270 DEG C) after this master batch polymer and this PET-C by hopper with the weight ratio of 25:75 are fed an axle extruder (temperature is 270 DEG C), is carried out measuring by gear pump, spued, spins through spinning spinneret, carry out cooling and solidifying, being oiled by feeding means again.Spinning speed is 2500m/min, obtains as-spun fibre, then by 2.2 times of deep processings, as-spun fibre is obtained polyester fiber.After tested, in gained polyester fiber, the average dispersion footpath of PVP is 250nm, and obtained fiber has good fibrous physical property, absorb-discharge humid, dry-hot shrinkage, but the tone of fiber is undesirable.
Comparative example 3
Polyester is changed to copolymerization PET-D, and other are with embodiment 1.Obtained by fiber there is good fibrous physical property, absorb-discharge humid, dry-hot shrinkage, but the tone L-value of fiber, b value difference, it is impossible to actually used.
Comparative example 4
Polyester is changed to copolymerization PET-G, and other are with embodiment 1.Obtained by fiber there is good fibrous physical property, absorb-discharge humid, tone, but the dry shrinkage of fiber becomes big, difficulty time actually used.
Comparative example 5
Changing the content of the phosphorus system heat stabilizer of interpolation in terms of P element 30ppm, other are with embodiment 1.Obtained by fiber there is good fibrous physical property, absorb-discharge humid, dry-hot shrinkage, but the tone of fiber is undesirable.
Comparative example 6
PVP content in polyester fiber is reduced to 2wt%, and other are with embodiment 1.Obtained fiber has good fibrous physical property, but moisture adsorption and releasing are poor.
Comparative example 7
Improving PVP content in polyester fiber to 18wt%, other are with embodiment 1.Obtained fiber has the moisture adsorption and releasing of excellence, but fibrous physical property, tone are deteriorated, it is impossible to actually used.
Comparative example 8
Using L/D when making master batch polymer is the mixing roll of 35, and other are with embodiment 1.Obtained fiber has good fibrous physical property, but the dispersibility of PVP is poor.
Comparative example 9
The PVP using K value to be 120 carries out mixing, and mixing process is with embodiment 1.Owing to the K value of PVP is relatively big, mixing relatively difficult.Obtained master batch such as embodiment 1 carries out spinning, and it is bad that obtained fiber has good fibrous physical property, and the dispersibility of PVP is poor.

Claims (10)

1. an absorb-discharge humid polyester fiber, is characterized in that: containing fusing point in this polyester fiber is 200~240 DEG C of polyester, poly N-ethylene lactams, phosphorus system heat stabilizer and sodium system nucleator, and wherein poly N-ethylene lactams accounts for the 3~15wt% of polyester fiber weight;The content of phosphorus system heat stabilizer accounts for the 50~500ppm of polyester fiber weight in terms of P element;The content of sodium system nucleator accounts for the 10~100ppm of polyester fiber weight in terms of Na element;And in this polyester fiber antimony element content at below 5ppm.
Absorb-discharge humid polyester fiber the most according to claim 1, it is characterized in that: described polyester is the cation dyeable polyester containing the construction unit formed by the M-phthalic acid or derivatives thereof with sodium group, in polyester, sulfur content is 0.1~1.0wt%.
Absorb-discharge humid polyester fiber the most according to claim 1, is characterized in that: described poly N-vinyl lactams accounts for the 5~12wt% of polyester fiber weight.
4. according to the absorb-discharge humid polyester fiber described in claim 1 or 3, it is characterized in that: described poly N-ethylene lactams is polyvinylpyrrolidone.
Absorb-discharge humid polyester fiber the most according to claim 4, is characterized in that: the dispersion footpath of described poly-polyvinylpyrrolidone is below 300nm.
Absorb-discharge humid polyester fiber the most according to claim 4, is characterized in that: the K value of described polyvinylpyrrolidone is 15~90.
Absorb-discharge humid polyester fiber the most according to claim 1, is characterized in that: described sodium system nucleator in terms of Na element, account for the 20~60ppm of polyester fiber weight.
Moisture absorption type polyester fiber the most according to claim 1, is characterized in that: the hygroscopicity parameter, Δ MR of this polyester fiber is more than 1.0%, and hue b value is below 5.0, and light fastness is more than 3 grades, and the dry-hot shrinkage at 180 DEG C is below 12%.
9. the preparation method of absorb-discharge humid polyester fiber described in a claim 1, it is characterized in that: by polyester and poly N-ethylene lactams with the weight ratio of 95:5~60:40, the double screw extruder using screw slenderness ratio more than 40 carries out melting mixing, obtains master batch polymer;Then mixed with the weight ratio of 60:40~10:90 with polyester by gained master batch polymer in device for spinning, melt spinning prepares moisture adsorption and releasing polyester fiber;In terms of P elements, account for the phosphorus system heat stabilizer of polyester fiber weight 50ppm~500ppm in blended stage or the interpolation of melt spinning stage simultaneously;Containing the sodium system nucleator being equivalent to weight polyester 10~120ppm in terms of sodium element in described polyester, the amount of antimony element is at below 5ppm.
The preparation method of absorb-discharge humid polyester fiber the most according to claim 9, is characterized in that: described phosphorus system heat stabilizer added in the blended stage.
CN201410821360.8A 2014-12-25 2014-12-25 Polyester fiber with moisture absorption/desorption performance and preparation method thereof Pending CN105780188A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950724A (en) * 2018-07-23 2018-12-07 含山县海达服饰有限公司 Polyester fiber is taken in a kind of movement of wash resistant

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950724A (en) * 2018-07-23 2018-12-07 含山县海达服饰有限公司 Polyester fiber is taken in a kind of movement of wash resistant

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