CN104711704A - Antistatic polyester composite fiber and application thereof - Google Patents
Antistatic polyester composite fiber and application thereof Download PDFInfo
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- CN104711704A CN104711704A CN201310675678.5A CN201310675678A CN104711704A CN 104711704 A CN104711704 A CN 104711704A CN 201310675678 A CN201310675678 A CN 201310675678A CN 104711704 A CN104711704 A CN 104711704A
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Abstract
The invention discloses an antistatic polyester composite fiber. The fiber is obtained by compounding a component A with a component B, wherein the component A is polyester, and the component B is modified polyester obtained through a reaction of aromatic dicarboxylic acid or an esterification derivative thereof, alkylene glycol and polyether olefine acid ester. The antistatic polyester composite fiber has excellent and durable antistatic performance, still maintains high antistatic performance after dyeing treatment, and can be widely used in fibers, resins and films.
Description
Technical field
The present invention relates to a kind of antistatic polyester composite fibre and application thereof of antistatic excellent in te pins of durability.
Background technology
Dielectric constant and the electric conductivity of conventional macromolecular material are all very low, and the fiber made with macromolecular material easily produces electrostatic when rubbing, this problem such as contamination, binding dust bringing difficulty and fabric to use to weaving aft-loaded airfoil.Therefore, these macromolecular material antistatic behaviours are given more and more important.
The current method improving macromolecular material electric conductivity has antistatic additive is coated in products formed surface, or antistatic additive is joined by copolymerization or blended mode the antistatic behaviour improving material in polymer.But the antistatic products that a kind of front method obtains also can slowly come off along with the antistatic additive extending surface coating service time, does not have permanent antistatic behaviour; A kind of rear method, the general low molecular weight antistatic additive used easily post-processed particularly obtained fabric separate out from material after the process of heat tinting look and do not have antistatic property.
Patent CN101230186A discloses a kind of antistatic pet material and preparation method thereof, by polyethylene terephthalate is blended obtained with antistatic additive, antioxidant, wherein antistatic additive is the product of nano silver colloidal sol and kayexalate complex reaction.The method not only cost compare is high and also this antistatic additive due to just and polyester blend, so easily come off in post-production, weaken antistatic effect.
Summary of the invention
The object of the present invention is to provide the antistatic polyester composite fibre that a kind of durability is lasting.
Technical solution of the present invention is:
The antistatic polyester composite fibre be composited by composition A and composition B, on filament cross section, the area ratio of composition A and composition B is S
a: S
b=5/95 ~ 95/5.Wherein composition A is polyester, the modified poly ester that composition B is obtained by reacting by aromatic binary carboxylic acid or its esterification derivative, aklylene glycol and polyethers olefin(e) acid ester, in composition B containing come from polyethers olefin(e) acid ester such as formula the construction unit shown in 1 and formula 2,
formula 1,
formula 2,
In formula 1, R is the alkylidene of carbon number 2 ~ 4, preferred ethylidene, and n is the integer of 10 ~ 500.
The area of described A composition is unsuitable too small, otherwise composite fibre be island-in-sea type composite fiber or core sheath composite fibre time sheath or the phenomenon that can break of sea.The area of B component is also unsuitable too small simultaneously, otherwise the antistatic behaviour of fiber is bad.
Mentioned component A polyester can be polymer-modified any one of polyethylene terephthalate (PET), polybutylene terephthalate (PBT) (PBT), polytrimethylene terephthalate (PTT), PLA (PLA) and above polymer.
Described composition B is the electrostatic source of resistant fiber, and wherein the ehter bond of polyethers olefin(e) acid ester plays antistatic property, and the existence of diolefin key makes this material in polymerization, have the possibility being certainly polymerized to more macromolecule polyethers, thus improves the moisture absorption antistatic behaviour of polyester.The existence of ester bond in addition, that can improve with polyester portion is compatible and reactive, make it can be uniformly dispersed in polymerization and in aft-loaded airfoil not easily stripping come off.
More specifically, described polyethers olefin(e) acid ester can be the compounds such as polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, 2-methacryloyl ethyoxyl butenoate, 2-acryloyloxyethyl pentenoate, polypropylene glycol dimethacrylate, polypropyleneglycol diacrylate.
Antistatic polyester composite fibre of the present invention can be core sheath composite fibre, island-in-sea type composite fiber, parallel composite fiber and multicore composite fibre etc., wherein preferred core sheath composite fibre or island-in-sea type composite fiber.When fiber is core sheath composite fibre, composition A is sheath, and composition B is core; When fiber is island-in-sea type composite fiber formula, composition A is sea, and composition B is island.
The molal quantity being set as construction unit shown in point B Chinese style 1 is G1, and the molal quantity of aromatic binary carboxylic acid or its esterification derivative construction unit is C, and the molal quantity of construction unit shown in formula 2 is G2, and the relation between them is such as formula shown in 3 and formula 4:
G1/C=0.05 ~ 0.5 formula 3,
G2/G1=0.01 ~ 0.03 formula 4,
Wherein G1/C more preferably 0.05 ~ 0.35.If the content of construction unit is too low relative to polyester shown in composition B Chinese style 1, will antistatic behaviour be there is no, and if the content of construction unit is too high relative to polyester shown in polyester Chinese style 1, the heat resistance of polyester can be caused to be deteriorated and the pelletizing difficulty that spues after polymerization.
Also preferred in described composition B is one or more in the sulfonate of structure as shown in Equation 5 of 0.1 ~ 10wt% containing accounting for composition B weight,
formula 5,
Wherein, R
3for the straight chained alkyl of carbon number 10 ~ 40 or the aromatic radical having alkyl substituent of carbon number 10 ~ 40, M is alkali metal or alkaline-earth metal, and as sodium, potassium, magnesium etc., m is the integer of 1 ~ 2.
Above-mentioned sulfonate as shown in Equation 5 can be neopelex (DBS), sodium cetanesulfonate (MS), Kui sodium alkyl sulfonate etc.
Because above-mentioned sulfonate does not have the functional group that can react with polyester segment, so the fraction that easily comes off from polyester in aft-loaded airfoil process, among a small circle, the antistatic property of polyester is caused to decline.
Therefore, containing the construction unit shown in formula 6 in preferred composition B of the present invention, in its molal quantity S and composition B, the relation of the molal quantity C of aromatic binary carboxylic acid or its esterification derivative is such as formula 7,
formula 6,
S/(S+C)=0.01 ~ 0.05 formula 7.
Due to same containing sulfonate groups in said structure unit, thus improve the polarity of polyester segment, according to the principle of similar compatibility, the large sulfonate shown in formula 5 of Polarity comparision just more easily combines with polyester, thus decreases sulfonate compound shown in formula 5 and come off in aft-loaded airfoil.
In addition, the heat resistance of modified poly ester can be made to be deteriorated owing to adding a large amount of ehter bond, xanthochromia occurs, so in order to suppress the oxidative thermal decomposition of modified poly ester, also preferably containing Hinered phenols antioxidant in composition B, its structure as shown in Equation 8,
formula 8,
Its addition is equivalent to 0.01% ~ 0.5% of composition B weight.
In formula 8, R
4, R
6be respectively the alkyl of protium or carbon number 1 ~ 5, R
5for the alkyl of protium, carbon number 1 ~ 5, sulfo-thing, phosphonate ester, ester group or benzyl.Work as R
4, R
5and R
6when being alkyl, the preferably alkyl of 3 ~ 4.Described hindered phenol antioxygen can be four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (Ir1010), 1,3,5-trimethyl-2,4,6-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) benzene (Ir1330), 4,4 '-thiobis (6-tertiary butyl metacresol) (Ir300), BHT (Ir264) etc.
The preparation method of composition B modified poly ester of the present invention is:
Aromatic binary carboxylic acid or its esterification derivative and aklylene glycol are added esterifying kettle by a certain percentage, at 220 ~ 250 DEG C of temperature, esterification 2 ~ 6 hours, reaction terminates rear immigration polycondensation vessel; Add before polycondensation and be the polyethers olefin(e) acid ester as shown in Equation 9 of 0.05 ~ 0.5 with aromatic binary carboxylic acid or its esterification derivative mol ratio and stir, in high vacuum, polycondensation 1 ~ 4 hour obtained modified poly ester at temperature 260 ~ 290 DEG C;
formula 9,
Wherein, R
7for the alkyl of hydrogen atom or carbon number 1 ~ 4, R is the alkylidene of carbon number 2 ~ 4, and n is the integer of 10 ~ 500.
Meanwhile, in order to improve the uniformity of the antistatic behaviour of modified poly ester, heat resistance, tone and the material strip that spues, also preferably before polycondensation, also add the sulfonate being as shown in Equation 5 equivalent to polyester 0.1 ~ 10wt%; Also add before ester exchange or before polycondensation with modified poly ester weight ratio be 0.01% ~ 0.5% Hinered phenols antioxidant as shown in Equation 8.In order to the stripping of sulfonate in aft-loaded airfoil process, also preferably add the 5-sodium sulfo isophthalate or derivatives thereof being equivalent to the molal quantity 0.01 ~ 0.05 of aromatic binary carboxylic acid or its esterification derivative in modified poly ester in the reaction.
Other catalyst used in the preparation process of composition B and auxiliary agent are all conventional known, as added catalyst acetic acid slaine cobalt acetate, magnesium acetate, manganese acetate, lithium acetate, calcium acetate etc. in the ester exchange stage, at catalyst such as the antimony system that polymerization stage adds, titanium system, germanium systems, described auxiliary agent can comprise defoamer, phosphorus system stabilizing agent, delustering agent etc.
The antistatic polyester composite fibre that the present invention is composited by composition A and composition B can be prepared by conventional melt spinning method.Such as composition A and composition B is dropped into bicomponent spin machine respectively, by the discharge-amount of measuring pump difference dose ingredients A and composition B after heating and melting, in press-in bi-component assembly, then spued by compound mouth gold, be the lateral blowing of 10 ~ 50m/min by wind speed again, oil to oil nozzle, the up-coiler being finally 800 ~ 6000m/min by coiling speed batches.When one-step method (DSD), directly obtain extending silk.When two-step method, the silk that do not extend obtained is carried out extending or DTY processing obtains final fiber.
Composite fibre of the present invention is except having excellent antistatic property, and antistatic durability is also very excellent, can meet fibre as fabric requirement to long-acting antistatic in service life.The fabric that fiber is obtained thus through JIS standard testing friction belt voltage be below 3000V.
The evaluation method that the present invention relates to is as follows:
(1) area ratio of composition A and composition B on fiber cross section
Use paraffin method to carry out process to fiber and obtain fiber cross section sample, by microscope, observation is carried out to sample in cross section and take pictures, then contrasted by the area of photo to A and B.
(2) mol ratio of construction unit shown in structural unit content shown in composition B Chinese style 1 and formula 2, formula 1
A certain amount of Modified polyester chips is dissolved in trifluoroacetic acid, carries out H-NMR test.The mol ratio of construction unit and aromatic binary carboxylic acid or its esterification derivative construction unit shown in formula 1 is calculated according to the peak area of the characteristic peak of protium on the peak area of the characteristic peak of protium on ehter bond and aromatic binary carboxylic acid compounds phenyl ring.The mol ratio of construction unit shown in formula 2, formula 1 is calculated according to the peak area of the characteristic peak of protium on the peak area of the characteristic peak of protium on alkene and ehter bond.
(3) sulfonate content
Use fluorescent X-ray to carry out the content that S atom is measured in spectrum analysis, inferred the content sulfonate by the structural formula of sulfonate.
(4) friction belt voltage determination
Be that benchmark measures according to JISL 1094 friction belt voltage test method.Condition determination: temperature 20 ± 1 DEG C, relative humidity 40 ± 2%.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Bishydroxyethyl terephthalate is added esterification groove, keep temperature 250 DEG C, pressure 1.2 × 10
5pa, the TPA(terephthalic acid (TPA) by 10 weight portions) and the EG(ethylene glycol of 4.5 weight portions) slurry joined esterification layer gradually, then carry out the esterification of 1 hour in 4 hours.Finally from the reactant of esterification obtained, get 12.3 weight portions joins polycondensation reaction layer.
Esterification reaction product is remained on 250 DEG C, under normal pressure, add the defoamer (methyl-silicone oil) being equivalent to weight polyester 0.01%, stirring interpolation and terephthalic acid (TPA) mol ratio after five minutes is polyethylene glycol (n=23) dimethylacrylate of 0.3, add phosphorus atoms amount again after stir about 30min and be equivalent to the antimonous oxide that the phosphoric acid of weight polyester 18ppm and antimony atoms amount be equivalent to weight polyester 230ppm, cobalt atom amount is equivalent to the catalyst of the cobalt acetate of weight polyester 15ppm.Start decompression after 5 minutes, heat up, temperature by 250 DEG C rise to 290 DEG C, Pressure Drop is to 40Pa.Final temperature, final pressure is reached after 60 minutes.After arriving certain stirring extent, in reaction system, import nitrogen be back to normal pressure, stop polycondensation reaction.Polymer is that uniform strip spues, and obtains composition B Modified polyester chips in the sink after cooling.
PET is dropped into bicomponent spin machine respectively with the composition B obtained and carries out melting, be metered into bi-component assembly, the proportioning of PET and composition B is 50/50, by core sheath spinnerets, 3000m/min coiling machine reels, and obtains pre-oriented yarn, then obtains DTY by processing.Carry out frictional electrification pressure after using the obtained textile dyeing of this DTY to measure, result is 2500V.
Embodiment 2 ~ 3
Change the proportioning of PET and composition B during spinning, other are with embodiment 1, and acquired results is as shown in table 1.
Embodiment 4 ~ 5
Change the addition of polyethylene glycol (n=23) dimethylacrylate during prepared composition B, other are with embodiment 1, and acquired results is as shown in table 1.
Embodiment 6 ~ 7
Polyethylene glycol (n=100) dimethylacrylate and polyethylene glycol (n=500) dimethylacrylate is added respectively during prepared composition B, and before adding catalyst, add hindered phenol antioxidant four [β-(3 being equivalent to composition B weight 0.2wt%, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (Ir1010), other are with embodiment 1, and acquired results is as shown in table 1.
Embodiment 8
Polypropylene glycol (n=10) diacrylate is added, R during prepared composition B
7for hydrogen base, other are with embodiment 1, and acquired results is as shown in table 1.
Embodiment 9
When preparing composite fibre, filament spinning component changes to island composite component, and other are with implementing 1, and acquired results is as shown in table 1.
Embodiment 10
During prepared composition B, interpolation and terephthalic acid (TPA) mol ratio are polyethylene glycol (n=50) dimethylacrylate of 0.4, add after polycondensation phase adds polyethers olefin(e) acid ester and be equivalent to the neopelex (DBS) that composition B weight is 0.8wt%, and before adding catalyst, add the hindered phenol antioxidant 1 being equivalent to composition B weight 0.5wt%, 3,5-trimethyl-2,4,6-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) benzene (Ir1330), during spinning, the proportioning of PET and composition B is 90/10, and other are with embodiment 1, and acquired results is as shown in table 1.
Embodiment 11 ~ 12
Change the addition of DBS during prepared composition B, other are with embodiment 10, and acquired results is as shown in table 1.
Embodiment 13
During prepared composition B, add after polycondensation phase adds polyethers olefin(e) acid ester and be equivalent to the cetyl benzenesulfonic acid sodium (MS) that composition B weight is 0.8wt%, other are with embodiment 10, and acquired results is as shown in table 1.
Embodiment 14
During prepared composition B, interpolation and terephthalic acid (TPA) mol ratio are polyethylene glycol (n=80) dimethylacrylate of 0.1, adding with terephthalic acid (TPA) molal quantity relation in polycondensation phase is the 5-sodium sulfo isophthalate of 0.01 such as formula 7, and before adding catalyst, add the hindered phenol antioxidant 2 being equivalent to composition B weight 0.1wt%, 6-di-tert-butyl methyl phenol (Ir264), during spinning, the proportioning of PET and composition B is 40/60, the complex morphological of obtained fiber is islands-in-sea type fibre, other are with embodiment 10, and acquired results is as shown in table 1.
Embodiment 15
Change the addition of 5-sodium sulfo isophthalate during prepared composition B, other are with embodiment 14, and acquired results is as shown in table 1.
Embodiment 16 ~ 17
When preparing composite fibre, change the proportioning of PET and composition B, other are with embodiment 14, and acquired results is as shown in table 1.
Embodiment 18
When preparing composite fibre, filament spinning component changes to core sheath composite component, and other are with implementing 14, and acquired results is as shown in table 1.
Embodiment 19
During prepared composition B, before adding catalyst, add hindered phenol antioxidant four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (Ir1010) being equivalent to composition B weight 0.01wt%.When preparing composite fibre, changing A composition is PBT, and during spinning, the proportioning of PBT and composition B is 60/40, and the complex morphological of obtained fiber is core sheath fiber, and other are with embodiment 14, and acquired results is as shown in table 1.
Embodiment 20
During prepared composition B, before adding catalyst, add hindered phenol antioxidant four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (Ir1010) being equivalent to composition B weight 0.05wt%.When preparing composite fibre, changing A composition is PTT, and during spinning, the proportioning of PTT and composition B is 70/30, and the complex morphological of obtained fiber is core sheath fiber, and other are with embodiment 14, and acquired results is as shown in table 1.
Comparative example 1
During prepared composition B, be the PEG replacement polyethers olefin(e) acid ester as shown in Equation 9 of 8300 with molecular weight, other are with embodiment 1, and carry out frictional electrification pressure after the DTY obtained being obtained textile dyeing and measure, result is 3500V.
Table 1
Claims (8)
1. an antistatic polyester composite fibre, is characterized in that: this fiber is composited by composition A and composition B, and on filament cross section, the area ratio of composition A and composition B is S
a: S
b=5/95 ~ 95/5; Described composition A is polyester, the modified poly ester that composition B is obtained by reacting by aromatic binary carboxylic acid or its esterification derivative, aklylene glycol and polyethers olefin(e) acid ester, in composition B containing come from polyethers olefin(e) acid ester such as formula the construction unit shown in 1 and formula 2,
formula 1,
formula 2,
In formula 1, R is the alkylidene of carbon number 2 ~ 4, and n is the integer of 10 ~ 500.
2. antistatic polyester composite fibre according to claim 1, is characterized in that: this fiber is core sheath composite fibre or island-in-sea type composite fiber, and wherein composition A is sheath or sea, and composition B is Xin Huo island.
3. antistatic polyester composite fibre according to claim 1 and 2, it is characterized in that: shown in described composition B Chinese style 1, the molal quantity of construction unit is G1, the molal quantity of aromatic binary carboxylic acid or its esterification derivative construction unit is C, the molal quantity of construction unit shown in formula 2 is G2, the relation of G1 and C as shown in Equation 3, the relation of G2 and G1 as shown in Equation 4
G1/C=0.05 ~ 0.5 formula 3,
G2/G1=0.01 ~ 0.03 formula 4.
4. antistatic polyester composite fibre according to claim 1 and 2, is characterized in that: be one or more in the sulfonate of structure as shown in Equation 5 of 0.1 ~ 10wt% containing accounting for composition B weight in described composition B,
formula 5
Wherein, R
3for the straight chained alkyl of carbon number 10 ~ 40 or the aromatic radical having alkyl substituent of carbon number 10 ~ 40, M is alkali metal or alkaline-earth metal, and m is the integer of 1 ~ 2.
5. antistatic polyester composite fibre according to claim 1, is characterized in that: containing the construction unit shown in formula 6 in described composition B modified poly ester, in its molal quantity S and composition B, the relation of the molal quantity C of aromatic binary carboxylic acid or its esterification derivative is such as formula 7,
formula 6,
S/ (S+C)=0.01 ~ 0.05 formula 7.
6. antistatic polyester composite fibre according to claim 2, is characterized in that: described composition B also contains Hinered phenols antioxidant as shown in Equation 8, and its addition is equivalent to the Hinered phenols antioxidant of composition B weight 0.01% ~ 0.5%,
formula 8,
Wherein, R
4, R
6be respectively the alkyl of protium or carbon number 1 ~ 5, R
5for the alkyl of protium, carbon number 1 ~ 5, sulfo-thing, phosphonate ester, ester group or benzyl.
7. antistatic polyester composite fibre according to claim 1, is characterized in that: in described formula 1, R is ethylidene.
8. the application of antistatic polyester composite fibre on antistatic polyester fabric described in a claim 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023080124A1 (en) * | 2021-11-02 | 2023-05-11 | 日本エステル株式会社 | Sheath-core type polyester composite fiber and method for producing same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023080124A1 (en) * | 2021-11-02 | 2023-05-11 | 日本エステル株式会社 | Sheath-core type polyester composite fiber and method for producing same |
| JP7340183B1 (en) | 2021-11-02 | 2023-09-07 | 日本エステル株式会社 | Core-sheath type polyester composite fiber and its manufacturing method |
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Application publication date: 20150617 |