JP2772926B2 - Method for producing antistatic polyester fiber - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an antistatic polyester fiber having excellent antistatic performance.

[0002]

2. Description of the Related Art Polyester fibers are widely used not only for clothing but also for industrial materials because of their excellent properties, but have the drawback that they have high electric resistance and are easily charged with static electricity. Therefore, various methods have been proposed in order to improve the disadvantage of being easily charged with static electricity.
One of the methods is to knead an antistatic agent into polyester. For example, JP-B-46-22200 and JP-B-47
Japanese Patent Application Laid-Open No. Sho 5-10246 and Japanese Patent Publication No. 47-11280 discloses a method in which polyoxyalkylene glycol and sodium alkylbenzene sulfonate are mixed as an antistatic agent.
Japanese Patent Application Publication No. 3-149247 proposes that a polyoxyalkylene glycol and sodium alkyl sulfonate are mixed as an antistatic agent, and Japanese Patent Publication No. 57-4724 discloses that an antistatic polymer is streaked in the fiber axis direction. It has also been proposed to disperse in a shape.

However, in the conventional method, a satisfactory antistatic performance cannot be obtained with a small amount of an antistatic agent.
Further, when the compounding amount of the antistatic agent such as polyoxyalkylene glycol is increased for the purpose of improving the antistatic performance, the yarn-forming stability, heat resistance, and the like are reduced, and there is a disadvantage that stain spots and the like are easily generated. In the conventional method, one of the reasons why a small amount of the antistatic agent is not sufficient to express sufficient antistatic performance is that the antistatic agent is present in the fiber in a continuous state in a streak shape in the fiber axis direction. In that the compounded antistatic agent does not function effectively.

[0004]

DISCLOSURE OF THE INVENTION The present invention relates to a method for producing an antistatic polyester fiber by a kneading method in a polymerization step into a polyester using a polyalkylene glycol and a metal salt of an organic sulfonic acid as an antistatic agent. The spinning method is improved to disperse the electric agent as a continuous phase in the fiber axis direction and to exhibit a high antistatic performance even with a small amount of the antistatic agent. Another object of the present invention is to efficiently provide an antistatic polyester fiber having excellent resistance.

The present invention relates to a polyalkylene glycol having an average molecular weight of at least 5,000 of 0.5 to 5% by weight and a general formula R
SO ₃ M (where R represents an alkyl group having 3 to 30 carbon atoms, an aryl group or an alkylaryl group having 7 to 40 carbon atoms, and M represents an alkali metal). In preparing a polyester fiber by melt-spinning a polyester polymer having ethylene terephthalate as a main repeating unit obtained by adding 2% by weight as an antistatic agent to a reaction system before completion of polycondensation, the following requirements (A) and The polymer is melt-spun from a spinneret under the conditions satisfying (B), and the spun yarn is once cooled to a temperature lower than the glass transition point of the polyester, and subsequently heated at a temperature higher than the glass transition point and lower than the melting point. Run through the band,
A method for producing an antistatic polyester fiber, comprising winding at a speed of 3,500 to 6,000 m / min.

[0006]

(A) The time required for the polymer to pass through a single-hole volume V ₁ represented by the product of the opening area S ₁ of the single hole of the spinneret and the length L ₂ of the single hole is 3 milliseconds. (B) Discharge linear velocity V ₀ of polymer from single hole of spinneret
Is 800cm / min or less

In particular, in the present invention, it is preferable to use a spinneret for a solid fiber having a circular cross section as a spinneret and to perform melt spinning under the conditions satisfying the following requirements (A ₁ ) and (B ₁ ). (A ₁ ) The time required for the polymer to pass through the single-hole volume V ₁ represented by the product of the opening area S ₁ of the single hole of the spinneret and the length L ₂ of the single hole portion is 10 ms or more ( B ₁ ) Linear velocity V ₀ of discharge of polymer from single hole of spinneret
Is less than 600cm / min

In the antistatic polyester fiber of the present invention, the polyester refers to a polyester containing ethylene terephthalate as a main repeating unit, terephthalic acid or an ester-forming derivative thereof as a dicarboxylic acid component, and ethylene glycol or an ester forming ester thereof. A typical example is a polyester having a derivative as a diol component.A part of the dicarboxylic acid component is a dicarboxylic acid component other than terephthalic acid or an ester-forming derivative thereof, and a part of the diel component is ethylene glycol or It may be replaced with another diol component other than the ester-forming derivative.

Other dicarboxylic acid components include isophthalic acid, 5-sulfoisophthalic acid monoalkali metal salt, naphthalenedicarboxylic acid, diphenyldicarboxylic acid, diphenylsulfondicarboxylic acid, adipic acid, sebacic acid, and 1,4-cyclohexanedicarboxylic acid. Dicarboxylic acids or esters thereof and p-oxybenzoic acid, p
And oxycarboxylic acids such as -β-oxyethoxybenzoic acid and esters thereof.

Further, as other diol components, 1,4
-Butanediol, alkylene glycol having 2 to 10 carbon atoms, 1,4-cyclohexanedimethanol, neopentyl glycol, 1,4-bis (β-oxyethoxy)
Examples include benzene and bisglycol ether of bisphenol A.

Further, as long as the polyester is substantially linear, polycarboxylic acids such as trimellitic acid and pyromellitic acid, polyols such as pentaerythritol, trimethylolpropane and glycerin, monohydric polyalkylene oxides and phenyl A polymer using a polymerization terminator such as acetic acid may be used.

The polyester may be synthesized by any known method. For example, in the case of polyethylene terephthalate, terephthalic acid and ethylene glycol are directly esterified, a lower alkyl ester of terephthalic acid such as dimethyl terephthalate is transesterified with ethylene glycol, or terephthalic acid is ethylene oxide. To synthesize a glycol ester of terephthalic acid or a low polymer thereof, followed by polycondensation of the product by a conventional method.

Further, in synthesizing the polyester,
Known catalysts, antioxidants, color inhibitors, ether bond by-product inhibitors, flame retardants, and other additives may be appropriately used.

The polyester constituting the antistatic polyester fiber of the present invention comprises 0.5 to 5% by weight of a polyalkylene glycol having an average molecular weight of 5,000 or more and a metal salt of an organic sulfonic acid represented by the above formula. 0.1 to 2% by weight as an antistatic agent. In the present invention, the polyalkylene glycol contained in the polyester needs to have an average molecular weight of 5,000 or more, and is preferably a polyalkylene glycol having an average molecular weight of 10,000 or more.

In the case of a polyalkylene glycol having an average molecular weight of less than 5,000, the proportion of the polyalkylene glycol copolymerized in the main chain of the polyester when added to the polyester polycondensation reaction system is increased. , The formation of an independent phase as a polyalkylene glycol is reduced, and it is difficult to exhibit sufficient antistatic performance. Examples of the polyalkylene glycol include polyethylene glycol, polypropylene glycol, and a copolymer of ethylene oxide and propylene oxide.
It is not limited to these.

In the present invention, the organic sulfonic acid metal salt represented by the above general formula contained in the polyester includes sodium, potassium or lithium salts of alkyl sulfonic acids having 3 to 30 carbon atoms, toluene sulfone. Examples include an acid, a sodium salt, a potassium salt or a lithium salt of dodecylbenzenesulfonic acid, or a mixture thereof.

In the antistatic polyester fiber of the present invention, at least one polyalkylene glycol of the antistatic agent forms a large number of independent phases oriented in the fiber axis direction in the fiber. The glycol independent phase is a highly dispersed and continuous phase. In addition, the organic sulfonic acid metal salt is distributed near the polyalkylene glycol.

In the fiber, the independent phase of the polyalkylene glycol has an average spacing of 0.2 μm or less between each independent phase in the cross section of the fiber perpendicular to the fiber axis and is parallel to the fiber axis. The ratio of the number of continuous independent phases to the total number of independent phases oriented in the fiber axis direction per 1 μm ² in the longitudinal fiber cross section in the direction is 30% or more. The average spacing between the polyalkylene glycol independent phases exceeds 0.2 μm, or the proportion of continuous independent phases, that is, independent phases having a length of 1 μm or more is 30%.
If it is less than 30, sufficient antistatic performance is not exhibited.

Hereinafter, a method for producing the antistatic polyester fiber of the present invention will be described. In the present invention, it is necessary to use a polyester polymer having ethylene terephthalate as a main repeating unit to which polyalkylene glycol and an organic sulfonic acid metal salt are added as an antistatic agent.

The amount of polyalkylene glycol added to the polyester must be 0.5 to 5% by weight, preferably 0.8 to 3% by weight. The amount added is 0.
If it is less than 5% by weight, the manifestation of antistatic performance becomes insufficient, and
If the amount is more than 10% by weight, not only the passing stability in the spinning process is lowered, but also the physical properties such as the strength and elongation of the obtained fiber are lowered.

When the polyalkylene glycol is added, it is preferable to use a small amount of a known stabilizer, antioxidant and the like in combination for the purpose of improving thermal stability. Examples thereof include hindered phenol compounds and thioether compounds. The addition amount of these compounds is 1 to polyalkylene glycol.
It is preferable that the content be 10 to 10% by weight.

The amount of the metal organic sulfonic acid salt to be added to the polyester must be 0.1 to 2% by weight.
Preferably it is 0.2 to 1.5% by weight. The amount added is 0.
If it is less than 1% by weight, the manifestation of antistatic performance becomes insufficient and
If the content exceeds the weight percentage, not only the passing stability in the spinning process is lowered, but also the resulting fiber has drawbacks such as fluffing.

In the present invention, the polyalkylene glycol and the metal salt of an organic sulfonic acid may be independently added to the polyester. However, it is preferable to add them as a mixture because they have a synergistic effect of exhibiting antistatic performance. It is. The mixing ratio between the polyalkylene glycol and the organic sulfonic acid metal salt is as follows:
It is preferable to set the organic sulfonic acid metal salt to 90:10 to 10:90 in order to obtain a synergistic effect of antistatic performance.

The amount of the mixture of the polyalkylene glycol and the metal salt of an organic sulfonic acid to be added to the polyester is 0.5 to 5% by weight, preferably 1 to 4% by weight as the total amount of the mixture. If the total amount is less than 0.5% by weight, the antistatic performance will be insufficient, and if it exceeds 5% by weight, not only will the passing stability in the spinning process be reduced, but also the strong elongation of the resulting fiber. And other problems, such as deterioration of physical properties, and fluffing of fibers.

The polyalkylene glycol and the metal salt of an organic sulfonic acid are preferably added to the reaction system before the completion of the polycondensation reaction of the polyester. More preferably, the polycondensation reaction is carried out in order to secure the stability in the spinning process. The polycondensation reaction is completed by adding to the intermediate system.

In the present invention, in melt-spinning a polyester polymer to which a polyalkylene glycol and a metal salt of an organic sulfonic acid have been added, the following requirements (A) are required.
It is necessary to spin from a spinneret under the conditions satisfying (B). (A) time required for a single pore volume V ₁ medium _{to the} opening area S1 of the single-hole represented by the product of the length L ₂ of a single hole spinneret to pass through the polymer is at least 3 ms (B) Discharge linear velocity V ₀ of polymer from single hole of spinneret
Is 800cm / min or less

In order for the polyester fiber to exhibit excellent antistatic performance, the dispersion state of the antistatic agent in the obtained fiber is extremely important. In the polyester fiber, the antistatic agent is oriented in the fiber axis direction and is long. Extremely excellent antistatic performance is exhibited when dispersed in a continuous phase in a streak shape.

In the present invention, polyalkylene glycol and an organic sulfonic acid metal salt are used as an antistatic agent.
The antistatic agent used in the present invention is incompatible with polyester in their molten state. Accordingly, by melt spinning the added polyester polymer antistatic agent when spun from a spinneret, a single hole having an opening area S ₁ and the area S ₁ of the single-hole spinneret length L ₂ By increasing the time required for the polymer to pass through the single pore volume V ₁ indicated by the product, the phase separation between the antistatic agent and the polyester immediately before discharge becomes clearer, and in the fiber thinning step immediately after discharge. A favorable state is formed in which the antistatic agent is oriented in the fiber axis direction.

In order to form a preferable state in which the antistatic agent is oriented in the fiber axis direction, it is necessary that the time required for the polymer to pass through the single pore volume V ₁ is 3 milliseconds or more. Preferably, it is 10 ms or more. Further, in order to highly orient the antistatic agent in the fiber axis direction, it is necessary to make the polymer discharge linear speed V ₀ which when ejecting polymer from single-hole spinneret with 800 cm / min or less, preferably 600cm / Min or less.

As long as the spinneret used in the present invention is capable of spinning a polymer under the conditions satisfying the requirements (A) and (B), the shape of the opening of the single hole is not limited to a circle, but may be non-circular. It may have a circular cross section, or may have a shape for obtaining hollow fibers.

In particular, in the present invention, when melt-spinning a polyester polymer to which an antistatic agent has been added using a spinneret for solid fibers having a circular cross section, the above requirement (A) is satisfied by the following requirement (A _1). ) And the requirement (B) are preferably melt-spun under conditions including the requirement (C) in which the requirement (B ₁ ) is replaced by the following requirement (B ₁ ). (A ₁ ) The time required for the polymer to pass through the single-hole volume V ₁ represented by the product of the opening area S ₁ of the single hole of the spinneret and the length L ₂ of the single hole portion is 10 ms or more ( B ₁ ) Linear velocity V ₀ of discharge of polymer from single hole of spinneret
Is less than 600cm / min

That is, in the spinneret for a solid fiber having a circular cross section, the time required for the polymer to pass through the single-hole volume V ₁ is 10 ms or more, more preferably 30 ms or more, Discharge linear velocity V ₀ of 600c
m / min or less, more preferably 400 cm / min or less, is desirable in order to obtain excellent antistatic performance and to obtain uniform fibers with extremely little stain spots.

In the present invention, the yarn spun from the spinneret is once cooled to a temperature below the glass transition point of the polyester in the cooling zone. This cooling is indispensable for improving the dyeability of the obtained fiber and for making the physical properties of the fiber practically sufficient.

Subsequently, the cooled yarn is heated to a temperature between the glass transition point and the melting point, preferably 120 to 2 ° C.
Heat treatment is performed by passing through a heating zone at a temperature of 30 ° C. If the temperature of the heating zone is lower than the glass transition point, the fiber physical properties become extremely poor fibers that cannot withstand practical use, and if the temperature is higher than the melting point, fusion between single fibers or yarn breakage is caused, and there is a problem in yarn production. In addition, the texture of the fabric obtained by weaving or knitting the obtained fiber is remarkably inferior.

As the apparatus for forming the heating zone, an indirect heating type apparatus which does not come into contact with the yarn is preferable, and an apparatus in which the opening area of the entrance and exit of the yarn is as small as possible is preferable. In other words, since the yarn runs at high speed, indirect heating without generating fluff and yarn spots due to contact with the heating unit is good, and a device for preventing temperature unevenness and thermal efficiency decrease due to high-speed airflow accompanying the yarn. Opening must be minimized.

As a heating method, any method such as a method in which a gas such as air is preliminarily heated and supplied into the apparatus, a method in which the atmosphere is directly heated by a heater provided around the running yarn, and the like can be used. You may. Further, the heating zone may be divided into two or more zones, each of which is under different temperature atmosphere. The yarn in the heating zone is heat treated during running and undergoes substantial stretching.

The yarn that has passed through the heating zone is applied with an oil agent as appropriate, then is taken up by a pair of take-up rollers, and is taken up by a take-up machine. ~ 6,000 m / min, preferably 4.0
It is performed at a speed of 00 to 6,000 m / min. If the winding speed is less than 3,500 m / min, the dyeability of the obtained fiber is inferior, and the fiber physical properties become extremely inferior fiber that cannot withstand practical use. It cannot be made into a heat-treated drawn yarn. The take-up speed is preferably set to be 0.5 to 1% higher than the take-up speed.

When winding the yarn through the take-up roller, it is preferable to provide a heat treatment device between the two take-up rollers and to reduce the stress of the yarn by heating under overfeed. Also, a fluid entanglement treatment device can be provided before or after this heat treatment device to increase the relaxation rate of the yarn.

According to the present invention, after normal spinning and winding,
It is easier to form a continuous independent phase of the polyalkylene glycol in the fiber than by the drawing method,
And although the number of independent phases is slightly reduced, thicker independent phases are formed. The polyester fiber obtained by the present invention,
A known arbitrary processing technique such as heat treatment or shaping to obtain a processed yarn, or alkali reduction processing or dyeing processing can be appropriately applied.

[0041]

The present invention will be described below in more detail with reference to examples. The percentages, parts and ratios in the examples mean weight%, parts by weight and weight ratio, respectively.
Each of the samples showed good, somewhat good and bad, and each characteristic value was measured by the following method.

[Intrinsic Viscosity] A sample was dissolved in a phenol / tetrachloroethane (50/50) mixed solvent and measured at 25 ° C. using an Ubbelohde viscometer.

[Antistatic performance] Warp: polyethylene terephthalate fiber yarn (50 denier / 18 filaments) Weft: antistatic polyester fiber yarn (100 denier / 48 filaments, 75 denier / 36 filaments) Warp density: 40 yarns / cm Weft density: after weaving under conditions of 26.6 yarns / cm and 30.5 yarns / cm, JIS L1094 (1988)
The charged voltage and the decay rate were measured according to the triboelectric discharge curve measurement method of the reference method. The measurement was performed using a friction voltage meter EST-3 manufactured by Kanebo Engineering Co., Ltd.
The test was performed at 0 ± 1 ° C. and a relative humidity of 30 ± 2%. Washing of the sample, washing of the friction cloth with hot water, and adjustment of the sample and the friction cloth were based on the JIS method, and wool was used as the friction cloth.

For each sample, the charged voltage V after 30 seconds and the decay rate D after 60 seconds were determined as an average value of each of the five times from the triboelectric discharge curves obtained by measuring five times. Further, each sample was performed five times, and the final average values of the charged voltage V ₃₀ after 30 seconds and the decay rate D ₆₀ after 60 seconds were determined. The unit of the charged voltage is volt (V, the sign is minus (-)), and the attenuation rate is represented by%.

[Observation by Transmission Electron Microscope] After dyeing the fiber obtained in the example with an aqueous solution of osmic acid, methyl methacrylate / butyl methacrylate (70/3) was used.
0), an ultra-thin section was prepared, and the dispersion state of the antistatic agent in the fiber was determined using a JEM100CX-2 transmission electron microscope manufactured by JEOL Ltd. with the dispersion state of polyethylene glycol. And observed and shown in photographs. The dispersion state of the polyethylene glycol can be observed as black streaks in the photograph.

(Example 1) 100 parts of terephthalic acid and 52 parts of ethylene glycol were charged into an esterification tank.
The esterification reaction was carried out at 260 ° C. under a pressure of 5 kg / cm ² , and 0.01% of trimethyl phosphate, 0.04% of antimony trioxide and 0.4% of titanium dioxide were added to the obtained reaction product. It was added as a glycol solution and transferred to a polymerization tank. Next, when the polycondensation reaction was performed at 285 ° C. for 70 minutes under high vacuum, the molecular weight was 20,000.
Polyethylene glycol (hereinafter abbreviated as PEG) and sodium alkyl sulfonate having an average carbon number of 15 (hereinafter referred to as RS).
(Abbreviated as O ₃ Na) at a mixing ratio of 5: 1 was added to the reaction system so as to be 2.4% with respect to the produced polymer, followed by a polycondensation reaction for a predetermined period of time. A terephthalate polymer was obtained.

The polymer was formed into chips by a conventional method and dried, and then spun at a spinning temperature of 280 ° C. using a spinneret for a solid fiber having a circular single-hole opening. The spinneret used had 48 single holes described below. Single hole opening S ₁ : 0.283 mm ² Single hole length L ₂ : 3.0 mm Single hole volume V ₁ : 0.849 mm ^{3 The} spinning conditions were as follows. Polymer passage time in single pore volume V ₁ : 65.9 ms Polymer discharge linear velocity V ₀ : 273 cm / min

After the spun yarn is cooled and solidified with cooling air,
Run through a cylindrical indirect heat treatment device set at 200 ° C., then apply an oil agent, perform fluid entanglement treatment with a fluid entanglement treatment device provided between take-off rollers, and overheat the heat treatment device set at 350 ° C. At a winding rate of 4,000 m / min.
A 0 denier / 48 filament drawn yarn was obtained. The obtained drawn yarn had a strength of 4.1 g / d and an elongation of 37%, and had no practical problem, and was a uniform yarn with no staining spots or the like.

The drawn yarn was woven by a conventional method, and the antistatic performance of the woven fabric was measured. The average charged voltage V ₃₀ after 30 seconds was 3800 V, and the average attenuation D ₆₀ after 60 seconds was 59%, which was extremely good. It showed excellent antistatic performance. In addition, the woven fabric is
%, The average charging voltage V ₃₀ was 3900 V and the average decay rate D ₆₀ was 55%.
And that the antistatic performance was hardly reduced even after the alkali weight reduction processing.

When the fiber of the obtained drawn yarn was cut in a direction perpendicular to the fiber axis, the average interval between the respective PEG independent phases in the fiber cross section was 0.040 μm,
When cut in a direction parallel to the fiber axis, the ratio of the number of continuous independent phases to the total number of independent phases oriented in the fiber axis direction per 1 μm ² in the fiber longitudinal section was 56%.
Met. FIGS. 3 and 4 show transmission electron micrographs (magnification: 40,000 times, visual field: 1 μm ² ) of fiber longitudinal sections and transmission electron micrographs (magnification: 40,000 times) of fiber cross sections.
showed that.

(Examples 2 to 4, Comparative Examples 1 to 4) Example 1
In the same manner as in Example 1 except that the addition amount of the mixture of PEG and RSO ₃ Na, the spinneret and the spinning conditions in Example 1 were changed as described in Table 1, a drawn yarn was obtained and the antistatic performance of the woven fabric was measured. Table 2 shows the measured results.

[0052]

[Table 1]

[0053]

[Table 2]

FIGS. 5 and 6 show transmission electron micrographs (magnification: 40,000 times, visual field: 1 μm ² ) of a longitudinal section of an example of a conventional antistatic polyester fiber and transmission electron microscope of a cross section of the fiber. As shown in the photograph (magnification: 40,000 times), in this conventional antistatic polyester fiber,
The ratio of the number of continuous independent phases to the total number of independent phases of PEG oriented in the fiber axis direction per 1 μm ² in the fiber longitudinal section is 16%, and the average interval between the PEG independent phases in the fiber cross section is 0.1%. It was 027 μm.

(Example 5) 100 parts of terephthalic acid and 52 parts of ethylene glycol were charged into an esterification tank.
The esterification reaction was carried out at 260 ° C. under a pressure of 0 kg / cm ² , and 0.01% of trimethyl phosphate, 0.04% of antimony trioxide and 0.46% of titanium dioxide were added to the obtained reaction product. It was added as a glycol solution and transferred to a polymerization tank. Next, when the polycondensation reaction was performed at 285 ° C. for 70 minutes under high vacuum, the molecular weight was 20,000.
A mixture of PEG and RSO ₃ Na at a mixing ratio of 50:50 was added to the reaction system so as to have a concentration of 2.0% with respect to the produced polymer. A polyethylene terephthalate polymer was obtained.

The polymer was formed into chips by a conventional method, dried, and then spun at a spinning temperature of 284 ° C. using a solid fiber spinneret having a circular single-hole opening. The spinneret used has 36 single holes described below. Single hole opening S ₁ : 0.283 mm ² Single hole length L ₂ : 3.0 mm Single hole volume V ₁ : 0.849 mm ^{3 The} spinning conditions were as follows. Polymer passage time in single pore volume V ₁ : 49.4 ms Polymer discharge linear velocity V ₀ : 205 cm / min

After the spun yarn is cooled and solidified with cooling air,
Run through a cylindrical indirect heat treatment device set at 210 ° C., then apply an oil agent, perform fluid entanglement treatment with a fluid entanglement device provided between take-off rollers, and overfeed the heat treatment device set at 350 ° C. At a winding rate of 4,000 m / min.
A denier / 36 filament drawn yarn was obtained. The obtained drawn yarn has a strength of 4.3 g / d and an elongation of 35%,
The product was homogeneous without any staining spots.

The drawn yarn was woven by a conventional method, and the antistatic performance of the woven fabric was measured. The average charged voltage V ₃₀ after 30 seconds was 3900 V, and the average attenuation D ₆₀ after 60 seconds was 71%, which was very good. It showed excellent antistatic performance. In addition, the woven fabric is
%, The average charge voltage V ₃₀ was 4100 V, and the average decay rate D ₆₀ was 70%.
And that the antistatic performance was hardly reduced even after the alkali weight reduction processing.

(Examples 6 to 9, Comparative Examples 5 to 9) Example 5
In the same manner as in Example 5 except that the mixing ratio of the mixture of PEG and RSO ₃ Na, the amount added, the spinneret and the spinning conditions in Example 3 were changed as described in Table 3, a drawn yarn was obtained to control the woven fabric. Table 3 shows the results of measuring the electric performance.

[0060]

[Table 3]

[0061]

According to the present invention, the polyalkylene glycol in the fiber is oriented as a long continuous continuous phase in the fiber axis direction while using a known antistatic agent with a relatively small amount of the antistatic agent. It is possible to disperse, and by fully exhibiting the function of the antistatic agent, it has extremely excellent antistatic performance and obtains a uniform antistatic polyester fiber without dyeing spots and the like with good yarn production stability. be able to.

[Brief description of the drawings]

FIG. 1 is a transmission electron micrograph (magnification: 6,000) of a longitudinal section of a fiber showing the dispersion state of polyethylene glycol in the antistatic polyester fiber obtained in Example 1.
Times).

FIG. 2 is a transmission electron micrograph (magnification: 6,000) of a longitudinal section of a fiber showing a dispersion state of polyethylene glycol in a conventional antistatic polyester fiber.

FIG. 3 is a transmission electron micrograph (magnification: 40, 0) of a longitudinal section of the antistatic polyester fiber obtained in Example 1.
The magnification is 00 and the visual field is 1 μm ² ).

FIG. 4 is a transmission electron micrograph (40,0 magnification) of a cross section of the antistatic polyester fiber obtained in Example 1.
00 times).

FIG. 5 is a transmission electron micrograph (magnification: 40,000 times, visual field: 1 μm) of a longitudinal section of a conventional antistatic polyester fiber.
m ² ).

FIG. 6 is a transmission electron micrograph (magnification: 40,000 times) of a cross section of a conventional antistatic polyester fiber.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Noboru Imabayashi 4-1, Ushikawa-dori, Toyohashi City, Aichi Prefecture Inside the Mitsubishi Rayon Co., Ltd. Toyohashi Plant (72) Inventor Hideto Kakita 20th Miyukicho, Otake City, Hiroshima Prefecture No. 1 Mitsubishi Rayon Co., Ltd. Central Research Laboratory (72) Inventor Yasuyuki Fujii 20-1 Miyukicho, Otake City, Hiroshima Prefecture Mitsubishi Rayon Co., Ltd. Central Research Laboratory (56) References JP-A-53-149247 (JP, A) (Japanese Patent Publication No. Sho 57-4724 (JP, B2)) (58) Field surveyed (Int. Cl. ⁶ , DB name) D01F ⁶ /62-6/92

Claims (2)

(57) [Claims] 1. 0.5 to 5% by weight of a polyalkylene glycol having an average content of 5,000 or more and a general formula of RSO ₃ M
(Where R is an alkyl group having 3 to 30 carbon atoms, 7 to
An aryl or alkylaryl group of 40, M represents an alkali metal) and 0.1 to 2% by weight of a metal salt of an organic sulfonic acid as an antistatic agent was added to the reaction system before completion of the polycondensation. In producing a polyester fiber by melt-spinning a polyester polymer containing ethylene terephthalate as a main repeating unit, the polymer is melt-spun from a spinneret under conditions satisfying the following requirements (A) and (B), and spun. The yarn is cooled once to a temperature below the glass transition point of the polyester, and subsequently run in a heating zone at a temperature equal to or higher than the glass transition point and lower than the melting point.
A method for producing an antistatic polyester fiber, comprising winding at a speed of 6,000 m / min. (A) the time required for the opening area S ₁ and the single-hole portion of the single-hole spinneret single pore volume V ₁ medium represented by the product of the length L ₂ to pass through the polymer is at least 3 ms (B ) Discharge linear velocity V ₀ of polymer from single hole of spinneret
Is 800cm / min or less 2. The antistatic device according to claim 1, wherein a spinneret for a solid fiber having a circular cross section is used as a spinneret, and the polymer is melt-spun under conditions satisfying the following requirements (A ₁ ) and (B ₁ ). Method for producing conductive polyester fiber. (A ₁ ) The time required for the polymer to pass through the single-hole volume V ₁ represented by the product of the opening area S ₁ of the single hole of the spinneret and the length L ₂ of the single hole portion is 10 ms or more ( B ₁ ) Linear velocity V of discharge of polymer from single hole of spinneret
₀ is 600 cm / min or less