JPS61152821A - Production of modified polyester fiber - Google Patents

Abstract

PURPOSE:A polyester mainly composed of ethylene terephthalate units is combined with microfine particles of a specific particle size and a higher fatty monocarboxylic acid ester and the composition is melt-extruded and heat-treated to give the titled fiber of good color tone, soft and velvety touch and high abrasion resistance. CONSTITUTION:100pts.wt. of polyester mainly composed of ethylene terephthalate repeating units are combined with 0.005-2.0pts.wt. of microfine particles of 0.05-3mu average particle size such as calcium carbonate particles and 0.1-10.0 pts.wt. of a compound mainly containing a 34-65C higher fatty monocarboxylic acid ester such as hexyl montanate, then they are melt-extruded into fiber and heat-set at a temperature satisfying the equation: 170<=T<=Tm-5( deg.C) (where T is heat-treatment temperature; Tm is the melting point of the polyester) for 0.1sec-30min to give the objective fiber.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method for producing polyester fibers having good color tone, sliminess and abrasion resistance, and a soft feel.

The present invention relates to a method for producing polyester fibers having good color tone and abrasion resistance, durable slimy feel, and soft texture.

[Prior art and its problems]

In recent years, various modifications have been made to polyester fibers in order to obtain an appearance and feel similar to natural fibers. Among these, many studies have been conducted on polyester fibers that have an appearance and texture similar to high-quality animal hair.

However, although various methods have been studied to provide either the slimy feel characteristic of animal hair or the soft texture characteristic of animal hair, no attempt has been made to create a polyester fiber that combines the characteristics of both. Furthermore, methods for imparting the sliminess characteristic of animal hair to polyester fibers include methods of incorporating polyorganic siloxane, polytetrafluoroethylene, etc., which are easily slippery polyesters, into polyester fibers, and adding wax or fluorine to polyester fibers after fiber formation. Although methods have been investigated for attaching slippery organic compounds such as metal compounds and silicone compounds to polyester fibers, no satisfactory results have been obtained.

In other words, it is true that adding slippery polymers such as polyorganosiloxane or polytetrafluoroethylene can give polyester fibers a slimy feel, but these slippery polymers are not compatible with polyester. Due to its poor solubility, a large amount must be added to give it a slimy feel.
As a result, it was significantly colored and could not be used as animal hair-like polyester fiber.

Meanwhile, wax and fluorine compounds after fiber formation.

When a slippery organic compound such as a silicone compound is attached to polyester fibers, it can give a slimy feel, but it comes off during washing, dry cleaning, etc., resulting in poor durability.

In addition, as a method of imparting the soft texture characteristic of animal hair to polyester fibers, a method of attaching a softening agent such as a surfactant after fiber formation has been studied, but although it is possible to impart flexibility, washing The fabric softener falls off from the fibers during dry cleaning, resulting in poor durability.

For this reason, it has been considered impossible in the art to obtain animal hair-like polyester fibers that have good color tone, durable sliminess, and soft texture.

[Purpose of the invention]

The object of the present invention is to provide a method for producing polyester fibers having good color tone and abrasion resistance, durable slimy feel, and soft hand.

[Structure of the invention]

The above purpose is to add 0.005 to 2.0 parts by weight of fine particles with an average particle size of 0.05 to 3μ to 100 parts by weight of polyester whose main repeating unit is ethylene terephthalate, and whose main component has 54 to 54 carbon atoms. 0.1 to 10 of a compound consisting of 65 higher aliphatic monocarboxylic acid esters
．． After melt-spinning a polyester containing 0 parts by weight, a modified polyester is heat-treated at a temperature T°C that satisfies 170≦T≦Tm 5 (°C) for a period of 0.1 seconds or more and 30 minutes or less. This is achieved by a fiber manufacturing method. (However, Tm refers to the melting point of the polyester.) The polyester in the present invention may be a homopolyester or a copolyester as long as it is a polyester mainly composed of polyethylene terephthalate.

Examples of components to be copolymerized include diethylene glycol, propylene glycol, neopentyl glycol, and tetraethylene glycol.

1.4-butanediol, polyalkylene glycol,
1. Diol components such as 4-cyclohexane dimetatool, adipic acid, sepacic acid, phthalic acid, isophthalic acid,
2.6-naphthalene dicarboxylic acid, 5-sodium sulfoisophthalic acid.

Examples include dicarboxylic acid components such as dodecanedioic acid and dimer acid, polyfunctional dicarboxylic acid components such as trimellitic acid and pyromellitic acid, and oxycarboxylic acid components such as p-oxyethoxybenzoic acid.

The fine particles in the present invention mean at least one type of inert particles selected from internal particles, inorganic particles insoluble in polyester containing polyethylene terephthalate as a main component, organic particles, and the like.

The internal particles here refer to those separated by the particle separation method described later, but internal particles include metal compounds (e.g. calcium compounds, magnesium compounds, manganese compounds) added during the synthesis of polyester whose main component is polyethylene terephthalate. These particles are produced by combining at least one of the phosphorus compounds and the components constituting the polyethylene terephthalate. Specific examples of metal compounds include calcium acetate, magnesium acetate, and manganese acetate.

Examples include lithium acetate and lithium carbonate.

As the phosphorus compound, one or more of phosphoric acid, phosphorous acid, phosphonic acid, and partial esters of these esters can be used.

On the other hand, calcium carbonate is an inert particle.

Wet silicon oxide, dry silicon oxide, aluminum silicate, barium sulfate, calcium phosphate.

Talc, titanium dioxide, aluminum oxide, aluminum hydroxide, calcium terephthalate.

Calcium silicate, fluorine-containing fine particle polymer.

Examples include fine powder of cross-linked polymer.

These inert particles can be processed by various methods commonly used for the purpose of removing coarse particles and adjusting the particle size, such as air classification, natural sedimentation separation as an ethylene glycol slurry or water slurry, centrifugal sedimentation separation, sand mill crushing, etc. It is preferable to use those that have been subjected to/or classification treatment.

The average particle size of the fine particles contained in the polyester in the present invention must be 0.05 to 3 μm, more preferably 0.1 to 2 μm.

Yarn of fibers obtained with an average particle size of less than 0.05μ
The system friction coefficient becomes high and the sliminess becomes insufficient.

On the other hand, if the average particle size exceeds 5 μm, the abrasion resistance of the resulting fibers will be poor.

In the present invention, the content of fine particles with an average particle size of 0.05 to 3μ must be 0.005 to 2.0 parts by weight, and 0.005 to 2.0 parts by weight.
．． 005 to 1.0 parts by weight is preferably 10.01 to 0.5
Parts by weight are more preferred.

If the particle content is less than 0.005 parts by weight, the yarn-based stiffness coefficient of the obtained fiber will be high and the sliminess will be insufficient.

On the other hand, if the particle content exceeds 2.0 parts by weight, large amounts of coarse particles will be generated, and the abrasion resistance of the resulting fibers will be poor.

Examples of compounds contained in the polyester of the present invention whose main components are higher aliphatic monocarboxylic acid esters having 34 to 65 carbon atoms include monohydric or dihydric alcohols and higher aliphatic monocarboxylic acid esters having 10 to 33 carbon atoms. A compound containing as a main component an ester reaction product obtained by reaction with an acid is preferably used. Specific examples include hexyl montanate, seryl montanate, octacosyl lignocerate, merisyl lignocerate, seryl lignocerate, merisyl cerotate, seryl cerotate, etc., and naturally occurring montan wax, carnauba wax, and beeswax. , candelilla wax,
Nukarou, Ibotaro and the like are also preferably used.

It is preferable that the acid value of the compound whose main component is a higher aliphatic monocarboxylic acid ester having 34 to 65 carbon atoms is 5 or less from the viewpoint of sliminess.

Further, the effects of the higher aliphatic monocarboxylic acid ester compound include the effect of finely dispersing particles in the polyester, and the effect of lowering the thread-system friction coefficient and imparting sliminess.

The higher aliphatic monocarboxylic acid ester compound in the present invention must have 34 to 65 carbon atoms, preferably 40 to 62 carbon atoms.

When the number of carbon atoms is less than 34, the heat resistance of the higher aliphatic monocarboxylic acid ester compound is poor, resulting in severe discoloration of the resulting polyester fiber.

On the other hand, those having more than 65 carbon atoms have poor compatibility with polyester, and therefore have a small sliminess imparting effect.

In the present invention, the compound whose main component is a higher aliphatic monocarboxylic acid ester having 34 to 65 carbon atoms needs to be contained in the polyester in an amount of 0.1 to 10.0 parts by weight, preferably 0.5 to 10.0 parts by weight. It is 8.0 parts by weight.

If the content is less than 0.1 part by weight, the effect of imparting slimy properties and soft texture is small. This is because by heat-treating the polyester fiber containing a compound whose main component is a higher aliphatic monocarboxylic acid ester used in the present invention, the compound oozes out onto the surface of the fiber, giving it a soft texture. However, if the amount is less than 0.1 part by weight, this effect cannot be exhibited.

Moreover, if the content of 1 exceeds 10.0 parts by weight, the resulting polyester fibers will be intensely colored, making them unsuitable for practical use.

The polyester of the present invention may contain a stabilizer, a heat resistant agent, a weather resistant agent, an antioxidant, and an antistatic agent, if necessary.

Any additives such as flame retardants may be included.

The method for producing the polyester of the present invention is not limited, and any known polymerization method may be used.

As a polymerization method, for example, after an esterification reaction between a dicarboxylic acid and a glycol, or after a transesterification reaction between a dicarboxylic acid ester and a glycol.

A method in which the obtained prepolymer is subjected to polycondensation at high temperature under vacuum, or a method in which the prepolymer itself is used as a starting material to undergo polycondensation is used.

The timing of addition of the compound to generate internal particles is not particularly limited, but the metal may be added at any time from the time when the esterification reaction or transesterification reaction is substantially completed to the early stage when the polycondensation reaction has not progressed very much. At least one of the compounds is preferably added to the reaction system as a glycol solution.

The inert particles and the higher aliphatic monocarboxylic acid ester compound may be added before the polyester polymerization reaction, during the polymerization reaction, after the completion of the polymerization, during chip drying, or immediately before spinning, but in the case of inert particles, it is especially important to add inert particles. Particles in water and/or
Alternatively, it is preferable to add a slurry dispersed in ethylene glycol before or during the polymerization reaction.

In the present invention, the polyester containing particles is produced separately and kneaded with a higher aliphatic monocarboxylic acid ester compound in a melting process, or the polyester containing a large amount of particles and/or higher aliphatic monocarboxylic acid ester compound is produced. A method of diluting and mixing is also preferably employed.

In order to melt-spun the polyester thus obtained, it is not necessary to employ any special method, and any ordinary melt-spinning method for polyester fibers may be employed.

The fibers spun here may be solid fibers without a hollow part or hollow fibers with a hollow part, and the outer shape and the shape of the hollow part in the cross section of the spun fibers are circular. It may be a strange shape.

The polyester fiber thus obtained may be heat-treated either simultaneously with or after stretching, during false twisting, or after being made into a fabric, but preferably after being made into a fabric.

The heat treatment temperature TC in the present invention is 170≦T≦Tm
It is necessary to be in the range of 5 (℃), and 200≦T≦
The range of Tm-10 (°C) is preferable. Heat treatment temperature is 17
If the temperature is less than 0°C, the higher aliphatic monocarboxylic acid ester compound will hardly ooze out onto the fiber surface, making it impossible to impart a soft texture.

Furthermore, if the heat treatment temperature is higher than Tm 5 (° C.), fusion of single yarns occurs, resulting in hardening of the texture.

The heat treatment time in the present invention must be 0.1 seconds or more and 30 minutes or less, preferably 1 second or more and 20 minutes or less. If the heat treatment time is less than 0.1 seconds, the exudation of the higher aliphatic monocarboxylic acid ester compound onto the fiber surface due to the heat treatment is insufficient, and a soft texture cannot be imparted.

If the heat treatment time is longer than 30 minutes, the higher aliphatic monocarboxylic acid ester compound will undergo thermal deterioration, resulting in poor color tone of the resulting polyester fiber.

The fineness of the obtained polyester fiber is not limited to %t, but it is preferably 3 deniers or less, since the smaller the fineness is, the more animal hair-like texture can be obtained.

Further, as a heat treatment method, known means such as an open method, a hot roller, and a hot plate can be used.

〔Effect of the invention〕

(1) Polyester fibers containing a specific amount of fine particles having a specific particle size and a specific amount of a compound consisting of a specific higher aliphatic monocarboxylic acid ester are heat-treated at a specific temperature for 1 hour, so the present invention The polyvarnished margin chill fiber obtained by this method has good color tone, abrasion resistance, slimy feel and soft texture. Therefore, it is a fiber suitable for use as an animal hair-like polyester fiber.

+21 Since the polyester fiber containing a compound consisting of a specific higher aliphatic monocarboxylic acid ester and specific fine particles inside the polyester fiber is subjected to a specific heat treatment, the polyester fiber obtained by the method of the present invention is easy to wash, dry clean, etc. Even after this process, there is no loss of sliminess or loss of flexibility, and the product has excellent durability.

The present invention will be explained in detail with reference to Examples below.

The method for separating fine particles in the present invention and the method for measuring each characteristic value of polyester and polyester fibers in Examples were carried out as follows.

(Particle separation method) After orthochlorophenol is dissolved in polyester, centrifugation is performed. After separation, the supernatant liquid is removed by decanting to obtain separated particles. Separated particles may be contaminated with polyester components due to insufficient separation, so to remove this component, orthochlorophenol at room temperature is added to the collected particles, and after homogeneous suspension, they are again superimposed. Repeat centrifuge treatment. The thus obtained separated particles are vacuum dried at 120° C. for 16 hours and weighed.

Note that the separated particles obtained by the above operation may contain both internal particles and inert particles.

Therefore, in order to separately determine the amount of internal particles and the amount of inert particles, the separated particles are depolymerized in ethylene glycol to dissolve only the internal particles. The remaining particles are centrifuged to obtain separated particles, which are dry weighed to determine the amount of inert particles. The difference between the initial total separated particle amount and the inert particle amount is defined as the internal particle amount.

(Intrinsic viscosity) Determined from the value measured at 25°C in an orthochlorophenol solution.

(Method for creating tubular knitted fabric) A tubular knitted fabric is knitted using the filament to be evaluated using a 27-gauge sock knitting machine (manufactured by Koike Kikai Seisakusho ■).

(Scouring method) The cylindrical knitted fabric to be evaluated was treated with 0.2% nonionic activator [Sanded G-900 (manufactured by Sanyo Kasei ■)] and 0.2% by a conventional method.
% of soda ash for 5 minutes, then washed with water and dried.

(Color tone) It is expressed as a b value measured by stacking six or more pieces of tubular knitted fabric to be evaluated and using a digital measurement color difference calculator [manufactured by Suga Test Instruments (I)] in a state where no irradiation light is transmitted. The larger the b value, the more yellowish the color tone becomes.

(Sliminess) 12 cylindrical knitted fabrics to be evaluated were touched by 10 panelists and subjected to a sensory test, and those with a thickness of 5 Å or more were evaluated as ○, and 2 to 4 panelists felt that the fabrics were slimy. Those with a slimy feel were rated △, and the others were rated ×.

(Particle size of particles) The average particle size is the diameter of a sphere having the same volume as the volume of the particles measured by optical or electron micrograph of the particles in the polyester.

(Abrasion resistance) Figure 1 shows a schematic diagram of the abrasion tester. Sample (tube knitted fabric) 1
is attached to the head 3 using the holder 4 so that the friction area with the friction cloth 2 is 12.5d, and the sum is 7
507 load 5 is placed on it. This was attached to a friction table 6 via anti-slip sandpaper 7, rotated eccentrically at 85 rpm, and after 10 minutes of friction, the sample 1 was removed and the degree of wear was judged visually.

In other words, when wear occurs, the rubbed area looks whiter than the non-rubbed area, so we observe the condition where the rubbed area looks white (frosting) and divide it into the following three stages. It was determined that

Grade 3: Frosting is not acceptable.

Grade 2: Some frosting is observed.

Grade 1: Frosting is significantly observed.

Among the above, when used for ordinary fabrics, the passing level is 2°3.

(Yarn-system friction coefficient) The filament yarn to be evaluated is made into a skein shape in advance,
JI using a radar set friction coefficient tester manufactured by Maede Seiki ■
Measure the static friction coefficient according to SL1074.

(Flexibility) A panel of 10 people evaluated the refined 1g tubular knitted fabric.
A sensory test was carried out by touching with hands, and those with a panel size of 5 Å or more judged to be flexible, those judged to be flexible by 012 to 4 panelists were marked as Δ, and the others were marked as x.

(Melting point) Using DSC-IB manufactured by Perkin-E1mer, the temperature was raised from room temperature at a rate of 16°C/min in a nitrogen gas atmosphere using 10 cm of sample polymer, and the minimum point of the melting peak was measured. And so.

Example 1 A transesterification reaction was carried out in a conventional manner using 100 parts by weight of dimethyl terephthalate and 62 parts by weight of ethylene glycol using 0.06 parts by weight of calcium acetate as a catalyst, and the resulting product was mixed with 0.04 parts by weight of antimony dioxide and 0 parts by weight of lithium acetate. ．．
After adding 0.07 parts by weight and 0.04 parts by weight of calcium acetate, 0.02 parts by weight of phosphorous acid and 0.10 parts by weight of trimethyl phosphate, a polycondensation reaction was carried out to obtain an intrinsic viscosity of 0.61. , melting point 260°C, internal particles (average particle size 1.0 μ) amount 0.35 parts by weight (based on polyester 100
(parts by weight) was obtained.

The internal particles contained 1.2 parts by weight of calcium element, 169% by weight of lithium element, and 4.9% by weight of phosphorus element. (Polyester: A) 100 parts by weight of terephthalic acid and 43 parts by weight of ethylene glycol were kneaded to prepare a slurry.

This slurry was continuously added at a constant rate to a reactant of 50 parts by weight of terephthalic acid and 21.5 parts by weight of ethylene glycol stored at 245°C in a reactor, and an esterification reaction was carried out at 245°C under normal pressure to produce a product. The water was continuously distilled out of the system from the rectification column. The slurry supply time is 3 hours 3
The esterification reaction was completed in 0 minutes, and the esterification reaction was completed in 4 hours. From the obtained reaction product, an esterification reaction product corresponding to 100 parts by weight of terephthalic acid was transferred to a polymerization apparatus, containing 0.045 parts by weight of phosphoric acid, 0.023 parts by weight of antimony dioxide, and having an average particle size of 1.5μ. 2.3 parts by weight of calcium carbonate was added as an ethylene glycol slurry, and a polycondensation reaction was carried out in a conventional manner. The obtained polymer has an intrinsic viscosity of 0.61
, had a melting point of 260° C., had no internal particles defined by the present invention, and contained 2 parts by weight of calcium carbonate. (
Polyester 2B) Polyester: Perform a 5-polycondensation reaction in the same manner as B without adding inert particles, and have an intrinsic viscosity of 0.62% and a melting point of 260°C.
obtained a polymer. (Polyester: C) Polyester: Carry out the polycondensation reaction in the same manner as B without adding inert particles, and after the reaction, carnauba wax 5
．． 0 parts by weight was added and mixed under reduced pressure for about 10 minutes to obtain a polymer having an intrinsic viscosity of 0.60 and a melting point of 260°C. (Polyester D) The thus obtained polyester A, polyester kB, and polyester CI polyester D were chip-blended, containing 98.7 parts by weight of polyester and 0 internal particles.
．． A composition consisting of 2 parts by weight, 0.1 parts by weight of calcium carbonate, and 1.0 parts by weight of carnauba wax was obtained.

After drying the composition under reduced pressure, it was melt-spun using a spinneret having 24 spinning holes with a diameter of 0.23 all at a spinning temperature of 290° C. and a discharge rate of 31 y/min, and then spun onto a bobbin at a winding speed of 1200 m/min. I wound it up.

The obtained undrawn yarn was heated with a hot roller at 87°C and 150°C.
It was stretched 3.7 times using a hot plate, and the strength was 4.
A 65 denier, 24 filament polyester filament with a 99/d 1 elongation of 37% was obtained.

After scouring using this polyester filament, 2
The friction coefficient and color tone were measured after heat treatment at 30° C. for 1 minute in an open environment. The friction coefficient was 0.30 and the %b value was good as Zl.

In addition, it has good sliminess and flexibility, and has a wear resistance of 3.
It was in good condition.

Example 2 (Experimental Examples 2 to 12) In the same manner as polyester B of Example 1, dry silica with an average particle size of 0.3μ (Nichita Aerosil Co., Ltd.) was prepared.
"Aerosil" manufactured by R-972) was added, and 1 silica was added.
．． A polyester containing 0 parts by weight was obtained. (Polyester: E) A polyester containing 3.0 parts by weight of kaolinite having an average particle size of 0.9 μm was obtained in the same manner as in Polyester 2B of Example 1. (Polyester: F) Polyester of Example 1 = Polyester containing 5.0 parts by weight of beeswax in the same manner as D (Polyester: O) Polyester containing 5.0 parts by weight of S-Montan wax C Polyester: H) A polyester (polyester) containing 5.0 parts by weight of hexyl montanate was obtained. These polyester E,
F, G.

The intrinsic viscosity and melting point of H and I are both 0.61°260°C
Met.

These polymers and the polymer obtained in Example 1 were each chip-blended to obtain the compositions shown in Experimental Examples 2 to 13 in Table 1 in the same manner as in Example 1, and yarn was spun in the same manner as in Example 1. A polyester filament was obtained. After scouring, these polyester filaments were heat-treated in an open environment at 230°C for 1 minute, resulting in a color tone with a Masatsu coefficient of 9, sliminess,
Abrasion resistance and flexibility were measured. The results are shown in Table 1.

Experimental Example Ya 2.5 does not contain higher aliphatic monocarboxylic acid ester compounds, so it has a high stiffness coefficient and is slimy.
Less flexible. Experimental Example 4 does not contain fine particles, so it has a high mass coefficient and is poor in sliminess. Experimental Example A6 had a low content of higher aliphatic monocarboxylic acid ester compounds, so it had a high stiffness coefficient and was inferior in sliminess and flexibility. Further, Experimental Example No. 12 had poor wear resistance due to the large amount of fine particles. Experimental Examples A5, 7°, 8.9, and 10.11 were within the scope of the present invention, and were excellent in color tone, sliminess, abrasion resistance, and flexibility.

Comparative Example 1 Butyl stearate (carbon atoms: 22) was blended into chips of the polyester 2E of Example 2 in an amount of 2% by weight based on the polyester. This polymer was spun in the same manner as in Example 1 to obtain polyester filaments. A cylindrical knitted fabric was created using this polyester filament, and after scouring, it was heat-treated in an open environment at 230°C for 1 minute. When the color tone was measured, the b value was 10.5, which had a strong yellowish tinge and was unusable. there were.

Comparative Example 2 Polyester of Example 1: Polyester having an intrinsic viscosity of 0.61 and containing 15 parts by weight of carnauba wax was prepared in the same manner as D. A polyester having a melting point of 260°C was obtained. This polyester and polyester IIB were chip-blended to obtain a polyester mixture containing 12% by weight of carnauba wax and 0.4% by weight of calcium carbonate. This polyester mixture was spun in the same manner as in Example 1 to obtain polyester filaments. A cylindrical knitted fabric was made using this polyester filament, and after scouring, it was heat-treated in an open environment at 230°C for 1 minute, and its color tone was measured.The b value was 12.2, and it had a strong yellowish tinge, making it unusable. Ta.

Comparative Example 3 Polyester of Example 1: The average particle size was 5 in the same manner as B.
Intrinsic viscosity 0 containing 2.0 parts by weight of calcium carbonate
．． 61. A polyester having a melting point of 260°C was obtained. This polyester is chip-blended with polyester di-Al polyester = CI polyester: D, and a polyester containing 0.2 parts by weight of internal particles, 0.1 parts by weight of calcium carbonate with an average particle size of 5 μm, and 1.0 parts by weight of carnauba wax. I got it. This polyester was spun in the same manner as in Example 1 to obtain polyester filaments. A cylindrical knitted fabric was prepared using this polyester filament, and after scouring, it was heat-treated in an open environment at 230° C. for 1 minute, and its abrasion resistance was measured.

Example 3 87 parts by weight of terephthalic acid and 42 parts by weight of ethylene glycol were charged into an autoclave and heated at 220°C to 1.5 kp/
(The esterification reaction is carried out under the pressure of J, and the reaction rate is 50%.
After reaching the temperature, the esterification reaction was completed while gradually increasing the temperature under normal pressure.

To this reaction product was added 0.06 parts by weight of wet silica having an average particle size of 0.8 μm as an ethylene glycol slurry. Additionally, 0.06 parts by weight of magnesium acetate, 0.05 parts by weight of lithium acetate, and 0.025 parts by weight of acetate
11 parts by weight, 0.08 parts by weight of trimethyl phosphate, and 0.01 parts by weight of arsenic acid were added, and a polycondensation reaction was carried out by a conventional method. Furthermore, after the completion of the polycondensation reaction, 2.0 parts by weight of carnauba wax was added under normal pressure, and then 15 parts by weight of carnauba wax was added.
The mixture was kneaded under reduced pressure for a minute.

The resulting polyester contains magnesium.

0.07 parts by weight of internal particles consisting of lithium and phosphorus elements,
Wet silica 0.06 parts by weight, carnauba wax 2.0
The intrinsic viscosity of polyester is o,
62, the melting point was 260°C.

The polyester was spun using a spinneret having 24 spinning holes with a diameter of 0.25 m at a spinning temperature of 290°C and a discharge rate of 312/3.
It was melt spun for 1 minute and wound onto a bobbin at a winding speed of 1200 m/min. The obtained undrawn yarn was stretched 3.7 times using a hot roller at 87°C and a hot roller at 150°C, and then heat-treated with a hot roller at 230°C by changing the heat treatment time as shown in Table 2. I did it.

A tubular knitted fabric was created using these polyester filaments, and after scouring, the sliminess and flexibility were measured. The results are shown in Table 2.

Table 2 Experimental Examples Nos. 17 and 18 had good flexibility because the heat treatment time was within the range of the present invention, but Experimental Example No. 16, whose heat treatment time was outside the range of the present invention, had poor flexibility.

Example 4 A cylindrical knitted fabric was created using the polyester filament of Example 2 Experimental Example 11, and after scouring, heat treatment was performed in an oven for 1 minute with the heat treatment temperature changed as shown in Table 3 to improve sliminess and flexibility. The sex was measured. The results are shown in Table 3.

Table 3 Experimental Example JllL20.21 had good flexibility because the heat treatment temperature was within the range of the present invention, but Experimental Example AI9.22, which had a heat treatment temperature outside the range of the present invention, had poor flexibility.

Example 5 A tubular knitted fabric was created using the polyester filament of Example 2 Experimental Example 1611, and after scouring, it
Heat treatment was carried out in an open environment at Q° C. while changing the heat treatment time, and the sliminess and flexibility were measured in two colors. The results are shown in Table 4.

Table 4 As is clear from Table 4, Experimental Example 12 is within the scope of the present invention.
3.24 had excellent sliminess and flexibility in two tones, but
Experimental example 25, which had a long heat treatment time, had poor color tone.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of an apparatus for measuring wear resistance. 1: Sample 2: Friction cloth 3: Head 4: Holder 5: Load 6: Friction table 7: Sandpaper

Claims (1)

[Claims] The average particle size is 0.05 to 100 parts by weight of polyester whose main repeating unit is ethylene terephthalate.
Contains 0.005 to 2.0 parts by weight of 3μ fine particles and 0.1 to 10.0 parts by weight of a compound whose main component is a higher aliphatic monocarboxylic acid ester having 34 to 65 carbon atoms. After melt spinning polyester, 170≦T
0.1 seconds or more at a temperature T℃ that satisfies ≦Tm-5 (℃) 3
A method for producing a modified polyester fiber, the method comprising heat treating for a time of 0 minutes or less. (However, Tm indicates the melting point of polyester.)