JPS58144118A - Polyester fiber structure with improved color - Google Patents

Abstract

PURPOSE:Polyester fibers containing a specific amount of inert fine particles are treated with alkali, dyed and coated with a polymer with a refractive index lower than the fibers to give the fibers with deep and bright color tones after dyed. CONSTITUTION:Polyester fibers containing 0.1-5wt% inert fine particles of less than 100mmu average primary particle size and less than 3 secondary coagulation particles of larger than 100mmu particle size in 10 squaremicron of the cross section are treated with alkali to leach off more than 2wt% based on the weight of fibers, then dyed and coated with a polymer with a lower refractive index than the fibers such as polytetrafluoroethylene, polydimethylsilane, ethylene-vinyl acetate copolymer or polyethyl acrylate. As inert fine particles, are used preferably silica sol, alumina sol or titanium oxide of extremely fine particles, especially fine particles formed by inner precipitation consisting of a metal compound of the formula and an alkaline earth metal compound. The above additive is added before completion of polymerization and included in the fibers preferably.

Description

[Detailed description of the invention] The present invention relates to a method for producing polyester fibers.

More particularly, the present invention relates to a method for producing polyester fibers that have special pores and exhibit improved color depth and clarity when colored.

Polyester has many excellent properties and is widely used as a textile fiber. However, compared to natural fibers such as wool and silk, woven fibers such as rayon and acetate, and acrylic fibers, polyester fibers do not have a deep color when dyed. Also color development,
It has the disadvantage of poor clarity.

Conventionally, attempts have been made to improve dyes, chemically modify polyester, etc. in an attempt to overcome this drawback, but none of them have been sufficiently effective. In addition, we have developed a method for forming a transparent thin film on the surface of polyester fibers, and a method for forming transparent thin films on the surface of polyester fibers, and
A method has been proposed in which SOO stomach A-187- is subjected to plasma irradiation to form fine irregularities on the fiber surface.

However, even with these methods, the effect of improving the depth of color is insufficient, and in addition, the transparent thin film formed on the fiber surface easily falls off when washed, etc., and its durability is insufficient. - In the method of applying q*tit, unevenness does not occur on the surface of the fiber in the part of the ridge that is shadowed by the irradiation, so the smooth fiber surface is not caused by the rolling of the thread within the fiber structure that occurs during wear. There is a drawback that it appears on both sides and becomes a color inspection.

On the other hand, Table 11 for polyester fibers! ! As a method of imparting convexity, polyoxyethylene glycol or polyoxyethylene glycol and a sulfonic acid compound are blended;-
A method for producing hygroscopic fibers in which wrinkle-like micropores arranged in the fiber axis direction are formed into a WINK shape by treating fibers made of polyester with alkaline water IIs waves, or by oxidation! plow.

A polyester fiber made by adding fine particles of an inert inorganic substance such as calcium sulfate to a polyester reaction system is treated with alkaline water to remove fine inorganic particles and form micropores. Methods for producing hygroscopic fibers have been proposed. However, the fibers obtained by these methods do not have the effect of improving the color intensity, but have a concentration lower than that of Cl11. water soluble 11
When the treatment with aqueous alkaline solution is not sufficient, no effect of improving the color depth is observed, and when the treatment with alkaline aqueous solution is sufficient, rather than improving the depth of the color, it may be due to the diffuse reflection of light by the micropores. , the line of sight density decreases, and even if it is colored, it appears white, the strength of the fibers overlaid on it decreases significantly, and it becomes easily fibrillated, making it unsuitable for practical use.

In addition, fibers made of polyester containing inorganic fine particles such as silica with a particle size of sO millimicrons or less are subjected to an alkali weight reduction treatment to impart irregular irregularities of 0) to O, Fumiku p on the fiber surface, and these irregularities. A method has been proposed in which the depth of color is improved by creating fine irregularities of 50 to 200 millimeters inside. However, even with this method, the effect of improving the depth of color is insufficient, and in addition, the unevenness is destroyed by external physical effects such as friction, probably due to the extremely complex shape of the unevenness. There are disadvantages in that the portion is significantly discolored or has a difference in gloss compared to other undestructed portions, and furthermore, it is easily fibrillated.

The inventors of the present invention have conducted intensive studies in an attempt to obtain polyester fibers with excellent color depth and clarity without the above-mentioned defects. Use inert inorganic fine particles with a diameter of 100JV/27 or more, or an average primary particle diameter of less than 100JV/27. Since a large number of the above-mentioned secondary agglomerated particles exist, as a result, each pigeon house has 11Kiooi within the polynisder fiber.
There are particles larger than one quinine, and therefore alkali ψ reduction treatment 1
1, the fibers have irregularities of the order of 111iKy#I-111iKy#I-1, which are in the wave-like range or higher than that of the light-colored fibers, which reduces the effect of improving the depth of color and dance properties, and also reduces the fibril resistance. I learned what I am doing.

As a result of studies based on this knowledge, the present inventor surprisingly found that if the average primary particle diameter is less than 1 turn and the secondary agglomerated particles of 10gIIψ1 turn or more are below a specific level. By treating polyester fibers with alkali, the fibers have irregularities smaller than the wavelength of visible light. Polyester fibers that are uniformly distributed over the entire surface of the strawberry are obtained, and furthermore, after dyeing, the depth and sharpness of color removal is significantly improved by coating with a polymer having a lower refractive index than the fibers, and the fibril resistance is excellent. They discovered that it was possible to improve meat quality and completed the present invention.

That is, the present invention is suitable for cases in which the average primary particle diameter is LOO19i, and the secondary agglomerated particles defined by
When polyester fibers containing 0.1 to lI weight percent of inert fine particles, which do not exist at least 3 per 10 square microns, are treated with alkali, at least 2 of the wrinkled fibers are treated with alkali.
After dyeing the eluted polyester fibers at weight%,
It is a polyester fiber structure coated with a polymer having a refractive index lower than that of armpit fibers. However, secondary agglomerated particles are particles in which the center-to-center distance of adjacent primary particles is closer to each other than the diameter of the -order particles when viewed in a single magnified electron microscope photograph that allows the diameter of the -order particles to be clearly distinguished. The inert particles referred to in the present invention have an average particle group of 1 @ 4.
149j Ripun Mino has to be thrown, and 106Il
Secondary agglomerated particles with more than 1 turns cross the fiber 1i10 square liters
There must not be more than three ripundoro. The average primary particle II is 1.61v1 chron or more, or tooj
If there are 8 or more secondary agglomerated particles of v1 size or more in the textile side*1g1to square On the other hand, if the alkali weight loss ratio is increased in order to obtain sufficient color depth and freshness and a nice texture, the abrasion resistance and fibril resistance will deteriorate.

As for the average-order particles, it is preferable to use ears of 1 coon or less; 3.・Range S of 1 sl Vn or less
is preferable to 41. Furthermore, it is preferable that the number of secondary agglomerated particles present in the fiber cross section 10 square turns is 41.

The primary particle diameter as used in the present invention means the diameter of an imaginary sphere having the same volume as the primary particle.

In addition, secondary agglomerated particles refer to particles in which the primary particles are smaller than the diameter of the primary particles (i.e., the distance between the centers of adjacent primary particles is less than or equal to the diameter of the water particles). The maximum distance from end to end of the secondary agglomerated particles is defined as the size of the secondary agglomerated particles. Secondary agglomerated particles according to this definition can be observed by electron microscope photography in which the primary particle diameter is magnified to a degree that allows identification.

The inert fine particles referred to in the present invention may be fine particles as long as they are inert to polyester and can be dispersed in polyester fibers.

For example, silica sol, fine particulate silica, alumina sol, fine particulate aluminum, a mixture of alumina and silica, ultrafine titanium oxide, calcium carbonate sol, I particulate Takeshun calcium, phosphorus compound and metal compound inside the polyester reaction system. Internally precipitated fine particles precipitated by reaction are preferable, and among them, the following general formula % formula % (t, where, W and W are hydrogen atoms or -extreme organic groups, and l!1 and W may be the same or different, M is an alkali metal or an alkaline earth metal, and the value is 1 when M is an alkali metal and =/z when M is an alkaline earth metal) Internally precipitated fine particles consisting of a metal-containing phosphorous compound and an alkaline earth metal compound represented by 41 are preferable for 41. The above inert fine particles 111 may be used alone or in combination of two or more. good.

If the content of inert fine particles is less than 0 or i% by weight, the front surface unevenness of the polyester fibers ultimately obtained will be insufficient, and it will be difficult to see the effect of improving coloration and sharpness. The depth and vividness of the color increases, but when the S weight exceeds -, the depth and vividness of the color no longer increases, and on the contrary, the fibril resistance deteriorates, and furthermore, spinning becomes extremely difficult. For this reason, the content of the inert fine particles needs to be in the range of 0.1 to S weight, and preferably in the range of 0.3 to 3 Illch. - The polyester in the present invention has terephthalic acid as the main acid component and at least 1811 glycols, preferably at least one fullkylene glycol selected from ethylene glycol, trimethylene glycol, and tetramethylene glycol as the main glycol component. The main target is polyester.

It may also be a polyester in which part of the terephthalic acid component is replaced with another difunctional carboxylic acid component, and/
Alternatively, it may be a polyester in which a part of the glycol component is replaced with the above-mentioned glycol other than the main component or another diol component.

The difunctional carboxylic acid other than terephthalic acid used here includes, for example, inphthalic acid.

7-trisine dicarboxylic acid, y phenyl dicarmono, diphenoxyethane dicarboxylic acid, /-human waxyethoxybenzoic acid, p-oxybenzoic acid, S-sodium sulfoin 7, adipine, sebacic acid, 1,4-
These include aromatic, aliphatic, and alicyclic difunctional carboxylic acids such as citrate and dipropylene acids. In addition, examples of diolized metals other than the above-mentioned dalicol include Schiff-hexane-1,4-dimetatool, neopentyl glycol, bisphenol, bisphenol 8, aliphatic, aromatic diol compounds, and polyoxyal+rendary. We meet at the pool or something.

Such polyester may be synthesized by any method. For example, polyethylene terephthalate) K and I
! - Then, usually, terephthalic acid and ethylene dalypool are subjected to a direct esterification reaction, or a lower alkyl ester of terephthalic acid such as terephthalic acid dimethyl is subjected to a varnish exchange reaction with ethylene dalycol. Alternatively, the first stage reaction is to react terephthalic acid and ethylene oxide to produce a glycol ester of terephthalic acid and/or its low polymer, and the reaction product of the first t stage is heated under reduced pressure. In the present invention, the polyester fiber containing 5 inert particles, which is produced by the second step of polycondensation reaction until the degree of polymerization reaches violet, has hollow parts even if it is a solid fiber without hollow parts. It may also be a hollow fiber. Further, the outer shape of the fiber in the transverse plane and the shape of the hollow portion may be circular or irregular.

Furthermore, even if it is a core-sheath composite fiber consisting of a modified polyester containing the above-mentioned inert mold softener and an unmodified polyester containing [,], the modified polyester is a sheath component and the unmodified polyester is a core component, A side-pie-side type composite fiber having two or more layers of modified polyester and unmodified polyester may be used.

In the present invention, ~S5 inactive mold particle-containing polyester fiber can be produced by any method, but the acid component constituting the polyester can be produced at any stage until the production of the polyester described above is completed. Against [-te 0.
5 to 3 mol of the following general formula % formula % (wherein, R1 and R@ are a hydrogen atom or a - organic group, R1 and W may be the same or different, and M is an alkali metal or alkaline earth For metal-containing phosphorus compounds, which are metal-containing metals, where ■ is x when the latter is an alkali metal, and 1/2 when MtiLy is an alkali earth metal; Then, 1.2 moles of alkaline earth metal compound (-) and () are added without reacting them in advance, and then the reaction of the polyester is completed, and the obtained polyester is mixed with 1lII! A method of Ik spinning is preferably employed.

The metal-containing metal phosphide used here is a phosphorus compound represented by the following general formula %, where R1 and R'' are hydrogen atoms or -valent organic groups. Specifically, alkyl groups and aryl groups.

Aralkyl group, or ←(C′H,)to]kR lid [7
, R is preferably a hydrogen atom, an alkyl group, a 7-aryl group, or an aralkyl group, t is an integer of 2 or more, and k is an integer of 1 or more), and R1 and W may be the same or different. V is an alkali metal or alkaline earth metal, Ll, N
a + K + MP * Cm + Sr * Ba
is preferred, and Ca I 8r l Bm is particularly preferred. m is 1 when M is an alkali metal, and 1/2 when M is an alkaline earth metal. When a phosphorus compound in which R' and/or R family is replaced with a metal (alkali metal or alkaline earth metal in 4!) is used, the micropores generated in the final polyester fiber become larger, resulting in a dark color similar to the original author. The sharpening effect cannot be obtained, and the fibril resistance also becomes poor.

In order to produce the above-mentioned metal-containing phosphorus compounds, phosphorous acid or the corresponding phosphorous ester (monophosphorous acid) is usually used.

When a predetermined amount of the corresponding metal compound is reacted with heating in the presence of a solvent, a volume of 14 is obtained. In this case, it is most preferable to use glycol, which is used as a raw material for polyester, as the solvent.

The alkaline earth metal compound used in combination with the metal-containing phosphorus compound may be any compound that reacts with the metal-containing phosphorus compound to form a metal salt insoluble in the polyester.

For example, Mg # Ca # BY *1 m of organic carboxylates such as acetates, oxalates, benzoates, heptatarates, and stearates, borates, sulfates, silicates, and sulfates. Inorganic acid salts such as monobicarbonate, hagenides such as chloride, chelate compounds such as ethylenecyaminetetraacetic acid complex, hydroxides, oxides, methyl F.

Alcola-F such as Motilado and Glyconte.

I can give you phenolate. In particular, organic carboxylic acid salts, hagnides, quinto compounds, and alcoholades that are soluble in ethylene dalicol are preferred, and organic carboxylic acid salts are particularly preferred.
The above alkaline earth metal compounds may be used alone or in combination of two or more.

When the above-mentioned metal-containing carbon compounds and alkaline earth metal compounds are added, the final polyester fiber @
In order to give excellent color depth and its friction durability, K is
It is necessary to specify the amount of the metal-containing phosphorus compound used and the ratio of the amount of the alkaline earth metal compound used to the amount of the wrinkled phosphorus compound used. That is, if the amount of the metal-containing phosphorus compound used in the present invention is too small, the color depth of the final polyester fiber obtained will be insufficient, and as the amount is increased, the color depth will increase. However, if the amount is too large, the depth of the color will no longer improve significantly, the abrasion resistance will deteriorate, and it will be difficult to obtain a polyester with a sufficient degree of polymerization and softening point, and furthermore, yarn breakage will occur during spinning. occurs frequently. Therefore, the amount of the metal-containing phosphorus compound added is 0.5 to 3 parts per 1 part of the acid component constituting the polyester.
In addition, when the amount of the alkaline earth metal compound added is less than .S times the amount of the metal-containing phosphorus compound added, The color depth of the resulting polyester fibers is insufficient, the polycondensation rate is reduced, making it difficult to obtain a polyester with a high degree of polymerization, and the softening point of the resulting polyester is greatly reduced. On the other hand, if an alkaline earth metal compound is used in an amount exceeding 1.2 times the mole of the metal-containing phosphorus compound, coarse particles of the alkaline earth metal salt of the polyester oligomer are generated, and the depth of color is not improved, but rather On the contrary, the line-of-sight density decreases, or the thermal decomposition of the polyester is severely accelerated, and the resulting polyester becomes yellowish brown in color.

Therefore, the amount of alkaline earth metal compound added to the metal-containing syn compound is O,S~! ,! It should be in the double molar range, and %6ca,t~! ,・A range of twice the mole is preferable.

It is necessary to add the metal-containing phosphorus compound and the alkaline earth metal compound to the polyester reaction system without reacting them in advance. By doing so, the insoluble particles can be formed in the polyester in the form of uniform ultrafine particles (5). If the above-mentioned metal-containing phosphorus compound and alkaline earth metal/compound are made to react with the alkaline earth metal/compound externally and added to the polyester reaction system in 11 to form insoluble particles, the dispersibility of the insoluble particles in the polyester will be poor and the particles will become coarse. Since the amount of agglomerated particles is increased to 5, the effect of improving the color depth of the finally obtained polyester fiber is no longer recognized, which is not preferable.

The addition of the metal-containing phosphorus compound and the alkaline earth metal compound can be carried out in any order at each step until the synthesis of the polyester is completed.

However, the completion of the first stage reaction may be inhibited at the time of addition of the gold-containing mVsyn compound or at a stage where the first stage reaction has not yet been completed. If it is added before the reaction of 1IR1IIl is completed, if this reaction is an esterification reaction, coarse particles may be generated during this reaction, or if it is an interesterification reaction, this reaction may proceed abnormally quickly and cause a bumping phenomenon. Therefore, in this case, the amount added is preferably less than 20% by weight of the alkaline earth metal compound. It is preferable that at least SO weight % of the alkaline earth metallized metal compound and the total amount of the metal-containing phosphorus compound be added after the stage where the reaction in the first stage of polyester synthesis has been substantially completed; If the compound and the alkaline earth metal compound are added at a stage when the reaction at the 11th N stage has progressed too much, particle aggregation and Il size increase are likely to occur, resulting in insufficient color depth of the final polyester fiber. I'm happy because there is a tendency
The intrinsic viscosity of the reaction mixture in the step reaction is 0. IK@
Preferably, before reaching that point.

Even if the above-mentioned metal-containing phosphorus compound and alkaline earth metal compound are added at the same time! It may be added dividedly to the collected balls or #JK may be added continuously.

Although any catalyst can be used in the first step reaction of polyester synthesis,
Among them, some compounds have the ability to catalyze the transesterification reaction in the first stage reaction, and when such compounds are used, it is not necessary to use a separate catalyst, and this alkaline earth metal compound can be used in the first stage reaction. Addition E7 before or during the reaction of
Although it can also be used as a catalyst, it may cause bumping phenomenon as described above, so it is recommended that the amount used be less than 20 parts by weight of the total amount of alkaline earth metal compound added. preferable.

It is necessary to remove a part of the inert fine particle-containing polyester fiber obtained by melt-spinning the polyester polymer thus obtained! This can be easily carried out by carrying out stretching heat treatment or false twisting depending on the FK, or by further treating the fabric with an aqueous solution of a 1-pull twisting compound.

Examples of the alkali compounds used here include sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide, sodium carbonate, and carbonate.

Among them, hydroxide) IJum, hydroxide★su? People are especially preferred.

The concentration of such an aqueous solution of an alkali compound varies depending on the type of alkali compound, processing conditions, etc., but is usually O0.1.
A thickness of ~4.weight- is preferred, and a thickness of 0.1 to 10 weight-〇S+S+ is preferred.

The treatment temperature is preferably in the range of room temperature to 100°C, and the treatment time is usually in the range of 1 minute to 4 hours. Moreover, the amount eluted and removed by the treatment 11 with the aqueous solution of the alkali compound is in the range 1 - 2 weight or more based on the weight of the fiber! IK
Should. By treating the polyester fiber with a water solution containing a fulkaline compound in step 5, a polyester fiber having a rough surface with roughness smaller than the wavelength of visible light can be obtained.

In addition, the polyester fiber obtained by the method of the present invention must have 1! Depending on the conditions, optional additives such as catalyst 1, color inhibitor, heat resistant agent, flame retardant, fluorescent whitening agent, matting agent 2, coloring agent, etc. may be included.

An example of a polymer with a small refraction length as used in the present invention is polytetrafluoroethylene.

Tetrafluoroethylene-bupyrene copolymer, detrafluoroethylene, -hexafluorobupyrene copolymer, tetrafluoroethylene-ethylene fubolymer, tetrafluoro Rz ethylene-tetrafluoropropylene copolymer.

Polyfluorovinylidene, polypentadecafluorotatylate, polyfluorethyl acrylate,
Polytrifluoroisoprobyl metatallate, BoV
)! Fluorine-containing polymers such as 7fluorop-ethyl methacrylate, silicon-containing compounds such as polydimethylsilane, polymethylhydride-dienesilxane, and polydimethylsiloxane, ethylene-acetic acid bifuromer, polyethyl acrylic
Examples include esters, acrylic acid esters such as polyethyl methacrylate, and polyurethane-based polymers. From these materials, one with a refractive index smaller than that of the fiber matrix may be selected and used. In this case, it is desirable to select a material that has as large a difference in fiber resistance as possible from the matrix fiber.

1. A method of coating porous polyester fibers with a low refractive index polymer; These include the spray method, batudeinda method, +throll method, and knife footing method.

(Ladleur method, gravure; - Tainda method, Rakuchu adsorption method, etc.).

In this way, after coating 4 m of porous polyester with the polymer, it is dried, and then heat-set may be performed as necessary.

The present invention also relates to tow, filament, and yarn.

It can be applied to all types of textile products such as woven and knitted fabrics and non-woven fabrics.

The polyester fiber structure obtained by the present invention has a high degree of general color effect that has not been obtained conventionally, has little discoloration due to external forces such as abrasion, and has sufficiently satisfactory practical performance.

The reason why the bathochromic effect is further improved when the acid polyester fiber is coated with a polymer having a lower refractive index than that of the cough fiber is considered to be as follows. In other words, since the surface of the polyester fiber is made into a surface by the micropores, the amount of specularly reflected light generated on the fiber surface is reduced, and the deep color level of the dyed product is improved, and the porous polyester fiber is coated with a low refractive index polymer. This is thought to be due to the synergistic effect of increasing the amount of absorbed light and improving the deep color level of the 1-1 dyed product. This effect is particularly noticeable when dyed to a very dark color.

Furthermore, coating #polyester fibers with a low refractive index polymer reduces the frictional resistance on the surface of porous polyester fibers.
．． Therefore, the degree of discoloration due to wear is reduced.

Furthermore, since the low refractive index polymer penetrates into the micropores of the porous polyester fiber, its durability against washing pressure is also poor.

The present invention will be explained in more detail with reference to Examples below.As a measure of the bathochromic effect, bathochromicity (K/8) is used, and this value is the spectral reflectance (R) of the sample.
It was measured using an O-type self-recording spectrometer needle and determined from the following Kubelker-Munk equation (Kub@lkm -Mw*). The larger this value is, the greater the deep color effect is.

B Note that S indicates an absorption coefficient and S indicates a scattering coefficient.

Abrasion resistance was measured using a Gakushin flat abrasion machine for abrasion fastness tests, using polyethylene/Tele7 Talley) 100 as the abrasion cloth.
Using Georgette F consisting of Is, the test cloth was heated to 5.0 fF.
) Abrasion was carried out both in place and in both directions under load, and the extent of discoloration was determined using the JIB standard gray scale for discoloration and fading. The case where the wear resistance was extremely low was rated 1, and the case where it was extremely high was rated 2. For practical purposes, a level 4 or above is required.

Example am: 100 parts of dimethyl terephthalate, ethylene dacol 6
0 parts, 1.6 parts of calcium acetate monohydrate O (6 moles of O per dimethyl terephthalate) were charged into a transesterification tank, and the electron gas IF1! 140℃ for 4 hours
The transesterification reaction was carried out while the temperature was raised from 230° C. to 230° C. and the generated methanol was distilled out of the system. Subsequently, the obtained reaction product was added in advance to the O, S parts of triethyl phosphite (o, s s s mol - relative to dimethyl terephthalate).
) and o, [-9.26 parts of a transparent lacquer solution of phosphite diester calcium salt prepared by the manufacturer at room temperature.
Mixed transparent solution of phosphorous acid diester calcium salt and calcium acetate obtained by melting 1 part of calcium acetate monohydrate (o, s s s times the mole relative to N triethyl phosphate) 9'IN@@ was added, and then 0.04 part of antimony trioxide was added and the mixture was transferred to a polymerization can. Next, the pressure was reduced from F@O■Hf to 1HP over 1 hour, and then the temperature was raised from 230℃ to zss℃ over 1 hour and 30 minutes [7
Under reduced pressure of less than 1.5 Hf, polymerization was carried out for an additional 3 hours at a polymerization temperature of tts°C, for a total of 4 hours and 1 minute, until the intrinsic viscosity was o, sss.
After the completion of the reaction, poly 1- containing inert fine particles 6.4- was obtained with a softening point of 25 I°C! i- was made into chips according to a conventional method.

The chips were dried by a conventional method and melt-spun at 290°C using a spinneret with 36 circular spinning holes with a hole diameter of 3-3. Then, γi denier/s6 filament hen Harahata was obtained.

This yarn K II IS z s o o T/m'
l and ZIllI! The material was hardened at a rate of 0.00 mm/m, and then the folds were subjected to aging heat treatment at 11 degrees Celsius for 1 minute with SO to fix the folds.

Anti-wrinkle strong thread with light 1 degree 47 threads/-, latitude degree m 1 thread/a
Two s and two zm are arranged alternately to weave a cold region fabric.The obtained gray fabric is boiled in a rotary washer for two times at a time.
Apply relatasu for 0 minutes, do grain raising, preset shield using the usual method, 3.5 t of sodium hydroxide, boil in a water moat, treat with 1 esi skin, IN I-1 reduction 1 rate #to-
, z@*mj and no- fabrics were obtained.

The fabric after these alkaline layers is coated with Dianix Bla.
@kHG-Fig (Mitsubishi Chemical Industries ■Product) 15%
After staining with OVF at 1111℃ for 60 minutes, hydroxylation) I
Jum 1 f/l and Heid p Sulfi) 1 f
A black dyed cloth was obtained by reduction washing with an aqueous solution of tlK containing /l at 'to°C for 20 minutes. These black fabrics had no fibril defects and were excellent in color depth and friction discoloration resistance after 200 wears as shown in Table 1.

As a result of observing the cross section of the single yarn of the black dyed cloth with the above weight loss rate of 2G- with an electron microscope magnified 10,000 times, the average primary particle diameter of the inert fine particles dispersed inside the fiber is tooR.
The number of secondary agglomerated particles less than 1,601 mm and 27 or more per square pn of fiber cross section w10.
There were three.・Next, 7soy of dimethylpolysiloxa with a viscosity of 10ocs measured at 25°C, 29.28% by weight of tall oil fatty acid containing basic oleic acid, 7% ammonia water, 0. i
f,) reethanolic acid, TIP, water @ @, 75
F was mixed with a homogenizer to obtain an emulsion. The obtained 7 diionic emuldigone treatment agent consisting of sy in terms of polymer solid content, 2F glacial acetic acid, and water SO.t was picked up by applying it to the black dyed fabric. 811), and after drying, it was heat-set at 1@O 0 C for 1 minute. /8 value and friction 1if! of the obtained treated fabric! As shown in Table 1, the friction discoloration resistance after 2.a was excellent.

Comparison Example In the example, the amount of calcium acetate l hydrate to be melted at room temperature during the preparation of a mixed transparent solution of diester calcium phosphite and calcium acetate added after the completion of the transesterification reaction was 0.6 parts (0.6 parts). A polymer containing inert fine particles with an intrinsic viscosity of 0.-4 and a softening point of 511° C. was prepared in the same manner as in Example **, except that C1,117 times the mole of triethyl phosphite was used. I got it.

Kjll yarn was made using this polymer as in the example.

Heating, hot section mm yarn, embossed, preset, alkali weight loss treatment, dyeing, and washing. The fiber obtained is 1.Oj!
It contained 5 secondary agglomerated particles with J'J turns or more per 10 square microns of fiber cross section. Then, the fibers were coated with a low refractive index finishing agent (polymer) in the same manner as in the example.

The results were as shown in Table 1.

Claims (1)

[Claims] (Heavy) Contains 0.1 to 5 by weight of inert fine particles with an average primary particle diameter of less than 100 Jjj" turns, and contains 1G (
1! The presence of 3 or more secondary agglomerated particles per 10 square microns of cross section of the fiber (the polyester fiber is treated with an alkali to elute at least the weight of the fiber, and then dyed and A polyester fiber structure coated with a polymer having a refractive index lower than that of the filler fiber.