JPS58163718A - Preparation of polyester fiber - Google Patents

Abstract

PURPOSE:To obtain the titled fibers having special micropores and depth and brightness of color in coloring, by drawing undrawn polyester fibers, containing specific inert fine particles, and having a specific birefringence and crystallinity under unheated conditions, and eluting the resultant drawn fibers partially with an alkali. CONSTITUTION:Undrawn polyester fibers, containing 0.1-5wt% inert fine particles having <100mmu average primary particle diameter and fine inert particles having >=100mmu particle diameter in such a state that >=3 secondary aggregated particles adjacent thereto at a distance between the centers of the primary particles of less than twice of the primary particle diameter may not be present in 10mu<2> cross-sectional area by observing in an enlarged electron microscopic photograph to such an extent as to discriminate the primary particle diameter, and having 0.07-0.14 birefringence (DELTAn) of the total fibers, <=0.06 birefringence (DELTAna) in the amorphous region and >=30% crystallinity (Xc) are drawn under unheated conditions at 1.05-1.35 draw ratio, and then treated with an alkali to elute >=2wt% fibers therefrom.

Description

[Detailed description of the invention] This article describes a method for producing poester fiber.

The present invention relates to a method for producing polyester fibers having improved color depth and clarity compared to K-11, which has a unique perforation and is colored.

Polyester fibers are widely used as synthetic fibers due to their excellent properties. However, polyester fibers can be used as natural fibers such as silk and silk, as well as fibers such as lace and acetate. **False color because there is no IINC color Kll color compared to iron ore fibers, etc.
It has the disadvantage of poor clarity.

In order to overcome this drawback, attempts have been made to modify dyes and chemically modify polyester, but none of them have been effective. How to make it glue or S
10. Proverbs: VM/-'s plastic
Nine methods have been proposed for forming mold-like irregularities on the surface of the surface.

However, even with these methods, the effect of improving the depth of a single 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 that uses plasma irradiation, the surface of the fiber in the weave part that is in the shadow of the irradiated surface! ! Since no convexity occurs, there is a drawback that the smooth fiber surface is exposed to the surface due to the rolling of threads within the fiber structure during wear, resulting in color spots.

On the other hand, as a method of imparting irregularities to the surface of polyester fibers, fibers made of polyoxyethylene glycol or polyester blended with polyoxyethylene glycol and a sulfonic acid compound are treated with an aqueous alkaline solution.
A method for producing hygroscopic fine pores on the fiber surface WK, or zinc oxide, in which kneaded micropores arranged in the fiber axis direction are formed.

A polyester fiber prepared by adding fine particles of an inert inorganic substance such as calcium phosphate to a polyester reaction system is mixed with alkaline water to remove inorganic mold particles to form micropores. Methods for producing AM fibers have been proposed. However, the fibers obtained by these methods do not have the effect of improving the depth of one color, and on the contrary, a decrease in one-sensitivity density is observed. In these methods, alkaline water droplets IIK
#! When it is not Mitsuhide, the effect of improving the brightness of the color cannot be taken into account, and when the treatment with alkaline water Ilk is light, it does not improve the greenness of the color.
Perhaps due to the irradiation of light from the micropores, the visual sense deteriorates, the color becomes dark, and the C color becomes white (1 to 5), and the stiffness of the fibers placed on top of it deteriorates, making it easier to see. It becomes difficult to form fipsyl.

In addition, a fiber made of polyester containing inorganic particles having a reversibility of less than a diameter of $/Juj turns was subjected to alkali weight reduction treatment, and both surfaces of the fiber were treated with an alkali weight reduction treatment of 1 to 0. In addition to imparting an irregular layer of irregularities to the IR turn, 1.~5oo is added within this M^.
A method has been proposed to improve the depth of color by making the unevenness of the surface appear uneven.
However, this method was not sufficiently effective in improving color stagnation, and the unevenness was destroyed by physical action from the outside, probably due to the extremely complex uneven layer. However, there are disadvantages in that the destroyed part is greatly discolored and has a difference in gloss compared to other unbroken parts, and furthermore, 4 is easily encapsulated.

The inventor of the present invention has conducted intensive studies to produce polyester fibers with excellent color depth and brightness that are free from shipping defects, and have found that the polyester fibers that are blended into polyester by conventional methods are
The primary particle diameter of the flat noodle of machine mold grains is 100 JJ JJ cron or more, or the average primary particle size is *ooivs.
When inert inorganic ultrafine particles of less than 1 micron are used, secondary agglomeration easily occurs due to the formulation, resulting in a large number of secondary agglomerated particles of 1 micron or larger. In the case of Target Izuku, 1.OJ is also inside the polyester fiber.
There are many particles larger than JJ turn, and therefore Alka Zeng Weight Loss - II & Kasu is formed by the late great wall of the 11th party - or more talent - 〆1 eye convex - iron - front both #I - and the color. It was found that the numeric effect of depth and trout resistance was reduced by 1% to 10%, which resulted in inferior fip resistance.
As a result of further investigation based on this knowledge, we found that the average primary soma @ is heavy...11ξ turns unreturned and 1...z
When a polyester fiber containing an inert 1,000-meter amount of secondary agglomerated particles with a turn or more is below a certain level is treated with an alkali, a convexity smaller than the wavelength of 1wm light is generated. A polyester fiber having a uniform gold coating on the surface of the fiber is obtained, and the dyed color has a brightness and vividness. I was the first to suggest that he would improve his skills to the next level.

However, since the polyester fibers obtained in the above manner can only be dyed by high-pressure dyeing, it is desirable to modify the amount of ink dyeing so that the voltage voids can be dyed.

-・The guest of honor has conducted various studies on methods for modifying the above-mentioned polyester fibers with ink-dyed sK, and surprisingly, he has found that the above-mentioned inert fine particle-containing polynisdel can be spun with high spin under specific conditions. Therefore, the microporous porous fiber obtained by forming an unstretched fiber having a high-order molded structure with vias, then stretching it to a specific magnification in a non-heated layer, and then carrying out a lucar treatment. It was discovered that the ester fiber has the effect of further improving the straightness and clarity of the IIK color of the ink dyeing effect, which is the desired purpose.The present invention is the result of further studies based on this knowledge. It is completed.

That is, the present invention contains 0.1 to S weight of inert fine particles having an average primary particle diameter of less than 10@J remicrons, The number of secondary AM particles defined below is 1/106111 or more per N16 square mitern across the fiber.
It is an inert mold particle-containing polyester fiber which does not contain more than 10 particles, and the multilayer folding pattern of the entire fiber is 01 to 0.14, and the birefringence a of the amorphous region is Oo. 3
1. 0% or more polyester unstretched Im in a non-heated state
．． It has been extended to 05~*ss@, but in the future Arca 1J611
To do this, use at least 3 weights of fiber #A
(This is a manufacturing method for polyester steel that prevents mold from tightening. However, secondary A-ken is a method of manufacturing polyester iron that prevents the mold from forming. Jisoko's original painting between the centers is 8 times the time immediately after the primary particle, and is a state in which they are completely close to each other.

According to the knowledge of the study results of numerous studies, the inert fine particles contained in the inert polyester fiber of the present invention have an average primary particle diameter of 10@jtJf.
The average primary If the particle size is 1 (1.1 turns or more) or 10
G19 When there are 3 or more secondary agglomerated particles of 1 turn or more per 1 square turn of the cross-fiber irises, sufficient color depth and clarity cannot be obtained with the low alkali loss rate, and finally, sufficient color depth and clarity cannot be obtained. In order to obtain depth and vividness of color or to create a stormy texture, increasing the alkali weight loss ratio deteriorates the abrasion resistance and fibrillation resistance, causing practical problems.

The average primary particle diameter is preferably in the range of 4 soi limiters or less, and more preferably in the range of 30 mm or less. In addition, the fiber cross section "1'O" square 1
The number of secondary agglomerated particles present per Ku'un' is:
Among these, it is preferable that the number is less than 2, and 4IK is preferably less than 111%.

'Immediately after the primary particle in the present invention means the diameter J of an imaginary sphere having the same volume as the primary particle.

In addition, secondary agglomerated particles are particles with a separation smaller than their primary particle diameter, that is, the distance between adjacent primary particles "to the center" is less than twice the diameter of the primary particle. This refers to particles in a state where they are mixed together, and the distance from one end to the other of these secondary agglomerated particles is the maximum, and the secondary agglomerated particles are considered to be primary particles according to the constant of decreasing size of the secondary agglomerated particles. IIN can be seen by an electron micrograph magnified in horizontal orientation with a diameter of 100 mm.

The inert particles in the present invention do not need to be defined as *@, as long as they are fine particles that are inactive to polynisfuls and can be dispersed in polyester fibers as described above (e.g., silica gel, etc.).
, containing or not containing aluminum, aluminum
A polyester reaction system in which a metal compound is combined with a 4-free compound or a phosphorus compound such as a particulate aluminum, a calcium carbonate sol, or a calcium carbonate sol, and a metallic compound. Preferably, PII is precipitated by internal reaction, and is particularly preferred, as will be explained in detail later. Preferably, the inert fine particles of 41 are precipitated, and even if the above-mentioned inert fine particles contain only one type of polyester fiber E, or if three or more types are partially contained, the content of such inert fine particles is If the amount is too small, the amount of polyester fibers finally obtained will be insufficient, resulting in color blurring and graininess (L-improving effect). , the intensity and sharpness of the image increases, but it is not very
When this happens, the depth and clarity of the colors will no longer be noticeable.
On the contrary, the filip resistance deteriorates, and moreover, the spinning speed becomes extremely high, which is practically an indispensable practice range.

For this reason, the content of the inert fine particles needs to be in the range of 1 to 100% by weight, and preferably 40.1 to 100% by weight.

The polyester in the term "zero starting" has terephthalic acid as its main acid component, and at least one kind of glycol, preferably ethylene glycol, trimethylene/vcol, tetramethylene dalycol, and at least nine full kylene dalycols as the main acid component. The main target is polyester, which is the specialty of Daso tools.

It may also be a polyester in which part of the terephthalic acid content is replaced with Lun's Erfukan Ik Carvone oxidative content, and/or a part of the terephthalic acid content is replaced with a material other than Lord Weixiu. It may also be a polyester substituted with the above-mentioned glycol or a diol component.

The difunctional carboxylic acid other than terephthalic acid used here is, for example, isophthalic acid.

Natsutason dicarboxylic acid, a) phenyl dicarboxylic acid,
Diaenoxyethane dicarboxylic acid, cybenzoic acid in I-hydroxyethane, cybenzoic acid in P-oxyethane s1. 1.4
- Aromatic, aliphatic, dicarboxylic acid,
Bifunctional carvone lI of the fatba family! can be given. In addition, examples of diol compounds other than the above-mentioned Dasokoru include Jitter to Nakanan! , 4-dimetatool, neopentyldalyl, bisphenol, bisphenol, aliphatic-alicyclic-aromatic diol compounds such as bisphenol 8, and polyoxydialkylene dalicols.

Such polyester can be produced by any method! Good, Confucian explanation about polyethylene terephthalate - 1 Usually, terephthalic acid and ethylene glycol are directly esterified, or lower alkyl esters of terephthalic acid such as dimethyl terephthalate are transesterified with ethylene glycol. Alternatively, the first stage reaction is to react 11-terephthalic acid with ethylene oxyhydride to produce a d-12-terephthalic acid ester and/or its low polymer, and the reaction product of the first stage is depressurized. Under heating, the product is produced by a polycondensation reaction S (sH stage reaction) until the desired polymerization JIK is obtained.

The inert fine particle-containing polyester referred to in Book 11 can be procured by any method, but at any stage until the polyester expansion is completed as described in 41 (s
l) For the acid component constituting the ester, 1~
By reacting (- and (-) in advance, the alkaline earth metal catabolism and/or the chloride represented by the following general formula % formula % of Shima Morura) (1 (- and - metal sacrificial quantity -
A preferred method is to add C to 1.3% to the total amount of polyester, and then to complete the removal of polyester.

The compound used here is a phosphorus compound represented by the general formula % below, where 1 and 1 are hydrogen atoms or organic groups. This -valent organic group is an alkyl group or an aryl group.

794 kyl group or it t(C&)4G)kl'' (However, rst water bulk atom, alkyl group, azol group or 7ralkyl group, I is an integer of 2 or more, and 3 is an integer of 1 or more) etc., and R' and V may be the same or different,
X is a hydrogen atom, a -valent organic group, or a metal! The -valent organic group is the same as the definition of the organic group in 1k'' and Il''K above, and may be the same as or different from SR@IR'', and the metal is particularly alkali metal-alkali. Earth gold is preferred, especially alkaline earth metals
1, m is an integer of O or 1.

Examples of such phosphorus compounds include orthophosphoric acid.

trimethyl phosphate, trimethyl phosphate;
Methyl 1 dephosphate.

Phosphorus-114 and diesters such as ethyl-dophos-7-ethopyl-dophos-7ate.

M phosphate - trimethyl, triethyl phosphate - triphenyl triphenyl, V ester - methyl acid phosphatide, butyl acid phosphite and diesters of phosphorous acid, phosphorus compounds obtained by reacting phosphorous compounds with dalicol and/or water, and phosphorous compounds as described above and a predetermined amount of the corresponding metal. The compound is reacted with 11-m in the presence of 4
It is also possible to use one or more sulfur compounds selected from phosphorus compounds and the like. In addition,
When reacting the above-described syn compound and metal compound, it is most preferable to use the Guso tool used as a raw material for the target polyester.

The metal compound selected from the group consisting of alkaline earth metal compounds and lithium compounds to be used in combination with the above phosphorus compound is one that reacts with the above phosphorus compound to form an uncastable metal salt in the polyester. There is no limit to 4I0
For example, Mg.

Cas are Baa Ll monosalt, oxalate,
Organic salts such as benzoates, phthalates, stearates, borates, sulfates, *a salts, inorganic salts such as carbon-11 bicarbonates, hagenides such as chlorides, Examples include chelate compounds such as ethylene cyanide 4-metallic salt, fluorates such as oxidized methylate, ethylate-glycolate, phenolate, etc.@41 is ethylene dalycol KWIl. Preferred are organic carboxylates, octogenides, chelated compounds, and Alturanisi, and among them, organic carboxylates are preferred for 41, the above-mentioned alkaline earth metal compounds, and alkaline earth metal compounds.
^ Compounds may be used alone or in combination of eight or more.

When adding the above-mentioned phosphorus compound and metal compound, in order to give the finally obtained Bo V ester fiber Iak excellent color depth and its friction durability 11, K is determined by the amount of the phosphorus compound used and * It is necessary to determine the ratio of the amount of metal compound used to the amount of metal compound used. However, if the amount of the compound used in the present invention is less than 1/9, the final color of the polyester yarn obtained will be insufficient.
El to increase this amount! As the color increases, the overall appearance of the color will increase, but if it becomes too large, the color will no longer show any signs of improvement.
On the contrary, the friction durability deteriorates, and in addition, it becomes difficult to obtain a polyester with a sufficient degree of polymerization and softening point, which causes problems such as threads forming when carrying. The amount of the compound to be added should be within the range of O, S to m4 to the acid component constituting the polyester, preferably in the range of 411 to S to 8 molar. If the total number of equivalents of metals contained in the metal compound is less than 7 times the amount of the phosphorus compound, the color of the obtained polyester fiber will be insufficient; The degree of polycondensation decreases, the degree of polymerization of the polyester becomes dissociated, and the tempering point of the polyester produced decreases significantly to 5. Conversely, this amount is 1. The proverbial trend 91 and tacky color are generated, and instead of improving the depth of color, the visual density actually decreases. Therefore, the total number of metal equivalents of the above-mentioned phosphorus compound and gold compound is j O
The amount should be ~3-3 times the range ■, which is 411!
, O-3.0 times is preferred.

It is necessary to add the compound mentioned above and the metal compound to the polyester reaction layer without reacting them in advance. As a result, it becomes possible to form insoluble particles in the polyester in the form of uniform ultrafine particles. If the external phosphorus compound and metal compound are reacted in advance to form insoluble particles and then added to the tAv Nistil reaction system, the dispersibility of the insoluble particles in the polyester becomes - (and the coarse agglomerated particles are completely contained). This is undesirable because the effect of improving the depth of the polyester fiber finally obtained cannot be diminished. ゛The addition of the above-mentioned phosphorus compound and metal compound is necessary until the polyester fabrication is completed. It can be carried out at any stage and with any layer thickness.However, if the timing of addition of 9741 compound is not completed before the reaction of stage 15 is completed, 481
Completion of the reaction on the 49th floor may be inhibited, and if such a large amount of metal compound is added before the completion of the 1st stage reaction, if this reaction is an esterification reaction, coarse particles may be generated during this reaction. If transesterification occurs or transesterification occurs, this reaction may proceed abnormally quickly and cause a mid-boiling phenomenon.

It is preferable that the amount of the metal compound (both 80% by weight) and the total amount of the phosphorus compound be added after the stage where the reaction in the first stage of polyester synthesis is substantially completed. If the time of addition of the metal compound and the reaction at the joint stage has progressed too much, agglomeration of one particle or 11 particles may occur.
(Because the final polyester fiber color tends to be insufficient, the limiting viscosity of the polyester compound in reaction #C of II 2nd step is e, s ec g.
Before it was suitable! It is preferable that there be.

The above-mentioned phosphorus compound' and gold compound may be added all at once, in portions of 8 g or more, or may be added continuously.

Any catalyst can be used in the first step reaction of polyester production, but in the above metal compound, tI
There are compounds that have some ability to catalyze the transesterification reaction in the m1 stage reaction, and if such compounds are used,
This metallized product does not require the use of a K catalyst.
It can also be added as a catalyst by adding it before or during the reaction, but as mentioned above it may cause the boiling phenomenon, so the amount to be used is not included. Total amount of 6 metal compounds! It is preferable to keep the weight to less than 0.
In the present invention, the undrawn ester fiber is made of polyester containing inert particles such as Sotsu, and the fiber as a whole has a fairly high degree of orientation and crystallinity. A fiber with a special fine structure in which the amorphous region has only a very low degree of orientation is used.

That is, in the wrinkled fiber, the multi-layer folding pattern a of the amorphous region and the koji crystallinity X- of the entire fiber meet the following conditions.

It is a side effect of Pete. -26mu・---・・・
t~@, 1-4C preferably 0.01~0.11)Xs
=-*・% or more (preferably 4・Ten or more) 8l
--・,・6 or less (preferably O,・1~G, (1
4) The stiff, non-carved stretching spear can be rolled in a non-heated state as described below, and furthermore, it has good self-adhesive properties due to such stretching.
It can be used as a ceramic material and as an iron with excellent thermal and mechanical properties.

However, the composite JiIFrm of the entire textile is...O! At lower temperatures, the amount of deformation of the molecular chains during II stretching is large, and the stress distribution (distribution of stress) acting on the molecular chains is large, resulting in poor stretchability in non-thin ingots, and the need for preheating rollers, etc. Even if you raise your eyebrows and raise your eyebrows, elongation spots are likely to occur.On the other hand, those who can wear MU of 0,14 need to run at high speed 't'#A for 1...17 minutes. Not only does this require a separate winding device for each tatami mat, which increases the equipment cost, but also the uniformity of denier decreases significantly due to air resistance, especially in the case of Kjl11 denier yarn. In addition, if the m is larger than 0.14, the stretching tension will be high during stretching in an unheated state (as a result, the mechanical properties of the drawn fibers will deteriorate).

On the other hand, if the crystallinity Xe of the undrawn fibers is less than SO%, the drawn fibers obtained therefrom will have a fine structure that can be called highly oriented-amorphous and lack stability against heat. It requires heat treatment at a temperature of 11 degrees Celsius, which is expensive.

In addition to increasing energy costs, it is difficult to avoid heat-setting unevenness, which worsens the level dyeing properties of fibers.

At Takaaki Moto, the undrawn fibers have temperature, birefringence An and crystals of the entire fiber! L degree
l・) orientation! Single-fold [, birefringence Δ of the amorphous region
It is necessary that na be equal to or less than O, am. - First, if the orientational cohesion of the amorphous molecular chains distributed in the amount of crystals is high, stretching will cause many molecular chains to be undone (unfoided), resulting in the destruction of the crystals and the stretching unevenness. Not only is it a must-have, but it's also a must-have for any chicken set! Sexuality has arisen.

In other words, only when crystals that are oriented at a certain degree of S or more and are connected by amorphous materials with low restraint can rearrange the crystals without destroying them by stretching at a low magnification under a non-magnifying glass. It is possible to obtain polyester fibers that have excellent dyeability and leveling properties without the need for severe setting, and have the same thermal and mechanical properties as ordinary ivy-drawn heat escape yarns.

In addition, here, 1 word Ram, 81, and Xe are values obtained by the following method, respectively.

Feng) Mu (value set 1: fiber - f which is polarized at right angles to the axis
The value of the compound M ratio (n) for f1K and the ratio (demonstration) for light polarized parallel to the fiber axis, *chi4
It is expressed as 1 \ 1 f a rin - n ↓. A polarizing mirror equipped with a Peretta convensator was installed and the field was fixed by the electric railway. (However, the immersion liquid used was Taresyl 7 osphate.) Δna (birefringence of amorphous region) 2 A parameter that indicates the orientation of molecular chains in the amorphous region, determined from the specific gravity p1
11$1 double J1 prayer rate, yuibugaigangga fe (41MM
@ 0-s si *m issue 'A report) klfi
Calculate using the following formula.

ff1LXz= (41,7491-')/QJ@17
8■) It is calculated by the following formula.

'(re/(Ia+4m)) X 1 tjDmX
e(%) “(Xall fold is Rigaku mD-1cal
The all setting is used, and the field conditions are ssl ma x y@m, set-filter use, divergence scatter linda slit t, receiver slit @, BM. ) The fly to produce the undrawn fibers of polyester containing non-talking particles having the mold structure is melted and discharged from a die using the above-mentioned polyester having an "immature particle permeability". After cooling and solidifying the rods, the raw material is collected at a rate of 4,000 to 7...m/min, preferably 41 to $600./min.
It is preferable because of its excellent properties and the uniformity of the resulting undrawn fibers.
Thick (and embroidery 4R rough) above the knees
There is a method in which the withdrawal rate is set to 31'0/min or more, and after the A east discharged from the spinneret is once cooled to below the glass transition -R of the polyester, it is heated, heated, heated, etc. 1 feces 0 to 6 in summer due to heat etc.
・'CKNJEIIIn, scold 11si...II/1
It is also possible to adopt the above-mentioned collection method.

here! #Ilm to issue is φ! ! Even if it is ≦ in the Zhongyi Sensho that does not have a part, it is in the middle! It may be a hollow fiber having a 11 m cross section Hk1, and the shape of the hollow part may be inland or irregular. A core-sheath III consisting of a modified polyester that contains a polyester and an unmodified polyester that does not contain a modified polyester, a sheath component that is a modified polyester, and a core component that is an unmodified polyester.
Even if it is a synthetic fiber, it has eight or more layers of modified polyester and unmodified polyester.
Side 1 Composite fibers may also be used.

According to the zero-hatsu 1jK, such a non-tsuta extension train is i, as ~1.1!1 times, preferably 1.1.~t1 in the heating form.
Stretch it twice as much. This heron stretching can be done with the knee after melt spinning and once it is put into the package, but
It is also possible to reduce the equipment space, save labor, etc. by subjecting the spun fibers to continuous (continuous) so-called casting straight 111 stretching.

Normally, polyester untsuta-stretched fibers are stretched at a temperature higher than the glass transition temperature of polyester, and then further stretched to approximately 130-100°C.
The inert mold-containing polyester unstretched woven fabric used in the present invention can be heat-set at a temperature of C. Fibers with excellent gluing properties and uniformity, and good dimensional stability can be obtained.

(11) However, when m-tsuta stretching is performed, the easily dyeable woven structure formed at the pongee thread stage only deteriorates the adhesion of dust stL''clII. However, it is preferable to uniformly heat the M fibers evenly, and C4m unevenness occurs due to slight temperature unevenness in the plating process, so uniform crystallization cannot be avoided. If the temperature of the glass rises above the temperature of the glass due to heat expansion,
--- Fill the inside with cooling water --- La table W at room temperature gK
It is better to carry a plow, the growth rate of vines is 1.・Bang #1-g, am
(preferably L<4!1,1@~1.1@x). When the lI elongation rate is less than 1.0@, the effectiveness of the heron elongation Jl is L<1, and the mechanical properties (chier toughness, cutting elongation, primary yield point value, etc.) are generally inferior, Tsuta - Magnification is 13
When 111 turns seven times, Tsutashin 11 not only crystallizes, but also 18
The strong fIK-non-lightning IC of the dish that is deceptive becomes low.

From the thus obtained non-talking fine particle-containing poly:f-sprue fiber, a portion of it is removed by &1 if necessary.
After the fabric has been subjected to a false twisting process or the like, it can be further made into a fabric and then washed with an aqueous solution of an alkali compound.

The alkaline compounds used here include sodium monohydroxide, potassium hydroxide, tetramethylammonium oxide, sodium carbonate, potassium carbonate, and the like.

Among them, sodium hydroxide and potassium hydroxide (b%) are particularly preferred.

Although it varies depending on the water of the alkaline compound, the type of the alkaline compound, the M type conditions, etc., it is preferably in the range of 0.01 to 40% by weight, and 0.1% to the tatami mat.
~SO weight is preferably in the range of -1°J6 temperature is room temperature~
A temperature range of 100° C. is preferable, and it is usually carried out at a temperature of 1 minute to 4 hours. In addition, the amount of Cs removed by this alkaline compound according to Book ** 4611 should be in the range of 2 weight or more relative to the weight of the fiber. By applying water **''em@k, unevenness smaller than the wavelength of the normal line can be uniformly applied to the children's picture on the fiber surface, and the *a higher order inside the fiber as described above can be made uniform. A microporous polyester fiber with a microstructure is obtained, and the normal Im! Compared to similar microporous polyester fibers having a lint structure, the dyed product exhibits improved color depth and #5.

In addition, the polyester obtained by the method of the present invention must have the following properties: Depending on the situation, optional additives such as GLK1M, anti-coloring agents, 11sam resistance, fluorescent sun increasing agents, gloss 11 & tin 0 colorants, etc. may be included.Examples are given below. ! -do. *Parts and weight percentages in the examples indicate weight parts and weight %.

Friction discoloration was determined using the following method. Silver color [(K/8) was used as the scale for the itchy color. This value calculates the tm emissivity (R) of the sample cloth by Shimadzu RC-
14811 using a spectrophotometer, and obtained from the following Kupelkerk equation (Kub@lKm - Mun k ). A large value indicates a large tortoise effect.

Note that ward indicates a collection coefficient and 8 indicates a scattering coefficient.

(■) Using a friction discoloration/friction failure test using a Gakusho flat wear machine, the friction cloth was made of dicarbonate made of 100% ethylene terephthalate, and the test cloth was subjected to a specified load of 50Jj. The degree of discoloration was determined using a gray scale for discoloration and fading. If wear resistance is extremely low, t1ml
and L, if the pole Tote is 14, 'f: 5InL4゜Practically 4
A: #1 or higher is required.

Solid line l1lt Dimethyl terephthalate 100I1. Ethylene Daenicol 611 Calcium Acetate Monohydrate (for dimethyl terephthalate), 6. Raise the temperature from No. 14°C to 3sO°C over 4 hours under reduced pressure and remove the generated methanol from the system. A transesterification reaction was carried out while distilling off.Then, the reaction product obtained was preliminarily treated with @, @ill #')l
For dimethyl terephthalate, -
9 s mol%) and 0.31 molar calcium acetate monohydrate (1/8 times the mol in methyl phosphate) and 7 S, S parts at a temperature of 1 s/°C in ethylene glycol.
1st stream - 31 parts of the transparent beak IIl of the prepared diester calcicum salt of oxalic acid was mixed with water and heated under heat.
The traces of t@ were obtained by dissolving and steeping calcium monohydrate (I@4). The relationship between salt and lImcalcicum*S performance 9
．． 8 parts of Hatake was added, and then 70.0 parts of antithene dioxide was added.
Added 4g and transferred it to the polymerization cage. 0 then 1111 hours to intimidate from 1...■HI to 1■ wing I, and at the same time E1 hour 3
- The temperature was raised from 5uet: to sai°C over a period of minutes. Under reduced pressure of 1 part ■・I or less, at a polymerization temperature of 8-1°C for an additional Km time,
Polymerization was carried out in SO for a total of 4 hours to obtain an inert bomer with an intrinsic viscosity of 6IIs and a softening point of 1.6%. Made into chips.

This chip was dried by a conventional method, and the spinning temperature was 2 mK' from a spinning hole in which 24 circular spinning holes with a hole diameter of .
C:, Discharge, wind speed directly below the nozzle...! Cool and solidify with cooling air at Isa/sec, then 4! ! 410 proverbs/
Pick up at a speed of 1 minute, wind on a bobbin, aS denier,
Cutting elongation 11%.

-Yield strength6. -I JF/ds Xe 4 @
%smu0,0? m m 1M1& @, @
! 6 Next, the undrawn yarn was drawn at a stretching ratio of 1.11 times without heating to obtain a denier of 1 s and an elongation at break of 10%.

It was made into a tsuta-shinmushi with a boiling water shrinkage rate of a%.

The number of twists of this vine drawn thread (warp) is soo'r/M, and the writing speed is 40.
Book/3. (Weft) OT/M, density 40 threads/wound, made into plain woven fabric, No. 5.

The obtained greige fabric was precessed using a straw bale, and then boiled with water and salted to obtain a reduced-strength fabric.

This fabric is DIamix B1m@k KG-Pa (
Mitsubishi Kawei Industries - Seisatsu) After staining with 1 yen/vf for 3 min/min at ℃, sodium hydroxide*I/I and ^ide wt
The cloth was washed with 1 m of an aqueous solution containing ruphite II/'l at TE.degree. C. for 20 minutes to obtain an ink-dyed cloth.

The depth of color and the abrasion resistance of this black dyed fabric after three cycles of polishing were as shown in Table 1.

Example: Dimethyl terephthalate 1... Iku, Ethylene Sokole...
・Pour 1 part of calcium acetate into a transesterification tank and heat it for 4 hours under a nitrogen gas atmosphere (14°C).
The transesterification reaction was carried out while the temperature was raised from 0°C to 50°C and the methanol produced was removed from the system. Subsequently, .64 parts of anhydrous lithium salt (1.1% based on dimethyl terephthalate) was added to the resulting reaction, and this i-minute aX. ψphosphoric acid (0.69 molar relative to dimethyl terephthalate), KO after WIK% min,
64 Tsuru's antimony dioxide@, 64°S was added and transferred to a polymerization vessel.Next, as a cationic dye-dyeable copolymerization component, sodium di-di(I-human-oxyethoxycarbonyl)benzenesulfonate A4. 6 parts (relative to dimethyl terephthalate: s mol %) were added to the polymerized rose. Look in the mirror and reduce the pressure to 160■H1 or 1-Hl over an hour.1. 1 hour and 3.0 minutes at the same time? t S @ 'Ct
p was also raised to 2IO°C. Under reduced pressure of 1 Hjl or less,
.

Polymerization was carried out for an additional 2 hours at a polymerization temperature of 1°C, for a total of 4 hours.
Intrinsic viscosity @, 11! , softening point! A polymer of ia°C was obtained.

Using the same machine as in Example 1, spinning, cold drawing, II fiber, pu-Vit, and 7" potash treatment were carried out using the same machine as in Example 1 to obtain a plain woven fabric with a weight loss rate of 0%. .

The voice after this alkali treatment is uneven @a Catkll
・n111ack CD-GLH (Hodogaya Chemical Yusho)
After dyeing in a bath containing Glauber's salt z I/I at 130°C for 1 minute, an ink-dyed cloth was obtained by annealing according to a conventional method. The color depth and abrasion discoloration resistance after abrasion 20@■ of this ink-dyed fabric were as shown in Table 1.

Note that the undrawn yarn obtained here had an Xs of 37%.

Mu@, @? It had a microstructure of ＠*na＠, 02 m.

Ground Comparison 1 Instead of the high-speed spinning and J'1 drawing carried out in Example 1, the take-up mode was 1'1'''OO''II, normal 'spinning for 7 minutes, and the stretching temperature was ss°C, and the draw ratio was 3. The same procedure as in Example 1 was carried out except that ordinary stretching was carried out by s times, and the same procedure as in Example 1 was carried out to obtain a black ms with a weight loss of 0%.

The swelling was as shown in Table 1.

Comparative Confucian example! In place of the high-speed # system and cold tsuta-shin that was done in
Over-current spinning and drawing temperature si with take-up mode of 11 @ 0 ■/min
Stretching ratio is 3. A 1s denier/24 filament Sagi-shinmushi was obtained by using the same machine as in Example 3, except for the normal stretching of z times. Ta.

The results were as shown in Table 1.

Chapter 1/Table

[Brief explanation of the drawing]

It is the XIHI@forced line for □, where le indicates a fifi due to crystal, and Ia indicates 1 Nm degree due to amorphous. Procedural Amendment Written April 20, 1927, Mr. Commissioner of the Japan Patent Office 1, Indication of Case Patent Application Showa @ 7 311311 No. 2, Name of Invention Process for Manufacturing Polyester 4Il #11 3, Person Making Amendment Relationship with Case Patent Applicant: 1-11 Minamihonmachi, Higashi-ku, Osaka (300), Teijin Ltd. Representative Tomoo Tokusue (11 Specification No. 10) [Correct the phrase "Sijikagel" in the first line to read "Silica Sol." (!1 In the same page, page 14, line 9, the word “mall road” is corrected to “the number of cells.” , Putelua IF phosphate" has been corrected to "ethyl acid phosphate, ethyl acid phosphate, butyl acid V phosphate". (4) Same as above! In the 20th line of the 3rd line, r (t+nfsid1n)
g) J and aruwo r (unfoldlmg) J
I am corrected. (5) On page 24, line 14 of the same page, it is corrected to read ``completion prayers''. (In 61, page 33, line 11, the text ``Gold #l cured - O-branch mater reaction'' is corrected to read ``R reaction for 60 minutes under total reflux.'')

Claims (1)

[Claims] We have an inert wafer with a weight of 0.1 to 2, whose average primary bond is only 1 @ 111 turns. The inert molten powder contains an inert molten powder that does not have a secondary stiffness defined below of 1 ton or more per fiber cross-stroke or 3 or more drops per turn. Polyester woven fabric with sewage anchor and two folds fiLO, @1740
, 14, a polyester unstretched fiber sheet in which the compound analysis Δl of the amorphous region is Oo・6 or less and the intensification jIx@ is 1@% or more is heated from 1.01 to t, S, S in a non-heated state. A method for manufacturing polyester fibers in which the tatami mold is made by stretching the vines and then exposing them to alkali to elute the 3 weight atom of the fibres. Electron magnified to S* where child i meets in the office ■ Overcame with mold mirror photograph, central interlayer of primary cladding next to cast - 3 pieces of diameter of primary soshi - #cIII intercepted state ■It refers to the Soshi group.