JPS6367582B2 - - Google Patents

Description

[Detailed description of the invention]

a. Industrial Application Field The present invention relates to a method for producing a non-gritter woven or knitted fabric made of polyester false twisted yarn. b. Prior Art False twisted yarns made of polyester long fibers are widely used because of their excellent properties. In such polyester false twisted yarn,
During false twisting, the long fibers constituting the yarn are almost densely packed in the cross section of the yarn due to the twisting tension, and the fibers are heated with lateral pressure acting between them, so the fibers are crushed. Therefore, even fibers with a circular cross section are deformed into deformed hexagons or deformed pentagons. Due to the optical reflection of the flat surface of the fibers, when exposed to strong incident light, such as under direct sunlight, false-twisted yarn woven and knitted fabrics exhibit a phenomenon called glitter, where parts of the fabric shine like stars in various places. . Such glitter is a property that is disliked by people who have become familiar with natural fibers as a luster peculiar to polyester false twisted yarns, and it is desired to eliminate glitter. Conventionally, in an attempt to eliminate this grittiness, the cross-section was made into a multi-lobed shape such as five-lobed, six-lobed, or eight-lobed, and even when it was transformed into a pentagonal or hexagonal shape by false twisting, it still remained. It is believed that if the multi-lobed portions were allowed to remain, there would be fewer flat surfaces and no glittering portions, resulting in a so-called non-glitter, and this problem seemed to be solved by taking such measures. However, from a practical manufacturing perspective, manufacturing multilobal fibers with irregular cross sections requires
In addition to the high nozzle cost, multi-leaf nozzles have a large discharge area due to nozzle manufacturing constraints.
Spinning tends to occur in an unstable direction and is sensitive to the intrinsic viscosity of the polymer that controls the leaf shape and the spinning temperature, which not only requires extremely strict control, but also reduces polymer decomposition compared to circular nozzles. Since the nozzle is easily contaminated by objects etc., it is necessary to frequently interrupt spinning to clean the nozzle, resulting in a high running cost. In addition, from a quality perspective, false-twisted yarn with a multi-lobed cross section will cause white discoloration when dyed in a deep color, and it may be necessary to increase the amount of dye or reduce the dye exhaustion rate compared to false-twisted yarn with a circular cross-section. There was a need for a means to improve the dyeing rate, such as increasing the fiber microstructure. On the other hand, it contains 0.5% by weight or more of fine particles such as silica or calcium carbonate having a single particle diameter of 100 mμ or less and having a refractive index that is within 0.3 of the refractive index of the fiber,
In addition, a non-gritter woven and knitted fabric made of false twisted yarn of polyester fibers having fine and random irregularities on the fiber surface has been proposed (Japanese Patent Application Laid-Open No. 1983-1999).
Publication No. 107547). However, according to this method, 0.5% by weight is required to obtain a non-glitter effect.
As mentioned above, it is necessary to contain fine particles in polyester fibers in a large amount, preferably 1.5 to 10% by weight, and furthermore, as much as 3.0% by weight (example in the above publication) in order to actually obtain a sufficient non-glitter effect. This may be due to insufficient compatibility between the fine particles and the polyester, and also because the irregularities on the fiber surface take on an extremely complex shape, and such fibers easily change color and become fibrillated due to wear and tear during wear. Not practical. c. Purpose of the Invention As a result of intensive studies in an attempt to obtain a non-glitter processed yarn woven or knitted fabric free from the above-mentioned drawbacks, the present inventor has developed fine particles that are precipitated by reacting a specific phosphorus compound and an alkaline earth metal compound within a polyester reaction system. By subjecting a woven or knitted fabric made of polyester false-twisted yarn containing so-called internally precipitated fine particles to alkali reduction treatment, the fine particle content can be reduced.
Not only does it have a sufficient non-glitter effect even with an extremely small amount of less than 0.5%, but it also has excellent color depth and clarity when colored, has minimal discoloration due to friction, and has excellent fibril resistance. It was discovered that a knitted fabric can be obtained. As a result of a comparative study of the fiber obtained here and the polyester fiber disclosed in JP-A-5-107547, the two were found to be significantly different in terms of the size of dispersed particles in the cross section of the fiber and the size of unevenness on the fiber surface. It was confirmed that the size of the dispersed particles and the size of the unevenness formed on the fiber surface were much smaller in the case of the former internally precipitated fine particles than in the latter case of the externally added fine particles. We also learned that this provides superior non-glitter effects and color effects even with a small content of fine particles, resulting in less discoloration due to external forces such as friction and greater fibrillation resistance. Ivy. The present invention was completed through further studies based on these findings. d Structure of the Invention The present invention provides the following general formula in a reaction system for producing polyester as a base of fibers. (In the formula, R ¹ and R ² are monovalent organic groups, X is a metal,
0.1% by weight or more of internally precipitated fine particles precipitated by reacting a phosphorus compound (n represents 1 or 0) with an alkaline earth metal compound;
1. A method for producing a non-gritter woven or knitted fabric, which comprises treating a woven or knitted fabric made of polyester false-twisted yarn containing uniformly dispersed content of less than 0.5% by weight with an aqueous solution of an alkaline compound to reduce the weight by at least 3% by weight. The polyester in the present invention is a polyester having terephthalic acid as the main acid component and at least one type of glycol, preferably at least one alkylene glycol selected from ethylene glycol, trimethylene glycol, and tetramethylene glycol as the main glycol component. The main target is It may also be a polyester in which a part of the terephthalic acid component is replaced with another difunctional carboxylic acid component, and/or a part of the glycol component is replaced with the above-mentioned glycol or other diol component other than the main component. It may also be polyester. Examples of difunctional carboxylic acids other than terephthalic acid used here include isophthalic acid, naphthalene dicarboxylic acid, diphenyl dicarboxylic acid,
Diphenoxyethanedicarboxylic acid, β-hydroxyethoxybenzoic acid, p-oxybenzoic acid, 5-
Examples include aromatic, aliphatic, and alicyclic difunctional carboxylic acids such as sodium sulfoisophthalic acid, adipic acid, sebacic acid, and 1,4-cyclohexanedicarboxylic acid. In addition, examples of diol compounds other than the above-mentioned glycols include cyclohexane-1,4-dimethanol, neopentyl glycol, bisphenol A, and bisphenol S.
Examples include aliphatic, alicyclic, and aromatic diol compounds such as, and polyoxyalkylene glycols. Such polyesters may be synthesized by any method. For example, in the case of polyethylene terephthalate, it is usually a direct esterification reaction between terephthalic acid and ethylene glycol, a transesterification reaction between a lower alkyl ester of terephthalic acid such as dimethyl terephthalate and ethylene glycol, or a transesterification reaction between terephthalic acid and ethylene glycol. The first stage reaction involves reacting oxides to produce terephthalic acid glycol ester and/or its low polymer, and the first stage reaction product is heated under reduced pressure and polymerized until the desired degree of polymerization is reached. It is produced by a second step of condensation reaction. In the present invention, the fine particles contained in the above polyester system have the following general formula: These are internally precipitated fine particles that are precipitated by the reaction between a phosphorus compound and an alkaline earth metal compound. Here, the internal precipitation system refers to the above-mentioned phosphorus compound and alkaline earth metal being added to the polyester reaction system without reacting in advance, allowing both to react inside the polyester reaction system, and producing fine particles that are substantially insoluble in the polyester. A system that allows particles to precipitate uniformly, and the particle size is adjusted to the desired particle size externally in advance.
It is distinguished from an external addition system in which fine particles substantially insoluble in polyester are dispersed, preferably in glycol, alcohol, water, etc., and added to the polyester reaction system. In the above formula representing a phosphorus compound, R ¹ and R ² are monovalent organic groups. Specifically, this monovalent organic group is an alkyl group, an aryl group, an aralkyl group, or [-
(CH ₂ ) _l O] _k R ³ (wherein R ³ is a hydrogen atom, an alkyl group, an aryl group, or an aralkyl group, l is an integer of 2 or more, k is an integer of 1 or more), etc., and R ¹ and
It may be the same or different from R ² . X is a metal, and in particular, the monovalent organic group is the above-mentioned R ¹ and R ²
This is the same as the definition of organic group in R ¹ , R ²
The metals may be the same or different, and the metals are particularly preferably alkali metals and alkaline earth metals, especially Li, Na, K, Mg1/2, Ca1/2, Sr.
1/2, Ba1/2 are more preferable, among which Ca1/2
is particularly preferred. n is 1 or 0. Examples of such phosphorus compounds include trimethyl phosphate, triethyl phosphate, tributyl phosphate,
Phosphate triesters such as triphenyl phosphate, trimethyl phosphite, triethyl phosphite,
Phosphite triesters such as tributyl phosphite and triphenyl phosphite, phosphoric acid diesters such as dimethyl phosphate, diethyl phosphate, dibutyl phosphate, diphenyl phosphate, etc., dimethyl phosphite, diethyl phosphite, A phosphite diester such as dibutyl phosphite, diphenyl phosphite, etc. is mixed with a predetermined amount of an alkali metal compound such as Li, Na, K, etc. or an alkaline earth metal compound such as Mg, Ca, Sr, Ba, etc. One or more phosphorus compounds selected from phosphorus compounds obtained by reaction can be used. The alkaline earth metal compound to be used in combination with the above phosphorus compound is not particularly limited as long as it reacts with the above phosphorus compound to form a salt insoluble in polyester, and alkaline earth metal acetates, oxalates, etc. , organic carboxylates such as benzoates, phthalates, stearates, inorganic acid salts such as borates, sulfates, silicates, carbonates, bicarbonates, halides such as chlorides, ethylenediamine 4 Chelate compounds such as acetic acid complexes, hydroxides, oxides,
Examples include alcoholates such as methylate, ethylate, and glycolate, and phenolates. organic carboxylic acid salts, halides, chelate compounds, which are particularly soluble in ethylene glycol;
Alcoholates are preferred, and organic carboxylates are particularly preferred. As an alkaline earth metal
Among them, Ca is particularly preferred. The above alkaline earth metal compounds may be used alone or in combination of two or more. In order to produce a polyester containing uniformly dispersed internally precipitated fine particles made of the above-mentioned phosphorus compound and alkaline earth metal compound, for example, at any stage until the synthesis of the above-mentioned polyester is completed,
(a) the above phosphorus compound and (b) the above alkaline earth metal compound without reacting (a) and (b) in advance, and (a)
A preferred method is to add so that the total number of metal equivalents of (b) and (b) is 2.0 to 3.2 times the number of moles of the phosphorus compound of (a), and then complete the synthesis of polyester. I can do it. The content of the internally precipitated fine particles, which are precipitated by the reaction between the above-mentioned phosphorus compound and alkaline earth metal compound, in the polyester should be in the range of 0.1% by weight or more and less than 0.5% by weight based on the polyester. If the amount is less than 0.1% by weight, the non-glitter effect of the final processed yarn woven or knitted product will be insufficient, and as this amount is increased, the non-glitter effect and the depth and clarity of the color will increase. When the amount exceeds 0.5% by weight, the non-glitter effect and color depth no longer show any significant improvement, and the abrasion resistance and durability deteriorate on the contrary. Here, the content of internally precipitated fine particles in polyester is obtained by making the polyester fiber into an o-chlorophenol solution, separating it with a glass filter, and then centrifuging the solution using an ultracentrifuge. It is determined by repeatedly washing the separated particles with o-chlorophenol until polyester is no longer observed, and then weighing them. The thus obtained polyester containing a specific amount of the internally precipitated fine particles uniformly dispersed therein is spun into fibers by arbitrarily adopting a conventional melt spinning method for polyester fibers. The spun yarn is subjected to a drawing heat treatment if necessary, and then subjected to a false twisting process. There are no particular restrictions on the false twisting method, and commonly used false twisting methods and conditions can be used as they are. That is, as the method of the false twisting device, a spindle method, a friction method, a belt method, etc. can be arbitrarily adopted. Also, by using a single heater machine, a double heater machine, etc. as necessary, non-heatset yarn or heatset yarn can be obtained. Furthermore, the raw yarn for false twisting may be one obtained by drawing and orienting the spun yarn using a normal method.
subjecting the spun yarn to stretching false twisting in an unstretched state;
The raw yarn for so-called in-draw DTY may also be POY, in which the degree of orientation is increased by setting the spinning winding speed to about twice to several times the normal speed, and DTY is particularly suitable for simultaneous stretching and false twisting. At this time, the flattening of the cross-sectional shape is significant and gritters are likely to occur.
The effects of the present invention are significantly manifested. Of course, the false twisted yarn used in the present invention is not limited to a single yarn, and even if it is a simultaneously false twisted yarn of two or more yarns with different orientations, it can be made of two or more yarns with different melting points. It may be a processed yarn, a processed yarn consisting of two or more types of yarns with different elongations, or a processed yarn consisting of spun yarn, in which the yarn constituting the processed yarn is The effects of the present invention can be achieved as long as the particles contain precipitated fine particles. When two or more types of yarn are combined, the effect will be recognized if only the yarn on the surface layer side of the processed yarn contains the fine particles, or even when simply mixed, the mixing ratio is at least 50%. If so, it will be effective in eliminating grit after alkali weight reduction treatment. Typical examples of such composite false twisted yarns are as follows. That is, (a) As typified by Special Publication No. 45-28018,
The sheath yarn containing the internally precipitated fine particles of the present invention is wound around the core yarn that is being false twisted in an alternately twisted yarn form. In this case, the core yarn may be an overfeed of 0 to several percent, or may be an indraw method using highly oriented undrawn yarn (POY). (b) The internally precipitated fine particles of the present invention are used as slab-forming threads (sheath threads) in the methods described in Japanese Patent Publication No. 50-35147, Japanese Patent Publication No. 47-49459, and Japanese Patent Publication No. 43-28258. The contained polyester fibers are applied to make slub yarn. (c) As described in JP-A-54-101946, the internally precipitated fine particles of the present invention are contained as a high elongation component when two yarns with different elongations are entangled and then subjected to indraw false twisting. It is also possible to use a method such as making a composite yarn using polyester fibers. In order to remove a part of the thus obtained polyester false twisted yarn containing the internally precipitated fine particles and form fine irregularities on the fiber surface, after weaving and knitting the processed yarn, an alkali compound is added. This can be easily carried out by heating in an aqueous solution or by padding/steaming an aqueous solution of an alkali compound. Examples of the alkali compound used here include sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide, sodium carbonate, potassium carbonate, and the like. Among these, sodium hydroxide and potassium hydroxide are particularly preferred. Further, alkaline weight loss accelerators such as cetyltrimethylammonium bromide, lauryldimethylbenzylammonium chloride, etc. can be used as appropriate. The amount of alkali compound eluted and removed by treatment with an aqueous solution should be in the range of 3% by weight or more based on the weight of the fiber, and if the weight loss rate is less than 3%, satisfactory surface irregularities will not be formed. A sufficient non-glitter effect cannot be obtained. By treating with an aqueous solution of an alkaline compound in this way, the fibers are oriented in the axial direction, and the maximum value of the frequency distribution is in the range of 0.1 to 0.3 μ in the direction perpendicular to the fiber axis, and the length in the fiber axial direction is Ultra-fine pores with a diameter in the range of 0.1 to 5μ can be formed on the entire fiber surface, preventing specular reflection on the flat fiber surface caused by deformation of the fiber cross section during false twisting. As a result, not only the grittiness of specially dyed woven and knitted fabrics is drastically reduced or eliminated, but also they exhibit excellent color depth. The cross-sectional shape of the fibers spun in the method of the present invention has a synergistic effect of reducing flat surfaces due to the multilobed cross-sectional shape and preventing specular reflection due to the fine pores, resulting in an even more glitter-free luster characteristic of natural fiber materials. A multi-lobed cross-section is even more effective because not only can a woven or knitted fabric with no texture be obtained, but also the white discoloration that normally accompanies multi-lobal cross-sections does not occur during dyeing. Here, the multilobal cross-sectional shapes include 4 lobes, 5 lobes, and 5 lobes.
Examples include leaf shape, six-lobed shape, seven-lobed shape, eight-lobed shape, etc., and it is preferable that the shape is sharp. Note that the woven or knitted fabric made of the polyester false twisted yarn obtained by the method of the present invention can be appropriately subjected to known post-deepening processing, post-hydrophilization processing, etc. As the post-deepening process, a method of coating the fiber surface with a polymer having a refractive index lower than that of polyester, such as dimethylpolysiloxane or tetrafluoroethylene-propylene copolymer, can be preferably employed. Examples of post-hydrophilization processing include a method of treating polyester fibers with an aqueous dispersion of a polyester polyether block copolymer consisting of terephthalic acid and/or isophthalic acid or their lower alkyl esters, lower alkylene glycols, and polyalkylene glycols. can be preferably adopted. The polyester false twisted yarn woven or knitted fabric according to the method of the present invention is preferred because the durability of such post-processing is greatly improved due to the presence of special micropores on the fiber surface. In addition, the polyester fibers constituting the processed yarn woven or knitted fabric obtained by the method of the present invention may contain optional additives, such as catalysts, color inhibitors, heat resistant agents, flame retardants, fluorescent brighteners, matting agents, etc. It may also contain additives, colorants, etc. e Effects of the Invention As explained above, in the present invention, in order to use a polyester that uniformly disperses specific internally precipitated fine particles, the polyester is significantly finer than when conventional externally added fine particles are used. Particle dispersibility is obtained, and even if the content of the fine particles is small, superior non-glitter effects and color effects are obtained, resulting in less discoloration due to external forces such as friction and increased fibrillation resistance. I was able to do that. f Examples The following examples will be further explained. Parts and % in Examples indicate parts by weight and % by weight, and the grittiness, depth of color, and friction discoloration resistance when dyeing the resulting processed yarn woven and knitted fabrics were measured by the following methods. <Glitter Property> Glitter was evaluated by visually inspecting the dyed fabric under direct sunlight. The larger the evaluation number, the greater the grittiness. <Depth of color> As a measure of the depth of color, bathochromicity (K/
S) was used. This value was determined by measuring the spectral reflectance (R) of the sample fabric using a Shimadzu RC-330 self-recording spectrophotometer.
Munk) formula. The larger this value is, the greater the deep color effect is. K/S=(1-R) ² /2R (measurement wavelength 500 mμ) In addition, K shows an absorption coefficient and S shows a scattering coefficient. <Friction discoloration resistance> Polyethylene terephthalate was used as the friction cloth using a Gakushin type flat abrasion machine for friction fastness testing.
Using a dioset made of 100%, the test fabric was
The surface was abraded a predetermined number of times under a load of g, and the degree of discoloration was determined using a gray scale for discoloration and fading. The case where the wear resistance was extremely low was rated as 1st grade, and the case where it was extremely high was rated as 5th grade. For practical purposes, level 4 or above is required. Example 1 100 parts of dimethyl terephthalate, 60 parts of ethylene glycol, and 0.06 parts of calcium acetate monohydrate (0.066 mol% relative to dimethyl terephthalate) were charged into a transesterification tank, and heated from 140°C over 4 hours under a nitrogen gas atmosphere. The transesterification reaction was carried out while raising the temperature to 230°C and distilling the generated methanol out of the system. Subsequently, 0.4 part of trimethyl phosphate (relative to dimethyl terephthalate) was added to the resulting reaction product.
0.554 mol%) and 0.25 parts of calcium acetate monohydrate (1/2 mole relative to trimethyl phosphate) in 6.8
At room temperature, 7.45 parts of a clear solution of phosphoric acid diester calcium salt prepared by reacting in 100% ethylene glycol at a temperature of 120°C for 60 minutes under total reflux was added.
7.9 parts of a mixed transparent solution of diester calcium phosphate and calcium acetate obtained by dissolving 0.45 parts of calcium acetate monohydrate (0.9 times the mole relative to trimethyl phosphate) were added, and then 0.04 parts of antimony trioxide was added. was added and transferred to a polymerization can. Next, the pressure was reduced from 760 mmHg to 1 mmHg over 1 hour.
At the same time, the temperature was raised from 230°C to 285°C over 1 hour and 30 minutes. Polymerize for an additional 3 hours at a polymerization temperature of 285℃ under a reduced pressure of 1 mmHg or less, for a total of 4 hours and 30 minutes, to reduce the intrinsic viscosity.
A polymer with a softening point of 0.640 and a softening point of 259°C was obtained. After the reaction was completed, the polymer was made into chips according to a conventional method. The content of internally precipitated fine particles in this chip was 0.45%. This chip is dried by a conventional method and spun to 1090
This was carried out at a winding speed of m/min, and then drawing was carried out in a conventional manner to obtain a drawn yarn of 48 filaments of 150 denier. Spindle rotation speed
274000rpm, number of twists 2580T/M, yarn speed 106.2m/min,
False twisting was performed under the conditions of a heater temperature of 210°C and an overfeed of 1.0%. Next, the obtained false twisted yarn is additionally twisted with Z twist of 150T/M, and the gray yarn density is 51 threads/inches x weft 49 threads/inches, and the finished warp is 150T/M.
I created a plain woven fabric of 56 pieces/inch x weft of 54 pieces/inch. After heat-setting this fabric in a conventional manner, it was treated with a 3.5% aqueous sodium hydroxide solution at boiling temperature to determine the weight loss rate.
A 10% fabric was obtained. After this alkaline weight loss treatment, the fabric is made into Dianix
Black HG-FS (Mitsubishi Chemical Industries, Ltd. product) 15% owf
After staining at 130℃ for 60 minutes, sodium hydroxide 1
A black dyed cloth was obtained by reduction washing at 70° C. for 20 minutes with an aqueous solution containing 1 g/g/g of hydrosulfite and 1 g/g of hydrosulfite. Table 1 shows the glitter properties, depth of color, and friction discoloration resistance after 200 wears of this black cloth. Comparative Example 1 The same procedure as in Example was carried out except that the alkali reduction treatment using an aqueous sodium hydroxide solution, which was carried out in the above Example, was not carried out. The results are shown in Table 1. Comparative Example 2 Instead of the polymer used in Example, silica sol with an average primary particle size of 15 mμ was used as a micropore forming agent, and the silicon oxide content in the polymer was
The same procedure as in Example was carried out except that polyethylene terephthalate having an intrinsic viscosity of 0.680 and obtained by adding 3.0% was used. The results are shown in Table 1. Comparative Example 3 The same procedure as Comparative Example 2 was carried out except that the alkali reduction treatment performed in Comparative Example 2 was not performed. The results are shown in Table 1.

【table】

[Table] Comparative Example 4 197 parts of dimethyl terephthalate, 124 parts of ethylene glycol, 4 parts of Na-5-carboxylate Na-3-carbomethoxybenzenesulfonate (1.3 mol% based on dimethyl terephthalate), and calcium acetate monohydrate Pour 0.118 parts into a transesterification can,
The temperature was raised from 140° C. to 230° C. over 4 hours under a nitrogen gas atmosphere, and the transesterification reaction was carried out while the methanol produced was distilled out of the system. Trimethyl phosphate was subsequently added to the resulting reaction product as a stabilizer.
0.112 parts and antimony trioxide as polycondensation catalyst
0.079 part was added and transferred to a polymerization can. Next, following a normal pressure reaction for 20 minutes, the pressure was reduced from 760 mmHg to 1 mmHg over 1 hour, and at the same time, the pressure was reduced to 230 mmHg over 1 hour and 30 minutes.
The temperature was raised from ℃ to 280℃. Polymerization was carried out for a further 3 hours at a polymerization temperature of 280°C under reduced pressure of 1 mmHg or less, for a total of 4 hours and 30 minutes, to obtain a polymer having an intrinsic viscosity of 0.602 and a softening point of 258°C. After the reaction was completed, the polymer was made into chips according to a conventional method. Using this polyester chip, chip drying, spinning, stretching, false twisting, weaving, presetting, alkali weight reduction treatment, dyeing, and reduction washing were carried out in the same manner as in the examples to obtain a black dyed cloth. The weight loss rate of this black cloth is 10%, the grittiness is 3, and the depth of color is
21.2, the friction discoloration resistance after 200 abrasions was grade 2-3. Example 2 760 mmHg in the polymer synthesis reaction of Example 1
Synthesis, yarn spinning, false twisting, additional twisting, weaving, presetting, alkaline reduction, dyeing, and washing were carried out in the same manner as in Example 1, except that the time required to reduce the pressure from 1 mmHg to 1 mmHg was shortened to 30 minutes. The results are shown in Table 2. Example 3 The same procedure as in Example 3 was conducted except that the time required to reduce the pressure from 760 mmHg to 1 mmHg in Example 2 was changed to 1 hour and 30 minutes, and the results are shown in Table 2. Comparative Examples 5 to 7 100 parts of dimethyl terephthalate, 60 parts of ethylene glycol, and 0.06 parts of calcium acetate monohydrate (0.066 mol% relative to dimethyl terephthalate) were charged into a transesterification tank, and 140 parts of dimethyl terephthalate was charged over 4 hours under a nitrogen gas atmosphere. A transesterification reaction was carried out while raising the temperature from ℃ to 230℃ and distilling the generated methanol out of the system. Subsequently, 1.5 parts of magnesium acetate tetrahydrate (based on dimethyl terephthalate) was added to the resulting reaction product.
1.38 mol%) and then after 5 minutes 1.06 parts of trimethyl phosphate (relative to dimethyl terephthalate) was added.
1.47 mol%) was added to the polymerization can. Then, increase the temperature from 760mmHg to 1mmHg over the time listed in Table 2.
At the same time, reduce the pressure to 230℃ over 1 hour and 30 minutes.
The temperature was raised to 285℃. The polymer was further heated at a polymerization temperature of 285° C. under reduced pressure of 1 mmHg or less for 3 hours, and after the reaction was completed, the polymer was made into chips according to a conventional method. Using this chip, yarn spinning, false twisting, additional twisting, weaving, presetting, alkaline reduction, dyeing, and washing were carried out in the same manner as in Example 1. As shown in Table 2, clear differences in glitter properties and depth of color were observed between Comparative Examples 5 to 7.

【table】

【table】

Claims (1)

[Claims] 1. In the reaction system for producing polyester, which is the base material of the fiber, the following general formula (In the formula, R ¹ and R ² are monovalent organic groups, X is a metal,
0.1% by weight or more of internally precipitated fine particles precipitated by reacting a phosphorus compound (n represents 1 or 0) with an alkaline earth metal compound.
1. A method for producing a non-gritter woven or knitted fabric, which comprises treating a woven or knitted fabric made of polyester false-twisted yarn uniformly dispersed in less than 3% by weight with an aqueous solution of an alkali compound to reduce the weight by at least 3% by weight. 2. The method for producing a non-gritter woven or knitted fabric according to claim 1, wherein the cross-sectional shape of the fibers constituting the processed yarn is multilobal.