JPS62250272A - Hot water weight reduction polyester cloth and its production - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention provides an NFT that is hygroscopic and opaque under high temperature and high humidity conditions.
This invention relates to polyester fabrics and their manufacturing methods.

(Prior art) Natural fibers, both cellulose-based and non-bacterial, contain water and other liquids from cell tissues, which are eliminated by leaving polymeric solid components, and the cell tissues are removed. It is thought that the microstructure possessed by the fibers gives it moisture absorption performance and the good glossy texture of natural fibers, as well as opacity without the plastic feel.

On the other hand, conventionally, polyester fibers are hydrophobic, so
The disadvantage is that the fiber itself is poor in water absorption and moisture absorption. 44-23134 is a technology for polyester fibers that contain polyalkylene glycol to improve water absorption.
, load 47-11280° load 47-43772. etc. have been proposed. However, with these techniques, the tearing strength of the resulting T-fabric is low, and the Mayu appearance and Motozawa appearance are glossy.
It has a unique plastic-like flat luster, and the light fastness of the dyed product is poor, making it unsatisfactory in terms of commercial value.

Synthetic fibers made of polyester and polyamide have a monotonous texture and luster compared to natural fibers such as silk, cotton, and hemp, and are plastic-like and have a low quality feel. In addition, recent trends in clothing needs include tennis wear used for leisure sports, etc.
Although there is an increasing demand for white coats and the like used in the medical field, they are insufficient to provide desirable opacity.

There is also a method of processing the fabric to make it opaque, but this has the problem of hardening the fabric due to the wind effect, and the additional disadvantage is that the opacity imparted by the process disappears when washed.

(Problems to be Solved by the Invention) The present invention is based on the realization that it is impossible to reduce the thickness of natural fibers to natural fibers, which are essentially formed from cell tissue, by using the above-mentioned small improvements. It is a challenge to change your way of thinking.

(Friendly means to solve the problem) In other words, the additive present in the fiber is made into a water column substance, this water-soluble substance is eluted with hot water, and a process similar to the dehydration of cells in natural fibers is carried out. It is applied to synthetic fibers, especially melt-spun fibers, in which a dispersion mixture of organic water-soluble polymers and inorganic water-soluble metal salts is added and dispersed as water-soluble substances into the fibers, and eluted with hot water to reduce hot water loss. This can only be achieved by doing so.

In the present invention, the polyester fabric reduced in hot water has a gloss and surface appearance similar to that of natural fibers, has a natural soft feel, and is hygroscopic under high temperature and high humidity conditions. However, in the present invention, it has been discovered that the opacity of the fiber is an important characteristic that allows the surface appearance to be said to be fabric-like and similar to natural fiber. It has been found that the opacity A expressed by the following general formula is effective as a measure for determining the appearance similar to fibers, especially natural fibers such as polyester fabrics. Particularly in uncolored white fabrics and light-colored fabrics, the appearance of natural fibers must be carefully judged.If the 0 opacity A, which can be effectively judged in Q7, is 80% or more, the appearance will be very close to that of natural fibers. I hope it's discovered. On the other hand, it has been found that if a cloth has appropriate hygroscopicity under high temperature and high humidity conditions, it will have a natural fiber-like appearance in terms of thermal properties. ,clr
It has been found that L can be achieved by using a polyester fabric having a moisture absorption fc of 196 or more, preferably 2% or more in an environment of relative humidity 90±54RH and temperature 30°C±3°C.

That is, in the non-invention, when the inorganic salt of the water-soluble substance and the water-bathable polymer substance are eluted from the polyester fiber by delicate interaction with each other due to hot water loss, extremely fine communicating pores and inorganic salt particles are formed. It can be seen that the independent pores of the polyester fabric are connected in a complicated manner, resulting in an opacity A of 80 degrees or more and a moisture absorption rate of 1% or more.

Such micropores cause a phenomenon of diffused reflection of light, and as a result, the natural fiber appearance and glossiness, which removes the plastic-like gloss characteristic of synthetic fibers and has a transparent appearance, exhibiting the opacity that is the aim of the present invention. It comes to have.

If the opacity A value of the fabric made of these fibers is less than 80%, when worn, especially if it is white or light-colored, the white coat, skin, and small body parts will be easily visible through the fabric, which is unsightly. However, when it exceeds 80 qb, it becomes less unsightly and looks like a natural fiber cloth.
When it is 2% or more, the opacity effect becomes even more remarkable, and the transparency prevention effect becomes sufficient.

Hereinafter, a method for manufacturing the fabric of the present invention as described above will be explained.

The polyester referred to in the present invention is mainly composed of polyethylene pre-7, tallate and/or polybutylene terephthalate, and if necessary, other components may be copolymerized in an amount of about 15 molar or less, such as t-polyester. Other components include copolymerized components such as diethylene glycol, neopentyl glycol, cyclohexane dimetatool, isophthalic acid, sulfoisophthalic acid, and polyalkylene glycol, as well as additives (e.g., pigments, carbon, silica, etc.), and flame retardants. Alternatively, it may contain a dyeability improving agent.

The next essential requirement for opacity A to exceed 80% gold and moisture absorption rate to be 1% or more is that at least 30% of the fibers must be eluted from the fibers in hot water of 90°C or higher, and less than 30%. Those that can only be eluted are less effective and are no different from conventional polyester fibers. If it is 30% or more, a good effect is shown, but preferably fibers that elute 60% or more are better.

In order to achieve this, the manufacturing process requires that the fibers contain at least 1% by weight of water-soluble polymer based on the polyester, and 0.5% by weight or more of the water-soluble inorganic salt based on the polyester. It is.

This more detailed flexibility is water-soluble and has a viscosity of 1 at room temperature.
5 poise or more, 1% by weight or more based on the polyalkylene glycol gold polyester in solution at room temperature, 4-fold i
%, and in addition, one or more water-soluble metal salts selected from compounds represented by the following general formulas [II] and [III] are added to the polyalkylene/glycol. 0.5 weight*% to polyester
] [A mixture dispersed so as to contain less than 100% of the polyester polymer was added to the polyester polymer molten fluid after the completion of polymerization of the polyester polymer and immediately before spinning, and then kneaded in layers using a static mixer with 15 or more elements. Using the leather fibers obtained by post-spinning and fiberizing, a fabric containing at least t-3c1 of the fibers is formed, and the fabric is heated with hot water of 90° C. or higher to remove 30- or more of the water-soluble substances contained therein. This is what allows it to elute.

The polyalkylene glycol contained in the polyester fiber constituting the fabric of the present invention means a polymer mainly containing alkylene needle units in the main chain, such as polyethylene oxide, polypropylene oxide, ethylene oxide and polypropylene. Refers to a copolymer of oxides.゛The polyalkylene glycol used in the present invention is water-soluble and has a viscosity of 1 at room temperature.
It needs to have a poise of 5 poise or more and be liquid at room temperature. Therefore, the number average molecular weight of the polyalkylene glycol is preferably in the range of 4,000 to 5,000.

When the viscosity is less than 15 poise, the polyalkylene glycol has poor high-temperature heat resistance during spinning, which induces a decrease in the viscosity of the polyester, resulting in poor mechanical properties during spinning, increased fuzz and yarn breakage, and poor yarn manufacturing process performance. It is unconventional in this respect.

The amount of polyalkylene glycol contained in the polyester is preferably 1% by weight or more and less than 4% by weight based on the polyester. If the content is less than 1% by weight, it will be impossible to satisfactorily and uniformly incorporate the metal salt compound of the general formula [■] [■] into the polyester polymer, and if the content exceeds 4% by weight or more, dyeing will occur. The light fastness of the fabric deteriorates, and the strength of the yarn is significantly reduced due to the alkali weight reduction treatment described below, which weakens the tear strength of the fabric, which is disadvantageous as it loses its value as a product.

The effects of the present invention can only be achieved by using the above-mentioned general formulas CU] and [II[] in combination with the polyalkylene glycol.
] Examples of compounds represented by Ka [Fe (C2
04)3], Kz(Fe(C204)2), K2(
Cu(CzO4)2), Kl(Zn(C204)2)
, Ka (AA(Cz04)3) and other oxalate complexes. Examples of the compound represented by the Mayu general formula (1113) include Naα, Ka, etc.

The content of these compounds is 0.0% relative to polyester.
A range of 5% to 3% by weight is preferred. The inorganic salt is 0.
If it is less than 5 Ik%, the number of pores after elution will be small, resulting in insufficient improvement in hygroscopicity and opacity. If the content exceeds 3% by weight, the compound will aggregate in the polyester fibers, causing fluff and yarn breakage during the drawing process, which is not preferable.

Next, a method for kneading such a compound into a polyester polymer will be described. That is, the characteristic of the kneading method of the present invention is that the compound (general formula [■] or general formula (in)) is added after completion of polymerization of the t-polyester polymer and immediately before spinning, and then kneaded.

According to the conventional kneading method, the compound t is
ll&add. However, the disadvantage of this technique is that it often inhibits the polymerization of the polyester, and it is impossible to uniformly disperse the compound into the polymer, resulting in yarn breakage during spinning, When the yarn is further drawn, fuzz occurs frequently, making operability difficult.

To explain in more detail the addition method of the present invention which avoids these disadvantages and has good operability, it is a continuous method in which the molten polymer is continuously fed into a spinning nozzle and discharged without going through the step of pelletizing after the completion of polyester polymerization. The process is convenient. That is, it is preferable to feed the compound in a fixed amount into the molten polyester polymer stream immediately before spinning, and then knead it with a static mixer and discharge it from a constant diameter spinning nozzle hole. When spinning polyester polymer pellets using an extruder, a predetermined amount of the compound used in the present invention is melt-extruded and then fed into a polyester polymer melting line, then kneaded with a static mixer and then discharged from a spinning nozzle. It's good to let them do it.

What is important when kneading using a static mixer is that it is necessary to knead using a static mixer with a certain number of elements or more. There are several types of static mixers currently in use, such as the Kenics 1800, which has 2n elements with twisted blades shifted 90 degrees to the left and right.
When using a static mixer that divides into layers, it is necessary to use one with at least 15 elements. In this case, if the number of elements is less than 15, yarn breakage will occur during spinning and the spinning process will be poor.
Undesirable. Therefore, it is preferable to carry out division into 215 layers or more. It goes without saying that even when using a static mixer made by a company other than Konituta, it is necessary to set the number of elements to correspond to 215 layer divisions or more and use a secondary mixer. Toshisha's Hi-Mixer and Charles & Ros
For the AIS G mixer made by S), the number of layer divisions when passing through n elements is 4n layers, so the number of elements must be 8 or more, more preferably 11 or more. It is.

The spinning method used in the present invention can be conventional spinning or so-called high-speed spinning. Yarn processing such as false twisting and crimping may be used as appropriate.

The fabric referred to in the present invention is a fiber in which the hot water reduced microporous fiber is used for either the weft or the warp, or it is used in the warp and weft, or it is also a fiber that is subjected to hot water loss. This refers to woven fabrics, knitted fabrics, non-woven fabrics, etc. using blended yarns, blended cotton yarns, etc. From the viewpoint of effectiveness, hot water reduction of fabrics must be carried out at a temperature of 90° C. or higher. This hot water weight loss treatment may be carried out in the ninth treatment step of Thermal Theory, but if, for example, the greige scouring and desizing steps are carried out at 90° C. or higher, this step can be used instead. Further, this hot water weight loss can be carried out in two stages: a weight loss process using hot water at 90° C. or higher before boiling, and a boiling hot water weight loss process in boiling water. In this case, the temperature of the boiling hot water treatment is preferably 110'C or higher and lower than 140C.

This hot water treatment creates fine pores in the polyester fibers that make up the fabric, where the inorganic salts and water-soluble polymer substances subtly interact with each other. It can be expanded by reducing the amount with an aqueous solution. This treatment needs to achieve a weight loss rate of 5% or more in order to achieve its purpose. However, since this treatment reduces the strength of the fiber, it is necessary to limit the alkali weight loss rate depending on the application. In other words, when the weight loss rate exceeds 40%, the strength of the yarn decreases significantly, and the tear strength of the fabric becomes weaker, so the alkali loss is reduced.
It is necessary to keep the fk rate below seven times.

The fine pores can be enlarged by this weight loss treatment with a hot alkaline aqueous solution, but when the pores have a width t[L of 0.1 to 1μ when viewed from the side, the opacity Ai increases and the heat A=82% or more. Then, the appearance effect of the fabric becomes significantly better.

The present invention will be described in detail below, and the present invention will be explained more specifically. However, the present invention is not limited to the scope of the following examples. Note that dr/f in the examples represents the number of Denny) L//filaments. The intrinsic viscosity [η] is 1. Phenol, tetrachloroethane f, 50:500
The t value is measured at 30° C. in a solvent with a weight ratio.

Examples 1 to 4 and Comparative Examples 1 to 6 The following additive A (water-soluble polymer) was added to a molten polymer stream of [77) 0.65 polyethylene terephthalate (hereinafter abbreviated as PET) containing 0.4% TiO2f. A mixture of
The fibers are spun using a 6H (hole) spinning nozzle at a spinning speed of 1100 m15+. Next, these undrawn tips were brought into contact with a heated roller at 75°C and a heated plate at 120°C and stretched to 102dr/36f (each of the multifilaments in D) was drawn. Its [η] was 0.62. As Comparative Example 5, the same PET used in Example 1 was spun under the same spinning conditions as Example 1 without a scavenger, and stretched to obtain a multifilament of 103 dr/36 f.
These multifilaments were used as T-warp and weft yarns and woven into tucks. Their raw material density is 82 warps/
These greige taffetas with 95 wefts/inch were treated with a 1 t/l aqueous solution at 80°C for 20 minutes or boiling for 20 minutes to reduce hot water weight. I'm thinking of going. Also, use this as a pin tenter ゛C180℃C1
Additional hot water loss was carried out by heating at 80°C at 130°C for 30 minutes. In addition, one part was subjected to alkali weight loss, and each taffeta was evaluated for opacity, hygroscopicity, water absorption, tear strength, and light fastness of the dyed product.

Measurement of LB and LW values Measured using a self-recording spectrophotometer manufactured by Hitachi. Light fastness evaluation of light fastness of dyed products using the same drop method.The taffeta after the intermediate cera 1f was dyed and reduced washed under the dyeing conditions indicated by the arrow, and the dyed products were tested according to JIS standards.
-L-0841 was used to evaluate light fastness and waxiness.

Staining conditions> Staining Dianix Blue BG-FS 3% o
wf Nikka Sunsalt Φ7000 0.5f/ ammonium sulfate 1 f/ vinegar CKit (48
%) 1 cc/reductive cleaning.

Hydrosulfide 1 t/l Sodium hydroxide 1 t/l Amyradin
11/l As shown in Example 1 and Comparative Example 3, in Comparative Example 3 in which Additive B was not used, good weight loss did not occur and the opacity did not reach 80. deer? As shown in Example 3, when Additive B is used in combination with Example 1, the opacity improves to 80 or more, the moisture absorption and water absorption are good, and the fabric has excellent tear strength that does not decrease even when the weight is reduced by alkali. This is the result.

Comparative Example 1 is a case in which the amount of Additive A exceeds the specified amount in the present invention, and although opacity is achieved by reducing the amount in hot water, the tear strength is reduced and there is no commercial value.Comparative Example 2 is an additive. This is an example where A does not reach the specified amount in the present invention, in which case the spinnability is poor and it is difficult to manufacture the fiber. Comparative Example 4 is a case in which the amount of additive B exceeds the specified amount, and in this case too, the spinnability is poor and fiber production becomes difficult.

In Example 4 and Comparative Example 6, additives A and B satisfy the specified amounts, but if the weight loss rate in alkaline hot water weight loss is high, the tear strength will decrease significantly and the commercial value will be lost. It shows. Comparative Example 5 shows the standard when neither additive A%Bl is used.

As shown in Table 1, polyalkylene glycol and the compound represented by the general formula (it) can be obtained by using the compound defined in the present invention within a predetermined content range, and the polyester fiber fabric can be heated to a predetermined hot water weight loss. If the weight loss of the applied or additional alkaline hot water is within the specified range, there will be no problems with spinnability, light fastness, tear strength, etc., and the moisture absorption rate may be 1.
Appearance of natural fibers with an opacity of 80ts or more,
A product with gloss and texture can be obtained.

Examples 5-6 and Comparative Example 7 Compound t-1A of the same additives A and B as in Example 1 was added to the same PET molten polymer stream as in Example 1.
9% by weight and 2.8% by weight of B (relative to PET), and kneaded with a static mixer while varying the number of elements as shown in Table 2.
110 from a spinning nozzle of 20mmφx36H (hole)
The yarn was spun at a spinning speed of 0 m/min, and the spinning process performance (degree of yarn breakage) was examined.

Table 2 As shown in Table 2, when the number of elements is as small as 13, yarn breakage occurs frequently and the spinning process becomes poor.

Examples 7 to 8 and Comparative Example 8 Ks (A4 (Cz04)a
) 2.5% by weight (based on PET) and a copolymer of pyrene oxide (PO) and polyethylene oxide (EO) (copolymerization ratio 25 /75) and 3.5% by weight (PET
), kneaded with a static mixer with 42 elements, and spun at a spinning speed of 1100 m15) from a spinning nozzle with a diameter of 0.20 mm x 36 H (hole). Compare process efficiency.

As shown in Table 3 (Table 3), when the solution viscosity of the PO-EO copolymer is low, the spinning processability is poor, but when the solution viscosity is 16 poise, the spinning processability is good.

Examples 9-10 and Comparative Examples 9-10 Naα to the same PET molten polymer stream used in Example 1
Then, the same PO-EO copolymer used in Example 1 was supplied in a predetermined amount (Table 4) and kneaded in a risk mixer with 42 elements, and then spun at 1100 fn/min from a spinning nozzle with a diameter of 0.20 mm and a diameter of 36 H (hole). Spin at spinning speed. Next, these undrawn yarns were drawn under the same conditions as in Example 1 to obtain each multifilament of 1 O2 dr/36f. did. Their gray density was 82 warps/inch and 95 wefts/inch. After scouring and desizing these gray tacks in hot water at 95°C,
Intermediate ceratra was carried out at 0°C. Next, we will evaluate the opacity, moisture absorption, etc. of these taffetas.

Table 4 As shown in Table 4, a fabric made of polyester fiber obtained from the compound defined by the present invention and represented by the general formula [nl] within the specified content range was subjected to the total hot water loss specified by the present invention. It can be seen that when carried out, a polyester fabric having a moisture absorption rate of 1% or more and an opacity of SOS or more can be obtained.

Example 11 and Comparative Examples 11-12 The same taffeta gray fabric used in Example 1 and Comparative Example 3
The same taffeta greige used in the above case was subjected to hot water treatment for 90 minutes at the hot water temperature shown in Table 5. These tacks were evaluated for tear strength and opacity.

Table 5 As shown in Table 5, in the case of gray fabric that is not used in combination with the compounds specified in the present invention, opacity does not appear even after hot water reduction at 135°C; However, even in the case of Hygiene, the opacity is also unsatisfactory when the hot water treatment temperature is low, indicating that it is necessary that the combination of the compounds specified in the present invention and the hot water treatment temperature are mutually satisfactory. It will be done.

Example 12 and Comparative Example 13 For the same tack gray fabric used in Example 7, the sixth
The tear strength, opacity, etc. of the taffeta of Toson et al., which was subjected to hot water treatment for 90 minutes at the hot water temperature shown in the table, were evaluated.

Table 6 As shown in Table 6, when a fabric made of polyester fiber containing a compound defined by the present invention and represented by the general formula [m] is subjected to the high-temperature hot water treatment defined by the present invention, sufficient tearing is achieved. It can be seen that a fabric with satisfactory strength and opacity of 80% or more can be obtained, and it can also be seen that even if the same gray fabric is used, a high opacity cannot be obtained if the hot water treatment temperature is low.

Comparative Example 14 Same PO-EO copolymer and fc used in Example 1
92.5 parts and 70 parts of a[Aj(C204)a], respectively
1 part, 2,500 parts of dimethyl terephthalate, 2,400 parts of ethylene glycol, and 0.5 part of zinc acetate were placed in a reaction vessel, heated to 180°C, stirred, and transesterified for 2 hours while removing by-produced methanol. Add 0.6 part of ate and 1 part of antiseptane oxide, and gradually raise the temperature and reduce the pressure to 280℃0.2-0.5mHg.
Let it react for 2 hours. The obtained polymer was passed through a spinning nozzle of 0.20 wmφ x 36H installed at the bottom of the reactor.
The spun yarn was wound at a spinning speed of 0 m/min. [η] of the obtained friend polymer was 0.48. Many aggregates of Ks (At(C204)3) were observed under an optical microscope in the resulting fibers, indicating that Ka (At(C20a)3)
The holes are uniformly distributed throughout the fiber. Next, this undrawn yarn was brought into contact with a heated roller at 75°C and a heated plate at 120°C to perform drawing. Yarn breakage and fuzz occurred frequently, and the drawing process was extremely poor. Thus, it can be seen that kneading methods other than those specified in the present invention are not preferable.

Claims (1)

[Scope of Claims] 1) Contains at least 30% of polyester fibers, which are premixed with additives of 3% by weight or more but less than 20% by weight, of which 30% or more is eluted from the fibers in hot water of 90°C or higher. A fabric whose moisture absorption rate is 1% or more in an environment of relative humidity 90% ± 5% and temperature 30°C ± 3°C, and the opacity A of the fabric is as follows: General formula [
A hot water-reduced polyester fabric characterized by having an opacity of 80% or more as measured by the numerical value I]. A=(L^*_B)/(L^*_W)×100 [I
] L^*_B: L^* value L^ when fabric is layered on black base
*_W: L^* value when fabric is layered on white base Black base: Black plastic board L^* Value: 12 White base: Standard white board
L^* value: 100 2) The elution micropores of the fabric reduced in hot water are enlarged with a hot alkaline aqueous solution, and the pores become 0.1 to 1 when viewed from the side.
The hot water-reduced polyester fabric according to claim 1, which has a width of μ and an opacity A of 82% or more. 3) Add the following general formula [II] to a liquid polyalkylene glycol that is water-soluble and has a viscosity of 15 poise or more at room temperature.
A mixture in which one or more water-soluble metal salts selected from the compounds represented by [III] are dispersed,
After completing the polymerization of the polyester polymer and immediately before spinning,
Adding the polyalkylene glycol to the polyester polymer melt fluid in an amount of 1 to 4% by weight based on the polyester, and adding the water-soluble metal salt in an amount of 0.5 to 3% by weight based on the polyester. Then, after layer-divided kneading with a static mixer having 15 or more elements, the yarn and/or fibers obtained by spinning and fiberization are used to form a fabric containing at least 30% of the fibers, A method for producing a hot water-reduced polyester fabric, which comprises eluting 30% or more of the water-soluble substances contained in the fabric with hot water at 90° C. or higher. [Mtn[D(C_2O_4)_m] [II] ACl
[III] Mt in formula [II]: Group I alkaline earth metal such as Na, K, etc. D in formula [II]: At least one of Fe, Zn, Ni, Cu,
Complex-forming atomic formula from Al, Ti, etc. n = 1 to 4, m = 2 to 4 A in formula [III]: Group I alkaline earth metal such as Na, K, etc.] 4) Reduced by hot water A method for producing a hot water-reduced polyester fabric according to claim 3, wherein the polyester fabric is additionally reduced in weight with hot water at a temperature of 110°C or higher and lower than 140°C, and the hot water weight loss is carried out in two steps. . 5) Production of the hot water reduced polyester fabric according to claim 3, wherein the polyester fabric that has been reduced in hot water is subjected to additional weight loss with a hot alkaline aqueous solution to achieve an alkali weight loss rate of 5% or more. Law.