JP2003129368A - Method for dyeing flame-retardant polyester fabric having rich design property - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a flame-retardant polyester fabric which has a chinchilla- like appearance quality, a soft touch and a rich design property and can not be realized by conventional flame-retardant polyesters. SOLUTION: This method for dyeing the flame-retardant polyester fabric having a rich design property and at least partially containing polyester multifilament yarns prepared by melt-spinning a copolyester containing a phosphorus compound represented by the general formula [R is a monovalent ester- forming functional group; R2 and R3 are each identically or differently a halogen, a 1 to 10C hydrocarbon or R1 ; A is a divalent or trivalent organic residue; (n1 ) is 1 or 2; (n2 ) and (n3 ) are each an integer of 0 to 4] and having a phosphorus atom content of 500 to 50,000 ppm, is characterized by subjecting the polyester fabric to a wet heat relaxing treatment comprising quickly heating from a lower temperature by 20 deg.C than a fiber shrinkage-starting temperature obtained from the heat shrinkage stress curve of the multifilament yarns to a higher temperature by 30 deg.C than the fiber shrinkage-starting temperature at a rate of +5 to +10 deg.C/min.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for dyeing and processing a flame-retardant fabric using a phosphorus atom-containing polyester, and more particularly, to the flame-retardant fabric having a soft touch, a swelling feeling and a chinchilla effect. The present invention relates to a method for dyeing and processing a flame-retardant polyester cloth suitable for daily use such as curtains, table cloths, etc., for the purpose of giving a certain textured cloth surface feeling.

[0002]

2. Description of the Related Art Conventionally, curtains, chair upholstery, bed covers, and other interior applications have been required to have flame retardancy, and in particular, many flame retardant products have been put on the market and deployed for use as equipment for public facilities. Most of these are by exhaustion method and padding method by post-processing, and include, for example, tris (1-aziridinyl) phosphine oxide, tris (2,3-dibromopropyl) phosphate, bis (2,3-diamine). A typical example thereof is a bromopropyl) phosphate compound.

These are substances which are being regulated as highly toxic and harmful substances, and particularly halides such as Cl and Br are very likely to be prohibited from being used in the future, and new flame-retardant substances with high safety should be selected immediately. I have a problem of having to do it. Further, although the flame-retardant treatment by the post-processing method is relatively inexpensive, it is not excellent in durability and has a problem that the flame-retardant performance is extremely deteriorated by repeated washing and the like. Further, there is a very high possibility that a highly toxic harmful substance may be mixed and leaked into the waste liquid during the processing step, and the possibility of developing an environmental problem cannot be denied.

[0004]

DISCLOSURE OF THE INVENTION The present invention improves the above-mentioned conventional method, and improves the flame-retardant durability by forming a yarn made of a polymer in which a flame-retardant substance is copolymerized with a raw material polyester into a fabric. It is an object to realize a chinchilla-like appearance quality and soft feeling which could not be realized by the conventional flame-retardant polyester, while improving the flame-retardant performance as compared with post-processing.

[0005]

The present invention has the following constitution. A fabric structure containing at least a part of a polyester multifilament yarn containing 500 to 50,000 ppm of phosphorus atom and melt-spun of a copolyester obtained by adding the phosphorus compound shown below. In the dyeing process, a wet heat relaxation treatment is performed from a temperature 20 ° C lower than the yarn shrinkage start temperature obtained from the heat shrinkage stress curve of the multifilament yarn to a temperature 30 ° C higher than the yarn shrinkage start temperature + 5 ° C / min or more +10. A method for dyeing and processing a flame-retardant polyester cloth having a high design property, which is characterized in that the temperature is rapidly raised at a rate of not more than ° C / min for processing.

[0006]

[Chemical 2] (In the formula, R 1 is a monovalent ester-forming functional group,
2, R3 are the same or different groups, each selected from a halogen atom, a hydrocarbon group having 1 to 10 carbon atoms, and R1, and A represents a divalent or trivalent organic residue. Further, n1 is 1 or 2, and n2 and n3 each represent an integer of 0-4. )

Further, the ratio of the woven width to the finished width and / or the ratio of the woven length to the finished length is from 1.00: 1.20.
The method for dyeing and processing a flame-retardant polyester fabric, which is characterized in that the treatment is carried out under a condition satisfying 1.00: 1.45.

A method for dyeing and processing a flame-retardant polyester cloth, which is characterized in that a wet heat relaxation treatment is carried out in an aqueous solution containing a nonionic surfactant having an HLB value of 8 to 15.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION The polyester flame-retardant polyester cloth of the present invention is a cloth using at least a part of a copolymerized polyester multifilament obtained by adding a phosphorus compound containing 500 to 50,000 ppm of phosphorus atoms. It is necessary to impart flame retardancy.
When the phosphorus atom content is less than 500 ppm, not only the flame retardancy is inferior, but also the molecular chain is easily oriented during melt spinning and drawing, so that the elastic modulus of the fiber is improved and it is difficult to obtain a soft feeling of the fabric structure. It is not preferable. Further, if the phosphorus atom content exceeds the range of 50,000 ppm, it is necessary to increase the copolymerization amount of the phosphorus compound containing the phosphorus atom, and the melting point of the obtained polymer is extremely lowered, resulting in poor spinnability. Not only that, the strength of the fiber is also reduced, and it cannot be put to practical use. The phosphorus atom content is preferably 1500 to 30000 ppm, more preferably 3000 to 10000 ppm.

The polyester in the present invention contains terephthalic acid or naphthalenedicarboxylic acid as a main acid component and at least one glycol, preferably at least one alkylene glycol selected from ethylene glycol, trimethylene glycol and tetramethylene glycol. This refers to polyester as a component, and is obtained by copolymerizing a phosphorus compound in order to impart flame retardancy.

The phosphorus compound used in the flame-retardant polyester cloth of the present invention is required to be a compound capable of reacting with the dicarboxylic acid or diol which is a constituent component of the polyester and copolymerizing with the polyester. In particular, a compound capable of introducing a phosphorus atom into a side chain and / or a terminal of polyester is desirable, and not only a single compound but also plural kinds of compounds may be used at the same time. However, in order to obtain a soft texture, it is preferable to suppress the orientation of the molecular chains to some extent and to slightly reduce the elastic modulus of the fiber, and therefore it is preferable to use a phosphorus compound having a phosphorus atom introduced into the side chain. In addition, if necessary, antioxidants, antistatic agents, pigments, matting agents,
If necessary, additives such as dyeability improving agent may be contained. Further, physical and / or chemical treatment may be carried out in the post-processing step, particularly in the dyeing processing step, to impart functions such as deodorant, antibacterial, moisture absorption, fragrance, antistatic and adsorption.
Needless to say, post-processing flame retardant treatment such as padding method, exhaust method, thermosol method and the like can be carried out as required, but special attention is required for processing waste liquid treatment in order to prevent environmental pollution.

The phosphorus compound used in the present invention is a compound represented by the following [Chemical Formula 3], and the phosphorus compound itself being a part of the copolyester, the consumption durability and the It is preferable from the viewpoint of preventing environmental pollution.

[0013]

[Chemical 3] (In the formula, R 1 is a monovalent ester-forming functional group,
2, R3 are the same or different groups, each selected from a halogen atom, a hydrocarbon group having 1 to 10 carbon atoms, and R1, and A represents a divalent or trivalent organic residue. Further, n1 is 1 or 2, and n2 and n3 each represent an integer of 0-4. )

The following can be mentioned as specific examples of [Chemical Formula 3]. Of course, it is not limited to the following,
All compounds satisfying the general formula [Chemical Formula 3] are included.

[0015]

[Chemical 4]

[0016]

[Chemical 5]

[0017]

[Chemical 6]

[0018]

[Chemical 7]

[0019]

[Chemical 8]

The copolyester obtained is Japanese Patent Publication Sho 55
It is possible to polymerize by a known method described in JP-A-41610, etc., and the copolyester can be formed into a yarn by a conventional melt spinning method. Although not particularly limited, the spinning take-up speed is 1500 to 400
After being wound as undrawn yarn in the range of 0 m / min, or continuously drawn without being wound, the high shrinkage yarn and the low shrinkage yarn can be made from the same polymer by variously changing the stretching conditions and heat treatment conditions. To get When a yarn obtained by mixing these during spinning or drawing is used as part of the warp and / or weft of the fabric, it gives the fabric an appropriate swelling feeling and can impart an appropriate chinchilla effect. Therefore, it is preferable to use. Further, the cross-sectional shape of the single yarn is not limited, and may be a solid cross section or a hollow cross section.
An irregular cross section such as a flat cross section can be appropriately adopted according to the purpose and application.

In order to obtain a different shrinkage mixed filament yarn, it is preferable to change the stretching condition and the heat treatment condition as described above to give a difference in shrinkage ratio. The heat treatment is performed by a plate heater, a hot roller or the like. Either contact heating or non-contact heating such as a tube heater may be used. Further, either a dry method or a wet method may be used. Productivity, although not particularly limited
From the viewpoint of quality, contact roller heating is preferably used.

The loom used for obtaining the fabric structure is not particularly limited, and any of an air jet loom, a rapier room, a projectile room and a water jet loom can be used. Especially, in order to impart a chinchilla feeling, it is necessary to avoid heat application before the dyeing process as much as possible. In the case of using a water jet room, it is preferable to perform the drying at a greige drying temperature of less than 55 ° C.

The structure of the fabric structure is not particularly limited, but a twill weave, plain double weave, double satin weave, satin weave, irregular twill weave, especially for the purpose of improving the chinchilla effect and the swelling feeling of the fabric. Woven designs such as irregular satin weave and jacquard weave that increase the floating number of warp and / or weft are preferably applied, but if the floating number of weft is increased more than necessary, pilling resistance and snag resistance deteriorate. Therefore, it can be said that it is preferable to keep the weft floating number at 6 or less. A more preferable weave design is a satin weave-based design, which is a double satin weave based on 5 warp satin, a 7 warp satin weave,
Various jacquard weaves are exemplified. 1 to 10 show specific examples of one perfect weave design, but of course, the present invention is not limited to this.

When obtaining the flame-retardant polyester cloth of the present invention, an oligomer component, a spinning oil agent component, a sizing agent, etc. attached to the yarns constituting the cloth in order to maintain a high degree of flame retardancy.
It is necessary to remove impurities such as wax components. The wet heat relaxing treatment in the dyeing processing method of the present invention is a step which also serves as a scouring treatment, and the wet heat relaxing treatment comprises a surfactant, a hydroxide of an alkali metal or an alkaline earth metal,
The treatment is carried out in an aqueous solution containing a scouring aid, various chelating agents, a bath softener and the like. Examples of hydroxides of alkali metals or alkaline earth metals include sodium hydroxide, potassium hydroxide, calcium hydroxide, and the like, and as scouring aids, sodium carbonate (soda ash), sodium sulfate (mirabilite), silicic acid as builders. Examples thereof include sodium and sodium aluminosilicate. The chelating agent is used for softening water, and sodium tripolyphosphate, sodium hexametaphosphate, and ethylenediaminetetraacetic acid sodium salt (EDTA) are preferably used. These are appropriately selected and selected according to the type and amount of impurities adhering to the yarn.
It can be used in combination.

It is desirable to use a nonionic surfactant which does not show ionicity, and has characteristics such as detergency, hard water resistance, biodegradability, emulsion dispersibility, and low foaming property during scouring. Have. Anionic, cationic, and zwitterionic surfactants all have a crafting point and do not exhibit surface activity until the temperature is raised above that temperature. It is not preferable because it causes problems such as redeposition of impurities.
As the nonionic surfactant, polyoxyethylene alkyl ether and polyoxyethylene alkylphenol ether are preferably used. It is desirable to use one having an HLB value of 8 to 15 as the nonionic surfactant.

Here, the HLB value (Hydrophile-Lipophile
Barance) is an American Atlas Powder Co. It was first derived by the company, and in the present invention,
Calculated based on 1]. [Formula 1] HLB = 7 + 11.7 log (Mw / Mo) (where Mw and Mo are the molecular weights of the hydrophilic part and lipophilic part in the activator) When using a plurality of nonionic surfactants Is the first one because HLB is additive.
[Formula 2] is established when HLB of the activator of (1) is HA and HLB of the second activator is HB, and a weight and a weight of each are mixed. [Formula 2] HLB = (a × HA + b × HB) / (a + b) The present invention naturally includes not only a single type of the above surfactants but also a combination of a plurality of nonionic surfactants.

The HLB value of the nonionic surfactant used in the present invention is in the range of 8 to 15, preferably 10 to 15, and more preferably 13 to 15. If the HLB value is less than 8, it will be difficult to remove the spinning oil, polyester oligomer and other impurities. Further, when the HLB value is in the range of more than 15, the molecular weight of the lipophilic part becomes extremely low, and as a result, the ability to trap spinning oil agents and other lipophilic impurities decreases, resulting in poor efficacy as a surfactant. It becomes a thing. The flame-retardant polyester cloth of the present invention has the HLB = HLB =
It is desirable to use 8-15 nonionic surfactants to completely remove them from the fabric.

A raw fabric is obtained using the polyester multifilament yarn, and after scouring and relaxing in the dyeing process, dyeing and finishing set are applied to obtain a cloth. Depending on the texture, it is possible to carry out alkali weight reduction processing in the process before dyeing, but in this case, after scouring / relaxing, use a heat setter, straighten the texture with the intermediate set, adjust the fabric width, and then It is preferable to carry out batch type reduction such as flow reduction or continuous reduction such as pad steam method.In the above refining / relaxation treatment, various oil agents such as spinning oil agent, sizing agent, false twist oil agent, etc. can be completely removed. It is desirable to maintain the flame retardant performance, so refrain from using antifoaming agents such as silicone, and wash thoroughly with hot water after the waste liquid so that it does not remain.

Also in the dyeing process, it is preferable to remove excess dyeing aids such as dispersants in the reduction washing process and the soaping process, and then dry and finish the set. It is possible to apply a flame-processing agent or the like by an exhaust method, a thermosol method, a padding method or the like. For finishing resins, it is not preferable to use chemicals such as melamine / formaldehyde finishing agents that reduce the flame retardant performance of the product, but softeners such as polyester, hard finishing agents, antifouling agents, etc. to the extent that flame retardant performance is not impaired. Can be used together depending on the application.

In order to obtain an appropriate chinchilla effect, the bath temperature is slightly suppressed from the thermal contraction start temperature of the above-mentioned yarn from -20 ° C to the same contraction start temperature +30 while slightly suppressing wrinkle movement in the scouring / relaxing process as compared with the conventional condition. It is effective to raise the temperature to + 5 ° C./min under the temperature rising condition of +5 to + 10 ° C./min in order to impart a chinchilla feeling. If the rate of temperature rise is less than + 5 ° C / minute, it is possible to prevent the fabric from being pushed in when wrinkled by heat and moisture, but the appearance becomes plain. If the condition exceeds + 10 ° C / min, indentation creases in the weft direction of the woven fabric and rope creases in the warp direction remain strong, impairing the appearance quality, and a large number of weft protrusion defects occur. , Not a preferable condition.

When the wet heat relaxation is carried out by liquid flow treatment, the bath ratio, nozzle pressure, impact plate shape, impact plate installation angle,
It is important to adjust the nozzle type and other factors. Regarding the nozzle shape, it is preferable to use a filament nozzle having a smaller Venturi angle than a span nozzle having a large Venturi angle used in ordinary liquid flow refining. Rope wrinkles tend to occur when the filament nozzle is used,
Although the material has a Yangyanagi-like finish, the rubbing effect increases, so it is effective in imparting appearance quality and bulging.

As a model used for moist heat relaxation, in addition to the above liquid flow relaxer, a high pressure rotary washer, etc.
It can be implemented using a known model. If necessary, various wet heat pretreatments and dry heat pretreatments may be used in combination. In the case of using a high-pressure rotary washer, a crushed wrinkle process in which a textile machine is finely pressed into a cylindrical cotton bag and subjected to scouring / relaxation to make wrinkles is effective for improving the chinchilla feeling and the appearance design. When the crushed wrinkle processing is performed, after completion of the above washer relaxation, dehydration treatment is performed, and the raw fabric is taken out from the cylindrical cotton bag and expanded, and then soaping with an open soaper or liquid scouring is performed again, and the spinning oil agent that cannot be completely removed It is desirable to completely remove impurities such as a sizing agent and an oligomer component.

It is desirable that the temperature rising temperature range in the wet heat relaxation is from the thermal contraction start temperature of the yarn of −20 ° C. to the thermal contraction start temperature of + 30 ° C. Although the high temperature range after the same heat shrinkage start temperature + 30 ° C is not specified, it is necessary to raise the temperature in stages while decreasing the temperature raising rate to give a rubbing effect of about 30 to 60 minutes at the maximum reached temperature. It is effective for making texture. The temperature near the thermal contraction start temperature of the yarn is a temperature region that occupies an important position particularly from the viewpoint of the appearance quality and texture of the fabric, and by controlling the heating rate in the above temperature region, a suitable appearance can be obtained. It is possible to obtain a feeling of quality and swelling.

The ratio of the woven width to the finished width of the cloth and / or the ratio of the woven length to the finished length of the cloth is 1.00: 1.20 to 1.00: 1 as a finish: woven ratio. 45 range,
Particularly preferably, it is in the range of 1.00: 1.30 to 1.00: 1.40. The weaving width and the weaving length referred to here are not the properties on the loom, but the properties in which the raw loom is taken out from the loom and put in a free state. Further, the finishing width and the finishing length are not the physical properties on the heat setter in the final finishing setting step, but the physical properties when the post-setting raw machine is in a free state.

If the finishing: weaving ratio is less than 1.00: 1.20, the swelling feeling of the cloth, the chinchilla effect of the appearance and the like are very poor, and various problems such as misalignment and slippage occur. Is unfavorable because of concern. Further, in the area where the finish: weave ratio exceeds 1.00: 1.45, the fabric feels fluffy, and the surface feel is also disturbed, resulting in a chinchilla feel, and warp and / or weft This is not preferable because it induces pilling and snag due to jumping out.

When the flame-retardant polyester cloth of the present invention is dyed, it is dyed with a disperse dye. However, in addition to dip dyeing with a jet dyeing machine, printing with a rotary screen, a flat screen, an ink jet or the like may be used. In the case of dip dyeing, a bath temperature of 120 to 130 ° C is preferable from the viewpoint of dyeing fastness, and in the case of printing, the cloth after wet heat relaxation treatment is subjected to straightening and width adjustment using a heat setter before dispersion for printing. A printing paste containing a dye, paste, etc., is applied to the surface of the cloth to give a surface temperature of 10
After preliminarily drying through a cylinder roll of 0 to 120 ° C, after removing unnecessary glue and dye by soaping through a coloring step of exhausting and fixing the dye at an ambient temperature of about 160 to 180 ° C with a color developing machine. Finish by performing a finishing set with a heat setter.

In any of the dyeing formulations, it is desirable to remove excess dyes, dispersion aids, etc. from the fabric in order to improve the flame retardancy, and especially in the case of a dark color, reduction washing is sufficiently carried out. Is desirable. If necessary, the fibers may be exhausted with the ultraviolet absorber by the same dyeing bath treatment.
Further, the dyed fabric may be treated with a nonionic polyester antistatic agent or a softening agent by a pad method or the like within a range that does not impair flame retardancy.

The flame-retardant polyester cloth obtained in the present invention is cut and sewn according to the use and used as a curtain, a upholstery material, a bedclothing bedding side material, a wallpaper material, and a table cloth. In order to maintain the flame-retardant performance of the product itself, it is preferable to use a sewing member such as sewing thread, zipper, button, seam tape, etc., which also has flame-retardant performance.

[Examples] The present invention will be described in more detail with reference to the following examples. The characteristic values described in the text and examples are based on the following methods. Further, the present invention is not limited to the following examples.

[Boiling water shrinkage rate (SHW)] A sample (thread) was used with a measuring machine having a frame circumference of 1.125 m and an initial load of 0.09 g /
Rewind at a speed of 120 times / min by applying dtex, and the number of windings is 2
Create a small skein 0 times, apply a load 40 times the initial load, and measure the skein length L0 (mm). Then, the load is removed, and the sample is immersed in boiling water at 98 ° C. ± 2 ° C. for 30 minutes under conditions where shrinkage is not hindered, and then kept horizontal and air dried. After air-drying, a load of 0.09 g / dtex is applied again to measure the length L1 (mm), and the boiling water shrinkage SHW is calculated based on the following formula. The average value of 5 times of experiments is taken as the measured value. [Equation 3] SHW (%) = (L0-L1) / L0 × 100 The boiling water shrinkage difference ΔSHW was measured and evaluated by the above method independently for the low shrinkage yarn and the high shrinkage yarn before mixing, and both The difference in shrinkage (%) is expressed.

[Dimensional change rate at a dry heat of 160 ° C.] 20 cm × 20 cm so that the cloth is along the grain without tension.
Mark the four corners of the square with oil-based ink, and in an oven adjusted to a dry heat of 160 ° C under conditions where shrinkage is not hindered.
After the treatment for a minute, the sample (dough) is taken out and air-cooled in a horizontal state until it reaches room temperature. The distance (L2 cm) marked with the oil-based ink is measured, and the dimensional change rate at the dry heat of 160 ° C. in the warp direction and the weft direction is obtained according to the following. Since two dimensional changes in the warp direction and the weft direction can be measured from one sample, two measurement samples (fabric) are prepared and the dimensional changes are measured at n = 4. To do. In the measurement of dimensional change, obtain the second decimal place. [Formula 4] Dimensional change rate (%) = (L2−20) / 20 × 100

[Flame retardant performance] 1999 version JIS L-
1091 A-1 method (45 ° micro burner method) 1
The burning area (cm ² ) after the minute heating, the afterflame time (seconds), and the remaining dust time (seconds) are evaluated. Furthermore, the Japan Flame Retardant Association
Performance test standards for flameproof products issued by the Flameproof Product Certification Committee (revised January 1, 1999) 1st Bedding-2 Flameproof performance test. 1. (1). Evaluation was performed according to the coil method described in 1.
The sample washing method (washing washing, dry cleaning) is JIS L-1018 8.58.4b).
F-2 method of 6.2, 8.58.4 of JIS L-1018
b) Carry out according to the method E-2 of 5.2), and evaluate the flame retardancy (afterflame time, residual dust time, burning area) at the initial stage of washing, after 5 washes with water and after 5 times of dry cleaning.

[Temperature of contraction of heat shrinkage of yarn] Using a heat shrinkage stress measuring device SSC-5000 manufactured by Seiko Instruments Inc., distance between chucks = 20 mm, heating rate = 20 ° C.
/ Min, initial load = 0.045 g / dtex, measurement atmosphere gas =
The heat shrinkage stress of the yarn was measured under each condition of air, and the heat shrinkage initiation temperature of the yarn was directly read from the heat shrinkage stress curve. In addition, the average value of 5 times of experiment was made into the measured value. In addition, FIG.
The method for reading the thermal contraction onset temperature from the thermal contraction stress curve is illustrated in Fig. Regarding the method for reading the heat shrinkage initiation temperature, the temperature at the intersection of the two tangents drawn on the heat shrinkage stress curve was directly read from the graph.

[Example 1] The phosphorus compound represented by the above [Chemical Formula 11] was used as a carboxylic acid component and a glycol component of terephthalic acid and ethylene glycol, respectively, and had a phosphorus atom content of 6
Using a phosphorus-containing copolyester copolymerized to a concentration of 000 ppm, melt spinning was performed at a spinning temperature of 265 ° C. and an undrawn yarn take-up speed of 1500 m / min to obtain a polyester multifilament undrawn yarn. Then, the unstretched yarn was stretched at a draw ratio of 3.0 times while being brought into contact with a hot roller having a surface temperature of 80 ° C. and a plate heater having a surface temperature of 160 ° C., to obtain a low shrinkage yarn of 42 decitex 24 filaments. The boiling water shrinkage SHW was 7.5%.

On the other hand, the polyester multifilament unstretched yarn obtained under the same spinning conditions was contacted only with a hot roller having a surface temperature of 80 ° C. and stretched at a draw ratio of 3.0 to obtain a highly shrinkable yarn of 42 decitex 24 filaments. Obtained. The boiling water shrinkage was 48.5%. The high shrinkage yarns and low shrinkage yarns thus obtained were subjected to an entanglement treatment with a normal temperature and high pressure air flow under the same rate supply condition to obtain 84 decitex 48 filament heterogeneous shrinkage mixed yarns. The difference in boiling water shrinkage ratio (ΔSHW) between the high shrinkage yarn / low shrinkage yarn constituting the heterogeneous shrinkage mixed yarn is 41.0.
%, The heat shrinkage onset temperature obtained from the heat shrinkage stress curve is 50
It was ℃.

A partially twisted yarn (PO) obtained by melt-spinning the phosphorus-containing copolyester used in the mixed yarn as a weft yarn by applying a sweet twist of 400 times / m to the mixed yarn
Y) was false-twisted, and a 167-decitex 48-filament false-twisted yarn was woven in an untwisted manner using an air jet loom into a double-satin design based on 5 sheets of satin.
Weaving density is 110 warp / cm, weft 26 / cm, weave width 15
The length is 2.5 cm and the weaving length is 63.5 m.

The obtained weaving looms were finely pushed into a cylindrical bag (made of cotton) having a diameter of 30 cmφ, the opening of the bag was tied with a string, and the bath temperature was raised from 30 ° C to 80 ° C using a high pressure rotary washer. Raise the temperature at + 7 ° C / min to reach the maximum temperature of 11
Treated at 0 ° C. As a nonionic surfactant [Chemical formula 9]
An aqueous solution in which 1 g / l of polyoxyethylene dodecyl glycol ether (HLB = 14.05) and 1 g / l of sodium hydroxide were prepared was subjected to wet heat relaxation treatment.

[0048]

[Chemical 9] After the waste liquid is dehydrated, the cylindrical bag is opened, the dough is taken out and spread, and after thoroughly soaping through an open soaper, a cylinder roller with a surface temperature of 110 ° C and a net conveyor dry heat relaxer with an ambient temperature of 160 ° C. Was subjected to a drying treatment under a condition that excessive tension was not applied in the warp direction and the weft direction.

Next, high-pressure dyeing with a disperse dye is performed using a jet dyeing machine, and after the waste liquid is sufficiently reduced and washed and soaped, a cylinder roller with a surface temperature of 110 ° C and a net conveyor type with an ambient temperature of 140 ° C are again used after dehydration. A finishing set was performed through a dry heat relaxer at a treatment temperature of 160 ° C. The resulting fabric has a finishing density of 137 warps /
cm, 32 wefts / cm, finished width 123 cm, finished length 50.8 m
Met. Finish width: woven width = 1.00: 1.24, finish length: woven length = 1.00: 1.25. The dimensional change rates at dry heat of 160 ° C are -0.5% and weft-1.5%, and even after the dry heat treatment, the settling and shrinkage are mild and the consumption performance is satisfactory. It was Other,
The physical property values such as flameproof performance are also summarized in Table 1. The cloth was used as a curtain. Moderate soft touch,
A swelling feeling, a surface feeling with a chinchilla effect can be obtained,
Finished curtain material suitable for public use such as theaters and home use.

[Example 2] Using the greige machine prepared in Example 1, a liquid-flow relaxer was used to increase the bath ratio from 1: 7.5 and the bath temperature from 20 ° C to 80 ° C at a heating rate of + 7 ° C / min. Then, scouring / relaxation treatment was performed at the maximum reaching temperature of 120 ° C. At the time of bath temperature 80 ℃, waste liquid is implemented and after repeated hot and cold washing, cylinder roller with surface temperature 110 ℃, ambient temperature 160 ℃
Was dried under the condition that excessive tension was not applied in the longitudinal direction and the weft direction. As the nonionic surfactant, polyoxyethylene nonylphenyl glycol ether (HLB =
An aqueous solution in which 1 g / l of 12.78) and 1 g / l of sodium hydroxide were prepared was subjected to a wet heat relaxation treatment.

[0051]

[Chemical 10]

Next, high-pressure dyeing with a disperse dye is carried out using a jet dyeing machine, and after the waste liquid is sufficiently reduced and washed and soaped, a cylinder roller with a surface temperature of 110 ° C and a net conveyor type with an ambient temperature of 140 ° C are again used after dehydration. A finishing set was performed through a dry heat relaxer at a treatment temperature of 160 ° C. The resulting fabric has a finishing density of 136 yarns /
cm, weft 31 strands / cm, finishing width 129 cm, finishing length 48 m, finishing width: woven width = 1.00: 1.18, finishing length: woven length = 1.00: 1.32, dry heat 160 The dimensional change rate at ° C was -1.0% and weft-1.0%, and even after the dry heat treatment, the settling and shrinkage were mild, and the consumption performance was satisfactory. Other physical properties such as flameproof performance are also summarized in Table 1.

The obtained flame-retardant polyester cloth is cut,
It was sewn and used on the seat surface of the sofa. A moderate soft touch and not too strong a chinchilla feel create a refined surface feeling, resulting in a sofa with an unpleasant appearance.

[Example 3] The 84-decitex 48-filament different-shrink mixed yarn and the 167 decitex 48-filament false twisted yarn used in Example 1 were used, and the different-shrink mixed-filament yarn was 400 times in the S twist direction. / M of sweet twist to form warp yarn, using the above-described false twisted yarn as the weft yarn in the rapier room without twisting, the weaving density is warp 74 yarns / cm, weft 26 yarns / cm, weaving width 193 cm, Weaving was carried out into a 7-sheet warp satin (upper right satin 6/1 (2 fly)) design with a weaving length of 71 m. Using the same method as in Example 1, the greige was used as a dyed fabric. Finishing density is 105 threads / cm, weft 35 threads / cm, finishing width 139 cm, finishing length 51 m, finishing width: weaving width = 1.00: 1.3
9, Finishing length: Textile length = 1.00: 1.39, dry heat 160 ° C
The dimensional change rate was −1.2% and the weft was −1.1%, and even after the dry heat treatment, the settling and the shrinkage were mild, and the consumption performance was satisfactory. Other,
Physical properties such as flameproof performance are summarized in Table 1.

The obtained flame-retardant polyester cloth is cut,
The sewn bedclothes bedding side cloth (bed cover) was obtained. It was a good bed cover with moderate soft touch, swelling, and chinchilla effect without dislike.

Comparative Example 1 A polyester multifilament drawn yarn (low shrinkage yarn) of 42 decitex 36 filaments was obtained by melt spinning and drawing treatment of polyester containing ethylene terephthalate as a main constituent unit according to a conventional method.
Got The boiling water shrinkage rate SHW of the drawn yarn was 6.0%. Further, a polyester obtained by copolymerizing 10 mol% of isophthalic acid as a carboxylic acid component other than terephthalic acid is melt-spun and stretched to obtain a 42 decitex 24 filament isophthalic acid-copolyester multifilament stretched yarn (high shrinkage yarn). Obtained. The boiling water shrinkage SHW of the drawn yarn was 55.5%.

The isophthalic acid-copolymerized polyester multifilament drawn yarn (high-shrinkage yarn) and the polyester multifilament drawn yarn (low-shrinkage yarn) were subjected to entanglement treatment with a normal-temperature high-pressure air stream at the same rate to obtain 84 decitex 6
A 0-filament polyester different shrinkage mixed yarn was obtained. The difference in the boiling water shrinkage ratio of the high shrinkage yarn / low shrinkage yarn of the different shrinkage drawn yarn (Δ
SHW) was 49.5%, and the heat shrinkage initiation temperature obtained from the heat shrinkage stress curve was 70 ° C.

400 times / m of sweet twist is applied to the mixed yarn to make a warp, and polyester multifilament normally drawn yarn 167 decitex 96 filament (trade name, Toyobo Ester) is used as weft 1500 times in S twist and Z twist directions. /
m real twist is inserted to make a twisted yarn, and using rapier room, weaving density is 75 yarns / cm, weft 24 yarns / cm, weave width 17
7 pieces of warp satin (upper right satin 6/1 (2 jumps)) of 2.5 cm and weaving length of 74 m were woven.

The weaving machine thus obtained was finely pressed into a cylindrical bag (made of cotton) having a diameter of 30 cm, the opening of the bag was tied with a string, and the bath temperature was raised from 30 ° C to 80 ° C using a high pressure rotary washer. The temperature was raised at a temperature rate of + 7 ° C / min, and the treatment was performed at the highest temperature of 110 ° C. The amounts of the nonionic surfactant and sodium hydroxide added and the formulation in the wet heat relaxation treatment were adjusted in the same manner as in Example 1. After the waste liquid is dehydrated, the cylindrical bag is opened, the dough is taken out and spread, and after thoroughly soaping through an open soaper, a cylinder roller with a surface temperature of 110 ° C and a net conveyor dry heat relaxer with an ambient temperature of 160 ° C. Was subjected to a drying treatment under a condition that excessive tension was not applied in the warp direction and the weft direction.

Then, when performing high-pressure dyeing with a disperse dye using a jet dyeing machine, the halogen-containing phosphoric acid ester flame retardant finishing agent was simultaneously exhausted by the in-bath exhaustion method. After the waste liquid is sufficiently reduced and washed and soaped, and after dehydration, the surface temperature of the cylinder roller is 110 ° C again, and the ambient temperature is 1
A net conveyor type dry heat relaxer at 40 ° C. was passed through, and a finishing set was performed at a processing temperature of 160 ° C. The obtained fabric has a finishing density of 87 warps / cm, 35 wefts / cm, a finishing width of 135 cm, and a finishing length of 57 m. Finishing width: woven width = 1.
28, Finishing length: Weaving length = 1.00: 1.30, dry heat 160
The dimensional change rate at ° C was -0.9% and weft-1.0%, and even after the dry heat treatment, the degree of settling and shrinkage was slight, and the consumption performance was satisfactory. Other physical properties such as flameproof performance are summarized in Table 1.

The post-processed flame-retardant polyester fabric was cut, sewn and finished as a curtain to give a soft and swelling feeling, and a finish with a chinchilla effect was obtained. Although the initial value is satisfied, the flameproof performance after 5 times of dry cleaning is extremely deteriorated and the washing durability is poor,
It did not have the desired performance as a flame-retardant curtain.

[0062]

[Table 1]

[0063]

As described above, according to the present invention, it is possible to obtain a polyester cloth having a flame-retardant property, a soft touch feeling, a bulge feeling, and a surface feeling of a cloth having a chinchilla effect.
In particular, it is a suitable material for daily use such as curtains, table cloths and wall coverings. Further, the conventional post-processed flame-retardant material had a problem in washing durability, but according to the present invention, the flame-retardant performance is semi-permanent, and further, since no flame-retardant agent is used in the post-process, it is environmentally friendly, An effect such as being able to impart performance economically and efficiently can be expected.

[Brief description of drawings]

FIG. 1 is an example of an embodiment (organization chart) of the present invention.

FIG. 2 is an example of an embodiment (organization chart) of the present invention.

FIG. 3 is an example of an embodiment (organization chart) of the present invention.

FIG. 4 is an example of an embodiment (organization chart) of the present invention.

FIG. 5 is an example of an embodiment (organizational chart) of the present invention.

FIG. 6 is an example of an embodiment (organizational chart) of the present invention.

FIG. 7 is an example of an embodiment (organization chart) of the present invention.

FIG. 8 is an example of an embodiment (organizational chart) of the present invention.

FIG. 9 is an example of an embodiment (organization chart) of the present invention.

FIG. 10 is an example of an embodiment (organizational chart) of the present invention.

FIG. 11 illustrates a method for reading the thermal contraction start temperature of the yarn from the thermal contraction stress curve of the yarn. The temperature at the intersection of the two tangents drawn on the curve is the heat shrinkage start temperature.

   ─────────────────────────────────────────────────── ─── Continued front page    F term (reference) 3B154 AA07 AA18 AB20 BA21 BB12                       BB32 BD07 BE05 BF01 BF06                       BF14 BF20 BF30 DA03 DA09                       DA13 DA16                 4H028 AA35 AA37                 4H057 AA02 DA01 DA17 DA40 FA17                       HA01 JA10 JB01                 4L035 BB32 BB89 BB91 EE14 GG01                       JJ25

Claims (3)

[Claims] 1. A fabric structure comprising at least a part of a polyester multifilament yarn containing 500 to 50,000 ppm of phosphorus atom and melt-spun of a copolyester obtained by adding the following phosphorus compound. In the dyeing process, a wet heat relaxation treatment is performed at a temperature of 20 ° C lower than the yarn shrinkage start temperature obtained from the heat shrinkage stress curve of the multifilament yarn to a temperature 30 ° C higher than the yarn shrinkage start temperature + 5 ° C / min. A method for dyeing and processing a flame-retardant polyester cloth having a rich design property, which is characterized in that the temperature is rapidly raised at + 10 ° C./min or less for processing. [Chemical 1] (In the formula, R 1 is a monovalent ester-forming functional group,
2, R3 are the same or different groups, each selected from a halogen atom, a hydrocarbon group having 1 to 10 carbon atoms, and R1, and A represents a divalent or trivalent organic residue. Further, n1 is 1 or 2, and n2 and n3 each represent an integer of 0-4. ) 2. The ratio of the weaving width to the finishing width and / or the ratio of the weaving length to the finishing length is finished: weave = 1.00:
The method for dyeing and processing a flame-retardant polyester cloth having excellent design properties according to claim 1, wherein the processing is performed under a condition satisfying 1.20 to 1.00: 1.45. 3. Dyeing of a flame-retardant polyester cloth having a high design property according to claim 1, wherein the wet heat relaxation treatment is performed in an aqueous solution containing a nonionic surfactant having an HLB value of 8 to 15. Processing method.