JPH08311766A - Polyester fiber fabric and its production - Google Patents

Abstract

PURPOSE: To give antifungal properties and flame retardancy simultaneously to a polyester fiber by admixing a halogenated cycloalkane, a quaternary ammonium salt and/or a compound bearing biguanide group and an aminoplast resin to a polyester fiber. CONSTITUTION: To the dye bath for a polyester ester fiber structure, 1.5-2.0% owf of a halogenated cycloalkane such as hexabromocyclododecane is added and the fiber structure is treated at a bath ratio of 1/50-1/5 at above 80 deg.C, then washed to dye the structure and simultaneously effect the flame-retardant processing. Then, a treating solution containing 0.04-2.1% owf of a compound bearing quaternary ammonium salts and biguanide groups on its main chains such as polyoxyethylene (dimethylimino)ethylene (dimethylimino)ethylene dichloride, <=10% owf of a halogenated cycloalkane and 0.01-0.35% owf of an aminoplast resin such as trimethylolmelamine is applied to effect the exhaustion treatment at 100-210 deg.C.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester fiber structure and a method for producing the same. More specifically, the present invention relates to a polyester fiber structure having antibacterial properties and flame retardancy, and a method for producing the same.

[0002]

2. Description of the Related Art Polyester fiber products are widely used for clothing and interiors. In such fiber products, human body sweat adhering to the fiber surface and atmospheric dirt are propagated as a nutrient source. There is a problem that a bad odor is emitted by microorganisms such as bacteria and mold.

On the other hand, the interior materials used in hotels, hospitals, movie theaters, etc. are regulated by the Fire Service Law in order to minimize damage caused by fires such as matches and cigarettes. Under these circumstances, in order to create a safe and comfortable living environment, it is desired to develop a textile product that has both antibacterial properties and flame retardancy.

Conventionally, various antibacterial processed products have been developed, and Japanese Patent Publication No. 2-30340 discloses a method of imparting an organosilicone having a quaternary ammonium base. , Cotton products can be washed with durability, but synthetic fiber products such as polyester fibers do not have long-lasting effect by themselves.

Further, in the processing method disclosed in JP-A-1-11076 in which a quaternary ammonium salt is used in combination with a melamine resin, antibacterial durability can be obtained, but when treated with a flame-retardant polyester fiber. However, the required flame retardancy cannot be obtained because the viscosity at the time of melting becomes high and the drip property deteriorates.

[0006]

SUMMARY OF THE INVENTION An object of the present invention is to provide a fiber product which imparts antibacterial properties and flame retardancy to a polyester fiber structure with durability against commercial washing.

[0007]

To achieve the above object, the polyester fiber structure of the present invention has the following constitution.

That is, 1.3% owf or more of a halogenated cycloalkane compound is contained inside the polyester fiber, and 0.04 to 2.1% of a compound having a quaternary ammonium salt or / and a biguanide group in the surface layer of the fiber. owf
It is a polyester fiber structure characterized by containing.

The method for producing a polyester fiber structure of the present invention has the following constitution.

That is, in a dyeing bath containing 1.5 to 20% owf of a halogenated cycloalkane compound, the bath ratio is 1:
50 to 1: 5, after treating at 80 ° C or higher and washing,
A treatment solution containing 0.04 to 2.1% ow of a quaternary ammonium salt or / and a compound having a biguanide group and 10% ow or less of a halogenated cycloalkane compound is applied to the fiber surface and heat treated at 100 to 210 ° C. Is a method for producing a polyester fiber structure.

[0011]

The polyester fiber structure of the present invention will be described in detail below.

The polyester fiber structure of the present invention comprises a polyalkylene terephthalate fiber typified by polyethylene terephthalate, polybutylene terephthalate, etc. or a copolymer fiber of these alkylene terephthalate units as a main component and a copolymerization component thereof. The following non-woven fabric, woven fabric, knitted fabric, sewn product, etc. can be used.

Further, the cross-sectional shape of the fiber is not particularly limited, such as round shape and irregular shape. It should be noted that these fiber structures may contain in advance a dye, a pigment, an antioxidant, an antibacterial agent or a flame retardant compound such as phosphorus-containing, halogen-containing or antimony-containing.

In the present invention, as the quaternary ammonium salt or the compound having a biguanide group, 3- (trimethoxysilyl) propyldimethyloctadecyl ammonium chloride, benzalkonium chloride, benzethonium chloride, polyoxyethylene trimethyl ammonium chloride, alkyl trimethyl Ammonium salt, phenododecium bromide, isooctylphenoxyethoxyethyldimethylbenzylammonium chloride, cetyldimethylbenzylammonium chloride, (3,4-dichlorobenzyl) dodecyldimethylammonium chloride, alkyldimethylethylammonium salt, alkylamidopropyldimethylbenzylammonium salt , Diisobutylcrezoxyethoxyethylbenzylammonium salt,
1,1'-hexamethylene bis [5- (p-chlorophenyl biguanide)] hydrochloride, dodecyl guaningin hydrochloride, poly-oxyethylene (dimethylimino) ethylene (dimethylimino) ethylene dichloride (hereinafter PMI
EC), bis- (p-chloro-phenyl biguanide) hexane, polyhexamethylene biguanidine hydrochloride and the like can be used, but not limited thereto.

A compound having a quaternary ammonium salt or a biguanide group, or a compound having a quaternary ammonium salt and a biguanide group is used in the range of 0.04 to 2.
1% owf is contained, and 0.1 to 1% o
It preferably contains wf.

If it is less than 0.04% owf, there is a problem that sufficient washing durability with antibacterial performance cannot be obtained. On the other hand, if it exceeds 2.1% owf, the flame retardancy is lowered. There is. Here, the fiber surface layer portion means a region from the surface of the single fiber to 1/2 of the radius of the single fiber. Whether or not the quaternary ammonium salt and the compound having a biguanide group are present in this region can be confirmed by dyeing the sample with a gold-containing dye or the like and observing the fiber cross section with an optical microscope.

In the present invention, the aminoplast resin is a melamine resin such as trimethylol melamine and hexamethylol melamine, a urea resin such as dimethylol propylene urea, dimethylol ethylene urea and dimethylol hydroxyurea, and a urone resin such as dimethylol urone. However, the present invention is not limited to this. The amount of resin attached is 0.01 to 0.3 with respect to the fiber.
5% owf is preferable, and 0.05 to 0.2% owf is more preferable.

Further, other urethane-based, epoxy-based or acrylic-based synthetic resins may be used in combination as long as the flame retardancy is not impaired.

The halogenated cycloalkane compound of the present invention is a cyclic saturated hydrocarbon compound or a saturated hydrocarbon compound having at least one cyclic saturated hydrocarbon group, wherein at least a part of hydrogen atoms is replaced by halogen. A compound. Specific examples of such compounds include:
For example, 1,2,3,4,5,6-hexabromocyclohexane, 1,2,3,4-tetrabromocyclooctane (hereinafter abbreviated as TBCO), 1,2,5,6,
9,10-Hexabulmocyclododecane (hereinafter referred to as HBC
Abbreviated as D), 1,2-bis (3,4-dibromocyclohexyl) 1,2-dibromoethane, or a compound obtained by substituting chlorine for bromine in these compounds. Among these compounds, most or all of the halogens are bromine because the exhaust efficiency is extremely high,
It is suitable for the present invention.

The content of the halogenated cycloalkane compound inside the fiber is 1.3% owf or more.

Generally, the upper limit is preferably 10% owf or less from the viewpoint of light fastness and exhaust efficiency.

If it is less than 1.3% owf, there is a problem that the flame retardant performance is deteriorated by antibacterial processing.
2% owf or more and 8% owf from the viewpoint of light fastness
It is preferable to set the following.

In the method for producing a polyester fiber structure of the present invention, for example, a halogenated cycloalkane compound for imparting the above flame retardancy is first charged in a dyeing bath,
Flame-retardant processing is performed at the same time as dyeing. In this case, the halogenated cycloalkane compound is 1.5 to
It is set to 20% owf. When the amount of the halogenated cycloalkane compound used is less than 1.5% owf, there is a problem that the flame retardancy is lowered by the antibacterial agent and stable flame retardant performance cannot be obtained. On the other hand, the amount exceeds 20% owf. In that case, there is a problem that the loss of the compound is large and it is not practical in terms of workability and cost.

Further, in addition to the dye, a pH adjusting agent, a leveling agent, a sequestering agent, a carrier and the like used in ordinary dyeing can be added as appropriate.

At this time, the bath ratio is 1:50 to 1: 5. From the viewpoint of loss of flame retardant or dye, color blur and color unevenness, 1:20 to 1: 5 is preferable. Bath ratio is 1: 5
If it is less than 0, the loss of the flame retardant or dye is large and there is a problem such as color blur. On the other hand, if it exceeds 1: 5, it is difficult to evenly distribute the flame retardant inside the fiber, and color unevenness occurs. There are problems such as easy to become.

The treatment temperature in the bath is 80 ° C. or higher. From the viewpoint of exhaustion, it is preferable to perform the treatment in a bath at 120 to 145 ° C. After that, cleaning is performed. The treatment time in the bath is usually about 20 to 60 minutes. When the temperature is lower than 80 ° C., the flame retardant is less likely to be exhausted by the fiber, and there is a problem that durability is lost.

Further, a halogenated cycloalkane compound or a phosphorus-based flame retardant compound is applied to the fiber surface before or after dyeing, or at 150 to 210 ° C.
It can also be treated with dry heat.

Thereafter, 0.04 to 2.1% of a compound having a quaternary ammonium salt or a biguanide group or a compound having a quaternary ammonium salt and a biguanide group is added.
ows, 0.1 to 1 halogenated cycloalkane compound
A treatment liquid containing 0% ows is applied to the fiber surface by an arbitrary method such as dipping treatment, spraying treatment, foaming treatment, and gravure treatment, followed by drying at 100 to 210 ° C. and heat treatment.

When the concentration of the quaternary ammonium salt or the compound having a biguanide group or the concentration of the quaternary ammonium salt and the compound having a biguanide group is less than 0.04% ow, sufficient antibacterial performance and washing durability can be obtained. There is no problem. On the other hand, if it exceeds 2.1% ows, the flame retardant performance is deteriorated, which is not practically preferable in terms of cost.

From the viewpoint of antibacterial durability and adverse effects on flame retardancy, the treatment liquid contains 0.0% aminoplast resin.
It is also preferable to contain 1 to 0.35% ows.

If the amount of the halogenated cycloalkane compound exceeds 10% ow, yellowing and deterioration of fastness are observed, which is not preferable. Further, the treatment liquid may contain an appropriate amount of an inorganic acid salt, an organic acid salt or the like as a catalyst for the aminoplast resin, and a phosphorus-based flame retardant or the like can be used together.

As the heat treatment, it is possible to adopt a tenter one-step finish for simultaneously performing drying and setting. 1
A heat treatment at a temperature lower than 00 ° C is not sufficient in terms of durability, while a temperature higher than 210 ° C causes problems such as yellowing and embrittlement of the fibers.

[0033]

The present invention will be described in more detail with reference to Examples and Comparative Examples.

The performance evaluation methods in the examples are shown below.

[Washing Method] JIS L 1042, 6.
According to 6.1 (1) (Washing machine), weak alkaline detergent "Zab" (registered trademark, manufactured by Kao Corporation) 0.1%, temperature 6
After treatment at 0 ° C. ± 2 ° C. and a bath ratio of 1:40 for 75 minutes, drainage is dehydrated and rinsing is repeated for 25 minutes three times. This is 5 times of washing.

[Evaluation of Flame Retardancy] JIS L 1091 D
Evaluation was performed according to the method (flame contact test).

[Evaluation of antibacterial property] As a test method, a bacterial count method was adopted. The test strain is Stapylococcus-au.
The reus IID1677 (MRSA) was used. The test method is as follows.
The number of viable cells after 18 hours of culture was measured, and the number of cells was compared with the number of cells to be inoculated, and the following criteria were followed.

Under the condition of log (B / A)> 2, log
(B / C) was defined as the difference in the increase / decrease value of the number of bacteria, and 1.6 or more was defined as the pass level.

Here, A represents the number of bacteria that were dispersed and recovered immediately after inoculation of the unprocessed product, B represents the number of bacteria that were dispersed and recovered after 18-hour culture of the unprocessed product, and C represents the number of bacteria that were dispersed and recovered in culture of the processed product for 18 hours. . [Light fastness] Measured according to JIS L 0842.

[Example 1 and Comparative Example 1] 1 g / g of "Sandet G-29" (manufactured by Sanyo Kasei Co., Ltd.) was knitted with a 150d-48fil processed yarn of 100% polyester fiber.
1 and sodium hydroxide (30%) 2g / l in a treatment liquid, scouring was carried out at 80 ° C for 15 minutes, then dried and intermediate set at 180 ° C for 30 seconds. Using a flame retardant treatment liquid, a jet dyeing machine was used and treated at 130 ° C. for 60 minutes with a bath ratio of 1:10.

<Compounding of Dyeing and Flame Retardant Treatment Liquid> Disperse Dye: Resolin Blue FBL (Resolin Blue FBL) 0.03% owf Auxiliary Agent: Ionet TD-208 1 g / l Fixa-PH-500 1 g / l Halogenated cyclo Alkane compound: HBCD 6% owf Next, "Sandet G-29" (manufactured by Sanyo Kasei Co., Ltd.) 1
In a bath consisting of g / l, sodium hydroxide (30%) 2 g / l and hydrosulfite 1 g / l, reduction washing was carried out at 80 ° C. for 20 minutes, hot water washing at 60 ° C. for 10 minutes, and further water washing. Then, it was dried at 120 ° C. for 2 minutes with a pin tenter.

Then, the PMIEC is 0.03% ows,
Trimethylolmelamine 0.16% ow in each aqueous solution containing 0.05% ows, 2.0% ows, 2.2% ows
s, HBCD at 5% ows to prepare a treatment liquid, the dyed fabric is dipped, squeezed at a pickup rate of 100%, dried with a pin tenter at 120 ° C. for 2 minutes, heat treated at 180 ° C. for 30 seconds to form a polyester fiber structure. I got a thing. The antibacterial property and flame retardancy of the obtained fiber structure were evaluated.

Further, for comparison, the dyed and flame-retardant fabric of Example 1 was dipped in a treatment liquid containing trimethylolmelamine at 0.5% ows and treated under the same conditions as in Example 1. As shown in Table 1, the content of the antibacterial agent is 0.0
When it was less than 4% owf (Comparative Example 1-1), the antibacterial property after washing was insufficient. When it exceeds 2.1% owf (Comparative Example 1-2), the flame retardancy is lowered. Further, when the content of the aminoplast resin was 0.35% owf or more, the flame retardancy was also lowered.

[0044]

[Table 1] [Example 2 and Comparative Example 2] HBCD was used in Example 1 except that HBCD was not included and the other conditions were the same.
After immersing the CD in a treatment solution prepared to 1.5% ows, 2% ows, 15% ows, squeezing it with a pickup rate of 100%, and drying it with a pin tenter at 120 ° C. for 2 minutes, 195
Heat treatment was performed at 30 ° C. for 30 seconds.

Next, the dyed and flame-retardant cloth was treated with PMICE at 0.5% ows and trimethylolmelamine at 0.2% o.
After immersing ws and Sumitex Accelerator in a treatment liquid containing 0.1% ows, squeeze with a pickup rate of 100%, and dry with a pin tenter at 120 ° C. for 2 minutes, then 180
Heat treatment was performed at 30 ° C. for 30 seconds to obtain a polyester fiber structure. The antibacterial property and flame retardancy of the obtained fiber structure were evaluated.

The results are shown in Table 2. As shown in Table 2, when the amount of the flame retardant attached was less than 1.3% owf (Comparative Example 2-1), the flame retardancy decreased. Also, the amount of HBCD adhered is 10% o
If it exceeds wf, the light fastness is lowered.

[0047]

[Table 2]

[0048]

EFFECT OF THE INVENTION The polyester fiber structure obtained by the present invention maintains the flame retardant performance that passes the flameproof standard and has antibacterial properties excellent in washing durability.

Further, it has become possible to combine the flame retardant and antibacterial properties of the polyester fibers, which has been difficult until now, and it is possible to broaden the product development in the curtain field and the like.

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Claims (6)

[Claims] 1. A polyester-based fiber containing 1.3% owf or more of a halogenated cycloalkane compound, and 0.04 to 2.1% of a compound having a quaternary ammonium salt or / and a biguanide group in the surface layer of the fiber. A polyester fiber structure containing owf. 2. Aminoplast resin is added in an amount of 0.01 to 0.35.
% Owf is contained, The polyester fiber structure of Claim 1 characterized by the above-mentioned. 3. The polyester fiber structure according to claim 1, wherein the quaternary ammonium salt has a quaternary ammonium salt in the main chain. 4. The polyester-based fiber structure according to claim 1, wherein the compound having a biguanide group has a compound having a biguanide group in the main chain. 5. A dyeing bath containing a halogenated cycloalkane compound of 1.5 to 20% owf in a bath ratio of 1:50 to 1:
5, treated at 80 ° C. or higher, washed, then 0.04 to
A treatment liquid containing 2.1% ow of a quaternary ammonium salt or / and a compound having a biguanide group and 10% ow or less of a halogenated cycloalkane compound is applied to the fiber surface, and exhaustion treatment is performed at 100 to 210 ° C. A method for producing a polyester fiber structure, which comprises: 6. The method for producing a polyester fiber structure according to claim 5, wherein the treatment liquid contains 0.01 to 0.35% ows of aminoplast resin.