JPH0434075A - Antimicrobial and deodorant polyester-based fiber structure and production thereof - Google Patents

Abstract

PURPOSE:To obtain the title structure having washing durability and dry cleaning durability, by providing a polyester-based fiber structure with an aqueous solution of a specific quaternary ammonium salt and subjecting to dry heat treatment. CONSTITUTION:(A) A polyester-based fiber structure is provided with an aqueous solution of a quaternary ammonium salt shown by the formula (R1 is 12-16C alkyl; R2, R3 and R4 are CH3 or C2H5; Bu is Butyl group) and subjected to dry heat treatment at 150-210 deg.C to give the objective antimicrobial and deodorant polyester-based fiber structure.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to an antibacterial and deodorizing polyester fiber structure and a method for producing the same.

[Prior art] Polyester fiber structures include various types of woven and knitted clothing such as women's blouses, Japanese clothing, uniforms, and sports clothing, as well as interlinings, linings, curtains, bedding products, interior products, nonwoven fabrics, threads, cotton, It is widely used in industrial materials, ammunition materials, etc., including woven and knitted fabrics.

For these polyester fiber structures, it is desirable to develop polyester fiber products that prevent the adhesion of microorganisms or suppress their adhesion and propagation, are durable against washing and dry cleaning, have a soft texture, and are highly safe. It is rare.

However, since polyester fibers have high crystallinity and few reactive groups, methods such as kneading metal zeolite into the fibers have been proposed, for example, in Japanese Patent Publication No. 63-5401.
Although it is disclosed in Japanese Patent No. 3, there are problems such as coloring of the fiber itself.

On the other hand, as a post-processing method, for example, JP-A-61-245
Publication No. 378 discloses a method of applying a reaction product of an acidic group-containing polyester copolymer and an antibacterial component to polyester fibers and then heat-treating the fibers to improve adhesion and impart durability. ing.

However, this method has the disadvantage that the resulting textile product has a hard feel due to the added polyester copolymer.

Furthermore, textile products treated with 2.4.4'-trichloro2'-hydroxydiphenyl ether as an antibacterial deodorant have the disadvantage that the antibacterial effect disappears when exposed to ultraviolet light or bleached with sodium hypochlorite.

Furthermore, Japanese Patent Publication No. 1-33589 proposes a polyester fiber structure having an antibacterial and deodorizing function treated with an amphoteric compound containing an alkyl phosphate quaternary ammonium salt, but it has poor mass fastness. It had drawbacks such as a decrease in

[Problems to be Solved by the Invention] An object of the present invention is to apply a highly safe antibacterial and deodorizing agent to a textile structure without causing a change in texture or a decrease in matt fastness. An object of the present invention is to provide a polyester fiber structure having durability and dry cleaning durability.

[Means for Solving the Problems] In order to achieve the above object, the antibacterial and deodorizing polyester fiber structure of the present invention has the following configuration.

That is, the quaternary ammonium salt represented by the following formula [I] is 0.0
It is an antibacterial and deodorizing polyester fiber structure containing 2% OW1 or more and less than 0.1% OWF.

(R□ is an alkyl group having 12 to 16 carbon atoms, R2゜R3,
R4 represents an alkyl group having 1 to 2 carbon atoms, and Bu represents a butyl group. ) Furthermore, the method for producing an antibacterial and deodorizing polyester fiber structure of the present invention has the following configuration. That is, after applying the aqueous solution of the quaternary ammonium salt represented by the above formula [I] to the polyester fiber structure,
This is a method for producing an antibacterial and deodorizing polyester fiber structure by dry heat treatment at 210°C.

The present invention will be explained in detail below.

First, the antibacterial deodorant used in the present invention will be described.

The antibacterial deodorant used in the present invention is a quaternary ammonium salt having the chemical structure as shown in the formula [I] above, and has the formula [I].
], R4 is an alkyl group having 12 to 16 carbon atoms, and if the number of carbon atoms is 11 or less or 17 or more, the antibacterial activity will be insufficient.

In addition, in the formula [I], R2, R3, and R4 have a carbon number of 1
or 2 alkyl groups, with a carbon number of 3
If it is more than that, the viscosity will increase and it is not favorable for manufacturing.
Solubility in water decreases.

As the anion used for neutralizing the quaternary ammonium base, an alkyl phosphate ion is selected for rust prevention reasons. Furthermore, the alkyl group has 4 carbon atoms, ie, a butyl group. As the butyl group, any of n-butyl group, 1so-butyl group, and Ierj-butyl group is preferably used.

If the number of carbon atoms in the alkyl group is 3 or less, it is unfavorable in terms of safety, and if the number of carbon atoms in the alkyl group is 5 or more, the viscosity becomes high (which makes synthesis difficult).
This results in a mixture of alkyl phosphate ions, which is unfavorable from a safety standpoint.

In the present invention, the quaternary ammonium salt of the above formula [I] is added to the polyester fiber structure from 0.02% owf to less than 0.1% owf, more preferably from 0.03 to 0.
By containing 09% owf, it is possible to obtain antibacterial and deodorizing performance that is safe and durable for washing.

When the content of the quaternary ammonium salt is less than 0.02% owf, the antibacterial performance of the original fabric can be obtained, but it is insufficient in terms of washing durability. On the other hand, if it is 0.1% owf or more, there is no problem in antibacterial performance, but it lowers practicality in terms of cost and color fastness of the dyed object, which is not preferred in practice.

Such antibacterial treatment agents are amphoteric reactants and have high compatibility;
It can be used in combination with other drugs, and if necessary, it can be used in the treatment bath.
Softeners, hard finishing agents, antistatic agents, water repellents, water absorbing agents, etc. can also be used together.

In the present invention, any method such as immersion treatment, spray treatment, foam treatment, and gravure treatment can be selected as the method for applying the quaternary ammonium salt. After incorporating an antibacterial component into a polyester fiber structure by any of the methods, a dry heat treatment at 150°C to 210°C is performed after a normal drying process.

As for the dry heat treatment, it is also possible to adopt a tenter single-stage finish in which drying and setting are performed simultaneously.

Heat treatment at less than 150°C can provide sufficient antibacterial performance after treatment, but is not sufficient in terms of washing durability, while heat treatment above 210°C poses a risk of fiber deterioration and embrittlement, making it impractical. Not desirable.

In the production method of the present invention, after applying the quaternary ammonium salt and before dry heat treatment, the temperature is 15
Incorporating a drying step at 0° C. or lower or performing a steaming treatment does not impede the effects of the present invention.

The polyester fiber structure referred to in the present invention includes fibers made of polyalkylene terephthalate such as polyethylene terephthalate and polybutylene terephthalate, fibers made of a copolymer of the polyalkylene terephthalate and a third component, and fibers made of the fiber as a base material. Examples include nonwoven fabrics, woven fabrics, knitted fabrics, sewn products, and slit yarns for films.

Further, the cross-sectional shape of the fibers may be round or irregular. Furthermore, it may contain core-sheath or bimetallic composite fibers.

[Example] Hereinafter, the present invention will be explained in more detail with reference to Examples.

Note that the performance evaluation in the examples was performed by the following method.

A. Washing method Using a household washing machine VB-3410 (manufactured by Toshiba ■), 0.2% neutral detergent "ZABU (manufactured by Kao ■), temperature 40℃±2℃,
Wash with strong inversion for 5 minutes at a bath ratio of 1:50, then drain the liquid.
After dehydration, the operation of rinsing for 2 minutes with overflow is repeated twice, and this is counted as one washing cycle.

B. As the antibacterial evaluation test method, a bacterial count measurement method was adopted. The test microorganism was Stapylococcus aureus.
ATTC6538p) was used. The test method is to pour the broth suspension of the above test bacteria onto a sterilized sample cloth, measure the number of viable bacteria after culturing at 37°C for 18 hours in a closed container, and measure the number of bacteria relative to the number of fertilized bacteria. The standards were followed.

Under the condition of Jog (B/^)〉2, jog (B/C) was defined as the difference in bacterial count increase/decrease value, and 1.6 or more was defined as a passing level.

However, A is the number of bacteria dispersed and collected immediately after inoculation of the unprocessed product, and B
C represents the number of bacteria dispersed and collected after 18-hour cultivation of the unprocessed product, and C represents the number of bacteria dispersed and collected after 18-hour cultivation of the processed product.

C1 washing fastness According to JIS LO844A-n method.

D. Rubbing fastness According to JIS LO849: Jakushin type (200g).

(Example 1, Comparative Example 1) Warp 1. Plain woven fabric made of 100% polyester fiber with 75d-36fil raw silk for weft (warp density 118/1n)
ch, weft density 90 threads/1 nch), “Sundet G
-29” (manufactured by Sanyo Chemical) 2g/A', soda ash 5g
/l, "Butrol WR-14" (manufactured by Meisei Kagaku Kogyo ■) 2g // in a processing chamber at 98°C.

After de-sizing and scouring for 20 minutes, it is dried and
Intermediate set at 80°C, disperse dye Dianix
Black BG-FS 200% (Mitsubishi Chemical Industries ■
) 8.0%owf X 80% acetic acid 0.5c as an auxiliary agent
c/I, RAP-50 (manufactured by Sanyo Chemical) 0 as a dispersant
．． Dyeing was carried out at 130° C. for 60 minutes in a bath consisting of 5 g/A′.

Next, Na0H (30%) 2g/l! , Sundead G-
29 (manufactured by Sanyo Chemical), 0. 5 g/A', hydrosulfide 1.0 g// bath for 20 minutes at 80°C, washed with hot water at 60°C for 10 minutes, further washed with water, and air-dried to obtain a black dyed fabric. .

The dyed fabric was treated with a novel antibacterial agent F (obtained by the manufacturing method described below).
8% pure) was weighed and 0.18% ows was obtained.

0625%ays, 0. 4%ows, 1.0%a
ys.

1.2%ows, 1.5%ows, 2.5%OWE
The antibacterial properties (bacterial count) of the fabric were determined by adjusting each of the seven treatment baths, squeezing them at a pick-up rate of 100%, drying them at 120°C for 2 minutes, and then dry-heating them at 170°C for 30 seconds using a pin tenter. (increase/decrease value difference) and abrasion fastness were evaluated. Antibacterial properties were expressed as the difference in the number of bacteria after washing 10 times.

The results are shown in Table 1.

The antibacterial agent F was prepared as follows.

100 g of dodecyltrimethylammonium chloride was dissolved in 100 g of isopropanol, 40 g of 40% aqueous sodium hydroxide solution was added, and the mixture was stirred for 30 minutes. The salt was removed by filtration. 200 g of water was added to this solution, and di-n-butyl phosphate was added. Add until neutrality, and in formula [I], a fourth compound with R1 as C□2H29 and R2-R4 as CH3
Aqueous solution containing 107g of ammonium salt type antibacterial agent F41
2g was obtained. Furthermore, antibacterial agent F is diluted with ion-exchanged water.
The purity was adjusted to 8%.

As is clear from Table 1, the new antibacterial agent content is 0.02
%owf or more and less than 0.1%owf (Example 1), the antibacterial performance and abrasion fastness are good.

On the other hand, at less than 0.02% owf, the abrasion fastness is good, but the antibacterial washing durability is insufficient.
At 1% owf or more (Comparative Example 1), although the antibacterial performance is sufficient, the abrasion fastness is insufficient.

(Comparative Example 2) 143 parts of an alkyl phosphoric acid ester prepared from 3 moles of n-butanol and 1 mole of phosphoric anhydride and having a monoalkyl substituted product/dialkyl substituted product mixing ratio of approximately 1/1 and 500 parts of water were placed in a reaction vessel. and neutralized by adding 260 parts of lauryl dimethylamine. This neutralized product contains 1 ethylene oxide
00 parts were charged and reacted at 100° C. for 3 hours, and ion-exchanged water was added to the obtained antibacterial agent to adjust the antibacterial agent purity to 6.5%.

The antibacterial agent was weighed and 0.4% ows, 0. 8%o
vs, 1.2%ows, 1.6%ows, 3.0%OV
Five treatment baths for S were adjusted, and the dyed fabric obtained in Example 1 was treated with a pick-up rate of 100% in the same manner as in Example 1.
Table 2 shows the results of measuring the antibacterial properties and abrasion fastness of the fabric obtained by squeezing, drying, and heat-treating the fabric. Either antibacterial properties or rub fastness were insufficient.

(Example 2. Example 3. Comparative example 3) The dry heat treatment temperature was 140°C (Comparative Example 2).

The antibacterial properties of the fabrics obtained after washing 10 times were evaluated in the same manner as in Example 1 except that the temperature was changed to 150°C (Example 2) and 160°C (Example 3). The results are shown in Table 3. As long as the dry heat treatment temperature is 150°C or higher, which is within the range of the method of the present invention, sufficient antibacterial performance is exhibited even after washing 10 times. On the other hand, temperatures below 150°C were insufficient in terms of antibacterial performance and washing durability.

[Effects of the Invention] According to the present invention, it is possible to provide a polyester fiber structure having good washing durability and good abrasion fastness.

Claims (2)

[Claims] (1) The quaternary ammonium salt represented by formula [I] is 0
．． An antibacterial and deodorizing polyester fiber structure containing 0.02% owf or more and less than 0.1% owf. ▲There are mathematical formulas, chemical formulas, tables, etc.▼ [I] (R_1 is an alkyl group with 12 to 16 carbon atoms, R_2, R
_3 and R_4 represent an alkyl group having 1 to 2 carbon atoms, and Bu represents a butyl group. ) (2) After applying an aqueous solution of a quaternary ammonium salt represented by formula [I] to the polyester fiber structure, 15
A method for producing an antibacterial and deodorizing polyester fiber structure, comprising dry heat treatment at 0°C to 210°C. ▲There are mathematical formulas, chemical formulas, tables, etc.▼ [I] (R_1 is an alkyl group with 12 to 16 carbon atoms, R_2, R
_3 and R_4 represent an alkyl group having 1 to 2 carbon atoms, and Bu represents a butyl group. )