JP2983306B2 - Method for producing antibacterial deodorant fiber - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for obtaining a fiber having an excellent antibacterial and deodorizing effect and an improved color tone without yellowing due to heat treatment. More specifically, the present invention relates to a method of fixing a specific antibacterial deodorant on a synthetic fiber and efficiently obtaining the antibacterial deodorant fiber having stable quality.

[0002]

2. Description of the Related Art Conventionally, carpets, mats, sheets, curtains, socks, and socks for the purpose of imparting antibacterial properties or preventing odors from being transmitted to hospitals and other sanitary fields for the purpose of preventing pathogen infection. Various methods for imparting antibacterial properties to tights have been proposed. However,
Its antibacterial properties are poorly persistent, and have the drawback that the antibacterial effect is lost during use even if it exhibits excellent effects immediately after processing, or yellowing of the fiber occurs due to decomposition of the antibacterial agent etc. . For example, 2,4,4'-trichloro-2'-
The method of adding hydroxydiphenyl ether as an antibacterial component has a disadvantage that the antibacterial component is decomposed by ultraviolet irradiation or sodium hypochlorite bleaching and the antibacterial effect is lost, and a benzalkonium chloride salt (alkyldimethylbenzylammonium) is used. The method of providing an antimicrobial component such as chloride) or a silicon-based quaternary ammonium salt has disadvantages such as the antimicrobial component falling off due to repeated washing and the like, and the fiber being yellowed by heat treatment.

In order to improve such disadvantages, Japanese Patent Laid-Open No. 59-192
No. 776 proposes a method in which an antibacterial component comprising a silicon-based quaternary ammonium salt is used in combination with a silicon compound having an epoxy group. Although this method certainly reduces the problem of yellowing of the fiber, there still remains a problem of durability such that the antibacterial agent falls off due to washing or the like and the antibacterial effect is reduced. Thus, a fiber which is excellent in durability of the antibacterial and deodorizing effect and at the same time prevents yellowing has not been proposed yet.

Further, depending on the type of antibacterial agent used, for example, a fiber product using 2,4,4'-trichloro-2'-hydroxydiphenyl may generate toxic dioxins and the like upon combustion. It is extremely dangerous in practice, and its safety has been pointed out.

[0005]

SUMMARY OF THE INVENTION Fibers having an antibacterial and deodorizing effect have durability that can withstand washing and do not cause yellowing or the like of fibers during use. That it does not cause toxic substances at the time of incineration, and that the amount of the antibacterial agent to be applied can exhibit a stable antibacterial effect without unevenness in the amount of adhesion, and to the fiber. It is required that it can be attached easily and does not require any special operation.

[0006] The present invention has been made in view of the above,
An object of the present invention is to provide a method for producing an antibacterial and deodorant fiber having the above-mentioned required characteristics.

[0007]

The present inventors have made intensive studies to achieve the above object, and as a result, the specific quaternary ammonium salt compound is excellent in heat resistance, and even under the condition that the melamine resin is fixed to the film by heating. It does not cause thermal yellowing and, unlike benzalkonium chloride, when melamine resin is used in combination, it is possible to obtain the antibacterial effect durability that can withstand washing because of the large surface hardness of the film. The present invention has been made, and as a result of further studies, the present invention has been achieved.

That is, according to the present invention, a synthetic fiber is treated with an N-polyoxyalkylene-N, N, N-trialkylammonium salt represented by the following general formula and a melamine resin as main active ingredients. Agent

Embedded image [Wherein, R ₁ represents an alkyl group having 8 to 22 carbon atoms or an alkyl group;
R ₂ and R ₃ are an alkyl group having 1 to 5 carbon atoms, and R is
An alkylene group having 2 to 4 carbon atoms, n is an integer of 1 to 5, X is
The counter anion, m indicates the valence of the counter anion. ] (1) below
And (2) was applied so as to satisfy equation _{simultaneously, (1) 0.01 ≦ W A} ≦ 1.0 (2) 0.01 ≦ W B ≦ 1.0 [ However, W _A and W _B, respectively N- polyoxyalkylene -N , N, N-trialkylammonium salt and melamine resin (wt% based on fiber weight). ]
Next, there is proposed a method for producing an antibacterial and deodorant fiber, wherein the film is heat-fixed by heat treatment.

[0009] N- polyoxyalkylene -N used in the present invention, N, N- trialkylammonium salt (hereinafter quaternary ammonium salt compound may be referred to) and a compound represented by the above following general formula der Ru.

[0010] Among them, those in which the counter anion represented by X in the above general formula is an alkyl phosphate anion (monovalent or divalent) have a small decrease in heat resistance and form an insoluble complex with an anionic surfactant. Particularly preferred is β-hydroxyethoxyethyldodecyldimethylammonium dibutoxyphosphate, β-hydroxyethoxyethylstearyldimethylammonium bis (2-ethylhexyl) phosphate, and the like.

The quaternary ammonium salt compound is different from benzalkonium chloride which has been widely used in the past,
It is presumed that the quaternary ammonium salt has a hydroxyl group in the substituent and is partially reacted with and fixed to the melamine resin used in combination. However, the durability of the antibacterial effect is extremely improved. In addition, although it is considered that the compound does not have a benzylamino group, the problem of yellowing due to heating or light is significantly improved. In addition, the agent has little phytotoxicity to the human body, does not generate harmful substances when incinerated, and has extremely high safety.

On the other hand, the melamine resin used in combination with the quaternary ammonium compound is usually produced by reacting melamine and formalin. In the present invention, the film is treated by heating after treating the fiber. There is no particular limitation on the reaction ratio between melamine and formalin as long as it forms.

In the present invention, the treating agent containing the quaternary ammonium salt compound and the melamine resin is added to the synthetic fiber. At this time, other components such as an emulsifier are contained in the treating agent. Any compounding agent such as a smoothing agent and an antistatic agent may be added.

For applying such a treating agent, any method can be adopted, and the timing is also arbitrary as long as it is after fiber formation. Above all, the method of applying in the yarn-making and cotton-making processes is more uniform than in the case of short fibers,
This is preferable because the process is simplified. In particular, a method of applying after stretching and before heat treatment is more preferable since warm water stretching becomes possible. Usually, the treatment agent is made into an emulsion of 1 to 15% by weight and applied to the drawn fiber by a dipping method, an oiling roller method, a spray method or the like. The amount of the quaternary ammonium salt compound is 0.01 to 1.
It must be 0% by weight, preferably 0.02 to 0.15 % by weight. If the amount is less than 0.01% by weight, a sufficient antibacterial effect cannot be obtained and it cannot be put to practical use. Conversely 1.
When the amount exceeds 0% by weight, the antibacterial property is sufficiently achieved, but there is no point in increasing the applied amount, and conversely, the cost is increased and the post-processing properties of the fiber are undesirably reduced.

On the other hand, the amount of the reactive melamine resin applied is 0.01
If the amount is less than this range, durability problems such as a decrease in the antibacterial and deodorant effects due to washing occur. If the amount exceeds this range, the texture of the obtained fiber becomes firm. It is not preferable because it becomes too much and the product application is restricted.

When the quaternary ammonium salt compound and the melamine resin are applied in an excessively small amount, sufficient antibacterial and deodorant performance is difficult to be exhibited, and conversely, when the amount is large, film formation is insufficient. And the durability tends to be reduced. Therefore, the latter is 1 to 1 part by weight of the former.
It is desirable to use 5 parts by weight.

After the treatment agent is applied, the fiber is subjected to a heat treatment, whereby the melamine resin in the treatment agent can be formed into a film-like, microscopically network-like film having high hardness on the fiber. By doing so, the antibacterial agent component is fixed on the fiber surface, and as a result, antibacterial and deodorant performance having extremely excellent durability can be obtained.

The heat treatment conditions vary depending on the type of melamine resin used, the presence or absence of a reaction accelerator, the type of fiber to be treated, and the like, and cannot be specified unconditionally.
If the temperature is too low, it takes a long time, and the film formation becomes insufficient, so that the effect of improving the durability cannot be obtained sufficiently.If the temperature is too high, the physical properties of the fiber deteriorate and yellowing occurs. Ordinarily, the processing temperature is 100 ~ 170 ℃,
A processing time of 10 to 60 minutes is employed. Of course, the optimal heat treatment time depends on the heat treatment temperature, and it is 15 to 25 at 140 ° C.
Min, 160 ° C. for 5 to 15 minutes is desirable in view of the state of film formation on the fiber surface and production efficiency.

The synthetic fiber to be used in the present invention is not particularly limited as long as it is composed of a fiber-forming polymer which can be spun and drawn. Melt-spun drawing of polyester fiber, polyamide fiber, polyolefin fiber, etc. Any of the fibers obtained by dry or wet spinning, such as the prepared fibers, acetate fibers, acrylic fibers, and aramid fibers, are preferably used.

[0020]

The fiber obtained by the method of the present invention exhibits excellent washing durability since the antibacterial agent is fixed in the melamine resin film formed in a film. Moreover, since the quaternary ammonium salt compound used as an antibacterial agent has excellent heat resistance, it can be sufficiently heat-treated without causing yellowing of the fiber, and can sufficiently achieve fixation of the melamine resin film. Therefore, it shows more excellent durability.

In addition, while antibacterial treatment has conventionally been applied mainly to fiber aggregates such as raw cotton and web, in the present invention, it can be applied in the fiber manufacturing process, so that the treatment agent has very little unevenness. It also has a feature that extremely stable antibacterial and deodorant performance can be obtained even when the amount of the treatment agent is reduced.

[0022]

The present invention will be described in more detail with reference to the following examples. The performance evaluation in the examples was measured according to the following method. (1) Measurement of antibacterial activity Place the test sample on an agar medium inoculated with Staphylococcus aureus, incubate the bacteria at 37 ° C for 24 hours, and determine the antibacterial effect by the presence or absence of growth of Staphylococcus aureus around the sample. judge. (Judgment) ：: No growth of bacteria around the sample was observed, and halos were generated. X: Halo does not occur around the sample. (2) Washing method After washing for 5 minutes in a 40 ° C. aqueous solution containing 2 g / l of a neutral detergent New Beads (manufactured by Kao Corporation) using a household electric washing machine, washing with running water was performed for 2 minutes, and dehydration was performed. Then, it is washed with running water for 2 minutes, dehydrated, and dried. Repeated washing is performed by repeatedly performing the above operation. (3) Thermal yellowing The color tone of the test sample was measured using a colorimetric colorimeter (Color Machine No. 80-5Z manufactured by Nippon Denshoku Co., Ltd.).
Value) was measured. A sample having a b value of less than 5 was evaluated as good (○), and a sample having a value of 5 or more was evaluated as unacceptable (x).

[0023]

Example 1 Polyethylene terephthalate having an intrinsic viscosity of 0.64 was melt-extruded from a spinneret having a pore diameter of 0.3 mm and 140 holes at a spinning temperature of 300 ° C. and a discharge rate of 300 g / min, and spun at a take-up speed of 800 m / min. Then, the obtained undrawn yarn was drawn 4.0 times in hot water at 70 ° C., and then converted into N-oxyalkylene-N, N, N-trialkylammonium salt.

[0024]

Embedded image A melamine resin (Euramine T-33) manufactured by Mitsui Toatsu Co., Ltd. was used as a melamine resin, and immersed in a bath of a treatment liquid in which a quaternary ammonium salt compound and a melamine resin were mixed at the ratios shown in Table 1. Then, it was squeezed with a crimper so that the total adhesion amount was 0.20% by weight, and at the same time, crimping was applied. Next, heat treatment was performed under the conditions described in (Table 1), and the polyester fiber was cut to a length of 51 mm to obtain polyester short fibers (single fiber fineness: 6 denier).

The obtained short fibers are passed through a card and the basis weight is 100
A web of g / m ² was prepared and subjected to needle punching to obtain a nonwoven fabric. The results of evaluating this nonwoven fabric according to the above method are shown together with (Table 1).

The results obtained when benzalkonium chloride outside the present invention or the following quaternary ammonium chloride-containing trimethoxysilane was used as the quaternary ammonium salt compound (Comparative Example) are also shown in Table 1. ).

[0027]

[Table 1]

From the above results, it can be seen that the fiber obtained by the method of the present invention does not yellow during heat treatment and exhibits antibacterial performance with excellent washing resistance. When a quaternary ammonium salt is used or when a melamine resin is not used in combination, it can be seen that yellowing at the time of heat treatment increases, the durability of antibacterial performance decreases, or at least one of the performances decreases.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁶ Identification code FI D06M 13/46

Claims (1)

(57) [Claims] 1. A synthetic fiber represented by the following general formula:
It is N- polyoxyalkylene -N, N, a processing agent whose main active ingredient and N- trialkylammonium salt and a melamine resin, ## STR1 ## [Wherein, R ₁ represents an alkyl group having 8 to 22 carbon atoms or an alkyl group;
R ₂ and R ₃ are an alkyl group having 1 to 5 carbon atoms, and R is
An alkylene group having 2 to 4 carbon atoms, n is an integer of 1 to 5, X is
The counter anion, m indicates the valence of the counter anion. ] (1) below
And (2) was applied so as to satisfy equation _{simultaneously, (1) 0.01 ≦ W A} ≦ 1.0 (2) 0.01 ≦ W B ≦ 1.0 [ However, W _A and W _B, respectively N- polyoxyalkylene -N , N, N-trialkylammonium salt and melamine resin (wt% based on fiber weight). ]
Next, a method for producing an antibacterial and deodorant fiber, comprising heating and heat-fixing the film.