JPH03180571A - Deep coloration of fiber structure - Google Patents

Abstract

PURPOSE:To impart an excellent and durable deep color effect to a dyed fiber structure containing wool in good productivity by applying a corona discharge treatment to the fiber structure, imparting a silicon resin solution to the pre- treated fiber structure and subsequently subjecting the fiber structure to a low temperature plasma treatment. CONSTITUTION:A dyed fiber structure containing wool (e.g. wool/polyester black-dyed product) is subjected to a corona discharge treatment, coated with a resin solution containing a silicon resin, a catalyst, a crosslinking agent, thermally dried, subjected to a low temperature plasma treatment and subsequently thermally treated to provide the fiber structure having a durable excellent deep color effect and withstanding home washing works in good productivity.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a process for deep-coloring dyed fibrous structures containing wool.

(Conventional technology) Conventionally, deep color processing of dyed yarns, woven and knitted fabrics, and other fiber structures has mainly been applied to polyester fibers, which have a high reflectance on the fiber surface and are difficult to obtain deep colors. It is being done. Generally, the following two methods can be cited as methods for this.

(1) Low refractive index resin 1 For example, a method of applying silicone resin or the like to the surface of polyester fibers.

(2) A method in which the above-mentioned resin or the like is applied to the surface of polyester fiber, and then plasma treatment is performed using oxygen plasma or the like.

However, the conventional method described above is a method used to deepen the color of polyester fibers, and even if this method is applied as is to polyester/wool or wool, its deep coloring effect will be lower than that of polyester. There was a problem that it was small.

The following may be the cause of this. Wool has scales, and the inside of the scale is hydrophilic, but the outside of the scale is hydrophobic. When applying a low refractive index resin, the inside of the scale is hydrophilic, so the resin easily enters the scale, but the outside of the scale is hydrophobic, so it is difficult for the resin to adhere to it.

Therefore, when applying a resin with a low refractive index, the resin is absorbed inside the scale, and is not attached to the outside of the scale, that is, the surface of the wool. Because the amount of adhesion is small, a deep color effect cannot be obtained much. do not have.

The same can be said for polyester/cool blends, as the inside of wool's scales is hydrophilic, while polyester is a hydrophobic fiber.

A resin with a low refractive index is absorbed inside the hydrophilic wool scale, and the amount of resin attached to the polyester surface or wool surface is small.

(Problems to be Solved by the Invention) In order to solve these drawbacks, the present inventors previously applied low-temperature plasma treatment to dyed fiber structures containing wool in Japanese Patent Application No. 63-58094. First, we proposed a method in which a resin liquid containing silicone resin as the main ingredient and a catalyst and a crosslinking agent is applied, and after drying, low-temperature plasma treatment is performed again.

According to this method, polar groups such as hydroxyl and carboxyl groups are introduced to the outside of the wool scale and to the polyester by low-temperature plasma treatment, making the surface hydrophilic. This results in uniform adhesion to the entire surface of the fiber, resulting in an excellent deep color effect, but since low-temperature plasma treatment is performed in a vacuum, batch processing cannot be avoided.

Moreover, since the low-temperature plasma treatment was performed twice, there was a problem of a lack of productivity.

The present invention solves these drawbacks.

The object of the present invention is to obtain a method for deep-coloring a fiber structure that can bring about an excellent deep-color effect with good productivity on a fiber structure containing wool.

(Means for Solving the Problems) The present invention achieves the above object and has the following nine configurations.

That is, in the present invention, a dyed fiber structure containing wool is subjected to a corona discharge treatment, and then a resin liquid mainly composed of silicone resin and a catalyst and a crosslinking agent is applied, and after drying,
The gist of this paper is a deep color processing method for dyed fiber structures containing wool, which is characterized by performing low-temperature plasma treatment.

Hereinafter, one aspect of the present invention will be explained in detail.

In the present invention, a dyed fiber structure containing wool is used as an object of deep color processing. Textile structures containing wool are
This means that it contains wool as a component, and the other components include 9 synthetic fibers (polyester fiber, nylon fiber, acrylic fiber, etc.), semi-synthetic fibers (acetate fiber, etc.), natural fibers, etc. Any material with a lower quality than wool will suffice.

Naturally, fiber structures containing wool, including those made of 100% wool, are also subject to the method of the present invention. In particular, when the method of the present invention is applied to fiber structures made of 100% wool or fiber structures of polyester/wool blend, the deep coloring effect of the present invention becomes noticeable.

The fiber structures mentioned here include threads, fabrics, a-products, non-woven fabrics, etc.
The fiber structure may be in any form.

In the present invention, as a first step, a dyed fiber structure containing wool as described above is subjected to a corona discharge treatment.

Corona discharge occurs when a needle-like electrode and a plate-like electrode are placed in the air with a gap between them, and a voltage is applied to them to cause dielectric breakdown. Usually 5-200K) using AC of Iz,
It is carried out in the atmosphere at normal pressure.

This corona discharge is caused by the unit surface area (1m”) of the fiber structure.
It is preferable to use a discharge power amount of 1 joule or more and 106 joules or less per unit.

When the amount of energy supplied becomes less than 1 joule.

If the effect of the discharge treatment becomes insufficient and the amount exceeds 106 joules, the fiber structure may be burnt or holes may occur, which is not preferable.

This corona discharge treatment makes the outside of the wool and the surface of the hydrophobic polyester fiber hydrophilic, improving wettability9.
This has the effect of making it easier for the low refractive index resin used in the next step to adhere to the fiber surface.

Since this corona discharge treatment is carried out in the atmosphere at normal pressure, continuous treatment is possible as a pre-process to the primary resin liquid application process.

In the second step of the present invention, a resin liquid mainly composed of silicone resin and containing a catalyst and a crosslinking agent is applied to the dyed fiber structure whose surface has been made hydrophilic in the previous step by a pad-dry method. ,dry.

Examples of the silicone resin used here include methylhydrodienepolysiloxane and dimethylpolysiloxane having an amino group or a silanol group as a functional group. As these resins, water emulsion resins that are generally commercially available for processing fibers can be used.

The amount of silicone resin to be used is about 0.5 to 5% based on the weight of the fiber, either of methylhydrodienepolysiloxane or dimethylpolysiloxane having an amino group or a silanol group as a functional group.

Within this range, the optimum usage amount is determined as appropriate depending on the dyed fiber structure.

As the crosslinking agent, an isocyanate-based, polyol-based, polyamine-based compound, etc. can be used, and as the catalyst, an organic amine salt, an organic metal salt, etc. can be used. The crosslinking agent and catalyst are used in an amount of 0.1 to 3% based on the weight of the fiber.

The drying conditions may be the usual drying conditions for resin processing, and may be appropriately determined depending on the dyed fiber structure to be used. This second step imparts a low refractive index resin to the fiber surface.

By performing the first and second steps in this manner, a sufficient deep color effect is imparted to the dyed fiber structure, but as it is, it lacks dry cleaning durability and home washing durability, so its durability is In order to improve the properties, low-temperature plasma treatment is performed as a third step.

Low-temperature plasma is argon or nitrogen under low pressure.

Non-equilibrium plasma is a non-equilibrium plasma in which gas particles generated by glow discharge in a gas such as oxygen, carbon oxide, or air are ionized and excited and activated. To generate low-temperature plasma, a vacuum container containing a sample is evacuated and depressurized using a vacuum pump, and a predetermined gas is introduced to bring the sample to zero.
．． l~2. A method is used in which after adjusting the degree of vacuum to a certain degree within the range of OTorr, electric energy is applied to cause glow discharge. The energy source at this time may be either DC voltage application or AC voltage application;
Usually a high frequency of IKI (z ~ 3000MI (z) is used, especially a high frequency of 13.56M & 0.1 ~ IW/CT
A typical method is to apply the signal at the output of i. Even in the present invention.

A low temperature plasma generated in the manner described above is used.

The low-temperature plasma treatment conditions are not particularly limited; for example, a gas such as air, argon, nitrogen, or oxygen is used.

0.5-2. Plasma generated by applying a high frequency of 13.56MHz at 0.5W/cnf9 with OTorr,
Treat for 30 seconds to 3 minutes.

By performing the low-temperature plasma treatment in the third step, the dry cleaning durability and home washing durability are improved, and along with this improvement in durability, the bathochromic degree becomes deeper than that after the second step.

After the third step, use a pin tenter at 150℃ if necessary.
Heat treatment is performed for 30 seconds.

Through the above steps, the deep color performance targeted by the present invention can be imparted to a dyed fiber structure containing wool.

(Function) When a resin liquid with a low refractive index is applied to a dyed fiber structure containing wool (especially wool or a polyester/wool blend), the resin is deposited inside the scale, which is usually the hydrophilic part of the wool. It gets absorbed.

However, because resin is difficult to adhere to the outside of the scale, which is hydrophobic, and to the surface of polyester fiber, which is hydrophobic fiber, this method produces a small bathochromic effect.

In the method of the present invention, by performing corona discharge treatment in advance before applying the low refractive index resin, hydrophobic parts such as the outside of the wool scale and the surface of the polyester fiber are made hydrophilic, and in this way, the entire fiber structure is wetted. If the resin liquid is applied in a state where the properties are improved and the resin is easily adhered to the fiber surface uniformly, the low refractive index resin will be uniformly adhered to the entire surface of the fiber, and the deep coloring effect will be significantly improved.

In the present invention, by further performing low-temperature plasma treatment after applying the low refractive index resin, the low refractive index resin coating on the fiber surface has a high crosslinking density. The durability of the deep color effect is improved by suppressing swelling and falling off.

(Example) The present invention will be explained in more detail with reference to Examples, and the measurement and evaluation of the performance of the fabric in the Examples will be as follows.

It was done in the following way.

[1] The LI value of the sample was measured and evaluated using a bathochromic effect colorimeter Macbeth MS-2020. The LI value is.

The smaller the value, the better the deep color effect.

(2) Durability of deep color effect The LI value after treatment by the dry cleaning method or home washing method described below was measured by the method (1) above, and durability was evaluated by the difference in L* value before and after treatment. The smaller the LI value difference, the better the durability.

A. Dry cleaning method Turpentine washing was performed during dry cleaning in cloth.

B. Home washing method Using a home electric washing machine, bath ratio 1:40, water temperature 40
℃, detergent "Liquid Top" (product of Lion Corporation, neutral detergent) 1.3 g/l, washing was carried out for 10 minutes, followed by rinsing and spin-drying to complete one wash.

Repeat this process 5 times, then dry.

It was washed at home 5 times.

Example 1 As a dyed fiber structure containing wool, a plain woven fabric (wet weight: 146 g/rn'') with a blend of 55% black dyed polyester and 45% wool was prepared.

This was subjected to corona discharge treatment, which is the first step of the present invention.

For this corona discharge treatment, a corona discharge treatment machine manufactured by Kasuga Electric ■ was used, and the high frequency power supply was a 30KHz HF.
Corona discharge treatment was performed using a 5S-101 model, a ■-shaped discharge electrode, and a silicone rubber treatment roll. What is the amount of discharged power at this time?

It was set at 30,000 joules/mI.

Next, in the second step, the above-mentioned corona discharge treated cloth was immersed in a resin solution having the following formulation 1, squeezed with a mangle, and then dried for 2 minutes at 110° C. using a pin tenter.

[Formulation 1] Isocyanate crosslinking agent 0.5% by weight catalyst
0.5% by weight (However, the resin concentration indicates the adhesion concentration of the resin with respect to the weight of the fabric.) Next, low temperature plasma treatment, which is the third step of the present invention, was performed.
The treatment was carried out under the following low-temperature plasma treatment conditions 1.

[Low temperature plasma treatment conditions 1] Gas used: Oxygen gas flow rate: 200mj! /min Vacuum degree:
0.7 Torr Output: 0.5 KW High frequency: 13.56 MHz Treatment time: 30 seconds After this, heat treatment was performed at 150° C. for 30 seconds using a pin tenter.

For comparison with the present invention, two comparative deep-colored fabrics (Comparative Example 1) were obtained in the same manner as in the nine embodiments, except that the corona discharge treatment in the first step was omitted.

In addition, for comparison with the present invention, a comparison was made using the exact same method as in Example 1, except that low-temperature plasma treatment according to the low-temperature plasma treatment condition 1 was performed in place of the corona discharge treatment in the first step in Example 1. Deep-colored processed cloth (Comparative Example 2)
I got it.

The bathochrome effect and durability of the bathochrome-treated fabrics of the present invention and comparative fabrics were measured, and the results are shown in Table 1.

In addition, the LI values of the fabrics before deep color processing are also shown in Table 1.

(The following is a blank space) Table 1 As is clear from Table 1, the fabric according to the present invention has an L0 value of 11.9 after processing, and the LI value of the processed fabric of Comparative Example 1 is 11.9.
Although the value is 14.5, it can be seen that it has an excellent bathochromic effect.

Furthermore, regarding the durability of the deep color effect, the LI value difference before and after dry cleaning and before and after home washing of the processed fabric according to the method of the present invention is significantly smaller than the L0 value difference of Comparative Example 1. It turns out that it is excellent.

In addition, the LI value of the processed fabric of Comparative Example 2 is 12.2, showing the same deep color effect as the processed fabric of the present invention (L" value of 11.9), but in the first step of Comparative Example 2, Low-temperature plasma treatment (vacuum-based treatment) is performed in a batch manner, which requires a lot of time and effort in production, whereas the corona discharge treatment in the first step of the present invention is a treatment at normal pressure. By simply installing a corona discharge treatment machine in front of the resin bath in the second pad-dry method, continuous processing to the second resin processing step is possible, and productivity is far superior.

(Effects of the Invention) The present invention applies a corona discharge treatment and a silicone resin application treatment to a dyed fiber structure containing wool.

The present invention has a configuration in which three steps of low-temperature plasma treatment are combined and performed sequentially, and according to the present invention having such a configuration, it is possible to impart an excellent deep color effect to a dyed fiber structure containing wool with high productivity. .

Claims (1)

[Claims] (1) A dyed fiber structure containing wool is subjected to corona discharge treatment, and then a silicone-based resin is used as the main component, a catalyst,
A deep color processing method for a dyed fiber structure containing wool, which comprises applying a resin liquid containing a crosslinking agent, drying it, and then subjecting it to low-temperature plasma treatment.