JPH0544159A - Coloring of fiber - Google Patents

Abstract

PURPOSE:To provide a coloring method for fiber capable of imparting a fiber with flame-proofing property or flame-retarding property and easily coloring even glass fiber, etc., which has been difficult to color by conventional coloring method. CONSTITUTION:A coating liquid prepared by dispersing a pigment in a solution of a metal compound such as an alkoxysilane is applied to a fiber and heat- treated. A thin film of a pigment-containing metal oxide gel is fixed to the fiber surface by sol-gel process to color the fiber.

Description

Detailed Description of the Invention

[0001]

The present invention relates to a method for coloring fibers,
In particular, the present invention relates to a fiber coloring method capable of imparting flameproofness or flame retardancy to fibers, and further easily coloring glass fibers and the like, which have been difficult to color conventionally.

[0002]

2. Description of the Related Art In recent years, from the viewpoint of disaster prevention, textile products used for interior materials such as houses and vehicles, furniture, etc.
Flameproof and flame retardant performance is required. However, due to the pursuit of flame retardant performance, a new problem has arisen, in which toxic gas is generated due to decomposition of fibers and flame retardants due to heat during a fire.

Therefore, as a measure for solving such a problem, conventionally, inorganic fibers such as glass fibers and carbon fibers have been used alone, or mixed with organic fibers, and heat-resistant synthetic fibers have been used. Etc. have been proposed. However, in general, interior materials such as houses and vehicles, furniture, etc. are often required to be colored in order to make them aesthetically pleasing or to enhance the product value. , Because it is difficult to color
Conventionally, it has hardly been used for the above-mentioned interior materials and furniture.

[0004]

DISCLOSURE OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and in particular, it is possible to impart flameproofness or flame retardancy to fibers, and moreover, conventional methods. An object of the present invention is to provide a method for coloring fibers, which can easily color even glass fibers which have been difficult to be colored.

[0005]

The method for coloring a fiber according to the present invention is characterized by forming a metal oxide gel containing a dye on the surface of the fiber. As a method for forming a metal oxide gel, a sol-gel method has been well known in the past. In this method, an organic or inorganic compound of a metal is made into a solution, the metal compound is hydrolyzed in the solution, a sol is made into a gel through a polycondensation reaction, and dried and solidified by heat treatment to obtain a solid metal oxide. The product gel is produced. Such a solid metal oxide gel is a porous gel. Therefore, according to this method, a coating liquid containing the above-mentioned metal compound is applied to the surface of the fiber and heat-treated to form a thin film of the solid metal oxide gel on the surface of the fiber. The metal oxide gel thin film thus formed has flame resistance and flame retardancy equivalent to or higher than that of glass fiber. It is also known that the above-described porous gel produces amorphous glass by heating and burning it at a high temperature.

The method for coloring fibers according to the present invention is such a sol-gel method in which a dye is dispersed or dissolved in a solution of the metal compound to prepare a coating solution, and the coating solution is applied to the fiber. The heat treatment is performed to form a thin film of the colored metal oxide gel containing the dye as described above on the fibers, thereby coloring the fibers.

In the method of the present invention, the metal compound may be an organic metal compound such as metal alkoxide, metal acetylacetonate or metal carboxylate,
Inorganic metal compounds such as nitrates, oxychlorides and chlorides can be mentioned. However, in the method of the present invention,
Among these, an organometallic compound is preferable because it has high reactivity and easily forms a metal oxide gel.
Particularly, metal alkoxide is preferably used.

The metal alkoxide is represented by the general formula (I) M (OR) n (wherein M represents a metal element, R represents an alkyl group,
n is the oxidation number of the metal. ).

In the method of the present invention, among such metal alkoxides, those in which the metal element is silicon, that is, tetraalkoxysilane, are preferably used, and the metal element is, for example, zinc, titanium, or the like. Alkoxides of aluminum, iron, cobalt, nickel, lithium and the like can also be used. Further, the metal alkoxide may be a mixture. Further, R is preferably an alkyl group having 1 to 5 carbon atoms, for example, an isopropyl group or n-
An alkoxide which is a butyl group is preferably used.

The organic solvent for dissolving the metal alkoxide is appropriately selected in consideration of the solubility of the metal compound and the viscosity of the resulting solution, but alcohol is usually used, and among them, those having 1 to 5 carbon atoms. Aliphatic alcohols are preferably used. For example, ethanol, isopropanol, n-butanol and the like are preferably used. Almost all dyes, organic pigments and inorganic pigments can be used as the pigment. As the dye, for example, an acid dye, a metal-containing dye, an oil-soluble dye or the like can be used, and as the pigment, for example, an azo pigment such as benzidine yellow, carmine FB, perylene, perinone, dioxazine, thioindigo, isoindo, etc. Examples thereof include condensation pigments such as linone, quinophthalone, quinacridone, organic pigments such as phthalocyanine pigments, and inorganic pigments such as titanium white, red iron oxide, yellow lead, cobalt blue, and carbon black. Such a dye, depending on the type of dye used and the required coloring concentration, is usually 0.01 to
Used in the range of 200% by weight.

In the method of the present invention, it is preferable to use a dispersant when dispersing or dissolving the above dye in the solution after the metal. Such a dispersant is appropriately selected in consideration of a dye, a metal compound, an organic solvent, etc. to be used, but generally, a dispersant which has an adsorbing power for the dye and is compatible with the metal compound solution is preferably used. .. Examples of such dispersants include silane coupling agents, titanium coupling agents, metal coupling agents such as aluminum coupling agents, polyvinyl alcohol resins, polyvinyl butyral resins, acrylic resins, ethyl cellulose, unsaturated polycarboxylic acids, and phosphoric acid esters. Examples of the surfactant include a resin-based dispersant such as a surfactant and a polyester resin. These dispersants are usually used in the range of 5 to 100% by weight based on the dye. Normally,
The dye is dispersed in the solvent using such a dispersant, and the obtained dispersion is mixed with the metal compound solution.

The coating solution can be prepared, for example, by mixing the metal compound solution with a dye or a dispersion thereof, dispersing the mixture, adding water and an acid as a reaction catalyst, and stirring the mixture. Metal compounds in coating liquid,
The amount of the dye and the dispersant is usually in the range of 0.1 to 50% by weight, preferably 5 to 25% by weight.

In order to apply such a coating liquid to the fiber, a method such as a deep coating is usually used. That is, a uniform coating can be formed on the surface of the fiber by immersing the fiber in the coating liquid and then pulling it up. The temperature for immersing the fiber in the coating liquid may be room temperature. In this way, according to the method of the present invention, the coating liquid is applied to the fibers and heat-treated to form a gel through the sol by the polycondensation reaction of the metal compound, as described above, This gel is fixed on the fiber as a metal oxide thin film to form a colored film,
Thus, the fibers are colored.

The fibers used in the method of the present invention include, for example, inorganic fibers such as glass fibers, carbon fibers, metal fibers and ceramic fibers, polyamide fibers including aromatic polyamide fibers, organic fibers such as polyester fibers and polyvinyl alcohol fibers. Fibers can be mentioned. In particular,
According to the method of the present invention, it is possible to easily color inorganic fibers such as glass fibers and aromatic polyamide fibers, which have been difficult to color conventionally.

In the method of the present invention, the heat treatment temperature of the gel thin film is not higher than the decomposition temperature of the dye and not higher than the heat resistant temperature of the fiber. Often 300 ° C
The following are preferred: As described above, if the heat treatment is performed at a temperature of 300 ° C. or lower, most dyes can be used regardless of whether they are organic or inorganic. is there. However, according to the method of the present invention, a gel thin film of a metal oxide having a practical film strength can be obtained practically at a temperature near 100 ° C. However, depending on the dye or fiber used, the temperature may be 300 ° C.
The heat treatment may be performed at the above temperature.

[0016]

As described above, according to the method of the present invention,
Since a thin film made of a metal oxide gel containing a dye is formed on a fiber to color the fiber, the degree of freedom in color selection is high, and the fiber can be provided with flameproof performance or flame retardancy. Further, it is possible to easily color glass fiber or the like, which has been difficult to be colored conventionally.

Further, by using the method of the present invention, various functions can be imparted to the fiber. For example, a material such as a functional dye can be introduced on the surface of the fiber and applied to an electronic material or the like. Further, if a metal oxide gel such as lithium is used, it is possible to impart an antistatic effect to the fiber.

[0018]

The present invention will be described below with reference to examples.
The present invention is not limited to these examples. Example 1 2.5 parts by weight of a pigment (permanent carmine FBB-02), 0.5 parts by weight of a dispersant (Goselan L-301 (polyvinyl alcohol)) and 97 parts by weight of a solvent (isopropyl alcohol) were mixed, and a disperser was used. The pigment was dispersed for 10 minutes to prepare a pigment dispersion.

Next, 6.0 g of tetraethoxysilane, 6.0 ml of ethanol, 6.0 g of water, 0.75 ml of concentrated hydrochloric acid, 12.0 ml of the above pigment dispersion and 19.0 ml of n-butanol were mixed, and the mixture was mixed at room temperature for 2 hours. The coating liquid was prepared by stirring for a time. Dip the glass fiber woven cloth in this coating solution, then
The glass fiber was pulled up at a speed of mm / sec, the coating liquid was applied onto the glass fiber, and this was heat-treated at 100 ° C. for 15 minutes in an oven to obtain a colored glass fiber. Example 2 Tetraethoxysilane 6.0 g, ethanol 6.0 ml, water 9.
6 g, concentrated hydrochloric acid 0.75 ml, pigment "Supilon Blue 3BH conc.
A liquid mixture (2.0 ml) and n-butanol (25.0 ml) were prepared and stirred at room temperature for 2 hours to prepare a coating solution.

The glass fiber woven cloth is dipped in this coating solution, and then pulled up at a speed of 3 mm / sec to apply the coating solution on the glass fiber, which is then placed in an oven for 1 minute.
Heat treatment was carried out at 00 ° C. for 15 minutes to obtain a colored glass fiber. Example 3 An aramid (aromatic polyamide) fiber woven fabric (Technora manufactured by Teijin Ltd.) was dipped in the coating liquid prepared in Example 1, and then pulled up at a speed of 3 mm / sec.
Apply the coating liquid on the fiber and put it in the oven.
It heat-processed at 100 degreeC for 15 minutes, and obtained the colored aramid fiber. Example 4 An aramid (aromatic polyamide) fiber woven fabric (Technora manufactured by Teijin Ltd.) was dipped in the coating liquid prepared in Example 2 and then pulled up at a speed of 3 mm / sec.
Apply the coating liquid on the fiber and put it in the oven.
It heat-processed at 100 degreeC for 15 minutes, and obtained the colored aramid fiber. Example 5 The flame retardancy test of the colored aramid fiber prepared in Example 3 was performed. As a comparative example, a nonflammable aramid fiber was subjected to a flame retardancy test before being colored according to the present invention.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Kazuo Sakai 2- 1-43 Kiyowadai Higashi, Kawanishi City, Hyogo Prefecture

Claims (5)

[Claims] 1. A method for coloring a fiber, which comprises forming a metal oxide gel containing a dye on the surface of the fiber. 2. A metal oxide gel having the general formula (I) M (OR) n (wherein M represents a metal element, R represents an alkyl group,
n is the oxidation number of the metal. The method for coloring fibers according to claim 1, wherein the metal alkoxide represented by the formula (4) is formed by a sol-gel method. 3. The method for coloring a fiber according to claim 2, wherein the metal element is silicon, zinc, titanium, aluminum, iron, cobalt, nickel or lithium. 4. The method for coloring a fiber according to claim 2, wherein the alkyl group has 1 to 5 carbon atoms. 5. A method for coloring a fiber according to claim 1, wherein the metal oxide gel is formed from tetraalkoxysilane by a sol-gel method.