JP3144841B2 - Fiber coloring method - Google Patents

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 a flameproofing property or a flame retardant property to a fiber, and further capable of easily coloring a glass fiber or the like, which has been conventionally difficult to color.

[0002]

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

In order to solve such a problem, conventionally, inorganic fibers such as glass fibers and carbon fibers have been used alone or in combination with organic fibers, or heat-resistant synthetic fibers have been used. Etc. have been proposed. However, in general, interior materials and furniture, such as houses and vehicles, are often required to be colored in order to give them an aesthetic appearance or enhance product value. , Because coloring is difficult,
Conventionally, it is hardly 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, can provide a fiber with a flameproofing property or a flameproofing property. It is another object of the present invention to provide a fiber coloring method which can easily color glass fiber or the like which has been difficult to color.

[0005]

The method for coloring fibers according to the present invention is characterized in that a metal oxide gel containing a dye is formed on the surface of the fibers. As a method for forming a metal oxide gel, a sol-gel method has been well known. In this method, a metal organic or inorganic compound is converted into a solution, the metal compound is hydrolyzed in the solution, the sol is converted into a gel through a polycondensation reaction, and the sol is dried and solidified by heat treatment to form a solid metal oxide. To produce a product gel. 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, whereby a thin film of a solid metal oxide gel can be formed on the surface of the fiber. The thin film of the metal oxide gel formed in this manner has flame resistance and flame resistance equal to or higher than that of glass fiber. In addition, it is also known that the above-mentioned porous gel generates an amorphous glass by heating and firing it at a high temperature.

In the method for coloring a fiber according to the present invention, in the sol-gel method, a pigment is dispersed or dissolved in a solution of the metal compound to prepare a coating liquid, and the coating liquid is applied to the fiber. The fiber is colored by heat treatment to form a thin film of the colored metal oxide gel containing the above-mentioned dye on the fiber.

In the method of the present invention, the metal compound may be an organic metal compound such as metal alkoxide, metal acetylacetonate, metal carboxylate, etc.
Inorganic metal compounds such as nitrates, oxychlorides and chlorides can be mentioned. However, in the method of the present invention,
Among these, organometallic compounds are preferred because they are highly reactive and easily form a metal oxide gel,
In particular, metal alkoxides are preferably used.

The metal alkoxide has 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, in particular, those in which the metal element is silicon, that is, tetraalkoxysilane, are preferably used. Alkoxides such as aluminum, iron, cobalt, nickel, and lithium can also be used. Further, the metal alkoxide may be a mixture. R is preferably an alkyl group having 1 to 5 carbon atoms, for example, an isopropyl group or n-
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. Usually, an alcohol is used. 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 gold-containing dye, an oil-soluble dye, etc. can be used. Examples thereof include condensed pigments such as linone, quinophthalone, and quinacridone; organic pigments such as phthalocyanine pigments; and inorganic pigments such as titanium white, red iron, graphite, cobalt blue, and carbon black. Such a dye depends on the type of the dye to be used and the required coloring concentration, but is usually 0.01 to 0.01 to the metal compound.
It is 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-described dye in the solution after the metal. Such a dispersant is appropriately selected in consideration of a dye or a metal compound to be used, an organic solvent, and the like. Generally, a dispersant having an adsorptive power to a dye and being compatible with a metal compound solution is preferably used. . Such dispersants include, for example, 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 phosphate esters. And a resin-based dispersant such as a polyester-based surfactant and a polyester resin. These dispersants are generally used in the range of 5 to 100% by weight based on the dye. Normally,
The dye is dispersed in the solvent using the dispersant, and the resulting dispersion is mixed with the metal compound solution.

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

In order to apply such a coating liquid to fibers, a method such as a dip coating is usually used. That is, a uniform coating can be formed on the surface of the fiber by immersing the fiber in the above-mentioned coating solution and then lifting the fiber. The immersion temperature of the fiber in the coating liquid may be room temperature. In this manner, according to the method of the present invention, the fiber is coated with the coating liquid and heat-treated to form a gel via the sol by the polycondensation reaction of the metal compound as described above, This gel is fixed as a metal oxide thin film on the fiber to form a colored coating,
Thus, the fibers are colored.

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

In the method of the present invention, the heat treatment temperature of the gel thin film is lower than the decomposition temperature of the dye and lower than the heat resistance temperature of the fiber. Often 300 ° C
The following are preferred. As described above, when the heat treatment is performed at a temperature of 300 ° C. or less, most of the dyes can be used regardless of whether they are organic or inorganic, so that the selection range of the hue is expanded, which is advantageous in coloring the fiber. is there. However, according to the method of the present invention, a gel thin film of a metal oxide having practical film strength at a temperature near 100 ° C. can be obtained in practice. However, depending on the pigments and fibers used, 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 the fiber is colored by forming a thin film made of a gel of a metal oxide containing a dye on the fiber, the degree of freedom of color selection is large, and the fiber can be provided with a flameproofing property or a flame retardant property. In addition, glass fibers and the like, which have conventionally been difficult to color, can be easily colored.

Furthermore, various functions can be imparted to the fiber by utilizing the method of the present invention. For example, a material such as a functional dye can be introduced into the surface of a fiber and applied to an electronic material or the like. If a metal oxide gel such as lithium is used, an antistatic effect can be imparted to the fiber.

[0018]

EXAMPLES The present invention will be described below with reference to examples.
The present invention is not limited by these examples. Example 1 2.5 parts by weight of a pigment (permanent carmine FBB-02), 0.5 parts by weight of a dispersant (Gohselan L-301 (polyvinyl alcohol)) and 97 parts by weight of a solvent (isopropyl alcohol) were mixed, and a dispersing machine was used. 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-mentioned pigment dispersion and 19.0 ml of n-butanol were mixed, and mixed at room temperature. After stirring for a time, a coating solution was prepared. A glass fiber woven fabric is immersed in the coating solution,
The coating liquid was applied on the glass fiber by pulling up at a speed of mm / sec, and this was heat-treated in an oven at 100 ° C. for 15 minutes to obtain a colored glass fiber. Example 2 6.0 g of tetraethoxysilane, 6.0 ml of ethanol, 9.0 of water.
6 g, concentrated hydrochloric acid 0.75 ml, pigment “Supilon Blue 3BH conc.
A mixture comprising 2.0 ml of "liquid" and 25.0 ml of n-butanol was prepared and stirred at room temperature for 2 hours to prepare a coating solution.

A glass fiber woven fabric is immersed in the coating liquid, and then pulled up at a speed of 3 mm / sec. To apply the coating liquid on the glass fiber, which is placed in an oven for 1 hour.
Heat treatment was performed at 00 ° C. for 15 minutes to obtain a colored glass fiber. Example 3 Aramid (aromatic polyamide) fiber woven fabric (Technola manufactured by Teijin Limited) was immersed in the coating solution prepared in Example 1, and then pulled up at a speed of 3 mm / sec.
Apply the coating liquid on the fiber, and in an oven,
Heat treatment was performed at 100 ° C. for 15 minutes to obtain a colored aramid fiber. Example 4 Aramid (aromatic polyamide) fiber woven fabric (Technola manufactured by Teijin Limited) was immersed in the coating solution prepared in Example 2, and then pulled up at a speed of 3 mm / sec.
Apply the coating liquid on the fiber, and in an oven,
Heat treatment was performed at 100 ° C. for 15 minutes to obtain a colored aramid fiber. Example 5 A flame retardancy test of the colored aramid fiber prepared in Example 3 was performed. As a comparative example, an uncolored aramid fiber before being colored according to the present invention was subjected to a flame retardancy test.

Continuation of the front page (72) Inventor Kazuo Sakai 2-43, Higashi-Kawawa-shi, Hyogo Pref. JP-A-2-26474 (JP, A) JP-A-63-6164 (JP, A) JP-A-50-17417 (JP, A) JP-A-54-47798 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) D06M 11/00-13/535 D06P 1/673

Claims (5)

(57) [Claims] (1) A glass fiber or an aromatic polyamide fiber is attached.
A method of coloring, wherein a dye and tetra
Sol-gel from coating solution containing alkoxysilane
A method for coloring a fiber, comprising forming a silicon oxide gel by a method. 2. The method for coloring fibers according to claim 1, wherein the alkoxy group has 1 to 5 carbon atoms. 3. The method according to claim 1, wherein the pigment is a pigment.
The method for coloring fibers according to claim 1. 4. The coating liquid contains a dispersant.
The method for coloring a fiber according to claim 1, wherein 5. The method according to claim 1, wherein the dispersant is a polyvinyl alcohol resin,
Vinyl butyral resin, acrylic resin, ethyl cellulose
, Unsaturated polycarboxylic acid, phosphoric ester based surfactants
Selected from the group consisting of the agent and polyester resin
5. The method for coloring a fiber according to claim 4, wherein the fiber is colored.