JPH06104783B2 - Colored powder and manufacturing method thereof - Google Patents

Description

TECHNICAL FIELD The present invention relates to a colored powder and a method for producing the same, and in particular, it is excellent in physical strength, heat resistance, light resistance, dispersibility, and feel. The present invention relates to a colored powder suitable for use as a cosmetic base, a paint base, a resin coloring, and the like, and a method for producing the same.

(Conventional technology and its problems) Conventionally, as a method for obtaining a colored powder used in various cosmetic bases, paint bases, etc., a pigment is mixed and dispersed in a molten resin and then pulverized to obtain a powder. A known method is a melt blending method, or a dry blending method in which a resin powder and a pigment are simply mixed and stirred.

However, in the case of the melt blending method, the pigment is dispersed in the resin by a heating roll, an extruder, etc., and then mechanically pulverized by, for example, a ball mill or an air jet pulverizer to obtain a powder. Has a disadvantage in that the particle size distribution is wide and the average particle size is small or a resin having high toughness is used, the pulverization efficiency is deteriorated and it is difficult to obtain a desired product.
Therefore, when it is used as a base material for cosmetics, it has a bad feel, and in a paint base material, it cannot be expected to have excellent hiding properties, and it causes pinholes and see-through, which is an undesirable aspect. . Further, in the case of the dry blending method, since the pigment is merely electrostatically or mechanochemically attached to the resin powder, there is a problem in terms of stability over time. It has been very difficult to attach the pigment particles to the powder.

On the other hand, in recent years, various electric and electronic devices have been widely spread due to the development of electronic technology. However, in these devices, the influence of electromagnetic waves between the devices is regarded as a problem. Along with the expansion of usage, there is an increasing demand for resin to have electromagnetic wave shielding properties. At present, the metal powder is mixed with the resin to impart electromagnetic wave shielding property to the resin. However, since such a metal powder originally has a large specific gravity, it is difficult to uniformly disperse it. However, there is still room for improvement in these respects, since it is difficult to achieve the purpose of, and the cost is increased due to metal.

(Means for Solving Problems) The present invention has been made in view of the above circumstances, and has a dispersibility,
As a result of earnest research to obtain excellent colored powders that exhibit excellent effects in terms of various properties such as touch and durability and are suitable for coloring various cosmetic bases, paint bases, and resins. 、 Finally completed.

That is, the present invention comprises a colored powder in which a myriad of fine pores are formed on the surface of a powder made of a resin, and a colloid made of a metal or a metal oxide is deposited and deposited in the fine pore, and a resin. A gist of the present invention is to provide a method for producing a colored powder in which innumerable fine pores are formed on the surface of powder by etching, and a colloid consisting of metal or metal oxide is deposited and deposited in the fine pores by a reducing agent. .

As the resin powder in the present invention, the one whose average particle size is adjusted to be substantially constant is used in advance. Specific examples of the material include natural fiber, natural resin, polyethylene, polypropylene, polyvinyl chloride, polystyrene, polybutene, Thermoplastic resins such as polyamide, polyacrylic acid ester, polyacrylonitrile, polyacetal, ionomer, polyester, alkyd resin, phenol resin,
Examples of the thermosetting resin include urea resin, melamine resin, xylene resin, silicone resin and diallyl phthalate resin, which may be used alone or in admixture.

Innumerable fine pores are formed on the surface of such a resin powder, and chemical etching is mainly adopted when forming an example of the fine pores.
That is, the above resin powder is used as an etching solution for hydrochloric acid, hydrofluoric acid, borofluoric acid, ammonium acid fluoride, sulfuric acid, phosphoric acid, nitric acid, chromic acid, dichromate, permanganate, etc. It may be dipped after sufficiently considering the characteristics, but a surfactant such as a fluorine-based surfactant may be added to the etching solution in order to improve the dispersibility of the resin powder during etching. On the surface of the resin powder obtained in this manner, innumerable micropores having a pore diameter of about 1 mμ to 10 μm are formed.

The resin powder with innumerable fine pores formed on the surface is then made of stannous chloride such as stannous chloride, tartrate, formaldehyde, formic acid, glycerin, glucose, N, N-diethylglycine sodium, hypochlorous acid. One or two colloids of a metal such as nickel, cobalt, copper, silver, gold, palladium, rhodium, platinum, ruthenium or its oxide or oxide thereof are contained in the fine pores by a reducing agent such as a phosphate or a borohydride compound. It is deposited with more than one seed, and as a result,
A desired colored resin powder can be obtained. At this time, however, there is a possibility that the colloid particles may agglomerate with each other during deposition and precipitation of the colloid, which may make uniform coloring of the powder difficult. In order to prevent colloidal secondary particles as much as possible, the treatment may be carried out by using high speed stirring, a colloid mill or the like, or by applying ultrasonic waves.

The thus-obtained resin-made colored powder has an average particle size that is substantially constant, and while the characteristics of the resin can be utilized, colloids can uniformly exhibit various color tones in a state close to primary particles. It will be a very advantageous thing that can eliminate the problems of.

(Example) Hereinafter, the present invention will be described in detail based on examples.

Example 1 5 g of nylon powder having an average particle size of 5 μm (manufactured by Toray Industries, Inc.) was washed with a chlorofluorocarbon solvent, the solvent was removed by filtration, and the solution was dispersed in 20% hydrochloric acid (etching solution) at room temperature to completely remove it. High-speed stirring treatment was performed for 2 hours until the powder was dispersed to form numerous fine pores on the surface of the powder. Then filter this nylon powder,
After washing with ion-exchanged water, the solution was put into a reducing tin salt solution (stannous chloride 20 g / l, 35% hydrochloric acid) for complete dispersion and then filtered, and this nylon powder was dispersed in 100 ml of ion-exchanged water. Then, 20g / l of silver nitrate was completely dissolved in this dispersion solution with an alkaline ammonia solution, thoroughly stirred, filtered, washed and vacuum dried to deposit a colloid of metallic silver and silver oxide. Got

Example 2 5 g of the same nylon powder as in Example 1 was washed with a Freon solvent, the solvent was removed by filtration, and dispersed in a hydrochloric acid solution prepared by adding stannous fluoride 0.5 g / l to 20% hydrochloric acid at room temperature. Then, high-speed stirring treatment was carried out for 1 hour until the powder was completely dispersed, and innumerable fine pores were formed on the powder surface. Next, this nylon powder is filtered, washed with ion-exchanged water, and then a reducing tin salt solution at 30 ° C (palladium chloride 0.2 g / l, stannous chloride 10 g / l, hydrochloric acid 100
(ml / l) to completely disperse and then filter, the nylon powder was dispersed in 100 ml of deionized water. Next, in this dispersion solution, nickel chloride 10 g / l, sodium hypophosphite 4 g / l
l, 400 ml of sodium hydroxyacetate 20 g / l solution was added, stirred well, the liquid temperature was set to 60 ° C, and ultrasonic waves were applied.
Let stand for 10 minutes. Then, the nylon powder was filtered, washed, and vacuum dried to obtain a black nylon powder in which metallic nickel colloid was deposited and deposited.

Example 3 5 g of polystyrene powder having an average particle size of 15 μm (Fine Pearl, manufactured by Sumitomo Chemical Co., Ltd.) was washed with a chlorofluorocarbon solvent,
After removing the solvent by filtration, it was dispersed in a 42% hydrofluoric acid solution at 35 to 40 ° C., and stirring treatment was carried out for 1 hour until it was completely dispersed to form numerous fine pores on the powder surface. Then, this polystyrene powder is filtered, washed with ion-exchanged water, and then placed in a reducing tin salt solution (palladium chloride 0.2 g / l, stannous chloride 10 g / l, hydrochloric acid 100 ml / l) for complete dispersion. Then, this polystyrene powder was dispersed in 100 ml of deionized water. Next, add 30 g / l of copper sulfate, 7 g / l of nickel chloride, 25 g / l of hydrazine sulfate, 90 g / l of potassium sodium tartrate, 25 g / l of sodium hydroxide, 400 ml of sodium carbonate 7 g / l solution to this dispersion solution, and stir well. Then, the liquid temperature was set to 40 to 50 ° C and the mixture was left for 5 minutes while applying ultrasonic waves. Thereafter, the polystyrene powder was filtered, washed, and vacuum dried to obtain a black polystyrene powder in which metallic nickel colloid was deposited and deposited.

(Effects of the Invention) The specific gravities of the colored resin powders obtained in Examples 1 to 3 are 1.10, 1.295, and 1.305, respectively, which are remarkably lighter than the conventional metal powders, and have a number of characteristics unique to the resin. It has been confirmed that the characteristics can be fully exhibited, and that the coloring state is stable over time and the dispersibility is several times superior, which is extremely advantageous in terms of production efficiency and cost.

The colored powder according to the present invention can be widely used as, for example, a cosmetic base, a paint base, a catalyst or an additive to an electromagnetic wave shielding resin molded product, and can exert various practical effects. It is also useful as a composite material.

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Claims (2)

[Claims] 1. A colored powder obtained by forming innumerable fine pores on the surface of a powder made of a resin and depositing a colloid of a metal or a metal oxide in the fine pores. 2. A method for producing a colored powder, which comprises forming innumerable fine pores on the surface of a powder made of a resin by etching and depositing a colloid made of a metal or a metal oxide in the fine pores by a reducing agent. Method.