Black ultrafine magnetite particles and process for preparing th

Chemistry of inorganic compounds – Oxygen or compound thereof – Metal containing

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Details

106456, 106460, 252 6256, 423632, 428403, 428404, 428405, 428406, 428407, 4301066, C09C 122, C01G 4908, C01G 4902, B32B 516

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active

060834765

DESCRIPTION:

BRIEF SUMMARY
TECHNICAL FIELD

This invention relates to black ultrafine magnetite particles mainly for use as the starting powder for an electrostatic copying magnetic toner, and a black pigment powder for paints, and a process for the production of the magnetite particles.


BACKGROUND ART

In recent years, the spread of electrostatic copiers or laser beam printers employing electrophotographic technologies has been remarkable. In harmony with this trend, the properties of printing graphics or photographs with high reproducibility have been desired. With the concurrent progress of techniques for the meticulous creation of latent images, there has been a demand for the accurate printing of thin lines by development. To fulfill these requirements, the particle sizes of magnetic toners have been made smaller. Magnetite added as a magnetic black pigment should also be formed into fine particles.
Magnetite in current use has a particle size of 0.1 to 0.3 .mu.m. Thus, the need for ultrafine magnetite with a particle size of 0.1 .mu.m or less is growing. However, 0.1 .mu.m or less ultrafine magnetite particles with a black tint sufficient for use as a black pigment is nonexistent as yet.
Fine magnetite particles for use as a magnetic black pigment to be incorporated into a magnetic toner are generally those obtained by adding an alkali to ferrous sulfate to obtain a suspension of Fe(OH).sub.2, and air oxidizing the suspension at a suitable temperature. Various attempts to obtain fine particles 0.1 .mu.m or less in diameter by this method have been made based on studies of conditions, such as pH, rate of oxidation and reaction temperature. However, it is difficult to make the particle size smaller than 0.1 .mu.m while retaining a black color.
It is well known to add an alkali to a mixed aqueous solution of a ferrous salt and a ferric salt to cause coprecipitation, and age the coprecipitates at 50 to 100.degree. C., thereby forming ultrafine magnetite with a particle size of 0.01 .mu.m or less.
The so obtained ultrafine particles are so fine that when they are taken out into the air, they are oxidized, making their use for a magnetic toner or the like difficult. Their use is restricted to applications excluded from the air, such as magnetic fluid.
As a method for overcoming the drawbacks of the foregoing two representative methods, Japanese Patent Publication No. 33655/90 discloses a process for producing ultrafine magnetite with a particle size of about 0.01 to 0.025 .mu.m.
The technique disclosed there makes the content of a ferrous salt higher than in the composition of magnetite when obtaining ultrafine magnetite by coprecipitation, to cause ferrous hydroxide to remain after coprecipitation, and air oxidizes the ferrous hydroxide to grow air oxidation-induced magnetite on the coprecipitated ultrafine magnetite particles, thereby somewhat enlarging the ultrafine magnetite particles for stabilization.
Even this method, however, poses the problem that when the particles are taken out into the air, they become reddish and cannot serve as a magnetic black pigment.
The present situation is, therefore, that there is no ultrafine magnetite 0.1 .mu.m or less in particle size which is black enough to be used as a magentic black pigment.
The object of the present invention is to provide black ultrafine magnetite particles for a black magnetic toner that earlier technologies were unable to produce, and a process for producing the black ultrafine magnetite particles.


DISCLOSURE OF THE INVENTION

The chemical composition of magnetite is expressed as FeO.Fe.sub.2 O.sub.3, and originally its FeO content is 31%. As its specific surface area increases, magnetite becomes more oxidizable. Actually, when magnetite is withdrawn into the air, its FeO content is difficult to maintain at 31%.
Fine magnetite particles in current use as a black magnetic pigment have a particle size of 0.1 to 0.3 .mu.m and a BET specific surface area to 2 to 10 m.sup.2 /g. Its FeO content is about 20 to 26% rather than 31%.
Increasing FeO content gives a reddish co

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Kim et al. Preparation and Characteristics of Magnetite Ferrofluid. Journal of the Korean Ceramic Society. vol. 27, No. 1, pp. 13-22, 1990.
Jung et al. Adsorption, Precipitation, and Electronkinetic Processes in the Iron Oxide (Goethite)-Oleic Acid-Oleate System. Journal of Colloidal and Interface Science, vol. 118, No. 2, 1987.

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