JPH06144840A - Magnetite particle powder and it production - Google Patents
Magnetite particle powder and it productionInfo
- Publication number
- JPH06144840A JPH06144840A JP4301298A JP30129892A JPH06144840A JP H06144840 A JPH06144840 A JP H06144840A JP 4301298 A JP4301298 A JP 4301298A JP 30129892 A JP30129892 A JP 30129892A JP H06144840 A JPH06144840 A JP H06144840A
- Authority
- JP
- Japan
- Prior art keywords
- magnetite
- particle powder
- toner
- particle
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002245 particle Substances 0.000 title claims abstract description 66
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000011777 magnesium Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 239000003518 caustics Substances 0.000 claims abstract description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 6
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 5
- 230000002378 acidificating effect Effects 0.000 claims abstract description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 abstract 1
- 150000008041 alkali metal carbonates Chemical class 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000395 magnesium oxide Substances 0.000 abstract 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000007789 gas Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 9
- 229960002089 ferrous chloride Drugs 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Developing Agents For Electrophotography (AREA)
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、電子写真法、静電記録
法、静電複写機用等のトナーに使用されるマグネタイト
粒子粉末及びその製造方法に関するものであり、特に鮮
明な複写画像が得られる小粒径トナー用マグネタイト粒
子粉末及びその製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a magnetite particle powder used in toners for electrophotography, electrostatic recording, electrostatic copying machines and the like, and a method for producing the same. The present invention relates to a magnetite particle powder for a small particle size toner and a method for producing the same.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】従来よ
り、電子写真法や静電記録法などに使用されているトナ
ー用の磁性材料としては、マグネタイトやフェライト等
の磁性酸化物粒子、又は磁性金属粒子が使用されてい
る。磁性トナーは一般的に、主原料の磁性材料にバイン
ダー樹脂の他に、必要に応じて染料、顔料、導電性材料
等を添加し、加熱、混練、冷却し次いで粉砕して分級を
して製造されている。このトナーの径は一般的に１０μ
ｍ前後である。一方、近年トナー粒径を微細化すること
で、画質が向上し特に解像度が良くなることが、各種の
分野で報告されている。この小粒径トナーに使用するた
めのマグネタイトは微細品で樹脂中への分散性が良く、
粒度分布幅の狭いものが良いとされているが、従来のマ
グネタイト粒子粉末は、未だ充分な特性を満たしていな
いのが現状である。2. Description of the Related Art Conventionally, as magnetic materials for toners used in electrophotography and electrostatic recording, magnetic oxide particles such as magnetite and ferrite, or magnetic materials have been used. Metal particles are used. Magnetic toners are generally manufactured by adding a dye, a pigment, a conductive material, etc. to the magnetic material of the main raw material, if necessary, in addition to the binder resin, heating, kneading, cooling, crushing and classifying. Has been done. The diameter of this toner is generally 10μ.
It is around m. On the other hand, in recent years, it has been reported in various fields that the image quality is improved and the resolution is particularly improved by reducing the toner particle size. The magnetite used for this small particle size toner is a fine product and has good dispersibility in the resin.
It is said that a powder having a narrow particle size distribution width is preferable, but the conventional magnetite particle powder does not yet have sufficient characteristics at present.
【０００３】本発明の目的は、上記欠点を解消し、特に
解像度に優れた小粒径トナーに必要とされる特性を十分
に有したマグネタイト粒子粉末及びその製造方法を提供
することにある。本発明の目的はまた、解像度に優れた
磁性トナーを提供することにある。An object of the present invention is to solve the above-mentioned drawbacks and to provide a magnetite particle powder having a sufficient characteristic required for a small particle diameter toner having excellent resolution, and a method for producing the same. Another object of the present invention is to provide a magnetic toner having excellent resolution.
【０００４】[0004]
【課題を解決するための手段】本発明は、Ｍｇ（マグネ
シウム）の酸化物が、Ｍｇ換算でＦｅに対し０．１〜
５．０重量％含有されており、且つ平均粒子径が０．１
０〜０．２５μｍであり、該粒子形状が実質的に六面体
であり、該六面体の各稜線が面状になっていることを特
徴とするマグネタイト粒子粉末、及び第一鉄塩水溶液
に、マグネシウム化合物を添加し、苛性アルカリ又は／
及び炭酸アルカリの存在下で、且つ弱酸性の条件下に酸
化性ガスを通気してマグネタイトを生成させることを特
徴とするマグネタイト粒子粉末の製造方法を提供するこ
とにより上記目的を達成したものである。本発明はま
た、上記マグネタイト粒子粉末を含有する磁性トナーを
提供することにより上記目的を達成したものである。According to the present invention, an oxide of Mg (magnesium) is 0.1 to Fe in terms of Mg.
It is contained in an amount of 5.0% by weight and has an average particle size of 0.1.
0 to 0.25 μm, the particle shape is substantially hexahedron, and each ridgeline of the hexahedron is planar, and a magnesium compound in a ferrous salt aqueous solution and a ferrous salt aqueous solution. Add caustic or
And, in the presence of an alkali carbonate, and by passing an oxidizing gas under weakly acidic conditions to produce magnetite, to provide a method for producing magnetite particles powder, which achieves the above object . The present invention also achieves the above object by providing a magnetic toner containing the magnetite particle powder.
【０００５】以下、本発明に係るマグネタイト粒子粉末
及びその製造方法、更にはそれを用いた磁性トナーにつ
いて詳説する。本発明に係るマグネタイト粒子粉末は、
その成分中にＭｇの酸化物がＭｇ換算でＦｅに対して
０．１〜５．０重量％、好ましくは０．２〜１．５重量
％であることが望ましい。また、マグネタイト粒子の平
均粒子径は０．１０〜０．２５と極めて狭い範囲にあ
り、その粒度分布はシャープであることが好ましい。マ
グネタイト粒子粉末の比表面積値（窒素法）は２．０〜
２０ｍ2 ／ｇで、見掛け密度値は０．２〜０．９ｇ／ｃ
ｍ3 であることが好ましい。更に、トナーに用いる場合
はマグネタイト粒子の黒味の着色力が顔料試験法による
測定値で＋９０〜＋１４０であることが望ましい。The magnetite particle powder according to the present invention, the method for producing the same, and the magnetic toner using the same will be described in detail below. Magnetite particle powder according to the present invention,
It is desirable that the content of Mg oxide in the component is 0.1 to 5.0% by weight, preferably 0.2 to 1.5% by weight, based on Fe. Further, the average particle size of the magnetite particles is in the extremely narrow range of 0.10 to 0.25, and the particle size distribution is preferably sharp. Specific surface area value (nitrogen method) of magnetite particles powder is 2.0-
Apparent density value of 0.2 to 0.9 g / c at 20 m 2 / g
It is preferably m 3 . Further, when it is used for a toner, it is desirable that the black tint strength of the magnetite particles is +90 to +140 as measured by the pigment test method.
【０００６】本発明に係るマグネタイト粒子形状は、実
質的に六面体であり、該六面体の各稜線が面状になって
いる。このような粒子形状は、従来のマグネタイト粒子
形状は不定形、球形状、八面体形状等と相違して、微細
であるにもかかわらず、赤褐色にならず黒味が保持さ
れ、比表面積が大きくても、酸化安定性に優れたものと
なる。従って、上記マグネタイト粒子粉末は、小粒径磁
性トナー及びその他の磁性粉として用いたとき、その製
品の性能を十分に高める。The shape of the magnetite particles according to the present invention is substantially a hexahedron, and each ridge of the hexahedron is planar. Such a particle shape is different from the conventional magnetite particle shape such as an amorphous shape, a spherical shape, an octahedron shape, and the like, although it is fine, it does not become reddish brown but retains blackness and has a large specific surface area. However, it has excellent oxidative stability. Therefore, when the magnetite particle powder is used as a small particle size magnetic toner or other magnetic powder, the performance of the product is sufficiently enhanced.
【０００７】次に本発明に係るマグネタイト粒子粉末の
製造方法について説明する。マグネタイトの反応条件
は、湿式の反応槽（攪拌式、循環式、気泡塔）内をＮ 2
ガスで置換しながら、塩化第一鉄に対し苛性アルカリ及
び／又は炭酸アルカリを当量程度加え、反応温度は７０
℃以上に保ち、その後Ｎ2 を酸化性ガスに切り替えて、
弱酸性下の条件で酸化反応を行うことでマグネタイトを
得ている。Next, the magnetite particle powder according to the present invention is prepared.
The manufacturing method will be described. Reaction conditions of magnetite
Is N in the wet reaction tank (stirring type, circulation type, bubble column). 2
While replacing the gas with ferrous chloride, caustic alkali
And / or alkali carbonate is added in an equivalent amount, and the reaction temperature is 70
Keep above ℃, then N2Switch to oxidizing gas,
Magnetite can be obtained by performing an oxidation reaction under conditions of weak acidity.
It has gained.
【０００８】本発明を更に詳しく説明すると、攪拌式反
応槽をＮ2 ガスで置換しながら、１〜２ｍｏｌ（第一鉄
塩１ｍｏｌ程度に対して。）の苛性アルカリ及び／又は
炭酸アルカリを加える。その反応温度を５０〜１００
℃、好ましくは７５〜９５℃に保ちながら、別に用意し
たＭｇの化合物をＦｅに対してＭｇが０．１０〜５．０
重量％で、好ましくは０．２〜１．５重量％となる量
を、塩化第一鉄水溶液と共に加える。その後Ｎ2 ガスを
空気等の酸化性ガスに切り替え、酸化反応を完結させ
る。従って、酸化反応開始前の含水鉄水溶液の中に、マ
グネシウム化合物を加えることにより、生成物はマグネ
シウムを含むスピネル構造を有するマグネタイトとな
る。その平均粒径は０．１０〜０．２５μｍで、しかも
粒度分布がシャープである。To explain the present invention in more detail, while substituting the stirring reaction tank with N 2 gas, 1 to 2 mol (based on about 1 mol of ferrous salt) of caustic alkali and / or alkali carbonate is added. The reaction temperature is 50-100
While maintaining at ℃, preferably 75 ~ 95 ℃, Mg compound prepared separately Mg 0.10 ~ 5.0
An amount of 0.2% to 1.5% by weight, preferably 0.2 to 1.5% by weight, is added together with the aqueous ferrous chloride solution. After that, the N 2 gas is switched to an oxidizing gas such as air to complete the oxidation reaction. Therefore, the product becomes magnetite having a spinel structure containing magnesium by adding the magnesium compound to the aqueous iron-containing solution before the start of the oxidation reaction. The average particle size is 0.10 to 0.25 μm, and the particle size distribution is sharp.
【０００９】上記反応に於いて、マグネタイト粒子サイ
ズは反応条件、例えば、酸化性ガスの流量変化や、塩化
第一鉄塩の濃度等でコントロールをすることができる。
酸化速度が速ければ粒子は微細となり、遅ければ粒子は
大きくなる。上記酸化反応のｐＨ値については、５以上
７未満であると目的の粒子形状となるが、それ以外は目
的とする粒子が得ることが困難になる。本発明に使用す
る苛性アルカリ、炭酸アルカリの具体例は、苛性ソーダ
や炭酸ソーダで、第一鉄塩は、塩化第一鉄が一般的であ
り、マグネシウム化合物としては、塩基性炭酸マグネシ
ウム、硝酸マグネシウム、塩化マグネシウム等を挙げる
ことができるが、これらマグネシウムの無機塩は一種単
独で使用しても良いし複数種を併用しても良い。In the above reaction, the magnetite particle size can be controlled by the reaction conditions such as the change of the flow rate of the oxidizing gas and the concentration of the ferrous chloride salt.
The faster the oxidation rate, the finer the particles, and the slower the rate, the larger the particles. Regarding the pH value of the above-mentioned oxidation reaction, if the pH value is 5 or more and less than 7, the desired particle shape is obtained, but otherwise it becomes difficult to obtain the desired particles. Specific examples of the caustic alkali and alkali carbonate used in the present invention are caustic soda and sodium carbonate, the ferrous salt is generally ferrous chloride, and as the magnesium compound, basic magnesium carbonate, magnesium nitrate, Magnesium chloride and the like can be mentioned, but these inorganic salts of magnesium may be used alone or in combination of two or more.
【００１０】上記条件で生成したマグネタイトの平均粒
径値は、ＳＥＭ写真による粒子実測２００個の結果、
０．１０〜０．２５μｍであり、窒素法によるい比表面
積値は２．０〜２０ｍ2 ／ｇであり、ホソカワミクロン
（株）製のパウダーテスターによる見掛け密度の測定値
は０．２〜０．９ｇ／cm3 で、マグネタイト中のＭｇ含
有量は、Ｍｇ換算でＦｅに対し０．１〜５．０重量％
で、黒味の着色力は顔料試験法に依る測定値で＋９０〜
＋１４０であった。The average particle size value of the magnetite produced under the above conditions is the result of 200 particles actually measured by the SEM photograph.
0.10 to 0.25 μm, the specific surface area value by the nitrogen method is 2.0 to 20 m 2 / g, and the measured value of the apparent density by the powder tester manufactured by Hosokawa Micron Co., Ltd. is 0.2 to 0. At 9 g / cm 3 , the Mg content in magnetite is 0.1 to 5.0 wt% with respect to Fe in terms of Mg.
Then, the tinting strength of blackness is +90 to a measured value according to the pigment test method.
It was +140.
【００１１】次に本発明に係るマグネタイト粒子粉末を
用いた磁性トナーについて説明する。常法により２本加
圧式熱ローラーで、上記マグネタイト粒子粉末及び樹脂
の溶融混練を行い、ジェットミル式粉砕機及び分級機
で、平均粒径１０μｍを有する磁性トナーを得た。次に
樹脂中への分散性の評価を行った。即ち、市販の一成分
系複写の現像剤ボックスを改良し、これを用いてブラシ
飛散法で、トナーの磁気分布を測定した結果、樹脂中へ
のマグネタイトの分散性は良好であった。ここで、ブラ
シ飛散法とはマグローラーの回転数を可変式に改良し、
仕込み量を一定化させた場合、回転数を速くすること
で、磁力の弱いトナー（磁性材含有量少ない）は遠心力
で飛ばされる。飛ばされた量とそのトナーの磁気測定を
することでトナー中のマグネタイトの分散性を知ること
ができる。何故ならば、樹脂中へのマグネタイトの分散
が悪いと、個々のトナー磁力が異なり、磁力の弱いもの
は速く飛ばされるからである。Next, a magnetic toner using the magnetite particle powder according to the present invention will be described. The magnetite particle powder and the resin were melt-kneaded by a two-pressure heat roller by a conventional method, and a magnetic toner having an average particle diameter of 10 μm was obtained by a jet mill crusher and a classifier. Next, the dispersibility in the resin was evaluated. That is, a commercially available one-component copying developer box was improved, and the magnetic distribution of the toner was measured by the brush scattering method using the developer box. As a result, the dispersibility of magnetite in the resin was good. Here, with the brush scattering method, the number of revolutions of the mag roller is modified to be variable,
When the charged amount is made constant, the toner having a weak magnetic force (the magnetic material content is small) is blown by the centrifugal force by increasing the rotation speed. The dispersibility of magnetite in the toner can be known by measuring the amount of the ejected toner and the magnetic measurement of the toner. This is because if the magnetite is poorly dispersed in the resin, the magnetic force of each toner is different, and a toner having a weak magnetic force is quickly ejected.
【００１２】その結果、本発明のマグネタイト粒子粉末
は、微細品ながら粒度分布がシャープで、見掛け密度が
大きく、分散性がよいこから、小粒径トナーに必要な条
件である、樹脂中への馴染みが良く磁気特性が均一とな
り、製造されたトナー１個当たりの、マグネタイト含有
量が平均化するので、コピー画質を向上させ解像度を良
くさせ、カブリやトナー飛散もなく鮮明な複写画像が得
られる。更に、本発明のマグネタイトは従来の不定形、
球状、多面体、八面体等のマグネタイトと異なり、微細
品ながら赤褐色にならず黒味を保ち、比表面積が大きく
ても、酸化安定性に優れている。As a result, the magnetite particle powder of the present invention is a fine product but has a sharp particle size distribution, a large apparent density, and good dispersibility. Since the magnetic properties are good and the magnetic properties are uniform, and the magnetite content per manufactured toner is averaged, the copy image quality is improved and the resolution is improved, and a clear copy image without fog or toner scattering is obtained. Furthermore, the magnetite of the present invention has a conventional amorphous shape,
Unlike magnetite such as spheres, polyhedra, and octahedra, it is a fine product that does not turn reddish brown but retains a black tint and has excellent oxidation stability even with a large specific surface area.
【００１３】[0013]
【実施例】以下、本発明の実施例を比較例と比較しなが
ら説明する。尚、本発明は本実施例に限るものではな
い。 実施例１ ガス吹き込み管を有する攪拌槽にＮ2 ガス（３リットル
／ｍｉｎ）を通気しながら、苛性ソーダ（１．１２０k
g、２８．０ｍｏｌ）を水（３０リットル）に溶解し攪
拌槽に加え、攪拌させながら９０℃まで昇温させ、所定
温度になったら別に用意した塩化第一鉄水溶液（４．１
４リットル、１４ｍｏｌ）と塩化マグネシウム（０．０
５６kg、０．２８ｍｏｌ）と水（５．８４リットル）と
の混合液を攪拌槽に添加し、窒素置換を続けながら、３
０分間攪拌混合する。その後、酸化性ガス（空気）に切
り替え（１リットル／ｍｉｎ）て反応、この時、苛性ソ
ーダ水溶液（１ｍｏｌ／リットル）で、ｐＨ値を５以上
７未満に保つ様にコントロールして、酸化反応を完結さ
せた。この様にしてできたマグネタイトは、常法により
濾過、水洗、乾燥、粉砕して得られた物は、図１に示す
ような六面体を基本とし、六面体の各稜線が面状になっ
ているマグネタイトであった。EXAMPLES Examples of the present invention will be described below in comparison with comparative examples. The present invention is not limited to this embodiment. Example 1 While agitating a tank having a gas blowing pipe with N 2 gas (3 l / min), caustic soda (1.120 k
g, 28.0 mol) was dissolved in water (30 liters), added to a stirring tank, heated to 90 ° C. with stirring, and when a predetermined temperature was reached, a separately prepared ferrous chloride aqueous solution (4.1
4 liters, 14 mol) and magnesium chloride (0.0
56 kg, 0.28 mol) and water (5.84 liters) were added to the stirring tank, and while continuing the nitrogen replacement, 3
Stir mix for 0 minutes. Then, switch to oxidizing gas (air) (1 liter / min) to react, and at this time, control the pH value with a caustic soda aqueous solution (1 mol / liter) to keep it at 5 or more and less than 7 to complete the oxidation reaction. Let The magnetite thus obtained is obtained by filtering, washing with water, drying and crushing by a conventional method. The magnetite is based on a hexahedron as shown in Fig. 1, and each ridge of the hexahedron is a plane. Met.
【００１４】実施例２〜５ 本発明の反応生成反応条件における、反応温度とガスと
量を同じにして、塩化第一鉄水溶液の量や塩化マグネシ
ウムの添加量及び、苛性ソーダの量を種々変化させた以
外は、実施例１と同様にしてマグネタイト粒子を生成さ
せた。更に、実施例６で、苛性ソーダを炭酸ソーダに代
えて試験をした。尚、反応組成条件は表１に示した。Examples 2 to 5 Under the reaction formation reaction conditions of the present invention, the amount of ferrous chloride aqueous solution, the amount of magnesium chloride added, and the amount of caustic soda were variously changed under the same reaction temperature and gas amount. Magnetite particles were produced in the same manner as in Example 1 except for the above. Further, in Example 6, a test was conducted by replacing sodium hydroxide with sodium carbonate. The reaction composition conditions are shown in Table 1.
【００１５】比較例１ ガス吹き込み管を有する攪拌槽にＮ2 ガス（３リットル
／ｍｉｎ）を通気しながら、苛性ソーダ（１．１２０k
g、２８．０ｍｏｌ）を水（３０リットル）に溶解し攪
拌槽に加え、攪拌させながら９０℃まで昇温させ、所定
温度になったら別に用意した塩化第一鉄水溶液（４．１
４リットル、１４ｍｏｌ）と水（５．８４リットル）の
混合液を攪拌槽に添加し、窒素置換を続けながら、３０
分間攪拌混合する。その後、酸化性ガス（空気）に切り
替え（１リットル／ｍｉｎ）て反応を開始した。この様
にして得られたマグネタイトは、常法により濾過、水
洗、乾燥、粉砕した結果、粒子形状は図２の如く、通常
の八面体で粒子形状は不揃いであった。COMPARATIVE EXAMPLE 1 A caustic soda (1.120 k) was passed through an agitating tank having a gas blowing pipe while passing N 2 gas (3 liter / min).
g, 28.0 mol) was dissolved in water (30 liters), added to a stirring tank, heated to 90 ° C. with stirring, and when a predetermined temperature was reached, a separately prepared ferrous chloride aqueous solution (4.1
4 liters, 14 mol) and water (5.84 liters) were added to the stirring tank, and while continuing the nitrogen substitution, 30
Stir mix for minutes. Then, the reaction was started by switching to oxidizing gas (air) (1 liter / min). The magnetite thus obtained was filtered, washed with water, dried and pulverized by a conventional method, and as a result, the particle shape was an ordinary octahedron and the particle shape was irregular as shown in FIG.
【００１６】比較例２ 比較例１の反応条件で塩化第一鉄水溶液の中に、塩化マ
グネシウム（０．０５６kg、０．２８ｍｏｌ）を混合さ
せて、反応させた。マグネタイトの粒子形状は八面体で
あった。 比較例３ 比較例１の反応条件で塩化第一鉄水溶液の中に、塩化マ
グネシウム（０．１１４kg、０．５６ｍｏｌ）を混合さ
せて、反応させた。マグネタイトの粒子形状は八面体で
不揃いの粒子であった。尚、比較例と実施例の主要製造
条件と、生成マグネタイトの諸特性を〔表１〕と〔表
２〕に示す。Comparative Example 2 Under the reaction conditions of Comparative Example 1, magnesium chloride (0.056 kg, 0.28 mol) was mixed in the ferrous chloride aqueous solution and reacted. The particle shape of magnetite was octahedron. Comparative Example 3 Under the reaction conditions of Comparative Example 1, magnesium chloride (0.114 kg, 0.56 mol) was mixed in the ferrous chloride aqueous solution and reacted. The particle shape of magnetite was octahedral and irregular. The main manufacturing conditions of Comparative Examples and Examples and various characteristics of the produced magnetite are shown in [Table 1] and [Table 2].
【００１７】[0017]
【表１】 [Table 1]
【００１８】[0018]
【表２】 [Table 2]
【００１９】[0019]
【発明の効果】本発明に係るマグネタイト粒子粉末は、
解像度に優れた小粒径トナーに必要とされる特性を十分
に有する。また、本発明に係る上記マグネタイト粒子粉
末を用いた磁性トナーは、解像度に優れた磁性トナーと
することができる。The magnetite particle powder according to the present invention is
It has sufficient characteristics required for a small particle size toner having excellent resolution. Further, the magnetic toner using the magnetite particle powder according to the present invention can be a magnetic toner having excellent resolution.
【図１】本発明に係るマグネタイト粒子粉末の顕微鏡写
真により粒子構造を示す図である。FIG. 1 is a view showing a particle structure of a magnetite particle powder according to the present invention by a micrograph.
【図２】従来のマグネタイト粒子粉末の顕微鏡写真によ
り粒子構造を示す図である。FIG. 2 is a view showing a particle structure by a micrograph of a conventional magnetite particle powder.
Claims (3)
換算でＦｅに対し０．１０〜５．０重量％含有されてお
り、且つ平均粒子径が０．１０〜０．２５μｍであり、
該粒子形状が実質的に六面体であり、該六面体の各稜線
が面状になっていることを特徴とするマグネタイト粒子
粉末。1. An oxide of Mg (magnesium) is Mg
It is contained in an amount of 0.10 to 5.0% by weight with respect to Fe, and has an average particle size of 0.10 to 0.25 μm.
Magnetite particle powder, wherein the particle shape is substantially hexahedral, and each ridge of the hexahedron is planar.
を添加し、苛性アルカリ又は／及び炭酸アルカリの存在
下で、且つ弱酸性の条件下に酸化性ガスを通気してマグ
ネタイトを生成させることを特徴とする上記請求項１記
載のマグネタイト粒子粉末の製造方法。2. A method for producing magnetite by adding a magnesium compound to an aqueous solution of ferrous salt, and aerating an oxidizing gas in the presence of caustic alkali and / or alkali carbonate and under weakly acidic conditions to produce magnetite. The method for producing magnetite particle powder according to claim 1, which is characterized in that.
末を含有する磁性トナー。3. A magnetic toner containing the magnetite particle powder according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4301298A JP2628967B2 (en) | 1992-11-11 | 1992-11-11 | Magnetite particle powder and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4301298A JP2628967B2 (en) | 1992-11-11 | 1992-11-11 | Magnetite particle powder and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06144840A true JPH06144840A (en) | 1994-05-24 |
| JP2628967B2 JP2628967B2 (en) | 1997-07-09 |
Family
ID=17895160
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4301298A Expired - Lifetime JP2628967B2 (en) | 1992-11-11 | 1992-11-11 | Magnetite particle powder and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2628967B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4889853A (en) * | 1987-07-09 | 1989-12-26 | Suntory Limited | Hydroquinonlyphenyl butyric acid amide derivative |
| US5885740A (en) * | 1996-09-27 | 1999-03-23 | Titan Kogyo Kabushiki Kaisha | Magnetite particles, a process for producing them and applications thereof |
| JP2006335614A (en) * | 2005-06-03 | 2006-12-14 | Mitsui Mining & Smelting Co Ltd | Multiple iron oxide particle for ferrite formed body |
| US7470494B2 (en) | 2004-10-08 | 2008-12-30 | Canon Kabushiki Kaisha | Magnetic toner |
-
1992
- 1992-11-11 JP JP4301298A patent/JP2628967B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4889853A (en) * | 1987-07-09 | 1989-12-26 | Suntory Limited | Hydroquinonlyphenyl butyric acid amide derivative |
| US5885740A (en) * | 1996-09-27 | 1999-03-23 | Titan Kogyo Kabushiki Kaisha | Magnetite particles, a process for producing them and applications thereof |
| US7470494B2 (en) | 2004-10-08 | 2008-12-30 | Canon Kabushiki Kaisha | Magnetic toner |
| JP2006335614A (en) * | 2005-06-03 | 2006-12-14 | Mitsui Mining & Smelting Co Ltd | Multiple iron oxide particle for ferrite formed body |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2628967B2 (en) | 1997-07-09 |
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