JPH0136864B2 - - Google Patents
Info
- Publication number
- JPH0136864B2 JPH0136864B2 JP59155419A JP15541984A JPH0136864B2 JP H0136864 B2 JPH0136864 B2 JP H0136864B2 JP 59155419 A JP59155419 A JP 59155419A JP 15541984 A JP15541984 A JP 15541984A JP H0136864 B2 JPH0136864 B2 JP H0136864B2
- Authority
- JP
- Japan
- Prior art keywords
- solution
- triiron tetroxide
- pigment
- producing
- hydroxosilicate
- 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.)
- Expired
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 239000000049 pigment Substances 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims 3
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000005415 magnetization Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- WPUINVXKIPAAHK-UHFFFAOYSA-N aluminum;potassium;oxygen(2-) Chemical compound [O-2].[O-2].[Al+3].[K+] WPUINVXKIPAAHK-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 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
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Developing Agents For Electrophotography (AREA)
Description
【発明の詳細な説明】
本発明は粒度分布の優れた、かつ酸化安定性を
改善した四三酸化鉄顔料の製造法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a triiron tetroxide pigment having an excellent particle size distribution and improved oxidative stability.
最近乾式電子複写機の一成分系高抵抗磁性トナ
ー用材料として、四三酸化鉄顔料が広く使用され
るようになつた。特に現像特性改善のために、磁
性トナーとして、比抵抗の大きいこと、粒径が適
度に小さいこと、粒度分布が良く揃つていること
が要求される。 Recently, triiron tetroxide pigments have come to be widely used as materials for one-component high-resistance magnetic toners for dry type electronic copying machines. In particular, in order to improve the development characteristics, the magnetic toner is required to have a high specific resistance, a suitably small particle size, and a well-defined particle size distribution.
これに対応出来る四三酸化鉄顔料は、電気伝導
度のより低い粒子であること、粒径も0.2〜0.3μ
等従来の一般的な四三酸化鉄顔料より、粒子径が
小さく、かつ色相も実用にたえる黒さを保つこ
と、更にトナーへの加工時に於て樹脂への分散が
容易であること等が要求されている。 Triiron tetroxide pigments that can handle this need to have particles with lower electrical conductivity and a particle size of 0.2 to 0.3μ.
Compared to conventional general triiron tetroxide pigments, the particle size is smaller, the hue maintains a black enough for practical use, and it is also easier to disperse into resin when processed into toner. requested.
一般に水溶液反応による四三酸化鉄顔料はスピ
ネル型の結晶構造をもつマグネタイトを基本とす
るもので、電気伝導度は高く、また粒径も0.2〜
0.3μ以下になると、その表面活性が強くなる為酸
化安定性に難点があり、空気中常温でも、γ―
Fe2O3への酸化進行が速まり、色相も茶味を帯び
た黒色になり易い。 In general, triiron tetroxide pigments produced by an aqueous solution reaction are based on magnetite with a spinel-type crystal structure, have high electrical conductivity, and have a particle size of 0.2~
If it is less than 0.3μ, the surface activity becomes strong, so oxidation stability becomes difficult, and even in air at room temperature, γ-
Oxidation to Fe 2 O 3 accelerates, and the hue tends to become brownish black.
本発明者はこのような四三酸化鉄顔料の欠点を
解決すべく検討を重ねた結果、鉄塩水溶液中から
合成する四三酸化鉄の製造法に於て、溶液中の
Fe++／Fe+++比が10〜1.0の時期に、ヒドロキソ
ケイ酸塩溶液あるいはヒドロキソアルミン酸塩溶
液を加えることによつて粒子径の小さい四三酸化
鉄顔料でも、熱安定性に優れ、色相も実用に耐え
る黒色を保持し、樹脂中分散に有利な粒度分布の
揃つた四三酸化鉄顔料を得ることを見出した。 As a result of repeated studies to solve these drawbacks of triiron tetroxide pigments, the present inventor has developed a method for producing triiron tetroxide, which is synthesized from an aqueous iron salt solution.
By adding a hydroxosilicate solution or a hydroxoaluminate solution when the Fe ++ /Fe +++ ratio is between 10 and 1.0, even triiron tetroxide pigments with small particle diameters can have excellent thermal stability. It has been found that a triiron tetroxide pigment can be obtained which maintains a black hue suitable for practical use and has a uniform particle size distribution that is advantageous for dispersion in resins.
即ち本発明は、硫酸第一鉄塩等の第一鉄塩溶液
に当量以上のアルカリ水溶液を添加して得たFe
（OH）2コロイドを含む水溶液を、60℃以上望ま
しくは80〜95℃の温度範囲で空気を通すことによ
つてスピネル型四三酸化鉄を製造する方法に於
て、Si／Fe3O4又はAl／Fe3O4に換算して0.5〜3.0
重量％のヒドロキソケイ酸塩溶液又はヒドロキソ
アルミン酸塩溶液を加えることによつて、熱安定
性に優れ、粒度分布の揃つた四三酸化鉄顔料を生
成させ、次いで塩類を水洗除去し105〜110℃で乾
燥して粒状の黒色四三酸化鉄粒子粉末を得る方法
である。生成する四三酸化鉄の大きさは、反応中
のPH値を7.5以上の値の中から選択し制御するこ
とによつて、0.03μ〜0.5μの範囲の中から選択し
た粒子径に比較的容易に調整出来ることも、この
製造法の特徴である。 That is, the present invention provides Fe obtained by adding an equivalent or more aqueous alkali solution to a ferrous salt solution such as ferrous sulfate.
In a method for producing spinel triiron tetroxide by passing air through an aqueous solution containing (OH) 2 colloid at a temperature range of 60°C or higher, preferably 80 to 95°C, Si/Fe 3 O 4 Or 0.5 to 3.0 in terms of Al/Fe 3 O 4
By adding a hydroxosilicate solution or a hydroxoaluminate solution of 105 to 110% by weight, a triiron tetroxide pigment with excellent thermal stability and uniform particle size distribution is produced, and the salts are then removed by washing with water. This is a method to obtain granular black triiron tetroxide particle powder by drying at ℃. The size of the produced triiron tetroxide can be adjusted relatively to the particle size selected from the range of 0.03μ to 0.5μ by selecting and controlling the pH value during the reaction from a value of 7.5 or higher. Another feature of this manufacturing method is that it can be easily adjusted.
また、かゝる方法で得た四三酸化鉄粒子を700
〜900℃の温度範囲で加熱酸化した後、300〜550
℃の温度で通常の方法で還元しても粒子相互間の
焼結の少い、粒度分布の均一な四三酸化鉄顔料を
得ることが出来る。 In addition, 700 triiron tetroxide particles obtained by the above method were used.
After heating oxidation in the temperature range of ~900℃, 300~550
Even if the pigment is reduced by a conventional method at a temperature of .degree. C., it is possible to obtain a triiron tetroxide pigment with a uniform particle size distribution and little sintering between particles.
ヒドロキソケイ酸塩溶液あるいはヒドロキソア
ルミン酸塩溶液の添加の時期については、反応溶
液中のFe++／Fe+++比が10〜1.0である時期に行
なうのが有利であり、Fe++／Fe+++比が10以前の
早い時期に添加すれば、概してマグネタイト粒子
の成長が阻害され粒子径の調整が難かしく、粒度
分布も劣つたものになり易く、色相も劣るもので
あつた。またFe++／Fe+++比が1.0以後の時期に
添加したものは酸化安定性のばらつきが大きいも
のであつた。 Regarding the timing of adding the hydroxosilicate solution or the hydroxoaluminate solution, it is advantageous to add it when the Fe ++ /Fe +++ ratio in the reaction solution is 10 to 1.0. If the Fe +++ ratio is added at an early stage of 10 or less, the growth of magnetite particles is generally inhibited, making it difficult to adjust the particle size, resulting in poor particle size distribution, and poor hue. Furthermore, those added when the Fe ++ /Fe +++ ratio was 1.0 or later had large variations in oxidation stability.
添加するヒドロキソケイ酸塩溶液あるいはヒド
ロキソアルミン酸塩溶液はSiO2／Na2Oモル比2.1
〜3.9のケイ酸ソーダ、あるいはNa2O／Al2O3モ
ル比1.3〜1.6のアルミン酸ソーダが一般的である
が、ケイ酸カリウムあるいはアルミン酸カリウム
等を用いることが出来る。またこれらは組合わせ
て用いることも出来る。 The hydroxosilicate solution or hydroxoaluminate solution to be added has a SiO 2 /Na 2 O molar ratio of 2.1.
Sodium silicate with a Na 2 O/Al 2 O 3 molar ratio of 1.3 to 1.6 is generally used, but potassium silicate or potassium aluminate can also be used. Moreover, these can also be used in combination.
次に実施例により本発明を更に詳細に説明す
る。 Next, the present invention will be explained in more detail with reference to Examples.
実施例 １
反応溶液中の35.8ｇ―モルの硫酸第一鉄溶液
（濃度1.07モル／）33に18／分の量の空気
を吹込みながら1.05当量の苛性ソーダ溶液を250
ml／分の速度で添加する。Example 1 1.05 equivalents of caustic soda solution was added to 35.8 g-mol of ferrous sulfate solution (concentration 1.07 mol/min) in a reaction solution while blowing air at a rate of 18/min.
Add at a rate of ml/min.
その後Fe++／Fe+++比が4.0の時期の反応液に、
SiO237ｇ／、Na2O12ｇ／のヒドロキソケイ
酸塩溶液1000mlを10分間で添加した。５時間反応
を続行し、Fe++／Fe+++比が0.5にて反応を終了
した。なお、反応中の温度は90℃に調節した。 After that, in the reaction solution when the Fe ++ /Fe +++ ratio was 4.0,
1000 ml of a hydroxosilicate solution containing 37 g of SiO 2 /12 g of Na 2 O was added in 10 minutes. The reaction was continued for 5 hours and ended when the Fe ++ /Fe +++ ratio was 0.5. Note that the temperature during the reaction was adjusted to 90°C.
反応終了したスラリーを洗滌乾燥して得た四三
酸化鉄顔料は次の特性値を示すものであつた。 The triiron tetroxide pigment obtained by washing and drying the slurry after the reaction had the following characteristic values.
SiO2 1.5 重量％
比表面積 9.0 m2／ｇ
水分 0.1 ％
吸油量 27 ml／100ｇ
抗磁力 133 Oe
飽和磁化 85.4 emu／ｇ
実施例 ２
実施例１によつて得られた四三酸化鉄顔料を
800℃で空気雰囲気中加熱酸化してα―Fe2O3粒
子とした。次いでこのα―Fe2O3粒子を水素80
％、窒素20％の還元性雰囲気中400℃で180分間加
熱還元した後粉砕して得た黒色の四三酸化鉄顔料
は次の特性値を示すものであつた。SiO 2 1.5% by weight Specific surface area 9.0 m 2 /g Water 0.1% Oil absorption 27 ml/100g Coercive force 133 Oe Saturation magnetization 85.4 emu/g Example 2 The triiron tetroxide pigment obtained in Example 1 was
It was heated and oxidized at 800°C in an air atmosphere to form α-Fe 2 O 3 particles. Next, this α-Fe 2 O 3 particle is converted into hydrogen 80
%, a black triiron tetroxide pigment obtained by heating reduction at 400° C. for 180 minutes in a reducing atmosphere of 20% nitrogen and then pulverization exhibited the following characteristic values.
SiO2 1.5 重量％
比表面積 8.2 m2／ｇ
水分 0.1 ％
吸油量 30 ml／100ｇ
抗磁力 330 Oe
飽和磁化 82.0 emu／ｇ
実施例 ３
実施例１によつて得た四三酸化鉄顔料を900℃
で加熱酸化した以外は実施例２と同様の方法で得
た四三酸化鉄顔料は次の特性値を示すものであつ
た。SiO 2 1.5% by weight Specific surface area 8.2 m 2 /g Water 0.1% Oil absorption 30 ml/100g Coercive force 330 Oe Saturation magnetization 82.0 emu/g Example 3 The triiron tetroxide pigment obtained in Example 1 was heated at 900°C.
A triiron tetroxide pigment obtained in the same manner as in Example 2 except that it was oxidized by heating had the following characteristic values.
SiO2 1.5 重量％
比表面積 7.8 m2／ｇ
水分 0.1 ％
吸油量 33 ml／100ｇ
抗磁力 310 Oe
飽和磁化 81.5 emu／ｇ
比較例 １
ヒドロキソケイ酸塩溶液の添加を行わない以外
は実施例１と同様な方法で得た四三酸化鉄顔料は
次の特性値を示すものであつた。SiO 2 1.5% by weight Specific surface area 7.8 m 2 /g Water 0.1% Oil absorption 33 ml/100g Coercive force 310 Oe Saturation magnetization 81.5 emu/g Comparative example 1 Same as Example 1 except that no hydroxosilicate solution was added. A triiron tetroxide pigment obtained in a similar manner exhibited the following characteristic values.
比表面積 7.0 m2／ｇ
水分 1.0 ％
吸油量 29 ml／100ｇ
抗磁力 120 Oe
飽和磁化 85.8 emu／ｇ
比較例 ２
比較例１によつて得た顔料を、実施例２と同様
の方法で加熱酸化、加熱還元した後粉砕して得た
黒色の四三酸化鉄顔料は次の特性値を示すもので
あつた。Specific surface area 7.0 m 2 /g Moisture 1.0% Oil absorption 29 ml/100g Coercive force 120 Oe Saturation magnetization 85.8 emu/g Comparative Example 2 The pigment obtained in Comparative Example 1 was heated and oxidized in the same manner as in Example 2. The black triiron tetroxide pigment obtained by heating reduction and pulverization exhibited the following characteristic values.
比表面積 4.2 m2／ｇ 水分 0.1 ％ 吸油量 20 ml／100ｇ 抗磁力 205 Oe 飽和磁化 86.2 emu／ｇSpecific surface area 4.2 m 2 /g Moisture 0.1% Oil absorption 20 ml/100g Coercive force 205 Oe Saturation magnetization 86.2 emu/g
Claims (1)
添加し、空気酸化を行なつてスピネル型四三酸化
鉄を製造するにあたり、水酸化第一鉄生成後の四
三酸化鉄への酸化反応中に、ヒドロキソケイ酸塩
溶液あるいはヒドロキソアルミン酸溶液を添加す
ることを特徴とする、粒度分布の優れた、そして
酸化安定度の改良された四三酸化鉄顔料の製造
法。 ２ ヒドロキソケイ酸塩溶液あるいはヒドロキソ
アルミン酸塩溶液の添加を反応溶液中のFe++／
Fe+++比が10〜1.0である時期に行なう特許請求の
範囲第１項記載の四三酸化鉄顔料の製造法。 ３ ヒドロキソケイ酸塩溶液を第一鉄塩溶液中の
鉄に対し、Si／Fe3O4に換算して0.5〜3.0重量％
の割合で加える特許請求の範囲第１項記載の四三
酸化鉄顔料の製造法。 ４ ヒドロキソアルミン酸塩溶液を第一鉄塩溶液
中の鉄に対し、Al／Fe3O4に換算して0.5〜3.0重
量％の割合で加える特許請求の範囲第１項記載の
四三酸化鉄顔料の製造法。 ５ 第一鉄塩溶液に当量以上のアルカリ水溶液を
添加し、空気酸化を行なつて、スピネル型四三酸
化鉄を製造するにあたり、水酸化第一鉄生成後の
四三酸化鉄への酸化反応中に、ヒドロキソケイ酸
塩溶液あるいはヒドロキソアルミン酸溶液を添加
することによつて得られた四三酸化鉄粒子を、空
気中700〜900℃の温度範囲で加熱酸化してα―
Fe2O3粒子とし、次いで還元性雰囲気中300〜550
℃の温度範囲で加熱して還元することを特徴とす
る四三酸化鉄顔料の製造法。[Claims] 1. When producing spinel-type triiron tetroxide by adding an equivalent or more aqueous alkali solution to a ferrous salt solution and performing air oxidation, A method for producing a triiron tetroxide pigment having an excellent particle size distribution and improved oxidation stability, which comprises adding a hydroxosilicate solution or a hydroxoaluminate solution during the oxidation reaction to iron. 2 Addition of hydroxosilicate solution or hydroxoaluminate solution to Fe ++ /
A method for producing a triiron tetroxide pigment according to claim 1, which is carried out at a time when the Fe +++ ratio is 10 to 1.0. 3 The hydroxosilicate solution is added in an amount of 0.5 to 3.0% by weight calculated as Si/Fe 3 O 4 based on the iron in the ferrous salt solution.
A method for producing a triiron tetroxide pigment according to claim 1, wherein the pigment is added in a proportion of . 4. Triiron tetroxide according to claim 1, in which the hydroxyaluminate solution is added in a proportion of 0.5 to 3.0% by weight in terms of Al/Fe 3 O 4 based on the iron in the ferrous salt solution. Pigment manufacturing method. 5 When producing spinel-type triiron tetroxide by adding an equivalent or more aqueous alkali solution to a ferrous salt solution and performing air oxidation, the oxidation reaction to triiron tetroxide after the production of ferrous hydroxide Triiron tetroxide particles obtained by adding a hydroxosilicate solution or a hydroxoaluminate solution are oxidized by heating in the air at a temperature range of 700 to 900°C to form α-
Fe 2 O 3 particles and then 300-550 in reducing atmosphere
A method for producing a triiron tetroxide pigment, which is characterized by reduction by heating in a temperature range of ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59155419A JPS6134070A (en) | 1984-07-27 | 1984-07-27 | Production of tri-iron tetroxide pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59155419A JPS6134070A (en) | 1984-07-27 | 1984-07-27 | Production of tri-iron tetroxide pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6134070A JPS6134070A (en) | 1986-02-18 |
| JPH0136864B2 true JPH0136864B2 (en) | 1989-08-02 |
Family
ID=15605584
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59155419A Granted JPS6134070A (en) | 1984-07-27 | 1984-07-27 | Production of tri-iron tetroxide pigment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6134070A (en) |
Families Citing this family (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62278131A (en) * | 1986-05-28 | 1987-12-03 | Canon Inc | Silicon element-containing magnetic iron oxide and production thereof |
| JP2521545B2 (en) * | 1989-12-29 | 1996-08-07 | 濱田重工株式会社 | Steel slag processing method and device |
| JP2521564B2 (en) * | 1990-06-13 | 1996-08-07 | 濱田重工株式会社 | Cooling method for steel slag |
| JP2974452B2 (en) * | 1991-06-19 | 1999-11-10 | キヤノン株式会社 | Magnetic toner |
| US5424810A (en) * | 1991-09-13 | 1995-06-13 | Canon Kabushiki Kaisha | Magnetic toner, magnetic developer, apparatus unit, image forming apparatus and facsimile apparatus |
| US5356712A (en) * | 1991-09-13 | 1994-10-18 | Mitsui Mining & Smelting Co., Ltd. | Magnetite particles |
| DE69408253T2 (en) * | 1993-09-30 | 1998-05-14 | Toda Kogyo Corp | Granular magnetite particles and process for their manufacture |
| EP0650097B1 (en) * | 1993-10-08 | 1999-04-07 | Canon Kabushiki Kaisha | Magnetic toner, process cartridge and image forming method |
| EP0686882B1 (en) | 1994-05-13 | 1999-08-11 | Canon Kabushiki Kaisha | Toner for developing electrostatic images, process cartridge, and image forming method |
| US6002895A (en) * | 1994-05-13 | 1999-12-14 | Canon Kabushiki Kaisha | Process cartridge |
| US5641600A (en) * | 1994-08-05 | 1997-06-24 | Canon Kabushiki Kaisha | Magnetic toner and image forming method |
| EP0851307B1 (en) | 1996-12-26 | 2005-04-27 | Canon Kabushiki Kaisha | Magnetic toner, process for producing magnetic toner, and image forming method |
| DE69828014T2 (en) | 1997-09-16 | 2005-12-01 | Canon K.K. | Magnetic toner and image forming process |
| DE19919791A1 (en) | 1999-04-30 | 2000-11-02 | Bayer Ag | Process for the production of precipitation magnetites |
| US6447969B1 (en) | 1999-06-02 | 2002-09-10 | Canon Kabushiki Kaisha | Toner and image forming method |
| EP1128225B1 (en) | 2000-02-21 | 2005-12-14 | Canon Kabushiki Kaisha | Magnetic toner and image-forming method making use of the same |
| CA2337087C (en) | 2000-03-08 | 2006-06-06 | Canon Kabushiki Kaisha | Magnetic toner, process for production thereof, and image forming method, apparatus and process cartridge using the toner |
| DE10043492A1 (en) | 2000-09-01 | 2002-03-14 | Bayer Ag | Use of magnetic particles and process for their manufacture |
| US6670087B2 (en) | 2000-11-07 | 2003-12-30 | Canon Kabushiki Kaisha | Toner, image-forming apparatus, process cartridge and image forming method |
| DE10209150A1 (en) | 2002-03-01 | 2003-09-11 | Bayer Ag | Process for the production of magnetite particles and their use |
-
1984
- 1984-07-27 JP JP59155419A patent/JPS6134070A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6134070A (en) | 1986-02-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |