JPH04238819A - Production of magnetite black pigment - Google Patents
Production of magnetite black pigmentInfo
- Publication number
- JPH04238819A JPH04238819A JP99591A JP99591A JPH04238819A JP H04238819 A JPH04238819 A JP H04238819A JP 99591 A JP99591 A JP 99591A JP 99591 A JP99591 A JP 99591A JP H04238819 A JPH04238819 A JP H04238819A
- Authority
- JP
- Japan
- Prior art keywords
- magnetite
- aqueous solution
- ferrous
- black pigment
- temperature
- 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.)
- Pending
Links
- 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 32
- 239000000049 pigment Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001448 ferrous ion Inorganic materials 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims abstract description 7
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 230000005587 bubbling Effects 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000013081 microcrystal Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000010419 fine particle Substances 0.000 abstract description 8
- -1 ferrous compound Chemical class 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002537 cosmetic Substances 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000011859 microparticle Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 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
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、マグネタイト黒色顔料
の製造方法に関するものである。更に詳しく述べるなら
ば、本発明は分散性が良好で二次凝集性のないマグネタ
イト黒色顔料を効率よく製造する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 method for producing a magnetite black pigment. More specifically, the present invention relates to a method for efficiently producing a magnetite black pigment with good dispersibility and no secondary agglomeration.
【０００２】0002
【従来の技術】マグネタイト黒色顔料（別名鉄黒、四三
酸化鉄）は、化粧品用顔料として有用なものである。す
なわち、０．１μｍ以下の粒径を有するマグネタイト黒
色顔料は、その粒径が可視光の波長と同等、またはそれ
以下であるため、透明感があり、このため、化粧品とし
て用いると、深みのある黒色が得られるという特徴を有
している。BACKGROUND OF THE INVENTION Magnetite black pigments (also known as iron black, triiron tetroxide) are useful as cosmetic pigments. In other words, magnetite black pigments with a particle size of 0.1 μm or less have a transparent appearance because their particle size is equal to or smaller than the wavelength of visible light, and therefore, when used in cosmetics, they have a deep and deep appearance. It has the characteristic of producing black color.
【０００３】しかしながら、従来のマグネタイト黒色顔
料の製造方法は、第一鉄イオン含有水溶液にアルカリを
加えて水酸化第一鉄を生成させて、さらに、空気や酸素
ガスを吹き込みながら加熱昇温してマグネタイトを生成
するものであるが、この方法により得られるマグネタイ
ト黒色顔料粒子の粒径は０．１μｍより大きく、従って
、これを水性分散液にしても分散粒子が沈降しやすく、
また、所望の透明感を得ることが困難であった。However, the conventional method for producing magnetite black pigments involves adding an alkali to an aqueous solution containing ferrous ions to produce ferrous hydroxide, and then heating and raising the temperature while blowing air or oxygen gas. Although magnetite is produced, the particle size of the magnetite black pigment particles obtained by this method is larger than 0.1 μm. Therefore, even if this is made into an aqueous dispersion, the dispersed particles tend to settle.
Furthermore, it was difficult to obtain a desired transparency.
【０００４】また他の方法として、第一鉄イオンと第二
鉄イオンとを含む水溶液において、そのモル混合比を１
：１とし、この水溶液にアルカリを加えてマグネタイト
を生成せしめると、粒径０．０１μｍ以下のマグネタイ
ト微粒子が得られるが、この微粒子は二次凝集力が強く
、これを化粧品に用いたとき、微粒子を安定な分散状態
に保持することが困難である。As another method, in an aqueous solution containing ferrous ions and ferric ions, the molar mixing ratio is set to 1.
:1, and when an alkali is added to this aqueous solution to generate magnetite, magnetite fine particles with a particle size of 0.01 μm or less are obtained, but these fine particles have a strong secondary cohesive force, and when used in cosmetics, fine particles It is difficult to maintain a stable dispersion state.
【０００５】化粧品以外の用途として、マグネタイトは
、静電複写機用磁気トナーにも用いられる。この場合に
は、画像を鮮明にするため、マグネタイト黒色顔料の粒
径が０．１〜０．０１μｍの範囲内にあることが求めら
れている。すなわち、粒径が０．０１μｍより小さな微
粒子は、トナー結着樹脂中に均一に分散することが困難
になる。In applications other than cosmetics, magnetite is also used in magnetic toners for electrostatic copying machines. In this case, in order to make the image clear, the particle size of the magnetite black pigment is required to be within the range of 0.1 to 0.01 μm. That is, fine particles having a particle size smaller than 0.01 μm are difficult to uniformly disperse in the toner binder resin.
【０００６】また、マグネタイト黒色顔料の原料として
、第一鉄化合物、および第二鉄化合物が用いられるが、
第二鉄化合物は高価であるため、第二鉄化合物を使用せ
ずに、第一鉄化合物のみからマグネタイト黒色顔料を製
造し得る方法の開発が強く求められている。Ferrous compounds and ferric compounds are also used as raw materials for magnetite black pigments.
Since ferric compounds are expensive, there is a strong demand for the development of a method for producing magnetite black pigments only from ferrous compounds without using ferric compounds.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、第一鉄化合
物を原料として、所望の微小粒径を有し、二次凝集性の
ないマグネタイト黒色顔料を効率よく製造し得るマグネ
タイト黒色顔料の製造方法を提供しようとするものであ
る。[Problems to be Solved by the Invention] The present invention is directed to the production of a magnetite black pigment that can efficiently produce a magnetite black pigment that has a desired microparticle size and is free from secondary agglomeration using a ferrous compound as a raw material. It is intended to provide a method.
【０００８】[0008]
【課題を解決するための手段・作用】本発明は、マグネ
タイト黒色顔料の製造に当り、第一鉄イオン含有水溶液
に不活性ガス（例えば窒素ガス、アルゴンガス等）をバ
ブリングして水溶液中の溶存酸素含有量を減少させなが
ら、これにアルカリ溶液を加えて水酸化第一鉄を沈澱せ
しめ、その後に、加熱、操作を施すことにより、上記課
題を解決したものである。[Means/Actions for Solving the Problems] The present invention involves bubbling an inert gas (for example, nitrogen gas, argon gas, etc.) into an aqueous solution containing ferrous ions in order to produce a magnetite black pigment. The above problem was solved by adding an alkaline solution to this to precipitate ferrous hydroxide while reducing the oxygen content, and then heating and operating.
【０００９】すなわち、本発明に係るマグネタイト黒色
顔料の製造方法は、第一鉄イオンを含有する水溶液に、
不活性ガスをバブリングして前記水溶液中の溶存酸素含
有量を減少させながら、これにアルカリ性物質を添加し
て、水酸化第一鉄を生成させ、この水溶液を６０〜 １
００℃の温度に加熱して、マグネタイト微結晶を生成さ
せることを特徴とするものである。That is, the method for producing a magnetite black pigment according to the present invention includes adding aqueous solution containing ferrous ions,
While bubbling inert gas to reduce the dissolved oxygen content in the aqueous solution, an alkaline substance is added to the aqueous solution to generate ferrous hydroxide, and the aqueous solution is heated to 60 to 1
It is characterized by heating to a temperature of 00°C to generate magnetite microcrystals.
【００１０】一般に、第一鉄イオン水溶液にアルカリを
添加し、生成した沈澱物を加熱酸化すると、得られるマ
グネタイト結晶粒子が成長し、その粒径が０．１μｍよ
り大きくなる。本発明者は、この結晶粒子の成長を抑止
する方法を検討し、その結果、第一鉄イオン含有水溶液
に不活性ガスをバブリングすることによって水溶液中の
溶存酸素含有量を減少させ、反応系の温度上昇中には晶
析を起こさせず、所定温度に到達した後に晶析を開始さ
せ、それによって、反応系中に最初に生成する析出晶の
数を増大させることによって結晶粒子の成長を抑止し、
所望の微小粒径を有するマグネタイト黒色顔料を製造す
ることに成功した。[0010] Generally, when an alkali is added to an aqueous ferrous ion solution and the resulting precipitate is heated and oxidized, the resulting magnetite crystal particles grow and have a particle size larger than 0.1 μm. The present inventor investigated a method for inhibiting the growth of crystal particles, and as a result, by bubbling an inert gas into an aqueous solution containing ferrous ions, the dissolved oxygen content in the aqueous solution was reduced, and the reaction system was Crystallization is not caused while the temperature is rising, but starts crystallization after reaching a predetermined temperature, thereby suppressing the growth of crystal particles by increasing the number of precipitated crystals that initially form in the reaction system. death,
A magnetite black pigment with a desired microparticle size was successfully produced.
【００１１】本発明方法に用いられる第一鉄化合物は第
一鉄ハロゲン化物、第一鉄硫酸塩、第一鉄硝酸塩、第一
鉄過塩素酸塩などの水溶性第一鉄化合物から適宜に選択
することができる。工業的には安価な第一鉄硫酸塩を用
いることが好ましい。The ferrous compound used in the method of the present invention is appropriately selected from water-soluble ferrous compounds such as ferrous halides, ferrous sulfates, ferrous nitrates, and ferrous perchlorates. can do. Industrially, it is preferable to use inexpensive ferrous sulfate.
【００１２】第一鉄イオン水溶液中の第一鉄イオン濃度
に格別の限定はないが、一般に、５〜５０ｇ／ｌの範囲
内にあることが好ましい。[0012] The ferrous ion concentration in the ferrous ion aqueous solution is not particularly limited, but it is generally preferably within the range of 5 to 50 g/l.
【００１３】本発明方法に用いられるアルカリ性物質に
は格別の限定はないが、アルカリ金属水酸化物（水酸化
ナトリウム、水酸化カリウムなど）およびアンモニアな
どのように、第一鉄イオン水溶液に添加してもアルカリ
分が沈澱することなく安定に溶解するものが好ましい。[0013] There are no particular limitations on the alkaline substances used in the method of the present invention; It is preferable to use one that can stably dissolve alkaline components without precipitating.
【００１４】本発明方法において、第一鉄イオン水溶液
にアルカリ性物質が添加されるが、このアルカリ性物質
の添加量は、第一鉄イオン水溶液を中和し、そのｐＨを
６〜１４の範囲に調整し得る量であればよい。一般にア
ルカリ性物質は、その水溶液の状態で第一鉄イオン水溶
液に添加される。アルカリ物質の添加温度には、格別の
限定はないが、一般に室温付近、例えば１０〜３０℃の
温度にあることが好ましい。In the method of the present invention, an alkaline substance is added to the ferrous ion aqueous solution, and the amount of the alkaline substance added is determined by neutralizing the ferrous ion aqueous solution and adjusting its pH to a range of 6 to 14. It is sufficient as long as it is possible. Generally, the alkaline substance is added to the ferrous ion aqueous solution in the form of an aqueous solution. There are no particular limitations on the temperature at which the alkaline substance is added, but it is generally preferred to be around room temperature, for example 10 to 30°C.
【００１５】不活性ガスのバブリングは、アルカリ性物
質を第一鉄イオン水溶液に添加する前に行われる。不活
性ガスとしては、例えば窒素ガス、炭酸ガス、ヘリウム
ガス、およびアルゴンガスなどから選択することができ
るが、工業的には窒素ガス或は、醗酵工業などから得ら
れる安価で純度の高い炭酸ガスを用いることが好ましい
。Bubbling of inert gas is performed before adding the alkaline substance to the aqueous ferrous ion solution. The inert gas can be selected from, for example, nitrogen gas, carbon dioxide gas, helium gas, and argon gas, but industrially nitrogen gas or carbon dioxide gas, which is inexpensive and has high purity obtained from the fermentation industry, is used. It is preferable to use
【００１６】本発明方法において、不活性ガスによるバ
ブリングによって第一鉄イオン水溶液中の溶存酸素含有
量が減少する。このバブリング操作の程度は、液温、不
活性ガスの吹き込み流量、泡の大きさ、バブリング槽の
形状、寸法などに応じて、適宜に設定することができる
。In the method of the present invention, the dissolved oxygen content in the aqueous ferrous ion solution is reduced by bubbling with an inert gas. The degree of this bubbling operation can be appropriately set depending on the liquid temperature, the flow rate of the inert gas, the size of the bubbles, the shape and dimensions of the bubbling tank, and the like.
【００１７】本発明方法において、不活性ガスバブリン
グされ、アルカリ添加により形成された水酸化第一鉄の
沈澱分散液を、６０℃〜 １００℃の温度に加熱する。
このとき、得られるマグネタイトの粒径をより小さくす
るためには、結晶析出の開始温度が高いことが好ましい
ので、液温が上記範囲内の所定温度に達する迄、不活性
ガスによるバブリングを継続することが好ましい。また
、昇温速度をなるべく早くして結晶析出を可及的に抑制
することが好ましい。In the method of the invention, a precipitated dispersion of ferrous hydroxide formed by addition of alkali and bubbled with an inert gas is heated to a temperature of 60°C to 100°C. At this time, in order to further reduce the particle size of the obtained magnetite, it is preferable that the starting temperature of crystal precipitation be high, so bubbling with an inert gas is continued until the liquid temperature reaches a predetermined temperature within the above range. It is preferable. Further, it is preferable to increase the temperature increase rate as much as possible to suppress crystal precipitation as much as possible.
【００１８】水酸化第一鉄は、前記バブリング操作中に
、上記温度において酸化され、マグネタイト微粒子を生
成させる。この時の温度が６０℃未満のときは酸化速度
が遅く、酸化開始時に形成されるマグネタイト微結晶の
数が少なく、これが次第に成長して粗大粒子になりやす
いという不都合があり、また、酸化温度を １００℃よ
り高くするには密閉耐圧容器の使用が必要になるため、
コストが高くなるという不都合を生ずる。Ferrous hydroxide is oxidized at the above temperature during the bubbling operation to produce magnetite fine particles. If the temperature at this time is less than 60°C, the oxidation rate is slow and the number of magnetite microcrystals formed at the start of oxidation is small, which tends to gradually grow and become coarse particles. To raise the temperature higher than 100℃, it is necessary to use a sealed pressure-resistant container.
This results in the inconvenience of increased costs.
【００１９】[0019]
【実施例】本発明方法を、更に下記実施例によって説明
する。EXAMPLES The method of the present invention will be further illustrated by the following examples.
【００２０】実施例１
０．３モル／ｌの硫酸第一鉄を含有する１０００ｍｌの
水溶液に窒素ガスを１０００ｍｌ／分の流量で反応容器
の底部より吹き込み１０分間バブリングした。次いで、
バブリングを続けながらこの水溶液に、水酸化ナトリウ
ム水溶液を、この水溶液のｐＨが１０になるように添加
した。Example 1 Nitrogen gas was blown into 1000 ml of an aqueous solution containing 0.3 mol/l of ferrous sulfate from the bottom of the reaction vessel at a flow rate of 1000 ml/min for 10 minutes. Then,
While bubbling was continued, an aqueous sodium hydroxide solution was added to the aqueous solution so that the pH of the aqueous solution was 10.
【００２１】その後加熱して、その温度を７０℃に上昇
させ、５時間バブリングを継続した。得られた反応液中
にはＦｅ２＋ が存在しないことを確認した。この黒色
微粒子を濾別し、洗浄し真空乾燥して２０ｇの黒色微小
粒子を得た。[0021] Thereafter, heating was performed to raise the temperature to 70°C, and bubbling was continued for 5 hours. It was confirmed that Fe2+ was not present in the obtained reaction solution. The black fine particles were filtered, washed, and vacuum dried to obtain 20 g of black fine particles.
【００２２】この黒色微小粒子は、Ｘ線回析法によりマ
グネタイトであることが確認された。また、電子顕微鏡
により黒色微小粒子の粒径を測定したところ０．０１〜
０．１μｍであった。[0022] The black microparticles were confirmed to be magnetite by X-ray diffraction. In addition, when the particle size of black microparticles was measured using an electron microscope, it was 0.01~
It was 0.1 μm.
【００２３】比較例１
実施例１と同一の操作を行った。但し、窒素ガスによる
バブリングを施すことなく、上記水溶液に反応容器の底
部から空気を１０００ｍｌ／分の流量で吹き込み１０分
間バブリングを施した後、水溶液を７０℃に加熱し、更
に５時間空気によるバブリングを継続した。褐色沈澱物
が得られた。Comparative Example 1 The same operation as in Example 1 was carried out. However, without bubbling with nitrogen gas, air was blown into the aqueous solution from the bottom of the reaction vessel at a flow rate of 1000 ml/min for 10 minutes, then the aqueous solution was heated to 70°C, and air was bubbled for another 5 hours. continued. A brown precipitate was obtained.
【００２４】この褐色沈澱物は、０．１〜０．２μｍの
粒径を有する黄色酸化鉄針状結晶と、０．３〜０．６μ
ｍの粒径を有する黒色マグネタイト六角板状結晶との混
合物であった。This brown precipitate contains yellow iron oxide needle crystals with a particle size of 0.1 to 0.2 μm and 0.3 to 0.6 μm.
It was a mixture with black magnetite hexagonal plate-shaped crystals having a particle size of m.
【００２５】[0025]
【発明の効果】本発明により、０．０１〜０．１μｍの
微小粒径を有し、二次凝集性のないマグネタイト黒色顔
料を効率よく製造することが可能になった。このように
微細なマグネタイト黒色顔料は、化粧品、および静電複
写用トナーなどの用途に有用なものである。According to the present invention, it has become possible to efficiently produce a magnetite black pigment having a microparticle size of 0.01 to 0.1 μm and having no secondary agglomeration. Such fine magnetite black pigments are useful in applications such as cosmetics and electrostatographic toners.
Claims (1)
活性ガスをバブリングして前記水溶液中の溶存酸素含有
量を減少させながら、これにアルカリ性物質を添加して
、水酸化第一鉄を生成させ、この水溶液を６０〜 １０
０℃の温度に加熱して、マグネタイト微結晶を生成させ
ることを特徴とするマグネタイト黒色顔料の製造方法。Claim 1: Bubbling an inert gas into an aqueous solution containing ferrous ions to reduce the dissolved oxygen content in the aqueous solution, and adding an alkaline substance to the aqueous solution to produce ferrous hydroxide. This aqueous solution has a concentration of 60 to 10
A method for producing a magnetite black pigment, which comprises heating to a temperature of 0° C. to generate magnetite microcrystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP99591A JPH04238819A (en) | 1991-01-09 | 1991-01-09 | Production of magnetite black pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP99591A JPH04238819A (en) | 1991-01-09 | 1991-01-09 | Production of magnetite black pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04238819A true JPH04238819A (en) | 1992-08-26 |
Family
ID=11489181
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP99591A Pending JPH04238819A (en) | 1991-01-09 | 1991-01-09 | Production of magnetite black pigment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04238819A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2954885A1 (en) | 2014-06-11 | 2015-12-16 | Titan Kogyo Kabushiki Kaisha | Black iron oxide for use with cosmetics, production method thereof, and cosmetic materials comprising the same |
-
1991
- 1991-01-09 JP JP99591A patent/JPH04238819A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2954885A1 (en) | 2014-06-11 | 2015-12-16 | Titan Kogyo Kabushiki Kaisha | Black iron oxide for use with cosmetics, production method thereof, and cosmetic materials comprising the same |
| US10131762B2 (en) | 2014-06-11 | 2018-11-20 | Titan Kogyo Kabushiki Kaisha | Black iron oxide for use with cosmetics, production method thereof, and cosmetic materials comprising the same |
| US10344141B2 (en) | 2014-06-11 | 2019-07-09 | Titan Kogyo Kabushiki Kaisha | Black iron oxide for use with cosmetics, production method thereof, and cosmetic materials comprising the same |
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