JPH01298028A - Illumenite powder and production thereof - Google Patents
Illumenite powder and production thereofInfo
- Publication number
- JPH01298028A JPH01298028A JP63128706A JP12870688A JPH01298028A JP H01298028 A JPH01298028 A JP H01298028A JP 63128706 A JP63128706 A JP 63128706A JP 12870688 A JP12870688 A JP 12870688A JP H01298028 A JPH01298028 A JP H01298028A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- particle
- ilmenite
- particle size
- 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.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000002245 particle Substances 0.000 claims abstract description 98
- 239000000725 suspension Substances 0.000 claims abstract description 8
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 23
- 239000002244 precipitate Substances 0.000 abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 6
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 abstract description 4
- 229910010062 TiCl3 Inorganic materials 0.000 abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 11
- 239000010936 titanium Substances 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000049 pigment Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 101000878457 Macrocallista nimbosa FMRFamide Proteins 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 235000019241 carbon black Nutrition 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 229910005438 FeTi Inorganic materials 0.000 description 1
- 229910005451 FeTiO3 Inorganic materials 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 etc. can be used Chemical compound 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical 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
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000011882 ultra-fine particle 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
- C01G49/0018—Mixed oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、平均径０．０５〜２．０μｍであって、粒子
が１個１個バラバラであり且つ粒度が均斉なＦｅＴｉＯ
４粒子からなるイルメナイト粒子粉末及びその製造法に
関するものである。Detailed Description of the Invention [Industrial Field of Application] The present invention is directed to FeTiO, which has an average diameter of 0.05 to 2.0 μm, each particle is disjoint, and the particle size is uniform.
The present invention relates to an ilmenite particle powder consisting of four particles and a method for producing the same.
その主な用途は、塗料用、トナー用黒色顔料粉末である
。Its main use is as a black pigment powder for paints and toners.
近時、省エネルギー時代における作業能率の向上並びに
塗膜物性の改良という観点から、塗料の製造に際して顔
料粒子粉末のビヒクル中での分散性、作業性及び耐熱性
の向上が益々要求されている。In recent years, from the viewpoint of improving work efficiency and improving the physical properties of paint films in the energy-saving era, there has been an increasing demand for improvements in the dispersibility of pigment particle powder in a vehicle, workability, and heat resistance when producing paints.
分散性及び作業性の向上の為には、顔料粒子粉末として
適度な粒度を有し、且つ、粒子が１個１個バラバラであ
り、しかも、粒度が均斉であることが必要である６
耐熱性について言えば、近年、複写機器の普及に伴って
、需要が増大している現像用トナーは、その製造工程に
おいて１５０℃以上の高温となる為、現像用トナーの着
色剤として用いられる顔料粒子粉末は、１５０”Ｃ以上
の温度においても色彩が安定していることが必要である
。In order to improve dispersibility and workability, it is necessary that the pigment particle powder has an appropriate particle size, that each particle is different, and that the particle size is uniform6. Heat resistance In recent years, with the spread of copying equipment, the demand for developing toner has increased, and since the manufacturing process involves high temperatures of 150°C or higher, pigment particle powder used as a coloring agent in developing toner is required. The color must be stable even at temperatures of 150"C or higher.
従来、黒色顔料粒子粉末としてマグネタイト粒子粉末、
カーボンブラック粒子粉末が広く一般に使用されている
。Conventionally, magnetite particle powder was used as black pigment particle powder,
Carbon black particulate powder is widely and commonly used.
また、黒色粒子粉末としてイルメナイト粒子粉末が知ら
れている。イルメナイト粒子粉末は、天然に産出するも
のと合成されるものがあり、合成法としては、例えば、
ジャーナル オブ フィジイ力ル ソサイエティ オブ
ジャパン（Ｊｏｕｒｎａｌｏｆ Ｐｈｙｓｉｃａｌ
５ｏｃｊｅｔｙ ｏｆ Ｊａｐａｎ）第１１巻第５号（
１９５６年）の第４９７頁に記載されている通り、Ｒｅ
ｇｏｓ 、ＴｉＯ□及び鉄粉を混合、成型し、次いで真
空管（１０−”ｎｎＨｇ）中、１３５０℃で焼成後、室
温まで冷却して粉砕することにより得られている。Ilmenite particles are also known as black particles. There are two types of ilmenite particle powder: naturally occurring ones and synthetic ones. Examples of synthetic methods include:
Journal of Physical Society of Japan
5ocjety of Japan) Volume 11 No. 5 (
(1956), page 497, Re
It is obtained by mixing GOS, TiO□ and iron powder, molding, firing at 1350°C in a vacuum tube (10-''nnHg), cooling to room temperature, and pulverizing.
〔発明が解決しようとする問題点１
分散性、作業性及び耐熱性に優れた黒色顔料粒子粉末は
、現在量も要求されているところであるが、上述した通
りの公知のマグネタイト粒子粉末は、平均径０．２〜０
．５μｍ程度の粒状又は立方状粒子であり、水溶液中か
ら生成する為粒子が１個１個バラバラであり、且つ、粒
度が均斉ではあるが、磁性を有する為粒子相互間で再凝
集が生じやすいものであるという欠点があった。また、
マグネタイト粒子粉末は、１５０℃以上の温度でマグネ
タイトに変態して黒色から茶褐色に変色し耐熱性に問題
があった。[Problem to be Solved by the Invention 1 There is a current demand for black pigment particles with excellent dispersibility, workability, and heat resistance, but the known magnetite particles as described above have an average Diameter 0.2~0
．． It is a granular or cubic particle of about 5 μm, and because it is generated from an aqueous solution, each particle is disjointed, and the particle size is uniform, but because it has magnetic properties, particles tend to reagglomerate among themselves. It had the disadvantage of being. Also,
Magnetite particle powder transforms into magnetite at a temperature of 150° C. or higher, changing its color from black to brown, and has a problem in heat resistance.
また、公知のカーボンブラックは、耐熱性に優れてはい
るが、０．ＯＩ〜０．０２μｍ程度の超微細粒子であり
かさ高い粉末である為取り扱いが困難で作業性が悪いも
のである。また、発ガン性等の安全、衛生面からの問題
点も指摘されている。Further, although known carbon blacks have excellent heat resistance, 0. Since it is an ultrafine particle with an OI of about 0.02 μm and a bulky powder, it is difficult to handle and has poor workability. In addition, safety and hygiene issues such as carcinogenicity have also been pointed out.
一方、黒色粒子粉末であるイルメナイト粒子粉末は、非
磁性である為再凝集を生起することがなく、また、耐熱
性に優れてはいるが、天然に産出するものは粒度が不均
斉であって、板状、塊状及び粒状等の粒子が混在した不
定形粒子粉末であり、また、特に、赤色へマタイトを数
乗量％程度含有していることによって暗褐色を呈するも
のであり、合成法によるものは、高温加熱焼成後粉砕す
る為、粒子相互間で焼結を生起しており、且つ、粒度が
不均斉な不定形粒子粉末である。On the other hand, ilmenite particles, which are black particles, are non-magnetic and therefore do not cause reagglomeration, and have excellent heat resistance, but naturally occurring particles have asymmetric particle sizes. It is an amorphous particle powder containing a mixture of plate-like, lump-like, and granular particles, and in particular, it has a dark brown color due to the fact that it contains about several percent of red hematite. Since the powder is pulverized after being heated and fired at a high temperature, sintering occurs between the particles, and the particles are irregularly shaped particles with asymmetric particle sizes.
そこで、黒色顔料粒子粉末として使用できる粒子相互間
の焼結がなく１個１個がバラバラであり、且つ、粒度が
均斉な合成イルメナイト粒子粉末が強く要求されている
。Therefore, there is a strong demand for a synthetic ilmenite particle powder that can be used as a black pigment particle powder, which has no sintering between the particles, each particle is discrete, and the particle size is uniform.
〔問題を解決する為の手段］
本発明者は、高温加熱焼成及び粉砕工程を経ることなく
、合成イルメナイト粒子粉末を得るべく種々検討した結
果、本発明に到達したのである。[Means for Solving the Problem] The present inventor has arrived at the present invention as a result of various studies aimed at obtaining synthetic ilmenite particle powder without going through high-temperature heating and calcination and pulverization steps.
即ち、本発明は、平均径０．０５〜２．０μｍであって
、粒子が１１１個バラバラであり且つ粒度が均斉なＦｅ
ＴｉＯ３粒子からなるイルメナイト粒子粉末及びＦｅ１
Ｉｌ及びＴｉ（ＩＩＩ）を含むｐＨ８．０〜１０．０の
アルカリ性Ｆｅ（ＯＨ）ｚ懸濁液を２００〜３００℃の
温度範囲で水熱処理することにより平均径０．０５〜２
．０μｍであって、粒子が１個１個バラバラであり且つ
粒度が均斉なＦｅＴｉＯｓ粒子を生成させることからな
るイルメナイト粒子粉末の製造法である。That is, the present invention provides Fe with an average diameter of 0.05 to 2.0 μm, 111 discrete particles, and uniform particle size.
Ilmenite particle powder consisting of TiO3 particles and Fe1
By hydrothermally treating an alkaline Fe(OH)z suspension containing Il and Ti(III) with a pH of 8.0 to 10.0 in a temperature range of 200 to 300°C, an average diameter of 0.05 to 2
．． This is a method for producing ilmenite particle powder, which consists of producing FeTiOs particles having a diameter of 0 μm, each particle being discrete, and uniform in particle size.
先ず、本発明において最も重要な点は、Ｔｉ（２）を含
むｐｕｅ、ｏ 〜１０．０のアルカリ性Ｆｅ （ＯＲ）
ｚ懸濁液を２００〜３００℃の温度範囲で水熱処理し
た場合には、水溶液中から直接ＦｅＴｉ０）粒子を生成
させることができるという事実である。First, the most important point in the present invention is that pue containing Ti(2), alkaline Fe (OR) of o ~ 10.0
The fact is that if the Z suspension is hydrothermally treated in the temperature range of 200-300°C, FeTi0) particles can be generated directly from the aqueous solution.
本発明に係るイルメナイト粒子粉末は、平均径０．０５
〜２．０μｍの黒色粒子粉末であり、反応ｐＨによって
粒子形態が異なった粒子が生成する。即ち、ｐＨ８．０
〜８．５においては粒状形態の粒子のみが、ｐＨ８．５
〜１０．０においては板状形態の粒子のみが生成する。The ilmenite particle powder according to the present invention has an average diameter of 0.05
It is a black particle powder of ~2.0 μm, and particles with different particle shapes are produced depending on the reaction pH. That is, pH 8.0
~8.5, only particles in granular form were present at pH 8.5.
~10.0, only plate-like particles are produced.
本発明に係るイルメナイト粒子粉末は、−Ｓ式ＦｅＴｉ
Ｏ３で示される通り、Ｔｉが４価であるにもかかわらず
後出実施例及び比較例に示す通り、Ｔｉ（５）を使用し
た場合には、ＦｅＴｊＯｓは生成せず、Ｔｉ（２）を使
用した場合にのみＦｅＴｉＯ３が生成する。The ilmenite particles according to the present invention are -S type FeTi
As shown by O3, although Ti is tetravalent, as shown in the Examples and Comparative Examples below, when Ti(5) is used, FeTjOs is not generated and Ti(2) is used. FeTiO3 is produced only in this case.
本発明者は、Ｔｉ（ＩＩＩ）を使用した場合にのみＦｅ
Ｔｉ０）が生成する理由について、Ｔｉ＠は強還元剤で
あり、高温の水溶液中においてＦｅ（Ｉｆの酸化を防止
すると共に、Ｔｉ＠が溶存酸素等により選択的に酸化さ
れてＴｉ面が徐々に供給される為、価数の差が大きい場
合には共沈が生じにくいという技術常識にもかかわらず
、Ｆｅ０ｒｌとＴｉ面の共沈が可能となったことによる
ものと考えている。The inventor found that Fe only when using Ti(III)
The reason for the formation of Ti0) is that Ti@ is a strong reducing agent and prevents the oxidation of Fe (If) in a high-temperature aqueous solution. We believe that this is due to the fact that coprecipitation between Fe0rl and Ti surfaces became possible, despite common technical knowledge that coprecipitation is difficult to occur when the difference in valence is large.
次に、本発明実施にあたっての諸条件について述べる。Next, various conditions for implementing the present invention will be described.
本発明におけるＦｅ（１１としては、硫酸第一鉄、塩化
第−鉄等を使用することができる。As Fe(11) in the present invention, ferrous sulfate, ferrous chloride, etc. can be used.
本発明におけるＴｉ（２）としては、三塩化チタン等を
使用することができる。As Ti(2) in the present invention, titanium trichloride or the like can be used.
本発明におけるアルカリとしては、炭酸ナトリウム、ア
ンモニウム水、水酸化ナトリウム等を用いることができ
、炭酸ナトリウム、アンモニア水が好ましい。As the alkali in the present invention, sodium carbonate, ammonium water, sodium hydroxide, etc. can be used, and sodium carbonate and ammonia water are preferable.
本発明における反応ｐＨは、８．０〜１０．０である。The reaction pH in the present invention is 8.0 to 10.0.
８．０以下の場合には、Ｆ ｅ ＴＩＩが沈澱すること
なく溶解し、アナターゼ型酸化チタン（Ｔｉｅ、）粒子
が単独で生成沈澱する。 ｉｏ、ｏ以上である場合には
、ＦｅＱ［ｌとＴｉ（ＩＶＩが共沈せずマグネタイト粒
子とイルメナイトとの混合物が生成する。When it is 8.0 or less, F e TII is dissolved without precipitating, and anatase-type titanium oxide (Tie) particles are independently formed and precipitated. io, o or more, FeQ[l and Ti(IVI) do not co-precipitate and a mixture of magnetite particles and ilmenite is produced.
本発明における反応温度は、２００〜３００“Ｃである
。 ２００℃以下である場合には、イルメナイト粒子
中にマグネタイト粒子やアナターゼ型酸化チタン（Ｔｉ
（ｈ）が混在する。３００℃以上である場合にもイルメ
ナイト粒子の生成は可能であるが、装置の安全性等を考
慮した場合、温度の上限は３００℃である。The reaction temperature in the present invention is 200 to 300"C. When the temperature is below 200"C, magnetite particles and anatase titanium oxide (Ti) are added to the ilmenite particles.
(h) is mixed. Although it is possible to generate ilmenite particles at a temperature of 300°C or higher, the upper limit of the temperature is 300°C when considering the safety of the apparatus.
次に、実施例並びに比較例により、本発明を説明する。 Next, the present invention will be explained with reference to Examples and Comparative Examples.
尚、以下の実施例並びに比較例における粒子の平均径は
電子顕ｖＩｉ鏡写真から測定した数値の平均値で示した
。In addition, the average diameter of particles in the following Examples and Comparative Examples is shown as the average value of numerical values measured from electron micrographs vIi.
実施例１
Ｆｅｓｏ、 ０．２１１１ｏｌ、 ＴｉＣｌ３ ０．
２ ｍｏｌと１ｌａ２ｃＯ＝ ｏ。Example 1 Feso, 0.2111 ol, TiCl3 0.
2 mol and 1la2cO = o.
５５ ｍｏｌとを混合して全ｇｌを３００ ｄとしたｐ
ｕ ８．３のアルカリ性Ｆｅ（ＯＨ）ｚ懸濁液をオート
クレーブに投入した後、２００℃まで加熱し、機械的に
攪拌しつつこの温度に５時間保持し、黒色沈澱を生成さ
せた。室温まで冷却後、黒色沈澱を常法により炉別、水
洗、乾燥した。55 mol to make the total gl 300 d.
After charging the alkaline Fe(OH)z suspension of u 8.3 into an autoclave, it was heated to 200°C and kept at this temperature for 5 hours with mechanical stirring to form a black precipitate. After cooling to room temperature, the black precipitate was separated in a furnace, washed with water, and dried in a conventional manner.
この黒色粒子粉末は、図１に示すＸ線回折図及びネール
点を評価した結果、ＦｅＴｉＯｓであり、図２に示す電
子顕微鏡写真（ｘ ５００００）に示す通り、平均径０
．０８μｍの粒状粒子であり、粒子が１個１個バラバラ
で粒度が均斉な粒子であった。図１中、ピークＡはイル
メナイトである。As a result of evaluating the X-ray diffraction pattern and Neel point shown in Figure 1, this black particle powder was found to be FeTiOs, and as shown in the electron micrograph (x 50000) shown in Figure 2, the average diameter was 0.
．． The particles were granular particles with a diameter of 0.08 μm, and each particle was dispersed and the particle size was uniform. In FIG. 1, peak A is ilmenite.
実施例２
ＦｅＳＯａ Ｏ，２ｍｏｌ、 ＴｉＣｌ３ ０．
２ ｍｏｌとＮａ、ＣＯｌ ０゜７５ ｍｏｌと
を混合して全容量を３００ｄとしたｐＨ９，５のアルカ
リ性Ｆｅ（ＯＨ）ｚ懸濁液をオートクレーブに投入した
後、２５０℃まで加熱し、機械的に攪拌しつつこの温度
に５時間保持し、黒色沈澱を生成させた。室温まで冷却
後、黒色沈澱を常法により炉別、水洗、乾燥した。Example 2 FeSOa O, 2 mol, TiCl3 0.
An alkaline Fe(OH)z suspension with a pH of 9.5 made by mixing 0.75 mol of Na, COl and 0.75 mol of Na, COl to a total volume of 300 d was charged into an autoclave, heated to 250°C, and mechanically This temperature was maintained for 5 hours with stirring to form a black precipitate. After cooling to room temperature, the black precipitate was separated in a furnace, washed with water, and dried in a conventional manner.
この黒色粒子粉末は、図３に示すＸ線回折図及びネール
点を評価した結果、ＦｅＴｉ０＊であり、電子顕微鏡観
察の結果、平均径２．０μｍの板状粒子であり、粒子が
１個１個バラバラで粒度が均斉な粒子であった。As a result of evaluating the X-ray diffraction diagram and Neel point shown in FIG. 3, this black particle powder is FeTi0*, and as a result of electron microscopy observation, it is plate-shaped particles with an average diameter of 2.0 μm, and each particle is 1. The particles were discrete and uniform in size.
比較例ｌ
Ｔ１Ｃｌ、の代わりにＴｉＣｌ４を用いた以外は、実施
例２と同様にして黒色沈澱を生成させた。室温まで冷却
後、黒色沈澱を常法により炉別、水洗、乾燥した。Comparative Example 1 A black precipitate was produced in the same manner as in Example 2, except that TiCl4 was used instead of T1Cl. After cooling to room temperature, the black precipitate was separated in a furnace, washed with water, and dried in a conventional manner.
この黒色粒子粉末は、図４に示すＸ線回折図に示す通り
、マグネタイト中に酸化チタンが混在した混合粒子粉末
であった。図４中、ピークＢはマグネタイト、ピークＣ
は酸化チタンである。As shown in the X-ray diffraction diagram shown in FIG. 4, this black particle powder was a mixed particle powder in which titanium oxide was mixed in magnetite. In Figure 4, peak B is magnetite, peak C
is titanium oxide.
比較例２
ＮａｚＣＯｓ ０．７５’＋＊ｏｌの代わりにＮａＯ
Ｈ３，Ｏｍａｔを用いてｐＨ１２のアルカリ性Ｆｅ（０
）１）ｚ Ｍ、濁液とした以外は、実施例２と同様にし
て黒色沈澱を生成させた。Comparative Example 2 NaO instead of NazCOs 0.75'+*ol
Alkaline Fe (0
)1)z A black precipitate was produced in the same manner as in Example 2, except that a turbid liquid was used.
室温まで冷却後、黒色沈澱を常法により炉別、水洗、乾
燥した。After cooling to room temperature, the black precipitate was separated in a furnace, washed with water, and dried in a conventional manner.
この黒色粒子粉末は、図５に示すＸ線回折図に示す通り
、マグネタイト中に少量のイルメナイトが混在した混合
粒子粉末であった。図５中、ピークＡはイルメナイト、
ピークＢはマグネタイトである。As shown in the X-ray diffraction diagram shown in FIG. 5, this black particle powder was a mixed particle powder in which a small amount of ilmenite was mixed in magnetite. In Figure 5, peak A is ilmenite,
Peak B is magnetite.
比較例３
１ＪａｚｃＯ３０，７５＋＊ｏｌの代わりにＮａＯＨ０
，４５ｅａｌを用いてＰＨ７，０のアルカリ性Ｆｅ （
ＯＨ） ｚ懸濁液とした以外は、実施例２と同様にして
黒色沈澱を生成させた。室温まで冷却後、黒色沈澱を常
法により炉別、水洗、乾燥した。Comparative Example 3 NaOH0 instead of 1JazcO30,75+*ol
, 45eal was used to prepare alkaline Fe (
A black precipitate was produced in the same manner as in Example 2, except that a suspension was used. After cooling to room temperature, the black precipitate was separated in a furnace, washed with water, and dried in a conventional manner.
この粒子粉末は、図６に示すＸ線回折図に、示す通り、
酸化チタンのピークのみが認められた。図６中、ピーク
Ｃは酸化チタンである。As shown in the X-ray diffraction diagram shown in FIG.
Only the peak of titanium oxide was observed. In FIG. 6, peak C is titanium oxide.
比較例４
反応温度１８０”Ｃとした以外は、実施例２と同様にし
て黒色沈澱を生成させた。室温まで冷却後、黒色沈澱を
常法によりｐ別、水洗、乾燥した。Comparative Example 4 A black precipitate was produced in the same manner as in Example 2, except that the reaction temperature was 180"C. After cooling to room temperature, the black precipitate was separated by p, washed with water, and dried in a conventional manner.
この粒子粉末は、図７に示すＸ線回折図に示す通り、イ
ルメナイト粒子中にマグネタイト粒子や酸化チタンが混
在した混合粒子粉末であった。図７中、ピークＡはイル
メナイト、ピークＢはマグ２タイト、ピークＣは酸化チ
タンである。As shown in the X-ray diffraction diagram shown in FIG. 7, this particle powder was a mixed particle powder in which magnetite particles and titanium oxide were mixed in ilmenite particles. In FIG. 7, peak A is ilmenite, peak B is mag2tite, and peak C is titanium oxide.
本発明に係るイルメナイト粒子粉末は、前出実施例に示
した通り、水溶液中から直接生成させることができるこ
とに起因して粒子が１個１個バラバラであり、且つ、粒
度が均斉である為ビヒクル中又は樹脂中での分散性に優
れ、また、平均径０゜０５〜２．０μｍの粒子である為
作業性に優れ、しかも、耐熱性に優れた粒子であるから
、塗料用、トナー用黒色顔料粒子粉末として好適である
。As shown in the above example, the ilmenite particles according to the present invention can be produced directly from an aqueous solution, so the particles are individually dispersed, and the particle size is uniform, so the vehicle The particles have excellent dispersibility in medium or resin, and have an average diameter of 0.05 to 2.0 μm, making them excellent in workability. Furthermore, the particles have excellent heat resistance, making them suitable for use in black paints and toners. Suitable as pigment particle powder.
ξた、本発明に係るイルメナイト粒子粉末は、周知の通
り、硬度５〜６程度を有するものであるから、研磨剤と
しての使用も期待される。In addition, since the ilmenite particles according to the present invention have a hardness of about 5 to 6, as is well known, it is also expected to be used as an abrasive.
図１及び図３乃至図７は、いずれもＸ線回折図であり、
それぞれ実施例１、実施例２及び比較例１乃至比較例４
で得られた粒子粉末である。
図２は電子顕微鏡写真（Ｘ ５００００）であり、実施
例１で得られた粒状イルメナイト粒子粉末である。1 and 3 to 7 are all X-ray diffraction diagrams,
Example 1, Example 2, and Comparative Examples 1 to 4, respectively.
This is the particle powder obtained in . FIG. 2 is an electron micrograph (X 50000) of the granular ilmenite particles obtained in Example 1.
Claims (2)
個１個バラバラであり且つ粒度が均斉なＦｅＴｉＯ＿３
粒子からなるイルメナイト粒子粉末。(1) The average diameter is 0.05 to 2.0 μm, and the particle size is 1
FeTiO_3 with individual pieces and uniform particle size
Ilmenite particle powder consisting of particles.
カリ性Ｆｅ（ＯＨ）＿２懸濁液を２００〜３００℃の温
度範囲で水熱処理することにより平均径０．０５〜２．
０μｍであって、粒子が１個１個バラバラであり且つ粒
度が均斉なＦｅＴｉＯ＿３粒子を生成させることを特徴
とするイルメナイト粒子粉末の製造法。(2) An alkaline Fe(OH)_2 suspension containing Ti(III) with a pH of 8.0 to 10.0 is hydrothermally treated in a temperature range of 200 to 300°C to obtain an average diameter of 0.05 to 2.
A method for producing ilmenite particle powder, which is characterized by producing FeTiO_3 particles having a size of 0 μm, each particle being discrete, and uniform in particle size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63128706A JPH01298028A (en) | 1988-05-25 | 1988-05-25 | Illumenite powder and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63128706A JPH01298028A (en) | 1988-05-25 | 1988-05-25 | Illumenite powder and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01298028A true JPH01298028A (en) | 1989-12-01 |
Family
ID=14991414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63128706A Pending JPH01298028A (en) | 1988-05-25 | 1988-05-25 | Illumenite powder and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01298028A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006317927A (en) * | 2005-04-15 | 2006-11-24 | Toda Kogyo Corp | Iron-based black particulate powder for toner |
| JP2007126348A (en) * | 2005-10-07 | 2007-05-24 | Mitsui Mining & Smelting Co Ltd | Low magnetic black pigment particle, electrophotographic toner and image forming method |
| US7327974B2 (en) | 2002-09-12 | 2008-02-05 | Ricoh Printing Systems, Ltd. | Electrophotographic toner and image-forming system |
| CN108298591A (en) * | 2018-04-13 | 2018-07-20 | 哈尔滨工业大学 | A kind of synthetic method of hexagon iron titanate nanometer sheet material and application |
-
1988
- 1988-05-25 JP JP63128706A patent/JPH01298028A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7327974B2 (en) | 2002-09-12 | 2008-02-05 | Ricoh Printing Systems, Ltd. | Electrophotographic toner and image-forming system |
| US7459252B2 (en) | 2002-09-12 | 2008-12-02 | Ricoh Printing Systems, Ltd. | Electrophotographic toner |
| JP2006317927A (en) * | 2005-04-15 | 2006-11-24 | Toda Kogyo Corp | Iron-based black particulate powder for toner |
| JP2007126348A (en) * | 2005-10-07 | 2007-05-24 | Mitsui Mining & Smelting Co Ltd | Low magnetic black pigment particle, electrophotographic toner and image forming method |
| JP4682063B2 (en) * | 2005-10-07 | 2011-05-11 | 三井金属鉱業株式会社 | Low magnetic black pigment particles, electrophotographic toner, and image forming method |
| CN108298591A (en) * | 2018-04-13 | 2018-07-20 | 哈尔滨工业大学 | A kind of synthetic method of hexagon iron titanate nanometer sheet material and application |
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