JPH0557213B2 - - Google Patents
Info
- Publication number
- JPH0557213B2 JPH0557213B2 JP24254385A JP24254385A JPH0557213B2 JP H0557213 B2 JPH0557213 B2 JP H0557213B2 JP 24254385 A JP24254385 A JP 24254385A JP 24254385 A JP24254385 A JP 24254385A JP H0557213 B2 JPH0557213 B2 JP H0557213B2
- Authority
- JP
- Japan
- Prior art keywords
- hematite
- particles
- iron complex
- vapor
- 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.)
- Expired - Fee Related
Links
- 229910052595 hematite Inorganic materials 0.000 claims description 45
- 239000011019 hematite Substances 0.000 claims description 45
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 45
- 239000000843 powder Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011882 ultra-fine particle Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 53
- 239000007789 gas Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000012535 impurity Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 229910000859 α-Fe Inorganic materials 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000010419 fine particle Substances 0.000 description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 7
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052748 manganese Inorganic materials 0.000 description 5
- 239000011572 manganese Chemical class 0.000 description 5
- 239000006200 vaporizer Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 4
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 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
- 238000004898 kneading Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011701 zinc Chemical class 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000010949 copper Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、β−ジケトン鉄錯体を加水分解して
得られる平均径500Å以下の高純度ヘマタイト超
微粒子粉末及びその製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a highly purified ultrafine hematite particle powder with an average diameter of 500 Å or less obtained by hydrolyzing a β-diketone iron complex, and a method for producing the same.
本発明に係る高純度ヘマタイト超微粒子粉末の
主な用途は、フエライト用原料粉末、塗料用顔料
粉末及び、ゴム・プラスチツク用着色剤、触媒等
である。 The main uses of the high-purity hematite ultrafine particle powder according to the present invention are raw material powder for ferrite, pigment powder for paints, coloring agents for rubber and plastics, catalysts, etc.
ヘマタイト粒子粉末は、フエライト用原料粉末
として現在広く使用されている。
Hematite particle powder is currently widely used as a raw material powder for ferrite.
即ち、フエライトは、ヘマタイト粒子粉末等の
主原料とBa、Sr若しくはPb化合物等、又は、
Zn、Mn、Ni、Mg、若しくはCu化合物等の副
原料とを混合し、加熱焼成、粉砕することにより
製造されている。 In other words, ferrite is produced by mixing the main raw material such as hematite particles with auxiliary raw materials such as Ba, Sr, or Pb compounds, or Zn, Mn, Ni, Mg, or Cu compounds, heating and sintering, and pulverizing the mixture. Manufactured.
また、ヘマタイト粒子粉末は、赤色を呈してい
る為、顔料とビヒクルとを混合して塗料を製造す
る際の塗料用顔料粉末として広く使用されてお
り、殊に、500Å以下の超微粒子は紫外線吸収効
果並びに透明性を発現する等の特徴がある為、紫
外線吸収フイルム用透明性顔料粉末として使用さ
れており、更に、ゴム・プラスチツクに混練・分
散して着色剤としても使用されている。 In addition, because hematite particles have a red color, they are widely used as pigment powders for paints when mixing pigments and vehicles to produce paints.In particular, ultrafine particles of 500 Å or less absorb ultraviolet rays. Because of its effectiveness and transparency, it is used as a transparent pigment powder for ultraviolet absorbing films, and is also used as a coloring agent by kneading and dispersing rubber and plastics.
更に、ヘマタイト粒子粉末は、触媒としても使
用されている。 Furthermore, hematite particle powder has also been used as a catalyst.
上記した通り、ヘマタイト粒子粉末は、様々の
分野で使用されているが、いずれの分野において
も共通して要求されるヘマタイト粒子粉末の特性
は、粒度の微細化と純度が高いことである。 As mentioned above, hematite particles are used in various fields, and the characteristics commonly required for hematite particles in all fields are fine particle size and high purity.
即ち、フエライトの製造にあたつては、主原料
であるヘマタイト粒子の粒度が微細化すればする
程、原料の均一混合が可能となり、その結果、フ
エライト化反応の進行が容易となり、また、ヘマ
タイト粒子の純度が高ければ高い程、最終製品で
あるフエライトの性能は向上する。 In other words, in the production of ferrite, the finer the particle size of hematite particles, which are the main raw material, the more uniform the raw materials can be mixed, and as a result, the progress of the ferrite reaction is easier. The higher the purity of the particles, the better the performance of the final ferrite product.
この事実は、例えば、粉体工学第７巻第８号
（1970年）第46頁の「フエライト化反応は粒度が
小さいほど反応性は増大する。」なる記載、及び、
特公昭49−15360号公報の「……酸化第２鉄（ヘ
マタイト）中には……不純物が蓄積され、高性能
化小型化を要求される磁性体、特に、ソフト系の
マンガン・亜鉛系或いはマンガン・マグネシウム
系等の複合フエライトには全く使用が出来ず…
…」なる記載からも明らかである。 This fact is reflected in, for example, the statement in Powder Engineering Vol. 7, No. 8 (1970), page 46, "The smaller the particle size, the greater the reactivity of the ferrite formation reaction."
Japanese Patent Publication No. 49-15360 states, ``...impurities accumulate in ferric oxide (hematite), and magnetic materials that require high performance and miniaturization, especially soft manganese/zinc-based or It cannot be used at all for composite ferrites such as manganese and magnesium...
It is clear from the statement "...".
次に、塗料の製造においては塗料化に際して、
ゴム・プラスチツクの製造においては混練に際し
てヘマタイト粒子粉末を均一、且つ、容易に分散
させることが必要であり、その為には、出来るだ
け微細なヘマタイト粒子粉末が要求される。ま
た、ヘマタイト粒子中の不純物が多くなる程、ヘ
マタイト粒子の色調は不鮮明となり、赤色から赤
褐色又は、赤紫色に変化する為、純度の高いこと
が要求される。 Next, in the production of paint, when converting it into paint,
In the production of rubber and plastics, it is necessary to uniformly and easily disperse hematite particles during kneading, and for this purpose, hematite particles as fine as possible are required. Furthermore, as the amount of impurities in the hematite particles increases, the color tone of the hematite particles becomes unclear and changes from red to reddish brown or reddish-purple, so high purity is required.
更に、ヘマタイト粒子を触媒として使用するに
際しては、粒子が微細化すればする程、また、純
度が高くなればなる程、触媒活性が向上する。 Furthermore, when using hematite particles as a catalyst, the finer the particles and the higher the purity, the better the catalytic activity.
従来、ヘマタイト粒子粉末の製造法としては、
第一鉄塩水溶液とアルカリとを反応させて得られ
た水酸化第一鉄を含む反応水溶液に酸素含有ガス
を通気することにより、水溶液中から出発原料と
してのマグネタイト粒子を生成させ、次いで、該
マグネタイト粒子粉末を空気中で加熱する方法が
知られている。 Conventionally, the manufacturing method of hematite particle powder is as follows:
By passing an oxygen-containing gas through a reaction aqueous solution containing ferrous hydroxide obtained by reacting an aqueous ferrous salt solution with an alkali, magnetite particles as a starting material are generated from the aqueous solution, and then A method of heating magnetite particle powder in air is known.
粒度が微細であり、且つ、純度の高いヘマタイ
ト粒子粉末は、現在最も要求されているところで
あるが、上記した通りの公知方法による場合に
は、反応条件により、種々の粒度を有するマグネ
タイト粒子を生成させることができるが、その大
きさは10000〜1000Å程度であり、1000Å程度以
下のマグネタイト粒子を生成させることは困難で
ある。従つて、水溶液中から生成したマグネタイ
ト粒子を空気中で加熱して得られるヘマタイト粒
子もその大きさは、10000〜1000Å程度であり、
1000Å程度以下、特に500Å以下のヘマタイト粒
子を得ることは非常に困難である。
Hematite particles with fine particle size and high purity are currently most in demand, but when using the above-mentioned known method, magnetite particles with various particle sizes can be produced depending on the reaction conditions. However, the size is about 10,000 to 1,000 Å, and it is difficult to generate magnetite particles with a size of about 1,000 Å or less. Therefore, the size of hematite particles obtained by heating magnetite particles generated from an aqueous solution in the air is about 10,000 to 1,000 Å,
It is very difficult to obtain hematite particles with a diameter of about 1000 Å or less, especially 500 Å or less.
また、公知方法による場合には、原料である第
一鉄塩水溶液がMn、Si等の不純物を含有してい
る為、水溶液中から生成するマグネタイト粒子は
一般に4.0〜1.0重量％の不純物を含有しており、
このマグネタイト粒子を空気中で加熱して得られ
るヘマタイト粒子も当然4.0〜1.0重量％の不純物
を含有するものとなる。 In addition, when using a known method, the raw material ferrous salt aqueous solution contains impurities such as Mn and Si, so the magnetite particles produced from the aqueous solution generally contain 4.0 to 1.0% by weight of impurities. and
Hematite particles obtained by heating these magnetite particles in air naturally also contain 4.0 to 1.0% by weight of impurities.
そこで、粒度が微細であり、且つ、純度の高い
ヘマタイト粒子粉末を得る為の技術手段の確立が
強く要望されている。 Therefore, there is a strong demand for the establishment of technical means for obtaining hematite particles with fine particle size and high purity.
本発明者は、粒度が微細であり、且つ、純度の
高いヘマタイト粒子粉末を得るべく種々検討を重
ねた結果、本発明に到達したのである。
The present inventor has arrived at the present invention as a result of various studies in order to obtain hematite particle powder with fine particle size and high purity.
即ち、本発明は、β−ジケトン鉄錯体を加水分
解して得られる平均径500Å以下の高純度ヘマタ
イト超微粒子粉末及びβ−ジケトン鉄錯体の蒸気
と水蒸気とを気相中500℃〜900℃の温度範囲で反
応して上記β−ジケトン鉄錯体を加水分解するこ
とによりヘマタイト超微粒子を生成させることよ
りなる高純度ヘマタイト超微粒子粉末の製造方法
である。 That is, the present invention provides high-purity hematite ultrafine particle powder with an average diameter of 500 Å or less obtained by hydrolyzing a β-diketone iron complex and steam of the β-diketone iron complex and water vapor at a temperature of 500°C to 900°C in a gas phase. This is a method for producing ultrafine hematite powder, which comprises producing ultrafine hematite particles by reacting in a temperature range and hydrolyzing the β-diketone iron complex.
先ず、本発明において最も重要な点は、β−ジ
ケトン鉄錯体の蒸気と水蒸気とを気相中で反応さ
せた場合には、粒度の微細な、殊に、500Å以下
の超微粒子であり、且つ、純度の高いヘマタイト
微粒子粉末が得られる点である。
First, the most important point in the present invention is that when the vapor of the β-diketone iron complex and water vapor are reacted in the gas phase, the particle size is fine, especially ultrafine particles of 500 Å or less, and The point is that fine hematite powder with high purity can be obtained.
本発明においては、鉄原料として蒸気となりや
すいβ−ジケトン鉄錯体を用い、且つ、β−ジケ
トン鉄錯体の蒸気と水蒸気との気相中における反
応であることに起因して、水溶液中での反応に比
べ、短時間裡に反応が生起し、また、ヘマタイト
中の不純物含量として一般に重視されているSi、
Mn、Al、Ca及びこれらを含む酸化物等の化合物
は高沸点である為、本発明の反応に寄与すること
なくそのまま原料β−ジケトン鉄錯体中に残存
し、しかも、工程中からの不純物の混入が防止さ
れることによつて、粒度が微細な、殊に、500Å
以下の超微粒子であり、且つ、純度の高いヘマタ
イト微粒子粉末を得ている。 In the present invention, a β-diketone iron complex that easily becomes vapor is used as the iron raw material, and since the reaction is performed in the gas phase between the vapor of the β-diketone iron complex and water vapor, the reaction in an aqueous solution is possible. Compared to Si, the reaction occurs in a short period of time, and Si, which is generally emphasized as an impurity content in hematite,
Compounds such as Mn, Al, Ca, and oxides containing these have high boiling points, so they remain in the raw material β-diketone iron complex without contributing to the reaction of the present invention, and moreover, they are free from impurities during the process. By preventing contamination, particles with fine particle size, especially 500Å
The following ultrafine and highly pure hematite fine particle powder was obtained.
次に、本発明実施にあたつ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β−ジケトン鉄錯体としては、
鉄アセチルアセトナート等が使用できる。本発明
におけるβ−ジケトン鉄錯体の蒸気は、β−ジケ
トン鉄錯体をN2ガス等の不活性ガスを通じた気
化器内に入れ、100〜180℃で加熱して気化させる
ことにより得られる。気化器内に不活性ガスを通
じるのは、β−ジケトン鉄錯体とO2又はH2Oと
の反応が生起するのを防止する為である。 As the β-diketone iron complex in the present invention,
Iron acetylacetonate, etc. can be used. The vapor of the β-diketone iron complex in the present invention can be obtained by putting the β-diketone iron complex into a vaporizer through which an inert gas such as N 2 gas is passed, and heating it at 100 to 180°C to vaporize it. The purpose of passing an inert gas into the vaporizer is to prevent a reaction between the β-diketone iron complex and O 2 or H 2 O.
加熱温度は、100〜180℃である。温度が高くな
る程、気化速度が速くなり、β−ジケトン鉄錯体
の蒸気濃度が高くなる為、生成ヘマタイト粒子の
粒度は大きくなる傾向にある。 Heating temperature is 100-180°C. As the temperature becomes higher, the vaporization rate becomes faster and the vapor concentration of the β-diketone iron complex becomes higher, so the particle size of the produced hematite particles tends to become larger.
温度が100℃未満である場合には、β−ジケト
ン鉄錯体の蒸気濃度が非常に低くなり、ヘマタイ
ト粒子を効率的に生成することができない。 If the temperature is less than 100°C, the vapor concentration of the β-diketone iron complex becomes very low, and hematite particles cannot be efficiently produced.
温度が180℃を越える場合には、β−ジケトン
鉄錯体が熱分解し、蒸気の発生が困難となり、ま
た、不純物が混入しやすくなる。 If the temperature exceeds 180°C, the β-diketone iron complex will thermally decompose, making it difficult to generate steam and making it easy for impurities to be mixed in.
本発明における水蒸気は、水の飽和器を50〜70
℃に加熱し、これにN2ガス等の不活性ガスをキ
ヤリアガスとして吹き込むことにより得られる。 The water vapor in the present invention has a water saturation capacity of 50 to 70
It is obtained by heating it to ℃ and blowing an inert gas such as N 2 gas as a carrier gas into it.
50℃未満である場合には、水蒸気の濃度が低く
なり、β−ジケトン鉄錯体の加水分解反応が不充
分となる。 When the temperature is lower than 50°C, the concentration of water vapor becomes low, and the hydrolysis reaction of the β-diketone iron complex becomes insufficient.
70℃を越える場合には、水蒸気の濃度が高くな
つてβ−ジケトン鉄錯体の加水分解反応が激しく
なる為、生成ヘマタイト粒子相互間において凝集
が生起しやすくなる。 If the temperature exceeds 70°C, the concentration of water vapor becomes high and the hydrolysis reaction of the β-diketone iron complex becomes intense, so that agglomeration is likely to occur between the produced hematite particles.
本発明における気相中における反応は、β−ジ
ケトン鉄錯体の蒸気と水蒸気とを500〜900℃に加
熱した反応炉に導入することにより行う。 The reaction in the gas phase in the present invention is carried out by introducing the steam of the β-diketone iron complex and water vapor into a reactor heated to 500 to 900°C.
反応炉への導入は、β−ジケトン鉄錯体の蒸気
と水蒸気の両者を別々に導入しても、又は、両者
を混合した後に導入しても良い。 Both the β-diketone iron complex steam and water vapor may be introduced into the reactor separately, or they may be mixed and then introduced.
気相中における反応濃度はβ−ジケトン鉄錯体
の蒸気の流量及び水蒸気の流量により調整するこ
とが出来る。反応蒸気濃度が高くなると生成ヘマ
タイトの粒度が大きくなる傾向にある。生成する
ヘマタイト粒子の粒度を考慮すれば、β−ジケト
ン鉄錯体の蒸気の流量は、50〜1500ml／分、水蒸
気の流量は、50〜300ml／分が望ましい。本発明
の気相中における反応温度は、500〜900℃であ
る。 The reaction concentration in the gas phase can be adjusted by controlling the flow rate of the β-diketone iron complex vapor and the flow rate of water vapor. As the reaction vapor concentration increases, the particle size of the produced hematite tends to increase. Considering the particle size of hematite particles to be produced, the flow rate of the β-diketone iron complex steam is preferably 50 to 1500 ml/min, and the flow rate of steam is preferably 50 to 300 ml/min. The reaction temperature in the gas phase of the present invention is 500 to 900°C.
500℃未満である場合には、β−ジケトン鉄錯
体の加水分解反応が十分生起しない。 When the temperature is lower than 500°C, the hydrolysis reaction of the β-diketone iron complex does not occur sufficiently.
900℃を越える場合には、生成ヘマタイト粒子
相互間で焼結が生起しやすくなる。 If the temperature exceeds 900°C, sintering tends to occur between the produced hematite particles.
次に、実施例により本発明を説明する。 Next, the present invention will be explained by examples.
尚、以下の実施例における粒子の平均径は電子
顕微鏡写真から測定した数値で示した。 In addition, the average diameter of particles in the following examples is shown as a value measured from an electron micrograph.
また、粒子中のFeは、「螢光Ｘ線分析装置
3063M型」（理学電機工業製）を使用し、JIS
K0119−1979の「けい光Ｘ線分析通則」に従つ
て、螢光Ｘ線分析を行うことにより測定した。 In addition, Fe in particles can be detected using a fluorescent X-ray analyzer.
3063M type" (manufactured by Rigaku Denki Kogyo), JIS
It was measured by performing fluorescence X-ray analysis in accordance with the "General rules for fluorescence X-ray analysis" of K0119-1979.
実施例 １
鉄アセチルアセトナート〔Fe（C2H7O2）3〕２
ｇを流量500ml／分の窒素ガスを通じた気化器に
入れた後、温度110℃に加熱して、上記アセチル
アセトナートの蒸気を生成した。Example 1 Iron acetylacetonate [Fe(C 2 H 7 O 2 ) 3 ] 2
g was put into a vaporizer through which nitrogen gas was passed at a flow rate of 500 ml/min, and then heated to a temperature of 110° C. to generate the acetylacetonate vapor.
別に、水の飽和器を50℃に加熱し、この飽和器
内に流量300ml／分の窒素ガスを吹き込むことに
より、水蒸気同伴ガスとした。 Separately, a water saturator was heated to 50° C., and nitrogen gas was blown into the saturator at a flow rate of 300 ml/min to produce water vapor entrained gas.
上記アセチルアセトナートの蒸気と上記水蒸気
同伴ガスとを連続的に混合して反応炉に導き、
500℃で加熱した。 The acetylacetonate vapor and the water vapor entrained gas are continuously mixed and introduced into a reactor;
Heated at 500℃.
得られた粒子粉末は、Ｘ線回折の結果、ヘマタ
イト相から成り立つており、図１の電子顕微鏡写
真（×30000）によれば、平均径70Åの超微粒子
であつた。また、このヘマタイト粒子粉末の
Fe2O3分は99.80重量％であり、不純物の少ないも
のであつた。 As a result of X-ray diffraction, the obtained particles were found to be composed of a hematite phase, and according to the electron micrograph (×30000) in FIG. 1, they were ultrafine particles with an average diameter of 70 Å. In addition, this hematite particle powder
The Fe 2 O 3 min content was 99.80% by weight, which was low in impurities.
実施例 ２
鉄アセチルアセトナート〔Fe（C2H7O2）3〕２
ｇを流量500ml／分の窒素ガスを通じた気化器に
入れた後、温度120℃に加熱して、上記アセチル
アセトナートの蒸気を生成した。Example 2 Iron acetylacetonate [Fe(C 2 H 7 O 2 ) 3 ] 2
g was put into a vaporizer through which nitrogen gas was passed at a flow rate of 500 ml/min, and then heated to a temperature of 120° C. to produce the acetylacetonate vapor.
別に、水の飽和器を60℃に加熱し、この飽和器
内に流量300ml／分の窒素ガスを吹き込むことに
より、水蒸気同伴ガスとした。 Separately, a water saturator was heated to 60° C., and nitrogen gas was blown into the saturator at a flow rate of 300 ml/min to produce water vapor entrained gas.
上記アセチルアセトナートの蒸気と上記水蒸気
同伴ガスとを連続的に混合して反応炉に導き、
700℃で加熱した。 The acetylacetonate vapor and the water vapor entrained gas are continuously mixed and introduced into a reactor;
Heated at 700℃.
得られた粒子粉末は、Ｘ線回折の結果、ヘマタ
イト相から成り立つており、電子顕微鏡観察の結
果、平均径200Åの超微粒子であつた。また、こ
のヘマタイト粒子粉末のFe2O3分は99.65重量％で
あり、不純物の少ないものであつた。 As a result of X-ray diffraction, the obtained powder particles were found to be composed of a hematite phase, and as a result of electron microscopic observation, they were ultrafine particles with an average diameter of 200 Å. Further, the Fe 2 O 3 content of this hematite particle powder was 99.65% by weight, indicating that there were few impurities.
実施例 ３
鉄アセチルアセトナート〔Fe（C2H7O2）3〕２
ｇを流量500ml／分の窒素ガスを通じた気化器に
入れた後、温度140℃に加熱して、上記アセチル
アセトナートの蒸気を生成した。Example 3 Iron acetylacetonate [Fe(C 2 H 7 O 2 ) 3 ] 2
g was put into a vaporizer through which nitrogen gas was passed at a flow rate of 500 ml/min, and then heated to a temperature of 140° C. to produce the acetylacetonate vapor.
別に、水の飽和器を60℃に加熱し、この飽和器
内に流量300ml／分の窒素ガスを含むことにより、
水蒸気同伴ガスとした。 Separately, by heating a water saturator to 60°C and containing nitrogen gas at a flow rate of 300 ml/min in this saturator,
Water vapor was used as a gas.
上記アセチルアセトナートの蒸気と上記水蒸気
同伴ガスとを連続的に混合して反応炉に導き、
900℃で加熱した。 The acetylacetonate vapor and the water vapor entrained gas are continuously mixed and introduced into a reactor;
Heated at 900℃.
得られた粒子粉末は、Ｘ線回折の結果、ヘマタ
イト相から成り立つており、電子顕微鏡写真観察
の結果、平均径350Åの超微粒子であつた。また、
このヘマタイト粒子粉末のFe2O3分は99.55重量％
であり、不純物の少ないものであつた。 As a result of X-ray diffraction, the obtained powder particles were found to be composed of a hematite phase, and as a result of electron micrograph observation, they were ultrafine particles with an average diameter of 350 Å. Also,
The Fe2O3 content of this hematite particle powder is 99.55 % by weight
It had few impurities.
〔効果〕
本発明に係るヘマタイト粒子粉末は、前出実施
例に示した通り、粒度の微細な、殊に、500Å以
下の超微粒子であり、且つ、純度の高いものであ
るから、フエライト用原料粉末、塗料用顔料粉
末、殊に、紫外線吸収フイルム用透明性顔料粉末
及びゴム・プラスチツク用着色剤、触媒として好
適である。[Effects] As shown in the above examples, the hematite particles according to the present invention have fine particle sizes, especially ultrafine particles of 500 Å or less, and are highly pure, so they can be used as raw materials for ferrite. It is suitable as a powder, a pigment powder for paints, especially a transparent pigment powder for ultraviolet absorbing films, a colorant for rubber and plastics, and a catalyst.
図１は、実施例１で得られたヘマタイト超微粒
子粉末の粒子構造を示す電子顕微鏡写真（×
30000）である。
Figure 1 is an electron micrograph showing the particle structure of the ultrafine hematite powder obtained in Example 1 (×
30000).
Claims (1)
平均径500Å以下の高純度ヘマタイト超微粒子粉
末。 ２ β−ジケトン鉄錯体の蒸気と水蒸気とを気相
中500℃〜900℃の温度範囲で反応して上記β−ジ
ケトン鉄錯体を加水分解することによりヘマタイ
ト超微粒子を生成させることを特徴とする高純度
ヘマタイト超微粒子粉末の製造方法。[Scope of Claims] 1. High purity hematite ultrafine particle powder with an average diameter of 500 Å or less obtained by hydrolyzing a β-diketone iron complex. 2. Ultrafine particles of hematite are produced by reacting the vapor of the β-diketone iron complex with water vapor in the gas phase in a temperature range of 500°C to 900°C to hydrolyze the β-diketone iron complex. A method for producing high-purity hematite ultrafine particle powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24254385A JPS62100420A (en) | 1985-10-28 | 1985-10-28 | Production of ultrafine grain powder of high-purity hematite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24254385A JPS62100420A (en) | 1985-10-28 | 1985-10-28 | Production of ultrafine grain powder of high-purity hematite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62100420A JPS62100420A (en) | 1987-05-09 |
| JPH0557213B2 true JPH0557213B2 (en) | 1993-08-23 |
Family
ID=17090671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24254385A Granted JPS62100420A (en) | 1985-10-28 | 1985-10-28 | Production of ultrafine grain powder of high-purity hematite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62100420A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0616447U (en) * | 1992-08-04 | 1994-03-04 | 株式会社アサヒ産業 | Material for gasket |
| DE19936868A1 (en) * | 1999-08-05 | 2001-02-15 | Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh | Method and device for producing oxidic nanocrystals |
| KR100487905B1 (en) * | 2002-10-02 | 2005-05-06 | 한국과학기술연구원 | Shape anisotropic iron oxide nano-particles and synthetic method thereof |
-
1985
- 1985-10-28 JP JP24254385A patent/JPS62100420A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62100420A (en) | 1987-05-09 |
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