JPH0340921A - Production of ferrite powder by spray roasting method - Google Patents
Production of ferrite powder by spray roasting methodInfo
- Publication number
- JPH0340921A JPH0340921A JP17558489A JP17558489A JPH0340921A JP H0340921 A JPH0340921 A JP H0340921A JP 17558489 A JP17558489 A JP 17558489A JP 17558489 A JP17558489 A JP 17558489A JP H0340921 A JPH0340921 A JP H0340921A
- Authority
- JP
- Japan
- Prior art keywords
- ferrite powder
- flow
- ferrite
- roasting
- chloride
- 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
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 68
- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000007921 spray Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 239000007789 gas Substances 0.000 claims abstract description 29
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 11
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000005507 spraying Methods 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 25
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 229910001035 Soft ferrite Inorganic materials 0.000 description 11
- 238000010586 diagram Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 238000000975 co-precipitation Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000011592 zinc chloride Substances 0.000 description 4
- 235000005074 zinc chloride Nutrition 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910018605 Ni—Zn Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000012717 electrostatic precipitator Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はフェライト粉体の製造技術に関し、更に詳しく
は、フェライトを構成する金属のその塩化物を含む溶液
を噴霧焙焼して一気にフェライト粉体を製造する技術に
関する。Detailed Description of the Invention [Industrial Application Field] The present invention relates to a technology for producing ferrite powder, and more specifically, a solution containing chlorides of metals constituting ferrite is spray roasted to produce ferrite powder all at once. Concerning the technology of manufacturing the body.
［従来の技術・課題］
フェライト粉体に要求される特性として（ａ）粒度分布
が狭いこと、（ｂ）化学ｆｆｌ戒が均一であること、（
ｅ）化学的に高純度であること等が挙げられる。これら
の要求される諸特性を満足するフェライト粉体を製造す
る方法を開発すべく、鋭意研究がなされてきた。[Prior art/problems] The characteristics required of ferrite powder are (a) narrow particle size distribution, (b) uniform chemical ffl, (
e) High chemical purity. Intensive research has been conducted to develop a method for producing ferrite powder that satisfies these required properties.
現在実用化されているフェライト粉体の製造方法は、Ｎ
）乾式法、（ＩＩ）共沈法、（Ｉ［［）ルスナ一方式に
よる噴霧焙焼法の三つの方法があるが、それぞれに問題
があり、満足のいく方法とは言えない。The manufacturing method of ferrite powder currently in practical use is N
There are three methods: (1) dry method, (II) coprecipitation method, and (1) spray roasting method using Rusna method, but each method has its own problems and cannot be said to be a satisfactory method.
（１）乾式法（工程系統図を第２図ａに示す）フェライ
トを構成する金属の酸化物または炭酸塩を所定のモル比
に湿式混合し、乾燥後造粒して仮焼を行い、フェライト
化させて得られる固い塊状物の粉砕により、フェライト
粉体を製造する方法である。(1) Dry method (The process diagram is shown in Figure 2a) Metal oxides or carbonates constituting ferrite are wet mixed at a predetermined molar ratio, dried, granulated, and calcined to produce ferrite. This is a method for producing ferrite powder by crushing the hard lumps obtained by oxidation.
本性は最も一般的な製造法であり、実用化されている製
造法の主流をなすものである。安定した特性のフェライ
ト粉体を製造できるという技術の面では完成の域に達し
つつある方法であるが、■粉砕により所定の粒度にフェ
ライト粉体を整えるが、粒度分布の狭い粉体を得ること
が困難である；
■フェライト化を固相反応により行うので、微視的なレ
ベルでは化学組成に不均一性が認められ、それを均質に
することは困難である；
■湿式混合と粉砕に長時間を要し、この操作において外
部より不純物く特に５ｉＯ２）の混入が避けられなく、
高純度の粉体を得難い、また、装置よりの鉄の混入があ
り、鉄の組成ずれが起こる；■フェライト化を行う仮焼
は８００〜１０００’Ｃの比較的高温下で長時間行う必
要があること、また、湿式混合及び粉砕もそれぞれ１０
〜４０時間という長時間の処理を要することにより、こ
れらに使用されるエネルギーコストが大きく、更に、仮
焼、湿式混合、粉砕に長時間を要するので生産効率が決
して良いとは言えない、
等の問題点がある。This is the most common manufacturing method and is the mainstream of the manufacturing methods in practical use. Although this method is nearing completion in terms of technology for producing ferrite powder with stable characteristics, it is difficult to obtain a powder with a narrow particle size distribution by grinding the ferrite powder to a specified particle size. ■Since ferrite formation is carried out by solid phase reaction, there is non-uniformity in the chemical composition at the microscopic level, and it is difficult to make it homogeneous; ■It takes a long time to wet mix and grind. It takes time, and in this operation, it is inevitable that impurities (especially 5iO2) are mixed in from the outside.
It is difficult to obtain high-purity powder, and there is iron contamination from the equipment, which causes a deviation in the iron composition; ■Calcination for ferrite formation must be carried out for a long time at a relatively high temperature of 800 to 1000'C. Also, wet mixing and grinding are each 10%
Since the long processing time of ~40 hours is required, the energy cost used for these is high, and furthermore, the production efficiency cannot be said to be good because calcination, wet mixing, and pulverization require a long time. There is a problem.
（ＩＩ）共沈法（工程系統図を第２図すに示す）フェラ
イトを構成する金属のその塩化物、硫酸塩または硝酸塩
を所定のモル比になるように水に溶解して、そこに強ア
ルカリ物質（ＮａＯＨ１ＫＯＨ等）を加えて金属の水酸
化物沈澱を生成させ、その沈澱物を空気酸化することに
よってフェライト化を行い、生成したフェライト沈澱物
をｒ過、乾燥してフェライト粉体を製造する方法である
。(II) Co-precipitation method (The process diagram is shown in Figure 2) The chloride, sulfate or nitrate of the metal constituting the ferrite is dissolved in water to a predetermined molar ratio, and then A metal hydroxide precipitate is generated by adding an alkaline substance (NaOH, KOH, etc.), the precipitate is oxidized in air to form ferrite, and the generated ferrite precipitate is filtered and dried to produce ferrite powder. This is the way to do it.
本性は乾式法の欠点の解消を意図して開発された方法で
あり、乾式法に比べて以下の点で優れた方法である：
■沈澱生成反応の条件（例えばｐＨ１温度、塩濃度及び
酸化条件）を制御することにより、沈澱の核生成速度を
抑制して粒度分布の狭いフェライト粉体を製造できる；
■フェライトを構成する金属のその金属塩が均一に溶解
した水溶液を原料とするため、化学組成の均一なフェラ
イト粉体が製造できる；
■長時間にわたる湿式混合、粉砕が不要のため、外部か
らのＳ ｉ ０２等の不純物の汚染がおきがたい。This method was developed with the intention of eliminating the drawbacks of the dry method, and is superior to the dry method in the following points: ■Precipitate formation reaction conditions (e.g., pH 1 temperature, salt concentration, and oxidation conditions) ), it is possible to suppress the nucleation rate of precipitates and produce ferrite powder with a narrow particle size distribution; Ferrite powder with a uniform composition can be produced; (1) Since long-term wet mixing and pulverization are unnecessary, contamination with impurities such as S i 02 from the outside is unlikely to occur.
このように本性により高品質のフェライト粉体を製造可
能であるが、
■工程数が多くて製造コストが高くなる；０強アルカリ
物質を添加するので、不純物のアルカリ金属（Ｎ ａ”
、Ｋｏ等）が、フェライト粉体中に残留する、
等の問題点があり、フェライト粉体の製造法の主流とな
っていない６
（ＩＩＩ）ルスナ一方式による噴霧焙焼法（工程系統図
を第２図Ｃに示す〉
本性は次の工程より構成される：
）フェライトを構成する金属のその塩化物が所定のモル
比で溶解している金属塩化物の溶液を得る工程；
ｉ〉噴霧液滴の流れと熱媒体となる高温ガスの流れとが
向流するように金属塩化物の溶液を噴霧し焙焼する工程
；
ｉ）焙焼反応により生成したフェライト粉体の流れとガ
ス流れとを逆向きとする工程；
−）フェライト粉体を回収すると共に焙焼反応により生
成する塩化水素ガスを回収する工程。In this way, it is possible to produce high quality ferrite powder due to its nature; however, the manufacturing cost is high due to the large number of steps; since a strong alkali substance is added, impurity alkali metal (N a ”
, Ko, etc.) remain in the ferrite powder, so it has not become the mainstream manufacturing method for ferrite powder.6 (III) Spray roasting method using the Rusna method (see the process diagram) The process shown in Figure 2C consists of the following steps: ) Obtaining a solution of metal chloride in which the chloride of the metal constituting the ferrite is dissolved in a predetermined molar ratio; i) Spraying liquid A process of spraying and roasting a metal chloride solution so that the flow of droplets and the flow of high-temperature gas serving as a heating medium flow countercurrently; i) The flow of ferrite powder produced by the roasting reaction and the flow of gas are -) Recovering the ferrite powder and recovering the hydrogen chloride gas produced by the roasting reaction.
本性は鉄鋼業において発生する鋼材の塩酸酸洗廃液より
塩酸を回収しつつ１Ｍ化鉄を副生させる処理に実用化さ
れている、ルスナ一方式による噴霧焙焼法を、フェライ
ト粉体の製造法に応用したものである。The essence is that the spray roasting method using the Rusna method, which has been put into practical use as a by-product of 1M iron while recovering hydrochloric acid from the hydrochloric acid pickling waste of steel materials generated in the steel industry, is a method for producing ferrite powder. It was applied to
本性も乾式法の改善をめざして開発された方法であって
、乾式法と比べて以下の点で優れた方法である：
■噴霧条件（ノズルの形状、塩濃度、噴霧速度等）を制
御することにより、発生する液滴の粒度を制御して粒度
分布の狭いフェライト粉体を製造することができる；
■共沈法での記載■と同様のことが期待できる；■共沈
法での記載■と同様のことが期待できる；■製造工程が
少なく、単純なので製造コストの低減が可能である。This method was developed with the aim of improving the dry method, and is superior to the dry method in the following points: ■Controlling spray conditions (nozzle shape, salt concentration, spray speed, etc.) By this, it is possible to control the particle size of the generated droplets and produce ferrite powder with a narrow particle size distribution; ■The same results as described in the coprecipitation method■ can be expected;■Description in the coprecipitation method The same thing as ① can be expected; ② The manufacturing process is small and simple, so it is possible to reduce the manufacturing cost.
しかし、拳法の問題点としてＺｎ成分の組成のずれが大
きいことが挙げられる。Ｚ ｎ Ｃｌ ２を含有する金
属塩化物の溶液をルスナ一方式で噴霧焙焼すると、得ら
れるフェライト粉末は金属塩化物の溶液より予想される
Ｚｎ濃度を大幅に下回るＺｎ量しか含有しておらず、Ｚ
ｎの組成ずれが大きいという欠点がある。しかしながら
、拳法は共沈法のように製造コストが高くなく、乾式法
に比べて優れた品質を有するフェライト粉体の製造が可
能なので、現在主流を占めている乾式法に代わり得る有
望なフェライト粉体の製造法と考えられ、拳法における
大きな問題であるＺｎ組成ずれを解決することが強く望
まれている。However, one of the problems with martial arts is that there is a large difference in the composition of the Zn component. When a metal chloride solution containing Z n Cl 2 is spray roasted using the Rusna method, the resulting ferrite powder contains an amount of Zn that is significantly lower than the expected Zn concentration from a metal chloride solution. ,Z
There is a drawback that the composition deviation of n is large. However, the manufacturing cost of Kempo is not as high as the coprecipitation method, and it is possible to produce ferrite powder with superior quality compared to the dry method, so it is a promising ferrite powder that can replace the currently mainstream dry method. It is strongly desired to solve the Zn composition deviation, which is a major problem in Kenpo and is considered to be a method for manufacturing body parts.
従って、本発明の目的は従来の製造法の問題点を解決す
ることにあり、特にルスナ一方式による噴霧焙焼法の大
きな問題であるＺｎの組成ずれを解決した点に特徴を有
し、現在フェライト粉体の製造法の主流である乾式法に
取り代わり得る製造法を提供するごとにある。Therefore, the purpose of the present invention is to solve the problems of conventional manufacturing methods, and is particularly characterized in that it solves the compositional deviation of Zn, which is a major problem in the spray roasting method using the Rusna method. The purpose of the present invention is to provide a manufacturing method that can replace the dry method, which is the mainstream method for manufacturing ferrite powder.
［課題を解決するための手段］
即ち、本発明は（＾〉フェライトを構成する金属のその
塩化物が所定のモル比で溶解している金属塩化物の溶液
を得る工程；（Ｂ）噴霧液滴の流れと熱媒体となる高温
ガスの流れが同じ方向になるように金属塩化物の溶液を
噴霧し、焙焼する工程：（Ｃ）焙焼反応により生成した
フェライト粉体の流れをガス流れと同じ方向とする工程
：及び（Ｄ）フェライト粉体を回収すると共に焙焼反応
により生成する塩化水素ガスを回収する工程、よりなる
ことを特徴とするフェライト粉体の製造方法に係る６［
作 用］
以下、本発明につき詳細に記載する。[Means for Solving the Problems] That is, the present invention comprises (^> a step of obtaining a solution of a metal chloride in which the chloride of a metal constituting ferrite is dissolved in a predetermined molar ratio; (B) a spray liquid; A process of spraying and roasting a metal chloride solution so that the flow of droplets and the flow of high-temperature gas serving as a heat transfer medium are in the same direction: (C) The flow of ferrite powder produced by the roasting reaction is directed to the gas flow. and (D) a step of recovering the ferrite powder and recovering the hydrogen chloride gas produced by the roasting reaction.
Effect] The present invention will be described in detail below.
本発明のフェライト粉体の製造方法を第１図ａに示す概
念図により、また、第１図すのルスナー方式による噴霧
焙焼法によるフェライト粉体の製造方法の概念図より説
明する。The method for manufacturing ferrite powder of the present invention will be explained with reference to the conceptual diagram shown in FIG. 1a, and the conceptual diagram in FIG.
第１図ａにおいて、金属塩化物の溶液（１〉を噴霧装置
（２）により焙焼炉（３）内に熱媒体となる高温ガス（
５）の流れと同じ方向に噴霧する。焙焼炉（３）内で生
成したフェライト粉体とガスとが同じ方向に流れるよう
にし、フェライト粉体の回収装置（４）によりまずフェ
ライト粉体を回収する。その後に、塩化水素回収装置（
７）によりガス中の塩化水素を回収する。In Figure 1a, a metal chloride solution (1) is sprayed into a roasting furnace (3) using a spraying device (2), and a high-temperature gas (
Spray in the same direction as the flow in 5). The ferrite powder produced in the roasting furnace (3) and the gas are made to flow in the same direction, and the ferrite powder is first recovered by the ferrite powder recovery device (4). After that, the hydrogen chloride recovery equipment (
7) recovers hydrogen chloride in the gas.
一方、第１図すでは、金属塩化物の溶液（１）が噴霧装
置（２）により焙焼炉（３）内へ高温ガス（５）の流れ
と向流するように噴霧され、焙焼炉（３）内でフェライ
ト粉体とガスとを分離し、フェライト粉体は焙焼炉（３
〉の下部よりフェライト粉体の回収装置（４）を経て回
収される。一方、ガス中の塩化水素は焙焼炉の上部より
塩化水素回収装置（７）を経て回収される。On the other hand, in FIG. 1, a metal chloride solution (1) is sprayed into the roasting furnace (3) by a spraying device (2) in a countercurrent flow to the flow of high-temperature gas (5). Ferrite powder and gas are separated in (3), and the ferrite powder is roasted in a roasting furnace (3).
> from the lower part of the ferrite powder through a ferrite powder recovery device (4). On the other hand, hydrogen chloride in the gas is recovered from the upper part of the roasting furnace via a hydrogen chloride recovery device (7).
上述のように本発明の重要な点は、従来法のルスナ一方
式の噴霧焙焼法と異なり、
◎熱媒体となる高温ガスの流れと同一方向に噴霧液滴が
流れるように金属塩化物の溶液を噴霧すること・
◎焙焼反応にまり生成したフェライト粉体の流れとガス
流れの方向が同一であること、
の条件で噴霧焙焼することである。As mentioned above, the important point of the present invention is that, unlike the conventional Rusna one-type spray roasting method, the metal chloride is Spraying the solution: ◎ Spray roasting under the following conditions: ◎The direction of the gas flow is the same as the flow of the ferrite powder produced by the roasting reaction.
本発明による噴霧焙焼を行うと、理由は明確ではないが
、ルスナ一方式による噴霧焙焼法で認められるＺｎの組
成のずれが発生せず、金属塩化物の溶液組成から予想さ
れるＺｎの組成を有するフェライトが得られる。When spray roasting according to the present invention is carried out, although the reason is not clear, the shift in the Zn composition observed in the Rusna one-method spray roasting method does not occur, and the Zn composition as expected from the metal chloride solution composition does not occur. A ferrite having the following composition is obtained.
Ｚｎの組成ずれの発生原因について、現在のところ以下
のように推定することができる。焙焼炉内の高温雰囲気
下では、未反応のＺｎＣｌ２はガス化していると考えら
れる。ルスナ一方式の噴Ｎ焙焼では、生成したＺｎの少
ないフェライト粉体の流れと逆方式にガス状のＺｎｃＩ
ｚが反応生成ガスと共に流れ去ってしまうため、Ｚｎの
少ないフェライト粉体とガス状ＺｎＣ１，及び水蒸気と
が反応する機会を失うので、その結果得られるフェライ
ト粉体にはＺｎの組成ずれが起こると推定している。一
方、本発明方法では、Ｚｎの少ないフェライト粉体とガ
ス状のＺｎＣｌ２とが同一方向に流れるため、それらと
水蒸気とが反応する機会がルスナ一方式に比べて多くも
てるために、得られるフェライト粉体のＺｎの組成ずれ
は生じないものと推定される。いずれにしても、本発明
のように噴霧液滴とガス体及びフェライト粉体の流れる
方向を同一にすることによってＺｎの組成ずれの発生を
なくすことができる。フェライト粉体の回収方法及び焙
焼反応により生成する塩化水素ガスの回収方法はそれぞ
れサイクロンやバグフィルタ−あるいは電気集じん機、
水に塩化水素ガスを吸収させて塩酸溶液として回収する
という既知の方法が適用でき、これら回収方法それ自体
については、本発明の特徴となるものではない。At present, the cause of the Zn composition deviation can be estimated as follows. It is thought that unreacted ZnCl2 is gasified under the high temperature atmosphere in the roasting furnace. In the Rusna one-type injection N roasting, gaseous ZncI is produced in the opposite direction to the flow of the generated Zn-poor ferrite powder.
Since z flows away with the reaction product gas, the ferrite powder with less Zn, gaseous ZnC1, and water vapor have no opportunity to react, and as a result, the resulting ferrite powder has a compositional shift in Zn. I'm guessing. On the other hand, in the method of the present invention, since Zn-poor ferrite powder and gaseous ZnCl2 flow in the same direction, there is more opportunity for them to react with water vapor than in the Rusna one-way method. It is estimated that no deviation in the composition of Zn in the powder occurs. In any case, by making the flow directions of the spray droplets, the gas body, and the ferrite powder the same as in the present invention, it is possible to eliminate the occurrence of compositional deviation of Zn. The methods for recovering ferrite powder and the hydrogen chloride gas produced by the roasting reaction are methods such as cyclones, bag filters, electrostatic precipitators,
Known methods of absorbing hydrogen chloride gas into water and recovering it as a hydrochloric acid solution can be applied, and these recovery methods themselves are not a feature of the present invention.
なお、本発明方法において、フェライトを精成する金属
のその塩化物溶液として種々のものを使用することがで
き、該溶液として例えばＦｅＣｌ２、Ｍ ｎ Ｃｌ ２
及びＺｎＣｌ２を主成分とする溶液またはＦｅＣｂ、Ｎ
：Ｃ１２及びＺｎＣ１ｚを主成分とする溶液を使用する
ことができる。In the method of the present invention, various chloride solutions of metals for refining ferrite can be used, such as FeCl2, MnCl2, etc.
and ZnCl2-based solution or FeCb, N
: A solution containing C12 and ZnC1z as main components can be used.
［実 施 例］
以下、“本発明の実施例につき説明するが、本発明はこ
の実施例に限定されるものではない。[Examples] Hereinafter, examples of the present invention will be described, but the present invention is not limited to these examples.
実施例１
目標とするＭｎＺｎ系ソフトフェライトの組成（Ｆｅ２
０，５０モル％、Ｍｎ０３４％、Ｚｎ０１６モル％）と
同じ組成の溶液を、水約０．１！にＦｅＣｊ！ｚ・４
Ｈ２０、Ｍ ｎＣ（ｌｘ ・４ Ｈ２０及びＺｎＣｌ２
をそれぞれ２６０ｇ、８８ｆＩ、２８ｇ溶解して調製し
た。なお、ＦｅＣ１ｚ、Ｍｎ（１！及びＺｎＣ１，合計
量が１１の溶液に対し約２５０ｇとなるように調製する
。得られた金属塩化物の溶液を１０１／時間の供給速度
で約７５０℃に保持された焙焼炉内に、熱媒体の高温ガ
スの流れと噴霧液滴の流れとが同一になるように噴霧し
、且つ焙焼反応により生成したソフトフェライト粉体と
ガスとが同一方向の流れとなる状態で焙焼反応を行った
。ソフトフェライト粉体はバグフィルタ−により回収し
た。そのソフトフェライト粉体の組成を第１表に示すが
、Ｚｎの組成ずれは認められなかった。Example 1 Target composition of MnZn-based soft ferrite (Fe2
0.50 mol%, Mn0 34%, Zn0 16 mol%) with about 0.1% water. niFeCj! z・4
H20, M nC(lx ・4 H20 and ZnCl2
were prepared by dissolving 260g, 88fI, and 28g of each. In addition, FeC1z, Mn (1! and ZnC1, the total amount is prepared to be about 250 g for a solution of 11. The obtained metal chloride solution was maintained at about 750 ° C. at a feeding rate of 101/hour. In the roasting furnace, the flow of high-temperature gas as a heating medium and the flow of sprayed droplets are the same, and the soft ferrite powder and gas generated by the roasting reaction flow in the same direction. The roasting reaction was carried out under the following conditions.The soft ferrite powder was collected using a bag filter.The composition of the soft ferrite powder is shown in Table 1, and no deviation in the composition of Zn was observed.
実施例２
目標とするＮｉ−Ｚｎ系ソフトフェライトの組成（Ｆｅ
２０３５０モル％、Ｎｉ０３５モル％、ＺｎＯ１５モル
％）と同じ組成の溶液を水約０．９１に、ＦｅＣｈ・４
Ｈ２０，ＮｉＣ＆ｚ・６Ｈ２０及びＺ ｎＣ１２をそれ
ぞれ２６０ｇ、１０８ｙ、２７ｇ溶解して調製した、な
お、ＦｅＣｌ２、ＮｉＣｌ２及びＺｎＣ１ｚの合計量が
溶液１１に対し約２５０２となるように調製する。得ら
れた金属塩化物の溶液を実施例１と同様に処理、し、回
収されたソフトフェライト粉体の組成を表１に示すが、
Ｚｎの組成ずれは認められなかった。Example 2 Composition of target Ni-Zn soft ferrite (Fe
20350 mol%, Ni0 35 mol%, ZnO 15 mol%) in about 0.91% water,
It was prepared by dissolving 260g, 108y, and 27g of H20, NiC&z·6H20, and ZnC12, respectively, and the total amount of FeCl2, NiCl2, and ZnC1z was prepared to be about 2502 to solution 11. The obtained metal chloride solution was treated in the same manner as in Example 1, and the composition of the recovered soft ferrite powder is shown in Table 1.
No compositional deviation of Zn was observed.
比較例１
実施例１と同じ金属塩化物の溶液を実施例１と同様にし
て作製し、この溶液を１０１７時間の供給速度で約７５
０℃に保持された焙焼炉内に、熱媒体の高圧ガスの流れ
と噴霧液滴の流れが向流するように噴霧し、且つ焙焼反
応により生成したソフトフェライト粉体と該高圧ガスと
が逆向きの流れとなる状態で焙焼反応を行った。ソフト
フェライト粉体はホッパーに堆積させて回収した。その
ソフトフェライト粉体の組成を表１に示したが、顕著な
Ｚｎの組成ずれが認められた。Comparative Example 1 A solution of the same metal chloride as in Example 1 was prepared in the same manner as in Example 1, and this solution was fed at a feed rate of about 75
In a roasting furnace maintained at 0°C, the flow of high-pressure heat medium gas and the flow of sprayed droplets are sprayed in countercurrent flow, and the soft ferrite powder produced by the roasting reaction and the high-pressure gas are mixed. The roasting reaction was carried out under conditions where the flow was in the opposite direction. The soft ferrite powder was deposited in a hopper and collected. The composition of the soft ferrite powder is shown in Table 1, and a significant difference in the composition of Zn was observed.
比較例２
実施例２と同じ金属塩化物の溶液を実施１４＋ ２と同
様にして作製し、この溶液を比較例１と同様に処理し、
ソフトフェライト粉体を得た。得られたソフトフェライ
ト粉体の組成を表１に示すが、顕著なＺｎの組成ずれが
認められた。Comparative Example 2 A solution of the same metal chloride as in Example 2 was prepared in the same manner as in Example 14+2, and this solution was treated in the same manner as in Comparative Example 1.
A soft ferrite powder was obtained. The composition of the obtained soft ferrite powder is shown in Table 1, and a significant difference in the composition of Zn was observed.
東−１（モル％）
異と５ｂ通 Ｌシエｇ ＭｎＯＺｎＯ原料液組戒
５０．０ ３４．０ １６．０実施例１
４９．９ ３４．２ １５．９比較例１ ５５
．１ ３７．４． ７．５凡上二ヱ１系 Ｌシ否ユ
歓匹皇 乙ユＱ原料液組成 ５０．０ ３５．
０ １５．０実施例２ ５０．２ ３４．９
１４．９比較例２ ５５．２ ３８．７ ６
゜１［発明の効果］
以上説明したように、本発明によれば、従来法のルスナ
一方式による噴霧焙焼法では達成できなかったＺｎの組
成ずれの問題を解決でき、且つ高品質のフェライト粉体
を少ない工程で製造できるので、現在製造法の主流とな
っている乾式法に取って代わり得る画期的な製造法を提
供できる。Higashi-1 (mol%) Ito 5b-tsu L-sieg MnOZnO raw material liquid assembly precepts
50.0 34.0 16.0 Example 1
49.9 34.2 15.9 Comparative example 1 55
．． 1 37.4. 7.5 Bonjo 2ヱ1 Series L Shinayu Kantoki Otsuyu Q Raw material liquid composition 50.0 35.
0 15.0 Example 2 50.2 34.9
14.9 Comparative Example 2 55.2 38.7 6
゜1 [Effects of the Invention] As explained above, according to the present invention, it is possible to solve the problem of Zn composition deviation, which could not be achieved with the conventional spray roasting method using the Rusna method, and to produce high-quality ferrite. Since the powder can be manufactured in fewer steps, it is possible to provide an innovative manufacturing method that can replace the dry method that is currently the mainstream manufacturing method.
第１図ａは本発明によるフェライト粉末の製法を示す概
念図であり、第１図すはルスナ一方式による噴霧焙焼法
の概念図であり、第２図ａは乾式法によるフェライト粉
体の製法を示す工程系統図であり、第２図すは共沈法に
よるフェライト粉体の製法を示す工程系統図であり、第
２図Ｃはルスナ一方式による噴霧焙焼法によるフェライ
ト粉体の製法を示す工程系統図である。図中、１・・・
金属塩化物の溶液、２・・・噴霧装置、３・・・焙焼炉
、４・・・フェライト粉体の回収装置、５・・・高温ガ
ス、６・・・反応生成ガス、７・・・塩化水素回収装置
。
第１図
本発明
す
第２図
く乾
式
％式％Fig. 1a is a conceptual diagram showing the method for producing ferrite powder according to the present invention, Fig. 1 is a conceptual diagram of the spray roasting method using the Rusna method, and Fig. 2a is a conceptual diagram showing the production method of ferrite powder using the dry method. FIG. 2C is a process diagram showing the manufacturing method of ferrite powder using the coprecipitation method, and FIG. FIG. In the figure, 1...
Metal chloride solution, 2... Spraying device, 3... Roasting furnace, 4... Ferrite powder recovery device, 5... High temperature gas, 6... Reaction product gas, 7...・Hydrogen chloride recovery equipment. Figure 1 The present invention Figure 2 Dry type % type %
Claims (3)
所定のモル比で溶解している金属塩化物の溶液を得る工
程； （Ｂ）噴霧液滴の流れと熱媒体となる高温ガスの流れが
同じ方向になるように金属塩化物の溶液を噴霧し、焙焼
する工程； （Ｃ）焙焼反応により生成したフェライト粉体の流れを
ガス流れと同じ方向とする工程；及び（Ｄ）フェライト
粉体を回収すると共に焙焼反応により生成する塩化水素
ガスを回収する工程、よりなることを特徴とするフェラ
イト粉体の製造方法。(1) (A) Step of obtaining a metal chloride solution in which the chloride of the metal constituting the ferrite is dissolved in a predetermined molar ratio; (B) The flow of the spray droplets and the high temperature gas serving as the heat medium. A step of spraying and roasting the metal chloride solution so that the flow is in the same direction; (C) A step of making the flow of the ferrite powder produced by the roasting reaction in the same direction as the gas flow; and (D) A method for producing ferrite powder, comprising the steps of recovering ferrite powder and recovering hydrogen chloride gas produced by a roasting reaction.
ｌ＿２、ＭｎＣｌ＿２及びＺｎＣｌ＿２を主成分とする
請求項１記載の方法。(2) The chloride of the metal constituting ferrite is FeC
2. The method according to claim 1, wherein the main components are l_2, MnCl_2 and ZnCl_2.
ｌ＿２、ＮｉＣｌ＿２及びＺｎＣｌ＿２を主成分とする
請求項１記載の方法。(3) The chloride of the metal constituting ferrite is FeC
2. The method according to claim 1, wherein the main components are l_2, NiCl_2 and ZnCl_2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17558489A JPH0340921A (en) | 1989-07-10 | 1989-07-10 | Production of ferrite powder by spray roasting method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17558489A JPH0340921A (en) | 1989-07-10 | 1989-07-10 | Production of ferrite powder by spray roasting method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0340921A true JPH0340921A (en) | 1991-02-21 |
Family
ID=15998641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17558489A Pending JPH0340921A (en) | 1989-07-10 | 1989-07-10 | Production of ferrite powder by spray roasting method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0340921A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5462686A (en) * | 1992-03-23 | 1995-10-31 | Nkk Corporation | Method of manufacturing composite ferrite |
-
1989
- 1989-07-10 JP JP17558489A patent/JPH0340921A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5462686A (en) * | 1992-03-23 | 1995-10-31 | Nkk Corporation | Method of manufacturing composite ferrite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6661665B2 (en) | Recovery method for used SCR denitration catalyst | |
| JP7376862B2 (en) | Wet synthesis method of NCMA high nickel quaternary precursor | |
| CN108838406B (en) | Multi-stage process and system for preparing cell material | |
| US8986632B2 (en) | Process for recovery of cobalt, ruthenium, and aluminum from spent catalyst | |
| JP4992003B2 (en) | Method for producing metal oxide fine particles | |
| CN101497432B (en) | Method for preparing single or composite metal oxide by atomizing and oxidizing solution | |
| CN102583503A (en) | Method for preparing activated zinc oxide by utilizing high-arsenic secondary zinc oxide resource ammonia-ammonium process | |
| CN101665263A (en) | Method for processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide | |
| CN106558695A (en) | A kind of nickel cobalt aluminum complex hydroxide, nickel cobalt aluminium composite oxide and preparation method thereof | |
| CN104762474B (en) | Method for preparing ammonium molybdate through molybdenite | |
| CN107434260B (en) | A kind of preparation method of big granularity vanadic anhydride | |
| CN102795653B (en) | Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass | |
| CN105540623A (en) | Method for preparing nanometer magnesia | |
| CN112755981B (en) | Solid solution structure adsorbent, preparation method and application in separating Cr (VI) contained in water body | |
| WO2016054952A1 (en) | Metallurgical process for tungsten mineral raw material with no pollutant discharge in entire process | |
| CN110331297B (en) | Method for preparing vanadium pentoxide from vanadium slag in short process | |
| CN103449511A (en) | Strontium titanate submicron crystal and preparation method thereof | |
| CN116477671A (en) | Lithium battery material precursor, preparation method and application thereof | |
| JPH0340921A (en) | Production of ferrite powder by spray roasting method | |
| JP7254830B2 (en) | Method for producing mixed metal oxide | |
| CN108796234B (en) | Method for separating antimony and arsenic from antimony-arsenic material | |
| JPS63288913A (en) | Production of zinc oxide | |
| CN110980809A (en) | Method for preparing ammonium metatungstate by utilizing tungsten-containing waste | |
| CN104118910A (en) | Method for selectively preparing vanadium oxides and recovering hydroxides through vanadate hydrogen reduction method | |
| CN113828323B (en) | Additional catalyst for acrylonitrile production, preparation method and application |