JPH05175033A - Manufacture of composite oxide and soft ferrite - Google Patents

Manufacture of composite oxide and soft ferrite

Info

Publication number
JPH05175033A
JPH05175033A JP3340983A JP34098391A JPH05175033A JP H05175033 A JPH05175033 A JP H05175033A JP 3340983 A JP3340983 A JP 3340983A JP 34098391 A JP34098391 A JP 34098391A JP H05175033 A JPH05175033 A JP H05175033A
Authority
JP
Japan
Prior art keywords
producing
composite oxide
chloride
roasting
soft ferrite
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.)
Withdrawn
Application number
JP3340983A
Other languages
Japanese (ja)
Inventor
Akira Chiba
明 千葉
Hiroshi Oyanagi
浩 大柳
Norio Tsukiji
憲夫 築地
Masanari Hara
勝成 原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Nisshin Co Ltd
Tokin Corp
Original Assignee
Tokin Corp
Nisshin Steel Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tokin Corp, Nisshin Steel Co Ltd filed Critical Tokin Corp
Priority to JP3340983A priority Critical patent/JPH05175033A/en
Publication of JPH05175033A publication Critical patent/JPH05175033A/en
Withdrawn legal-status Critical Current

Links

Abstract

PURPOSE:To provide a method of easily manufacturing a composite oxide for soft ferrite and soft ferrite by using a general spray roasting surface. CONSTITUTION:A method of manufacturing a composite oxide by spraying and roasting the mixed aqueous solution of one or more kinds of chlorides of Mn, Mg, Ni having the ferrite composition, that is, ferrous chloride and ferric chloride and a method of manufacturing a soft ferrite using a composite oxide and zinc compound manufactured as a result of the former method are employed.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、エレクトロニクス産業
において重要な高透磁率磁性材料や低損失磁性材料とし
て用いられるソフトフェライトの原料である複合酸化物
及びソフトフェライトの製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a composite oxide and a soft ferrite which are raw materials of soft ferrite used as a high permeability magnetic material or a low loss magnetic material important in the electronics industry.

【0002】[0002]

【従来の技術】従来、ソフトフェライトの原料用の複合
酸化物を製造する方法としては、鉄鋼業における鋼板等
の塩酸酸洗の際に生じる酸洗廃液等の塩化鉄を利用し、
この塩化鉄とMn,Mg,Ni,Zn等の塩化物とを混
合した混合水溶液を噴霧焙焼する手法が特公昭47−1
1550号公報に開示されている。
2. Description of the Related Art Conventionally, as a method for producing a complex oxide as a raw material for soft ferrite, iron chloride such as pickling waste liquid generated during hydrochloric acid pickling of steel sheets in the steel industry is used,
A method of spray roasting a mixed aqueous solution obtained by mixing iron chloride with chlorides such as Mn, Mg, Ni and Zn is disclosed in Japanese Examined Patent Publication No. 47-1.
It is disclosed in Japanese Patent No. 1550.

【0003】しかしながら、Znを含むソフトフェライ
ト原料酸化物を噴霧焙焼によって製造することは、Zn
の組成ずれが大きく困難である。この為、例えば特開昭
63−156017号公報や特開平3−83819号公
報,或いは本発明者等により提案された特開平3−40
921号公報に開示されている如く、焙焼方法に対する
工夫が必要となる。即ち、Znを含むソフトフェライト
原料酸化物を噴霧焙焼によって製造するには、特殊な焙
焼炉が必要であり、一般的に用いられているルスナー炉
やドラボー炉を使用することは困難である。
However, the production of soft ferrite raw material oxide containing Zn by spray roasting is
The compositional deviation is large and difficult. Therefore, for example, JP-A-63-156017, JP-A-3-83819, or JP-A-3-40 proposed by the present inventors.
As disclosed in Japanese Patent No. 921, it is necessary to devise a roasting method. That is, a special roasting furnace is required for producing the soft ferrite raw material oxide containing Zn by spray roasting, and it is difficult to use a commonly used Rusner furnace or Drabo furnace. ..

【0004】そこで、Znの組成ずれを対策する為、特
公昭63−17776号公報に開示されているように、
フェライト組成金属元素のうち、比較的その塩化物の蒸
気圧の低い金属については、その塩化物混合溶液を噴霧
焙焼して得た複合酸化物を原料として用いる一方、塩化
物の蒸気圧の高い金属については、その酸化物を原料と
して用いて,ソフトフェライトを製造する方法が提案さ
れている。
Therefore, in order to prevent the compositional deviation of Zn, as disclosed in JP-B-63-17776,
Among the metal elements of the ferrite composition, for the metal whose vapor pressure of chloride is relatively low, the compound oxide obtained by spray roasting the chloride mixed solution is used as a raw material, while the vapor pressure of chloride is high. Regarding metals, a method of producing soft ferrite using the oxide thereof as a raw material has been proposed.

【0005】[0005]

【発明が解決しようとする課題】従来のソフトフェライ
ト製造方法において、鉄の塩化物のソースとして汎用的
に用いられる鉄鋼塩酸酸洗廃液は、通常塩化第二鉄を含
んでいる。この塩化第二鉄は、沸点が約320℃であっ
て、一般的な噴霧焙焼温度である600℃以上において
は蒸気圧が非常に高くなってしまう。この塩化第二鉄の
蒸気圧は、フェライト組成金属の塩化物のうちでは、他
のものとの比較において圧倒的に高くなっている。
In the conventional method for producing soft ferrite, the steel hydrochloric acid pickling waste liquid generally used as a source of iron chloride usually contains ferric chloride. This ferric chloride has a boiling point of about 320 ° C., and has a very high vapor pressure at a general spray roasting temperature of 600 ° C. or higher. The vapor pressure of ferric chloride is overwhelmingly higher than that of other chlorides of ferrite-composing metals.

【0006】この為、特公昭63−17776号公報の
ソフトフェライト製造方法によれば、塩化第二鉄を除去
するか、或いは塩化第二鉄を蒸気圧の低い塩化第一鉄に
還元する必要がある。ところが、廃塩酸中の余剰塩酸を
利用するために、スケール等の酸化鉄を溶解すれば、塩
化第二鉄が増加する上、鉄鋼塩酸酸洗廃液に限らず塩化
第一鉄は空気中の酸素によっても塩化第二鉄に酸化され
るので、塩化第二鉄の処理が必要であるという点で複雑
になる。一方、ソフトフェライト原料の粉体特性に対す
る要求は厳しいものがあるが、噴霧焙焼により得られる
粉体はこの要求を満足するものである。
Therefore, according to the method for producing soft ferrite in Japanese Patent Publication No. 63-17776, it is necessary to remove ferric chloride or reduce ferric chloride to ferrous chloride having a low vapor pressure. is there. However, in order to use the surplus hydrochloric acid in the waste hydrochloric acid, if iron oxide such as scale is dissolved, ferric chloride will increase, and ferrous chloride is not limited to iron and hydrochloric acid pickling waste liquid, but oxygen in the air. Is also oxidized to ferric chloride, which complicates the treatment of ferric chloride. On the other hand, there are some strict requirements for the powder characteristics of the soft ferrite raw material, but the powder obtained by spray roasting satisfies this requirement.

【0007】ところで、噴霧焙焼法のためのMn,M
g,Ni等のソースとしては、主として組成が要求され
るのみであり、しかも一旦溶液とするので精製も容易で
あり、フェライト原料として調整された高価な酸化物原
料のような粉体は不用である。そこで、ソフトフェライ
ト原料としての複合酸化物の製造に、この噴霧焙焼法を
用いれば、ソフトフェライトを安価に製造することがで
きる筈である。
By the way, Mn, M for the spray roasting method
As the source of g, Ni, etc., the composition is mainly required, and since it is once made into a solution, it can be easily purified, and a powder such as an expensive oxide raw material prepared as a ferrite raw material is unnecessary. is there. Therefore, if this spray roasting method is used for producing the composite oxide as the soft ferrite raw material, the soft ferrite should be able to be produced at a low cost.

【0008】本発明は、かかる事情を鑑みなされたもの
で、その技術的課題は、一般的な噴霧焙焼炉を用いて簡
単にソフトフェライト用の複合酸化物を製造する方法及
びその複合酸化物を用いてソフトフェライトを製造する
方法を提供することにある。
The present invention has been made in view of the above circumstances, and its technical problem is to provide a method for easily producing a complex oxide for soft ferrite by using a general spray roasting furnace and the complex oxide. It is to provide a method of manufacturing soft ferrite using.

【0009】[0009]

【課題を解決するための手段】本発明によれば、フェラ
イト組成の主成分金属元素であるMn,Mg,Niのう
ちの少なくとも1種以上と、Zn及びFeとから成るソ
フトフェライトの原料としての複合酸化物の製造方法で
あって、フェライト組成のMn,Mg,Niのうちの1
種以上の塩化物,塩化第一鉄及び塩化第二鉄の混合水溶
液を噴霧焙焼する複合酸化物の製造方法が得られる。
According to the present invention, as a raw material for a soft ferrite composed of Zn and Fe, at least one or more of Mn, Mg and Ni which are main component metallic elements of the ferrite composition, and Zn and Fe. A method for producing a composite oxide, comprising one of Mn, Mg, and Ni having a ferrite composition.
A method for producing a composite oxide is obtained by spray roasting a mixed aqueous solution of at least one kind of chloride, ferrous chloride and ferric chloride.

【0010】又、本発明によれば、上記複合酸化物の製
造方法において、噴霧焙焼する際の熱源として水素元素
を含む燃料を使用した複合酸化物の製造方法や、噴霧焙
焼する際の熱源として水素元素を含む燃料を使用した複
合酸化物の製造方法の他、噴霧焙焼する際に、噴霧焙焼
設備の焙焼炉から得られる高温の排出ガスを、塩酸ガス
回収用の塩酸ガス吸収塔に導入する直前に塩化第一鉄を
含む塩化物水溶液と接触させることにより該塩化物水溶
液を濃縮させる濃縮工程を有する複合酸化物の製造方法
や、塩化第一鉄及び塩化第二鉄に鉄鋼塩酸酸洗廃液を使
用する複合酸化物の製造方法が得られる。
Further, according to the present invention, in the above-mentioned method for producing a composite oxide, a method for producing a composite oxide using a fuel containing a hydrogen element as a heat source for spray roasting, and a method for producing spray roasting. In addition to the method for producing complex oxides using a fuel containing hydrogen as a heat source, during spray roasting, the high-temperature exhaust gas obtained from the roasting furnace of the spray roasting equipment is used as hydrochloric acid gas for recovering hydrochloric acid gas. Immediately before introducing into the absorption tower, a method for producing a complex oxide having a concentration step of concentrating the chloride aqueous solution by contacting it with a chloride aqueous solution containing ferrous chloride, and ferrous chloride and ferric chloride A method for producing a composite oxide using an iron and hydrochloric acid pickling waste liquid is obtained.

【0011】更に、本発明によれば、上記複合酸化物の
製造方法により製造される複合酸化物と、亜鉛化合物と
を原料とするソフトフェライトの製造方法が得られる。
Further, according to the present invention, there is provided a method for producing soft ferrite using the composite oxide produced by the above method for producing a composite oxide and a zinc compound as raw materials.

【0012】[0012]

【作用】本発明は、一般的な噴霧焙焼法の特徴である比
較的短時間のうちに噴霧液滴が高温に達して瞬時に反応
が進行する現象において、反応の進行は蒸気圧の高低が
主要因ではなく、熱力学的な平衡と速度論とによるもの
との着想に基づいている。即ち、熱力学的な平衡と速度
論によれば、Znは平衡論的に反応は難いが、塩化第二
鉄は充分反応すると考えられる。そこで、Mn,Mg,
Niのうち1種の塩化物と塩化第一鉄と塩化第二鉄との
混合水溶液を、短時間高温に晒したものと、実際のルス
ナー炉で焙焼したものとを分析した結果、混合水溶液と
焙焼の結果得られた酸化物とは金属の組成比においてほ
ぼ同程度となる(実施例に示す)ことが判った。これに
より、Zn以外のMn,Mg,Ni,Feであれば蒸気
圧の高低に拘らず塩化物混合溶液の噴霧焙焼により複合
酸化物の製造が可能であり、特に塩化第二鉄を含むよう
な鉄鋼塩酸酸洗廃液を用いても複雑な処理が必要のない
ことも判った。
The present invention is characterized by the general spray roasting method, in which the spray droplets reach a high temperature within a relatively short time and the reaction proceeds instantaneously. Is not the main factor, but is based on the idea of thermodynamic equilibrium and kinetics. That is, according to thermodynamic equilibrium and kinetics, it is considered that Zn has a difficult equilibrium reaction, but ferric chloride reacts sufficiently. Therefore, Mn, Mg,
As a result of analysis of a mixed aqueous solution of one kind of Ni, chloride, ferrous chloride and ferric chloride, which was exposed to high temperature for a short time, and what was roasted in an actual Rusner furnace, the mixed aqueous solution was obtained. It was found that the metal composition ratios of the oxides obtained as a result of the roasting and the oxides were almost the same (as shown in the examples). As a result, if Mn, Mg, Ni, and Fe other than Zn are used, it is possible to produce a complex oxide by spray roasting a chloride mixed solution regardless of the vapor pressure. It was also found that complicated treatment is not required even with the use of various waste iron and steel hydrochloric acid pickling solutions.

【0013】この結果から、本発明は、フェライト組成
の主成分金属元素であるMn,Mg,Niのうちの少な
くとも1種以上と、Zn及びFeから成るソフトフェラ
イトにおいて、フェライト組成のMn,Mg,Niのう
ちの1種以上の塩化物,塩化第一鉄及び塩化第二鉄との
混合水溶液を噴霧焙焼して製造した複合酸化物と、亜鉛
化合物とを原料に用いることによりソフトフェライトを
比較的簡単に製造するものである。
From these results, according to the present invention, in the soft ferrite composed of Zn and Fe and at least one or more of the main component metal elements of the ferrite composition, Mn, Mg, and Ni. Comparing soft ferrite by using zinc oxide as a raw material and a composite oxide produced by spray roasting a mixed aqueous solution of one or more chlorides of Ni, ferrous chloride and ferric chloride It is easy to manufacture.

【0014】ところで、単純な噴霧焙焼法に塩化第二鉄
を使用すると、混合塩化物の焙焼反応の際の雰囲気とし
て水蒸気分圧が低い場合に、塩酸ガス以外にも少量であ
るが、塩素ガスが生成するという欠点を有することも判
明した。この塩素ガスは微量である場合は上記の製造方
法を実施できるが、この塩素ガスが大気中に放出された
場合、公害の規制物質でもある為、何らかの対策を施す
必要がある。一般に、塩化物水溶液の噴霧焙焼設備は排
ガスの処理設備として排ガスのアルカリによる洗浄設備
が設置されているが、塩素ガスの処理には対応できな
い。この問題の簡易な対策としては、焙焼設備の排ガス
の処理設備として塩素ガスの処理設備を設置することが
考えられる。しかしながら、この処理設備は高価であ
り、新たに設置することはコストアップの要因となり好
ましくない。この為、種々の検討を重ねた結果、以下に
説明する塩素ガス処理対策を施すことが望ましい。
By the way, when ferric chloride is used in a simple spray roasting method, when the steam partial pressure is low as an atmosphere in the roasting reaction of the mixed chloride, the amount is small in addition to hydrochloric acid gas, It has also been found to have the drawback of producing chlorine gas. When the amount of chlorine gas is very small, the above manufacturing method can be carried out. However, when this chlorine gas is released into the atmosphere, it is also a pollution control substance, and therefore some measures must be taken. Generally, the spray roasting equipment for an aqueous solution of chloride is equipped with a cleaning equipment for treating exhaust gas with an alkali of exhaust gas, but cannot handle chlorine gas. As a simple measure against this problem, it is conceivable to install a chlorine gas treatment facility as an exhaust gas treatment facility of the roasting facility. However, this processing facility is expensive, and it is not preferable to newly install it because it causes a cost increase. Therefore, as a result of various studies, it is desirable to take the chlorine gas treatment measures described below.

【0015】一つの方法は、焙焼反応の雰囲気を水蒸気
分圧の高い状態で行い、塩素ガスの生成を抑制する方法
である。具体的に云えば、噴霧焙焼する際の熱源として
水素元素を含む燃料を使用するもので、燃料の燃焼によ
り水蒸気を発生するようにする。或いは直接的に燃焼ガ
ス中に水蒸気を吹き込む方法を採用しても良い。これら
の方法は、前者は燃料の転換,後者は水蒸気の配管の設
置で比較的簡単に行うことができる。もう一つの方法
は、生成される塩素ガスを吸収する方法である。具体的
に云えば、噴霧焙焼する際に、噴霧焙焼設備の塩酸ガス
回収用の塩酸ガス吸収塔の直前に配置される焙焼炉から
得られる高温の排出ガスと、塩化第一鉄を含む塩化物水
溶液を接触させ、この塩化物水溶液を濃縮させる濃縮工
程を加えることである。塩素ガスは塩化第一鉄のように
被酸化性の物質を含む溶液に吸収される上、この塩化物
水溶液として噴霧焙焼用の水溶液を使用できる。更に、
噴霧焙焼用の水溶液の濃縮を行うことはランニングコス
トの削減にもなる。従って、この方法はトータルとして
コスト的にメリットがあり、工業的に適している。
One method is a method of suppressing the generation of chlorine gas by carrying out the roasting reaction atmosphere in a state where the partial pressure of water vapor is high. Specifically, a fuel containing a hydrogen element is used as a heat source for spray roasting, and steam is generated by burning the fuel. Alternatively, a method of directly blowing steam into the combustion gas may be adopted. These methods can be performed relatively easily by converting the fuel for the former and installing steam piping for the latter. Another method is to absorb the chlorine gas produced. Specifically, during spray roasting, the hot exhaust gas obtained from the roasting furnace arranged immediately before the hydrochloric acid gas absorption tower for recovering the hydrochloric acid gas of the spray roasting facility and ferrous chloride are It is to add a concentration step of bringing the chloride aqueous solution containing the solution into contact and concentrating the chloride aqueous solution. Chlorine gas is absorbed in a solution containing an oxidizable substance such as ferrous chloride, and an aqueous solution for spray roasting can be used as this chloride aqueous solution. Furthermore,
Concentrating the aqueous solution for spray roasting also reduces running costs. Therefore, this method has an advantage in cost as a whole and is industrially suitable.

【0016】[0016]

【実施例】以下に実施例を挙げ、本発明の複合酸化物及
びソフトフェライトの製造方法について詳細に説明す
る。
EXAMPLES The method for producing the composite oxide and soft ferrite of the present invention will be described in detail below with reference to examples.

【0017】実施例1は、ソフトフェライトの原料とし
ての複合酸化物の製造方法に関するものである。ここで
は実験的に塩化物溶液を瞬時に高温に晒して酸化焙焼す
ることにより得られる複合酸化物と、もとの塩化物溶液
との組成比較を行った。具体的には、石英ガラスの砕い
たものを15ml入れた石英坩堝(容量約30ml)を竪型
の電気炉の高温部に保持して一定の温度(700℃,8
00℃)に保ち、炉上部より塩化物混合溶液を石英坩堝
中に滴下して焙焼反応を行わせた。この焙焼反応中は炉
内雰囲気はAir気流と30%水蒸気を含むAir気流
との2通りの条件下で実験を行った。その後、石英坩堝
を炉より取り出して焙焼反応により生成した複合酸化物
を石英ガラスと共にビーカーに移し入れ、HC1(1+
1)を加えて複合酸化物を加熱溶解した。溶解完了後、
溶液を石英ガラスと濾別してメスアップ後、ICP分析
により金属組成を求めた。塩化物混合水溶液中と複合酸
化物中との金属組成(塩化物比率と金属比率)は、それ
ぞれ表1(焙焼温度700℃のもの)、表2(焙焼温度
800℃のもの)に示す通りとなった。
Example 1 relates to a method for producing a composite oxide as a raw material for soft ferrite. Here, the composition of the complex oxide obtained by experimentally exposing the chloride solution to high temperature instantaneously and oxidizing and roasting was compared with the original chloride solution. Specifically, a quartz crucible (capacity about 30 ml) containing 15 ml of crushed quartz glass was held in a high temperature part of a vertical electric furnace at a constant temperature (700 ° C, 8 ° C).
The temperature was kept at 00 ° C), and the chloride mixed solution was dropped into the quartz crucible from the upper part of the furnace to carry out the roasting reaction. During the roasting reaction, the experiment was conducted under two conditions of the atmosphere in the furnace: the air flow and the air flow containing 30% steam. Then, the quartz crucible was taken out of the furnace, and the composite oxide produced by the roasting reaction was transferred to a beaker together with the quartz glass, and the HC1 (1+
1) was added and the composite oxide was melted by heating. After dissolution is complete,
The solution was separated from the quartz glass by filtration, and after measuring up, the metal composition was determined by ICP analysis. The metal compositions (chloride ratio and metal ratio) in the chloride mixed aqueous solution and in the complex oxide are shown in Table 1 (for roasting temperature of 700 ° C) and Table 2 (for roasting temperature of 800 ° C), respectively. It became a street.

【0018】[0018]

【表1】 [Table 1]

【0019】[0019]

【表2】 [Table 2]

【0020】これらの結果から判るように、塩化第一鉄
と塩化第二鉄及びMn,Mg,Niのうち1種の塩化物
との混合水溶液の焙焼により得られる複合酸化物の組成
は、混合水溶液の組成と良い一致を示している。又、こ
の実験の際に排出されるガスは、10%水酸化ナトリウ
ム溶液を通した後、ヨウ化カリウム−でんぷん溶液に通
じた反応により塩素ガスを生成するか否かを調べたとこ
ろ、炉内雰囲気をAir気流としたときは青色に変色す
るのに対し、30%水蒸気を含むAir気流としたとき
には変色が起こらなかった。このことより、反応を水蒸
気分圧の高い状態で行うと塩素ガスの発生が抑制されて
いるのが判る。
As can be seen from these results, the composition of the composite oxide obtained by roasting the mixed aqueous solution of ferrous chloride and ferric chloride and one of Mn, Mg and Ni chlorides is as follows: It shows good agreement with the composition of the mixed aqueous solution. Further, the gas discharged in this experiment was passed through a 10% sodium hydroxide solution, and then it was investigated whether chlorine gas was produced by the reaction passed through the potassium iodide-starch solution. When the atmosphere was an Air stream, the color changed to blue, whereas when the Air stream containing 30% water vapor was used, the color did not change. From this, it can be seen that the generation of chlorine gas is suppressed when the reaction is performed in a state where the partial pressure of water vapor is high.

【0021】実施例2は、複合酸化物及びソフトフェラ
イトの製造方法に関するものである。ここでは塩化第一
鉄84.5g/1、塩化第二鉄108.3g/1、塩化
マンガン58.3g/1及び塩酸9.3g/1の混合水
溶液を700℃に保ったルスナー炉で噴霧焙焼を行っ
た。このルスナー炉は、塩酸ガスの吸収塔の直前に濃縮
設備が設置されており、実験の前半は濃縮装置に回収塩
酸を循環させて操業し、実験の後半は塩化第一鉄を約2
30g/1含む鉄鋼塩酸廃液を流して濃縮操業を行っ
た。このとき得られた複合酸化物を分析した組成結果を
塩化物混合水溶液の組成結果と比較して表3に示す。
Example 2 relates to a method for producing a composite oxide and soft ferrite. Here, a mixed aqueous solution of ferrous chloride 84.5 g / 1, ferric chloride 108.3 g / 1, manganese chloride 58.3 g / 1 and hydrochloric acid 9.3 g / 1 was spray roasted in a Rusner furnace kept at 700 ° C. I baked it. This Lusner furnace is equipped with a concentrating equipment immediately before the absorption tower for hydrochloric acid gas. In the first half of the experiment, the recovered hydrochloric acid was circulated through the concentrator to operate.
A concentration operation was performed by flowing a steel hydrochloric acid waste liquid containing 30 g / 1. The compositional results of the analysis of the composite oxide obtained at this time are shown in Table 3 in comparison with the compositional results of the chloride mixed aqueous solution.

【0022】[0022]

【表3】 [Table 3]

【0023】この場合も、それぞれの組成は良い一致を
示していることが判る。又、この実験中、排ガス中の塩
素ガスの測定を行った結果を実験の前半(濃縮を行わな
い場合)と後半(濃縮を行った場合)とに分けて表4に
示す。
Also in this case, it can be seen that the respective compositions show good agreement. Further, the results of measuring chlorine gas in the exhaust gas during this experiment are shown in Table 4 separately for the first half (when the concentration is not performed) and the second half (when the concentration is performed) of the experiment.

【0024】[0024]

【表4】 [Table 4]

【0025】これから判るように、実験の前半の塩化第
一鉄の濃縮を行わない場合は、塩素ガスが大気中に排出
されるのに対し、後半の濃縮を行う場合は、塩素ガスの
処理が効率良く行われることが判る。
As can be seen, when ferrous chloride is not concentrated in the first half of the experiment, chlorine gas is discharged into the atmosphere, whereas in the latter half, chlorine gas is treated. You can see that it is done efficiently.

【0026】更に、このとき得られた複合酸化物に酸化
亜鉛を用いてFe2 3 =52.5mol %,MnO=3
5.5mol %,ZnO=12mol %の組成を有する低損
失フェライトを常手法により作成した。この際、組成調
整の為に酸化鉄も添加されている。又、比較例として酸
化鉄、酸化マンガン、酸化亜鉛を原料として同組成のソ
フトフェライトを製造した。この本発明に係るソフトフ
ェライト及び比較例のソフトフェライトの磁気特性を表
5に示す。
Furthermore, using zinc oxide in the composite oxide obtained at this time, Fe 2 O 3 = 52.5 mol%, MnO = 3
A low-loss ferrite having a composition of 5.5 mol% and ZnO = 12 mol% was prepared by a conventional method. At this time, iron oxide is also added to adjust the composition. As a comparative example, a soft ferrite having the same composition was manufactured using iron oxide, manganese oxide, and zinc oxide as raw materials. Table 5 shows the magnetic characteristics of the soft ferrite according to the present invention and the soft ferrite of the comparative example.

【0027】[0027]

【表5】 [Table 5]

【0028】これより、本発明のソフトフェライト製造
方法により生成されるソフトフェライトは、比較例のも
のと比べて同程度以上の磁気特性を有することが判る。
From the above, it is understood that the soft ferrite produced by the method for producing soft ferrite of the present invention has magnetic characteristics which are about the same as or higher than those of the comparative example.

【0029】[0029]

【発明の効果】以上のように本発明によれば、組成ずれ
の問題なく、しかも鋼板の塩酸酸洗廃液の様な塩化鉄と
低価格のMn,Ni,Mg原料とを用いて一般的な噴霧
焙焼炉により簡単に複合酸化物を製造でき、更にこの複
合酸化物を原料として優れた磁気特性を有するフェライ
トを製造することが可能となる。殊に、複合酸化物の製
造時に生成される塩素ガスの処理対策を完全に施してい
るので、トータルとしてコスト的に有利であるばかりで
なく、工業的に重要な複合酸化物及びソフトフェライト
の製造方法が実現されている。
As described above, according to the present invention, there is no problem of composition deviation, and moreover, it is general that iron chloride such as a hydrochloric acid pickling waste liquid of steel sheet and low cost Mn, Ni, Mg raw materials are used. The composite oxide can be easily produced by the spray roasting furnace, and further, the ferrite having excellent magnetic properties can be produced by using the composite oxide as a raw material. In particular, since it completely takes measures against the treatment of chlorine gas produced during the production of complex oxides, it is not only economically advantageous in total, but also the production of industrially important complex oxides and soft ferrites. The method has been realized.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 築地 憲夫 千葉県市川市高谷新町7番地の1 日新製 鋼株式会社新材料研究所内 (72)発明者 原 勝成 千葉県市川市高谷新町7番地の1 日新製 鋼株式会社新材料研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Norio Tsukiji, No. 1 at 7 Shin Takamachi Shinmachi, Ichikawa City, Chiba Prefecture, Nisshin Steel Co., Ltd. New Materials Research Center (72) Inventor Katsunari Hara, 7 Takamachi Shinmachi, Ichikawa City, Chiba Prefecture 1 Nisshin Steel Co., Ltd., New Materials Research Center

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 フェライト組成の主成分金属元素である
Mn,Mg,Niのうちの少なくとも1種以上と、Zn
及びFeとから成るソフトフェライトの原料としての複
合酸化物の製造方法であって、前記フェライト組成のM
n,Mg,Niのうちの1種以上の塩化物,塩化第一鉄
及び塩化第二鉄の混合水溶液を噴霧焙焼することを特徴
とする複合酸化物の製造方法。
1. At least one or more of Mn, Mg, and Ni, which are the main metal elements of the ferrite composition, and Zn.
A method for producing a composite oxide as a raw material for soft ferrite, comprising:
A method for producing a composite oxide, which comprises spray roasting a mixed aqueous solution of one or more chlorides of n, Mg and Ni, ferrous chloride and ferric chloride.
【請求項2】 前記噴霧焙焼する際の熱源として水素元
素を含む燃料を使用することを特徴とする請求項1記載
の複合酸化物の製造方法。
2. The method for producing a complex oxide according to claim 1, wherein a fuel containing a hydrogen element is used as a heat source for the spray roasting.
【請求項3】 前記噴霧焙焼する際の高温の熱風中に水
蒸気を吹き込むことを特徴とする請求項1記載の複合酸
化物の製造方法。
3. The method for producing a composite oxide according to claim 1, wherein steam is blown into hot air at a high temperature during the spray roasting.
【請求項4】 前記噴霧焙焼する際に、噴霧焙焼設備の
焙焼炉から得られる高温の排出ガスを、塩酸ガス回収用
の塩酸ガス吸収塔へ導入する直前に前記塩化第一鉄を含
む塩化物水溶液と接触させることにより該塩化物水溶液
を濃縮させる濃縮工程を有することを特徴とする請求項
1記載の複合酸化物の製造方法。
4. When the spray roasting is carried out, the ferrous chloride is removed immediately before the high temperature exhaust gas obtained from the roasting furnace of the spray roasting equipment is introduced into a hydrochloric acid gas absorption tower for recovering hydrochloric acid gas. The method for producing a complex oxide according to claim 1, further comprising a concentration step of concentrating the chloride aqueous solution by bringing it into contact with a chloride aqueous solution containing the same.
【請求項5】 前記塩化第一鉄及び塩化第二鉄に鉄鋼塩
酸酸洗廃液を使用することを特徴とする請求項1乃至4
記載の複合酸化物の製造方法。
5. An iron and hydrochloric acid pickling waste liquid is used for the ferrous chloride and ferric chloride.
A method for producing the composite oxide described.
【請求項6】 請求項1乃至5記載の複合酸化物の製造
方法により製造される複合酸化物と、亜鉛化合物とを原
料とすることを特徴とするソフトフェライトの製造方
法。
6. A method for producing soft ferrite, characterized in that a composite oxide produced by the method for producing a composite oxide according to claim 1 and a zinc compound are used as raw materials.
JP3340983A 1991-12-24 1991-12-24 Manufacture of composite oxide and soft ferrite Withdrawn JPH05175033A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3340983A JPH05175033A (en) 1991-12-24 1991-12-24 Manufacture of composite oxide and soft ferrite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3340983A JPH05175033A (en) 1991-12-24 1991-12-24 Manufacture of composite oxide and soft ferrite

Publications (1)

Publication Number Publication Date
JPH05175033A true JPH05175033A (en) 1993-07-13

Family

ID=18342117

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JPH05175033A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9073760B2 (en) 2010-12-24 2015-07-07 Shoei Chemical Inc. Manufacturing method and manufacturing device for multiple oxide
CN115368125A (en) * 2022-06-18 2022-11-22 信丰天科磁业有限公司 Manganese-zinc soft magnetic ferrite material with high breaking strength and manufacturing method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9073760B2 (en) 2010-12-24 2015-07-07 Shoei Chemical Inc. Manufacturing method and manufacturing device for multiple oxide
CN115368125A (en) * 2022-06-18 2022-11-22 信丰天科磁业有限公司 Manganese-zinc soft magnetic ferrite material with high breaking strength and manufacturing method thereof

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