JPH0383819A - Production of oxide raw material for ferrite - Google Patents
Production of oxide raw material for ferriteInfo
- Publication number
- JPH0383819A JPH0383819A JP1218676A JP21867689A JPH0383819A JP H0383819 A JPH0383819 A JP H0383819A JP 1218676 A JP1218676 A JP 1218676A JP 21867689 A JP21867689 A JP 21867689A JP H0383819 A JPH0383819 A JP H0383819A
- Authority
- JP
- Japan
- Prior art keywords
- chloride
- roasting
- waste solution
- hydrochloric acid
- raw material
- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000002994 raw material Substances 0.000 title claims description 19
- 229910000859 α-Fe Inorganic materials 0.000 title description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002699 waste material Substances 0.000 claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 238000005554 pickling Methods 0.000 claims abstract description 18
- 229910001035 Soft ferrite Inorganic materials 0.000 claims abstract description 16
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 13
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 11
- 239000010959 steel Substances 0.000 claims abstract description 11
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 10
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 17
- 150000001805 chlorine compounds Chemical group 0.000 abstract description 7
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 23
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 16
- 239000011572 manganese Substances 0.000 description 15
- 238000004458 analytical method Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 235000005074 zinc chloride Nutrition 0.000 description 8
- 239000011592 zinc chloride Substances 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 235000002867 manganese chloride Nutrition 0.000 description 5
- 239000011565 manganese chloride Substances 0.000 description 5
- 229940099607 manganese chloride Drugs 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000004451 qualitative analysis Methods 0.000 description 5
- 229910052596 spinel Inorganic materials 0.000 description 5
- 239000011029 spinel Substances 0.000 description 5
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は、鉄鋼業における鋼板等の塩酸酸洗の際に生じ
る酸洗廃液中の塩化鉄を利用してソフトフェライト用原
料となる酸化物を製造する方法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention utilizes iron chloride in the pickling waste liquid generated during hydrochloric acid pickling of steel plates, etc. in the steel industry to produce an oxide that is a raw material for soft ferrite. The present invention relates to a method for manufacturing.
〔従来の技術１
従来より鉄鋼業においては鋼板等の塩酸酸洗廃液を回収
して濃縮し、これを焙焼することにより酸化鉄を製造し
ている。焙焼方法としては、■ ６００〜９００℃に保
持した炉内に、炉頂より塩酸酸洗廃液を噴霧し炉内にて
熱分解させ酸化鉄を炉底より取り出す噴霧焙焼法、
■ ６００〜９００℃に保持した流動層中に塩酸酸洗廃
液を噴霧し熱分解させ酸化鉄を炉頂より捕集する流動焙
焼法
などが行われている。[Prior Art 1] Conventionally, in the steel industry, iron oxide has been produced by collecting and concentrating waste liquid from hydrochloric acid pickling of steel plates, etc., and roasting it. Roasting methods include: (1) a spray roasting method in which hydrochloric acid pickling waste is sprayed from the top of a furnace maintained at 600 to 900°C, thermally decomposed in the furnace, and iron oxide is taken out from the bottom of the furnace; A fluidized roasting method is used in which hydrochloric acid pickling waste is sprayed into a fluidized bed maintained at 900°C, thermally decomposed, and iron oxide is collected from the top of the furnace.
ソフトフェライト用原料の製造に関しては、上記の方法
において、塩化鉄溶液の焙焼前に鉄以外のフェライト構
成成分を塩化物又は金属の形態にて溶解混合した後に上
記と同様の焙焼炉にて焙焼する方法が、噴霧焙焼法では
特公昭６３−１７７７６号公報に、流動焙焼法では特開
昭６３−１５６０１７号公報に報告されている。Regarding the production of raw materials for soft ferrite, in the above method, before roasting the iron chloride solution, ferrite constituents other than iron are dissolved and mixed in the form of chlorides or metals, and then in the same roasting furnace as above. As for the roasting method, the spray roasting method is reported in Japanese Patent Publication No. 17776/1982, and the fluidized roasting method is reported in Japanese Patent Application Laid-Open No. 63-156017.
これらの方法ではフェライト構成成分を塩化物原料にて
混合し焙焼することにより、均一に混合した酸化物が得
られるため、フェライト製造工程中、仮焼、粉砕工程を
省略することができ、かつ工程中の不純物汚染が少なく
なる利点があるとされている。In these methods, a uniformly mixed oxide is obtained by mixing the ferrite constituents with a chloride raw material and roasting it, so the calcination and crushing steps can be omitted during the ferrite manufacturing process, and It is said to have the advantage of reducing impurity contamination during the process.
しかし、前者については高温にて焙焼するために蒸気圧
の高い塩化亜鉛等は同時に焙焼することが不可能であり
、また後者についても６００℃以上の温度にて焙焼する
ために、１００ｍｍＨｇという塩化亜鉛の高い蒸気圧の
ために亜鉛の組成ずれが生じてしまう。However, since the former is roasted at a high temperature, it is impossible to roast zinc chloride, etc., which has a high vapor pressure, at the same time, and the latter is also roasted at a temperature of 600°C or higher, so the temperature is 100 mmHg. Due to the high vapor pressure of zinc chloride, a compositional shift in zinc occurs.
〔発明が解決しようとする課題Ｊ
以上のように従来技術では、塩化亜鉛等の蒸気圧の高い
原料を含む塩化物の混合物を焙焼して所定の組成のソフ
トフェライト用原料酸化物を直接に製造する方法がなか
った。[Problem to be Solved by the Invention J] As described above, in the prior art, a chloride mixture containing a raw material with a high vapor pressure such as zinc chloride is roasted to directly produce a raw material oxide for soft ferrite with a predetermined composition. There was no way to manufacture it.
［課題を解決するための手段］
そこで本発明者は鋭意研究の結果、焙焼前の塩化物の成
分調整を行うことによりこの問題を解決する方法を見出
した。すなわち、鋼材の塩酸酸洗廃液中の塩化第一鉄を
塩化第二鉄に酸化し、全鉄濃度に占める３価鉄濃度を７
０％以上とした後に、ソフトフェライト用原料に必要と
される元素であるＭｎ、Ｚｎ、Ｃｕ、Ｎｉ、Ｍｇ及びＧ
ｏのうちから選ばれた少なくとも一種を塩化物または金
属の形態にて添加、溶解、混合後に、従来方法よりも低
温である６００℃以下の温度にて焙焼することにより、
蒸気圧の高い元素を含んだ場合においても、直接に所望
のソフトフェライト用原料酸化物を製造できることが判
明した。[Means for Solving the Problem] As a result of intensive research, the present inventor found a method for solving this problem by adjusting the chloride component before roasting. In other words, ferrous chloride in the waste solution from hydrochloric acid pickling of steel materials is oxidized to ferric chloride, and the trivalent iron concentration in the total iron concentration is reduced to 7.
After making it 0% or more, Mn, Zn, Cu, Ni, Mg and G, which are the elements required for the raw material for soft ferrite,
By adding, dissolving, and mixing at least one selected from o in the form of chloride or metal, and then roasting at a temperature of 600 ° C. or less, which is lower than the conventional method,
It has been found that the desired raw material oxide for soft ferrite can be directly produced even when an element with a high vapor pressure is contained.
また、上記工程中、前記ソフトフェライト用原料に必要
とされる元素すなわちＭｎ、Ｚｎ。In addition, in the above process, elements required for the raw material for soft ferrite, namely Mn and Zn.
Ｃｕ、Ｎｉ、Ｍｇ及びＣｏのうちから選ばれた少なくと
も一種を先に塩酸酸洗廃液に添加、溶解、混合後に、塩
化第一鉄を塩化第二鉄に酸化して焙焼してもよい。At least one selected from Cu, Ni, Mg, and Co may be added to the hydrochloric acid pickling waste solution, dissolved, and mixed, and then ferrous chloride may be oxidized to ferric chloride and roasted.
〔作用１
本発明に至った基礎実験の結果について次に述べる。試
薬特級のＦｅＣβ２、ＦｅＣβ３、Ｍ ｎ Ｃ！２２、
ＭｇＣｌ２２、ＺｎＣ１；２２なる塩化物を２種又は３
種混合して乾燥した試料を作製した。各試料の組成を第
１表に示す。[Effect 1] The results of the basic experiments that led to the present invention will be described below. Reagent grade FeCβ2, FeCβ3, M n C! 22,
MgCl22, ZnC1; 2 or 3 chlorides
A dried sample was prepared by mixing the seeds. The composition of each sample is shown in Table 1.
これらの８試料を横型管状炉内にて種々の温度にて焼鈍
して、塩化物がすべて酸化物に熱分解する温度（酸化反
応終了温度）を調査した。生成酸化物はＸ線回折による
定性分析にて行った。その結果を第２表に示す。２価鉄
を３価鉄に置き換えて焙焼した場合には、試料ｌと２の
比較、試料３と４の比較より、５０℃以上低い温度にて
酸化物が生成できることがわかる。そのため、蒸気圧の
高いＺｎｃＩ２２を含んでいても、６００℃以下の温度
にて焙焼が可能となることが試料５と６の比較、試料７
と８の比較から明らかである。このように塩化第二鉄に
他の金属元素を添加した場合には、低温にて焙焼するこ
とができ、これより蒸気圧の高い元素を含む場合におい
ても酸化焙焼が十分に可能となる。These eight samples were annealed at various temperatures in a horizontal tubular furnace, and the temperature at which all chlorides were thermally decomposed into oxides (oxidation reaction completion temperature) was investigated. The produced oxide was qualitatively analyzed by X-ray diffraction. The results are shown in Table 2. Comparison of Samples 1 and 2 and Samples 3 and 4 shows that when bivalent iron is replaced with trivalent iron and roasted, oxides can be produced at a temperature lower than 50°C. Therefore, even if it contains ZncI22 with a high vapor pressure, it is possible to roast it at a temperature below 600°C, as compared with Samples 5 and 6, and Sample 7.
It is clear from the comparison between and 8. When other metal elements are added to ferric chloride in this way, roasting can be performed at low temperatures, and even when elements with higher vapor pressures are included, oxidative roasting is fully possible. .
第３表は更に、試料５と６について、酸化焙焼により塩
化物が酸化物になった温度でのＦｅ、Ｍｎ及びＺｎのの
組成を化学分析により求めた結果である。表中の値は、
Ｆｅ、Ｍｎ、Ｚｎの３元素成分の総和が重量％にて１０
０％となるように求めた。Table 3 further shows the results of chemical analysis of the compositions of Fe, Mn, and Zn for Samples 5 and 6 at the temperature at which chlorides became oxides through oxidative roasting. The values in the table are
The total of the three elemental components of Fe, Mn, and Zn is 10% by weight.
It was calculated to be 0%.
この化学分析から、試料６については、５１０℃、５６
０℃においては組成ずれは見られないが、６００℃を越
えると亜鉛の蒸発による組成ずれが発生している。試料
Ｓについては６００’Ｃ以上にて焙焼しているために亜
鉛の蒸発による組成ずれが顕著に発生゛しているゆこの
ように６ｏｏ℃以上での焙焼は組成のずれにより好まし
くない。From this chemical analysis, for sample 6, 510°C, 56°C
No composition deviation is observed at 0°C, but when the temperature exceeds 600°C, composition deviation occurs due to evaporation of zinc. Sample S was roasted at 600° C. or higher, and as a result, a significant compositional shift occurred due to the evaporation of zinc. As shown in the above, roasting at 600° C. or higher is not preferable due to the compositional shift.
以上の予備実験より、塩化第二鉄とＺｎ及び他のソフト
フェライト原料として必要となるＮｌ。From the above preliminary experiments, ferric chloride, Zn, and other Nl required as soft ferrite raw materials.
Ｍｇ、Ｍｎ、Ｃｕ等の元素を金属または塩化物の形態に
て混合し、低温にて焙焼することにより、蒸気圧の高い
元素の蒸発を防ぎながらフェライト用原料酸化物を製造
することが可能となることがわかる。By mixing elements such as Mg, Mn, and Cu in the form of metals or chlorides and roasting them at low temperatures, it is possible to produce raw material oxides for ferrite while preventing evaporation of elements with high vapor pressure. It can be seen that
塩化第一鉄から塩化第二鉄へ酸化する方法としては塩素
ガスを吹き込むことによる塩素酸化が適切であるが、そ
の他の方法としては、酸素の吹き込み、電解酸化、酸化
触媒添加等の酸化方法を用いてもよい。Chlorine oxidation by blowing chlorine gas is appropriate for oxidizing ferrous chloride to ferric chloride, but other oxidation methods include blowing oxygen, electrolytic oxidation, and adding an oxidation catalyst. May be used.
また、廃液の焙焼方法としては、ロータリーキルン焙焼
、流動層内焙焼、その他の焼成方法を使用することがで
きる。Further, as a method for roasting the waste liquid, rotary kiln roasting, fluidized bed roasting, and other firing methods can be used.
塩酸酸洗廃液中の３価鉄が全鉄中に占める割合を７０％
以上に限定した理由は、これ以下では、低温にて焙焼し
た場合に、未反応にて残留する塩化第一鉄が多量に生じ
、酸化物製造における歩留りが低下してしまう上に組成
ずれの原因になってしまい、効果が少ないからである。Trivalent iron in hydrochloric acid pickling waste accounts for 70% of total iron
The reason for this limitation is that if the temperature is lower than this, a large amount of unreacted ferrous chloride will be produced when roasting at a low temperature, which will reduce the yield in oxide production and cause a composition shift. This is because it becomes a cause and has little effect.
〔実施例］ 以下に実施例に従い本発明内容を詳述する。〔Example] The contents of the present invention will be explained in detail below according to Examples.
実施例１
塩酸酸洗廃液に塩素ガスを吹き込み塩化第一鉄を塩化第
二鉄に酸化した。この廃液を窒素雰囲気のグローボック
ス中にて１００℃にて乾燥した。Example 1 Chlorine gas was blown into the hydrochloric acid pickling waste solution to oxidize ferrous chloride to ferric chloride. This waste liquid was dried at 100° C. in a glow box with a nitrogen atmosphere.
これを化学分析にて組成を調べたところ第４表の結果を
得た。はとんど塩化第二鉄になっていることが確認でき
た。When the composition of this was investigated by chemical analysis, the results shown in Table 4 were obtained. It was confirmed that most of the material was ferric chloride.
この廃液に塩化亜鉛及び塩化マンガンを組成比にてＦｅ
：Ｍｎ：Ｚｎが６９．３重量％： ２２．８重量％ニア
、９重量％となるように混合し、５７０℃に保持した焙
焼炉内に炉頂より噴霧焙焼し、ソフトフェライト用原料
酸化物を得た。Zinc chloride and manganese chloride were added to this waste liquid in a composition ratio of Fe.
:Mn:Zn was mixed so that it was 69.3% by weight: 22.8% by weight and 9% by weight, and sprayed from the top of the furnace at 570°C and roasted to obtain a raw material for soft ferrite. An oxide was obtained.
得られた酸化物の平均粒径、は０．５〜１．０μｍであ
り、Ｘ線回折による定性分析では、Ｆｅ２Ｏ３、Ｍ ｎ
２０３、スピネルの３成分が存在し、塩化物の存在は
確認できなかった。The average particle size of the obtained oxide was 0.5 to 1.0 μm, and qualitative analysis by X-ray diffraction revealed that Fe2O3, Mn
Three components of 203 and spinel were present, and the presence of chloride could not be confirmed.
化学分析から、Ｆｅ、Ｍｎ、Ｚｎの重量組成比は第５表
の通りであり、Ｚｎの蒸発による組成ずれは見られない
。From the chemical analysis, the weight composition ratios of Fe, Mn, and Zn are as shown in Table 5, and no composition shift due to evaporation of Zn is observed.
比較例１
塩酸酸洗廃液を窒素雰囲気のグローボックス中にて１０
０℃にて乾燥した。これを化学分析にて組成を調べたと
ころ第１表の結果を得た。はとんどの成分が２価鉄であ
った。この廃液に塩化亜鉛及び塩化マンガン重量組成比
にてＦｅ：Ｍｎ：Ｚｎが６９．３重量％：２２．８重量
％ニア、９重量％となるように混合し、７８０℃に保持
したルスナー炉内に炉頂より噴霧焙焼し、ソフトフェラ
イト用原料酸化物を得た。Comparative Example 1 Hydrochloric acid pickling waste liquid was placed in a nitrogen atmosphere glow box for 10 minutes.
It was dried at 0°C. When the composition was investigated by chemical analysis, the results shown in Table 1 were obtained. Most of the components were divalent iron. This waste liquid was mixed with zinc chloride and manganese chloride so that the weight composition ratio of Fe:Mn:Zn was 69.3% by weight: 22.8% by weight, 9% by weight, and the mixture was placed in a Lussner furnace maintained at 780°C. The mixture was then spray roasted from the top of the furnace to obtain a raw material oxide for soft ferrite.
得られた酸化物の平均粒径は０．８〜２．０μｍであり
、ｘ１１回折による定性分析では、Ｆｅ２Ｏ３、Ｍ ｎ
２０ Ｂ、スピネルの３成分が存在し、塩化物の存在
は確認できなかったゆ化学分析から、Ｆｅ、Ｍｎ、Ｚｎ
の重量組成比は第５表のとおりであり、Ｚｎの蒸発によ
る組成ずれは非常に大きく、後工程での成分調整が避け
られないことがわかる。The average particle size of the obtained oxide was 0.8 to 2.0 μm, and qualitative analysis by x11 diffraction revealed that Fe2O3, Mn
20 B, three components of spinel were present, and the presence of chloride could not be confirmed. Chemical analysis revealed that Fe, Mn, and Zn were present.
The weight composition ratios are as shown in Table 5, and it can be seen that the composition deviation due to Zn evaporation is very large, and component adjustment in the subsequent process is unavoidable.
実施例２
塩酸酸洗廃液に塩素ガスを吹き込み塩化第一鉄を塩化第
二鉄に酸化した。この廃液に塩化亜鉛及び塩化マンガン
を重量組成比にてＦｅ ： Ｍｎ ：Ｚｎが６９．３重
量％：２２．８重量％ニア、９重量％となるように混合
した。これを乾燥した後に、乳鉢にて粉末状にし、ロー
タリーキルンを使用して５２０℃にて焙焼し、ソフトフ
ェライト用原料酸化物を得た。Example 2 Chlorine gas was blown into the hydrochloric acid pickling waste solution to oxidize ferrous chloride to ferric chloride. Zinc chloride and manganese chloride were mixed into this waste liquid so that the weight composition ratio of Fe:Mn:Zn was 69.3% by weight: 22.8% by weight and 9% by weight. After drying this, it was powdered in a mortar and roasted at 520°C using a rotary kiln to obtain a raw material oxide for soft ferrite.
Ｘ線回折による定性分析ではＦｅ２Ｏ３、Ｍ ｎ ２０
３、スピネルの３成分が存在し、塩化物の存在は確認で
きなかった。In qualitative analysis by X-ray diffraction, Fe2O3, M n 20
3. Three components of spinel were present, and the presence of chloride could not be confirmed.
化学分析から、Ｆｅ、Ｍｎ、Ｚｎの重量組成比は第５表
の通りであり、Ｚｎの蒸発による組成ずれは見られない
。From the chemical analysis, the weight composition ratios of Fe, Mn, and Zn are as shown in Table 5, and no composition shift due to evaporation of Zn is observed.
比較例２
塩酸酸洗廃液に塩化亜鉛及び塩化マンガンを重量組成比
にてＦｅ：Ｍｎ：Ｚｎが６９．３重量％：２２．８重量
％ニア、９重量％となるように混合した。これを乾燥し
た後に、乳鉢にて粉末状にしロータリーキルンを使用し
て６２０℃にて焙焼し、ソフトフェライト用原料酸化物
を得た。Comparative Example 2 Zinc chloride and manganese chloride were mixed into a hydrochloric acid pickling waste solution so that the weight composition ratio of Fe:Mn:Zn was 69.3% by weight: 22.8% by weight, near 9% by weight. After drying this, it was made into powder in a mortar and roasted at 620°C using a rotary kiln to obtain a raw material oxide for soft ferrite.
Ｘ線回折による定性分析ではＦｅ２Ｏ３、Ｍ ｎ ２０
３、スピネルの３成分が存在し、塩化物の存在は確認で
きなかった。In qualitative analysis by X-ray diffraction, Fe2O3, M n 20
3. Three components of spinel were present, and the presence of chloride could not be confirmed.
化学分析から、Ｆｅ、Ｍｎ、Ｚｎの重量組成比は第５表
の通りであり、Ｚｎの蒸発による組成ずれは相当に大き
いことがわかる。The chemical analysis shows that the weight composition ratios of Fe, Mn, and Zn are as shown in Table 5, and the composition shift due to Zn evaporation is quite large.
実施例３
塩酸酸洗廃液に塩化亜鉛及び塩化マンガンを重量組成比
にてＦｅ二Ｍｎ：Ｚｎが６９．３重量％：２２．８重量
％ニア、９重量％となるように混合した。これに塩素ガ
スを吹き込み塩化第一鉄を塩化第二鉄に酸化した。これ
を乾燥した後に、乳鉢にて粉末状にし、ロータリーキル
ンを使用して５２０℃にて焙焼し、ソフトフェライト用
原料酸化物を得た。Example 3 Zinc chloride and manganese chloride were mixed into a hydrochloric acid pickling waste solution so that the weight composition ratio of Fe2Mn:Zn was 69.3% by weight: 22.8% by weight, 9% by weight. Chlorine gas was blown into this to oxidize ferrous chloride to ferric chloride. After drying this, it was powdered in a mortar and roasted at 520°C using a rotary kiln to obtain a raw material oxide for soft ferrite.
Ｘ線回折による定性分析ではＦｅ２Ｏ３、Ｍ ｎ ２０
３、スピネルの３成分が存在し、塩化物の存在は確認で
きなかった。In qualitative analysis by X-ray diffraction, Fe2O3, M n 20
3. Three components of spinel were present, and the presence of chloride could not be confirmed.
化学分析から、 Ｆｅ、 Ｍ ｎ 。From chemical analysis, Fe, M n .
Ｚｎの重量組成比 は第５表の通りであり、 Ｚｎの蒸発による組成す れは見られない。Weight composition ratio of Zn is as shown in Table 5, Composition due to evaporation of Zn This cannot be seen.
第
表
単位は重量％
第
表
単位は重量％
［発明の効果］
以上のように本発明によれば鋼板の塩酸酸洗廃液中の塩
化第一鉄を塩化第二鉄に酸化した後に、ソフトフェライ
ト用原料として必要な成分元素を金属または塩化物の形
態にて混合し、その後焙焼するので、蒸気圧の低い元素
が存在する場合においても同時に焙焼することが可能と
なり、従来方法と比較して組成ずれがなく、低コストに
てソフトフェライト用酸化物磁性材料を製造することが
可能となる。The unit in the table is % by weight. [Effect of the invention] As described above, according to the present invention, after oxidizing ferrous chloride in the waste solution of hydrochloric acid pickling of steel sheets to ferric chloride, soft ferrite is produced. Since the component elements required as raw materials are mixed in the form of metals or chlorides and then roasted, it is possible to roast them at the same time even when elements with low vapor pressure are present, compared to conventional methods. Therefore, it becomes possible to produce an oxide magnetic material for soft ferrite at low cost without compositional deviation.
Claims (1)
酸化し、全鉄成分中の３価鉄の割合を７０％以上とした
後に、該廃液にＺｎ， Ｍｎ，Ｎｉ，Ｃｕ，Ｍｇ及びＣｏから選ばれた少なくと
も一種を金属または塩化物の形態にて添加、溶解、混合
した後、６００℃以下の温度にて焙焼することを特徴と
するソフトフェライト用原料酸化物の製造方法。 ２ 鋼材の塩酸酸洗廃液に、Ｚｎ，Ｍｎ， Ｎｉ，Ｃｕ，Ｍｇ及びＣｏから選ばれた少なくとも一種
を金属または塩化物の形態にて添加、溶解、混合した後
、該廃液中の塩化第一鉄を塩化第二鉄に酸化し、全鉄成
分中の３価鉄の割合を７０％以上とした後に、６００℃
以下の温度にて焙焼することを特徴とするソフトフェラ
イト用原料酸化物の製造方法。[Scope of Claims] 1. After oxidizing ferrous chloride in the waste solution of hydrochloric acid pickling of steel materials to ferric chloride and making the proportion of trivalent iron in the total iron component 70% or more, Zn is added to the waste solution. , Mn, Ni, Cu, Mg, and Co in the form of a metal or chloride, which is added, dissolved, and mixed, and then roasted at a temperature of 600°C or less. Method for producing raw material oxide for use. 2. After adding, dissolving, and mixing at least one selected from Zn, Mn, Ni, Cu, Mg, and Co in the form of metal or chloride to the waste solution from hydrochloric acid pickling of steel materials, the first chloride in the waste solution is After oxidizing iron to ferric chloride and increasing the proportion of trivalent iron in the total iron component to 70% or more, 600°C
A method for producing a raw material oxide for soft ferrite, which comprises roasting at the following temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1218676A JPH0383819A (en) | 1989-08-28 | 1989-08-28 | Production of oxide raw material for ferrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1218676A JPH0383819A (en) | 1989-08-28 | 1989-08-28 | Production of oxide raw material for ferrite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0383819A true JPH0383819A (en) | 1991-04-09 |
Family
ID=16723676
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1218676A Pending JPH0383819A (en) | 1989-08-28 | 1989-08-28 | Production of oxide raw material for ferrite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0383819A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07206445A (en) * | 1994-01-06 | 1995-08-08 | Kawasaki Steel Corp | Production of oxide as stock of ni-zn ferrite |
-
1989
- 1989-08-28 JP JP1218676A patent/JPH0383819A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07206445A (en) * | 1994-01-06 | 1995-08-08 | Kawasaki Steel Corp | Production of oxide as stock of ni-zn ferrite |
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