JPH03146422A - Method and apparatus for producing high purity iron oxide powder with chromium-containing iron sulfate solution - Google Patents
Method and apparatus for producing high purity iron oxide powder with chromium-containing iron sulfate solutionInfo
- Publication number
- JPH03146422A JPH03146422A JP28643089A JP28643089A JPH03146422A JP H03146422 A JPH03146422 A JP H03146422A JP 28643089 A JP28643089 A JP 28643089A JP 28643089 A JP28643089 A JP 28643089A JP H03146422 A JPH03146422 A JP H03146422A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- chromium
- soln
- iron
- stage
- 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
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910000358 iron sulfate Inorganic materials 0.000 title claims abstract description 25
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 title claims abstract description 9
- 239000011651 chromium Substances 0.000 title claims description 37
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims description 23
- 229910052804 chromium Inorganic materials 0.000 title claims description 23
- 238000000034 method Methods 0.000 title description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000006386 neutralization reaction Methods 0.000 claims description 12
- 238000005192 partition Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002923 metal particle Substances 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 abstract description 6
- 239000010959 steel Substances 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 238000005554 pickling Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 abstract 1
- 235000021110 pickles Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000003472 neutralizing effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229960002089 ferrous chloride Drugs 0.000 description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910001430 chromium ion Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910001035 Soft ferrite Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 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
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009279 wet oxidation reaction Methods 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〉
本発明は含クロム硫酸鉄溶液から高純度の酸化鉄粉を製
造する方法及びそれに用いる中和装置に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing high-purity iron oxide powder from a chromium-containing iron sulfate solution and a neutralization device used therein.
〈従来の技術〉
近年、酸化鉄粉はソフトフェライト、ゲーサイトメタル
鉄粉等の各分野で多用されている。この酸化鉄粉は鉄鉱
石を原料として粉砕・精製するか、あるいは塩酸廃液中
から塩化鉄等の化合物を処理して製造されている。この
酸化鉄粉は一般的Ｆｅ２０ｇ純度で９８〜９９％である
が用途に於いては更に高純度のものが要求され一層の不
純物の低減が要求されている。この様な酸化鉄を造る方
法の一つとして特公昭６０−８９８０号公報に示される
方法があり、これはクロムを多量に含む塩化第１鉄水溶
液を鉄材を溶液中に存在させてｐＨ１，５〜３．５にな
るまで酸素を多量に含む気体と接触させ、生成する沈澱
物を分離するクロムを殆ど含まない塩化第１鉄水溶液の
製造方法であってかなりの効果を上げている。<Prior Art> In recent years, iron oxide powder has been widely used in various fields such as soft ferrite and goethite metal iron powder. This iron oxide powder is produced by pulverizing and refining iron ore as a raw material, or by treating compounds such as iron chloride from hydrochloric acid waste liquid. This iron oxide powder has a general Fe20g purity of 98 to 99%, but it is required to have even higher purity and further reduction of impurities in applications. One of the methods for producing such iron oxide is the method shown in Japanese Patent Publication No. 60-8980, in which a ferrous chloride aqueous solution containing a large amount of chromium is mixed with an iron material in the solution to a pH of 1.5. This is a method for producing an aqueous ferrous chloride solution containing almost no chromium, in which the solution is brought into contact with a gas containing a large amount of oxygen until the temperature reaches 3.5%, and the resulting precipitate is separated.
〈発明が解決しようとする課題〉
しかし乍ら、この塩化鉄の処理方法では、ｐＨ制御の過
程で塩化鉄溶液中のフリー塩酸が完全に消滅しないと生
成したクロム水酸化物がフリー塩酸によって溶解する現
象が反応系内で同時に発生し、クロム水酸化物がコロイ
ド状態となる。従ってこの処理方式では、処理方式をバ
ッチ方法でせざるを得ない。つまりフリー塩酸が完全に
消滅するまでは反応系内へは新たなりロムを含有する塩
化第１鉄水溶液の供給を断つ必要があるのである。又後
工程であるクロム水酸化物と塩化第１鉄水溶液との分離
の容易化の為に中和材は鋼材を使用しなければならず、
中和材に鉄粉及び鉄粉を使用するとクロム水酸化物との
分離が困難で１処理毎に中和材を廃棄しなければならず
コスト高となる欠点がある。この様なことは、クロムを
含有する硫酸鉄溶液の処理でも同様の現象が発生する。<Problem to be solved by the invention> However, in this iron chloride treatment method, if the free hydrochloric acid in the iron chloride solution is not completely eliminated during the pH control process, the generated chromium hydroxide will be dissolved by the free hydrochloric acid. These phenomena occur simultaneously in the reaction system, and chromium hydroxide becomes a colloid. Therefore, in this processing method, the processing method must be a batch method. In other words, it is necessary to cut off the supply of new ferrous chloride aqueous solution containing ROM into the reaction system until free hydrochloric acid is completely eliminated. In addition, in order to facilitate the separation of chromium hydroxide and ferrous chloride aqueous solution in the subsequent process, steel must be used as the neutralizing material.
If iron powder or iron powder is used as a neutralizing agent, it is difficult to separate it from chromium hydroxide, and the neutralizing agent must be discarded after each treatment, resulting in high costs. A similar phenomenon occurs in the treatment of iron sulfate solutions containing chromium.
即ち、フリーの硫酸が存在する系の中でクロム水酸化物
を生成させるには、バッチ方式を採用しなければならず
、かつ中和材として鋼材の使用が必要となる。この為生
産性が低く、しかも中和材に鋼材を用いる為に中和材の
比表面積が小さく、フリー酸を含む含クロム硫酸鉄溶液
のフリー酸を消滅する為には膨大なフリー酸消減反応槽
が必要であり工業化は不可能であった。That is, in order to generate chromium hydroxide in a system where free sulfuric acid exists, a batch method must be adopted, and steel must be used as a neutralizing material. For this reason, productivity is low, and since steel is used as the neutralizing material, the specific surface area of the neutralizing material is small, and in order to eliminate the free acid in a chromium-containing iron sulfate solution containing free acid, a huge free acid elimination reaction is required. Industrialization was impossible because a tank was required.
本発明では、塩化鉄系では酸化鉄中の残留塩素による焼
結増粒という問題点があることから、硫酸鉄溶液系に着
目し、従来法の欠点であるフリー酸の完全消滅が出来な
いという点を解消し連続処理が可能な含クロム硫酸鉄溶
液からの酸化鉄の製造方法及びその装置を提供すること
を目的とする。In the present invention, since iron chloride systems have the problem of sintering and grain increase due to residual chlorine in iron oxide, we focused on iron sulfate solution systems, which have the drawback of not being able to completely eliminate free acids, which is the drawback of conventional methods. It is an object of the present invention to provide a method and apparatus for producing iron oxide from a chromium-containing iron sulfate solution that eliminates the above problems and allows continuous processing.
く課題を解決する為の手段〉
上記本発明の目的を達成する為の方法としては次の如く
である。即ち、含クロム硫酸鉄溶液に金属鉄粉を添加し
て、該含クロム硫酸鉄溶液中のフリー硫酸を完全に中和
してｐＨを２〜４にする第１工程と、第１工程で処理さ
れた溶液に更に金属鉄粉を添加してｐＨを４〜６とした
脱クロム溶液に前記第１工程の溶液を適下すると共に鉄
粉を添加し常時ｐＨを４〜６に調整してＣｒ（０）１）
３を生成させる第２工程と、第２工程で中和処理された
溶液からＣｒ（ＯＨｈを沈降分離させる第３工程と、第
３工程で沈降分離出来ない未成長のＣｒ（ＯＨ）３を濾
過分離する第４工程と、第４工程で得られた硫酸鉄溶液
から酸化鉄を得る方法である。又この第１工程と第２工
程とに用いる装置としては、一側が上広がり状に拡径し
た反応槽本体の内部で上記拡径側の手前に底部に間隙を
有する仕切板を設け、該仕切板よりも内側を反応槽、同
外側を沈降槽となし、しかも上記仕切板の中央付近には
所要数の貫通孔が設けられ、かつ反応槽内底部には攪伴
翼が、又沈降槽上部にはオーバーフロー液排出口がそれ
ぞれに設けられた中和反応装置である。Means for Solving the Problems> A method for achieving the above object of the present invention is as follows. That is, a first step in which metallic iron powder is added to a chromium-containing iron sulfate solution to completely neutralize free sulfuric acid in the chromium-containing iron sulfate solution to a pH of 2 to 4; The solution from the first step was added to the dechromized solution to adjust the pH to 4 to 6 by further adding metal iron powder to the solution, and iron powder was added to constantly adjust the pH to 4 to 6 to remove Cr. (0)1)
a second step in which Cr(OH)3 is produced, a third step in which Cr(OHh) is separated by precipitation from the solution neutralized in the second step, and ungrown Cr(OH)3 that cannot be separated by precipitation is filtered in the third step. This is a method for obtaining iron oxide from the iron sulfate solution obtained in the fourth step of separation and the fourth step.The equipment used for the first and second steps is one with an enlarged diameter on one side. Inside the reaction tank main body, a partition plate having a gap at the bottom is provided in front of the expanded diameter side, and the inside of the partition plate is the reaction tank, and the outside of the partition plate is the settling tank, and near the center of the partition plate. This is a neutralization reactor equipped with a required number of through holes, a stirring blade at the bottom of the reaction tank, and an overflow discharge port at the top of the settling tank.
く作用〉
フリー硫酸を含む含クロム硫酸鉄溶液から直接クロムの
中和析出分離しようとすると、生成するＣｒ（ＯＨ）、
がフリー硫酸に再溶解されコロイド状となって沈降分離
が出来ないが、本発明方法では、まず第１工程で、第１
図に示す様な反応槽本体１が仕切板２によって反応槽３
と沈降槽４に仕切られ、仕切板２の中央には貫通孔５が
有り、又仕切板２の下部には間隙６が設けられており、
更に反応槽３の底部には攪伴翼７が、沈降槽４の上部に
はオーバーフロー液排出口８がそれぞれに設けられた中
和反応装置を用い、含クロム硫酸鉄溶液９に金属鉄粉１
０を投入し、金属鉄粉ｌＯを貫通孔５と下部の間隙６を
通じ、自己循環させ乍らフリー硫酸と十分に反応させる
ので中和反応の促進と中和材のロスが皆無となる。なお
この第１工程でｐＨを２〜４とするのは、ｐＨが２未満
だとフリー硫酸が残り、一方ｐＨが４を超えるとコロイ
ドが生成するからである。この様にしてフリー硫酸が無
くなった含クロム硫酸鉄溶液は、次に第２工程でやはり
第１図に示す様な中和反応装置を用いて、更に金属鉄粉
ｌＯを添加してｐｌ−１を４〜６となしＣｒ（ＯＨ）１
を生成、成長させる。この時ｐＨを４〜６とするのは、
この範囲の値がＣｒ（０）１）ｓの生成、成長に適して
いるからである。クロムの析出は、溶液のｐＨによって
コロイド状急速沈降性の析出物といった形体をとる。こ
の為に溶液中の鉄粉による中和速度とその第１工程の溶
液の適下速度によってクロムの析出が不安定になる。こ
の為に事前に脱Ｃｒ後溶液（ｐＨ２４〜６）を予め入れ
ておくと安定した沈降性のいいクロム析出物が生成され
る。更に第２工程で後述する第３工程の沈澱物を一部抜
き取り第２工程に添加することによって、新たな析出核
を抑制して、析出物の粒子成長を促進させることから析
出物の一部添加が好ましい。Effect> When attempting to directly neutralize and separate chromium from a chromium-containing iron sulfate solution containing free sulfuric acid, the generated Cr(OH),
However, in the method of the present invention, in the first step, the
A reaction tank body 1 as shown in the figure is connected to a reaction tank 3 by a partition plate 2.
and a settling tank 4, a through hole 5 is provided in the center of the partition plate 2, and a gap 6 is provided at the bottom of the partition plate 2.
Furthermore, using a neutralization reactor equipped with a stirring blade 7 at the bottom of the reaction tank 3 and an overflow liquid outlet 8 at the top of the settling tank 4, metallic iron powder 1 is added to the chromium-containing iron sulfate solution 9.
The metal iron powder 1O is circulated through the through hole 5 and the lower gap 6, and is sufficiently reacted with the free sulfuric acid, so that the neutralization reaction is promoted and there is no loss of neutralizing material. The reason why the pH is adjusted to 2 to 4 in this first step is because if the pH is less than 2, free sulfuric acid remains, whereas if the pH exceeds 4, colloids are formed. The chromium-containing iron sulfate solution free of free sulfuric acid is then processed in the second step using a neutralization reactor as shown in Figure 1 and further added with metallic iron powder lO to pl-1. 4 to 6 and Cr(OH)1
Generate and grow. At this time, the pH is set to 4 to 6 because
This is because a value within this range is suitable for the production and growth of Cr(0)1)s. Chromium precipitation takes the form of a colloidal, rapidly settling precipitate depending on the pH of the solution. For this reason, the precipitation of chromium becomes unstable depending on the neutralization rate by the iron powder in the solution and the dropping rate of the solution in the first step. For this reason, if a post-Cr removal solution (pH 24 to 6) is added in advance, a stable chromium precipitate with good sedimentation properties will be generated. Furthermore, by extracting a portion of the precipitate from the third step (described later) in the second step and adding it to the second step, new precipitation nuclei are suppressed and particle growth of the precipitate is promoted. Addition is preferred.
第３工程では、第２工程より流出した溶液を沈澱槽に単
独毎かあるいは連続的に供給し、Ｃｒ（ＯＨ〉３を沈降
分離させ、この沈降物はスラッジとして排出され、一部
微細状Ｃｒ（ＯＨ）３を含む上澄液は、第４工程へ運ば
れて微細状Ｃｒ（Ｏ）Ｉ）３が濾過排出され、高純度の
硫酸鉄溶液が得られるこの［酸鉄溶液は例えば焙焼ある
いは湿式酸化法などによって高純度の酸化鉄粉を製造す
ることができる。In the third step, the solution flowing out from the second step is supplied individually or continuously to a sedimentation tank, and Cr(OH>3 is sedimented and separated. This sediment is discharged as sludge, and some fine Cr The supernatant liquid containing (OH)3 is transported to the fourth step, where fine Cr(O)I)3 is filtered out and a high-purity iron sulfate solution is obtained. Alternatively, high purity iron oxide powder can be produced by a wet oxidation method or the like.
なお、第１工程から第４工程はそれぞれをバッチ処理す
るかあるいは設備を連設して連続的に行うが処理作業、
反応効率の面から連続処理が好ましい。Note that the first to fourth steps are each performed in batches or continuously using equipment, but the processing work,
Continuous treatment is preferred from the viewpoint of reaction efficiency.
〈実施例〉
以下本発明の実施例及び比較例を示し、本発明を詳述す
る。<Examples> The present invention will be explained in detail below by showing examples and comparative examples of the present invention.
実施例１
この実施例１は、含クロム硫酸鉄溶液９として鉄鋼の硫
酸酸洗廃液を用い、それを第２図に示す様なフローシー
トに従って処理した。即ち、第１工程としては、第１図
に示した如き形態で内容積１．５ｇの中和反応装置を用
いこれに５倍に希釈した硫酸酸洗溶液を１．５〜２．＆
／ｈｒで供給しつ）、金属鉄粉１０を６０ｇ／ｈｒで投
入し、攪伴翼７で攬伴した。次いで第１工程のオーバー
フロー液をやはり第１図に示した如き形態で内容積３．
３ｇの中和反応装置に受け、第２工程の処理として金属
鉄粉を１０ｇ／ｈｒ投入した。なおこの第２工程では中
和反応装置に加温器１１を配置し５０〜６０℃に加温し
た。Example 1 In this Example 1, waste liquid from sulfuric acid pickling of steel was used as the chromium-containing iron sulfate solution 9, and it was treated according to the flow sheet shown in FIG. That is, in the first step, a neutralization reactor having an internal volume of 1.5 g as shown in FIG. 1 is used, and 1.5 to 2. &
Metallic iron powder 10 was introduced at a rate of 60 g/hr) and was stirred with a stirring blade 7. Next, the overflow liquid from the first step is brought to an internal volume of 3.5 mm in the form as shown in FIG.
3 g of the powder was placed in a neutralization reactor, and 10 g/hr of metallic iron powder was added as a second step treatment. In this second step, a warmer 11 was placed in the neutralization reaction apparatus and the temperature was heated to 50 to 60°C.
次いで第２工程からのオーバーフロー液を、容積３．４
ｊＩのシックナー１２に受け、ここで第３工程として
のＣｒ（ＯＨｈの沈降分離をせしめ沈降物はスラッジ１
３として排出し、上澄液を回収し、該上澄液を濾過装置
１４にかけて精製硫酸鉄溶液１５を得た。The overflow liquid from the second step was then pumped to a volume of 3.4
Cr(OHh) is subjected to sedimentation separation as the third step, and the sediment is collected as sludge 1.
3, the supernatant liquid was collected, and the supernatant liquid was passed through a filtration device 14 to obtain a purified iron sulfate solution 15.
大縫型ｌ
この実施例２は、やはり含クロム硫酸鉄溶液９として、
５倍に希釈した鉄鋼の硫酸酸洗溶液を用い、第１工程と
第２工程の反応装置に通常のタンクを用いる以外は上記
実施例１と同様の処理をして精製硫酸鉄溶液を得た。Large sewing pattern l In this Example 2, as the chromium-containing iron sulfate solution 9,
A purified iron sulfate solution was obtained by performing the same treatment as in Example 1 above, except that a 5-fold diluted sulfuric acid pickling solution for steel was used, and a normal tank was used as the reactor for the first and second steps. .
塩駒艷１
この比較例１は、上記実施例１．２と同じ硫酸酸洗希釈
液１．５１を、容［２，、＆のタンクに入れ、それに鉄
粉１２００ｇを投入し、２時間攬伴の後４時間静置した
ものであり、ｐＨは３．５となった。Shiokomaso 1 In Comparative Example 1, 1.51 of the same diluted sulfuric acid pickling solution as in Example 1.2 above was put into a tank with a volume of [2,, &], 1200 g of iron powder was added thereto, and the water was soaked for 2 hours. The solution was allowed to stand for 4 hours after being washed, and the pH was 3.5.
上記実施例１，２及び比較例１に於ける処理前及び処理
後のクロムイオン濃度並びに濾過性等の比較表を下記第
１表に示す。なおこの第１表の処理後のクロムイオン濃
度は、実施例１及び２については、第４工程迄済んだ後
の溶液について、又比較例１については上澄液を濾過し
た溶液についてのものである。A comparison table of chromium ion concentration, filterability, etc. before and after treatment in Examples 1 and 2 and Comparative Example 1 is shown in Table 1 below. Note that the chromium ion concentrations after treatment in Table 1 are for the solutions after completing the fourth step for Examples 1 and 2, and for the solutions obtained by filtering the supernatant liquid for Comparative Example 1. be.
〈発明の効果〉
以上述べて来た如く、本発明によれば、まず第１工程で
フリー硫酸を中和してしまい、その後の工程に進むので
コロイドの発生がなく濾過性も良いので硫酸鉄中からク
ロムを殆ど完全に除去出来、従って不純物の殆ど無い酸
化鉄を造ることが出来るものである。<Effects of the Invention> As described above, according to the present invention, free sulfuric acid is first neutralized in the first step, and then proceeding to the subsequent steps, so colloids are not generated and filterability is good, so iron sulfate is It is possible to almost completely remove chromium from the inside, making it possible to produce iron oxide with almost no impurities.
又本発明の中和反応装置によれば反応槽と沈降槽が別々
に設けられ、それらに両槽は仕切板中央の貫通孔と下部
の間隙でのみ連通されているので中和材が自己循環し反
応を促進させるものである。Further, according to the neutralization reaction apparatus of the present invention, the reaction tank and the settling tank are provided separately, and the two tanks are communicated only through the through hole in the center of the partition plate and the gap at the bottom, so that the neutralizing material can self-circulate. and accelerates the reaction.
第■図は本発明に係る中和反応装置の断面説明図、第２
図は本発明実施例１の概要説明図。
図 中 １：反応槽本体
３：反応槽
４：沈降槽
９：含クロム硫酸鉄溶液
ＩＯ＝金属鉄粉Figure 2 is a cross-sectional explanatory diagram of the neutralization reactor according to the present invention,
The figure is a schematic explanatory diagram of Embodiment 1 of the present invention. In the figure 1: Reaction tank body 3: Reaction tank 4: Sedimentation tank 9: Chromium-containing iron sulfate solution IO = metallic iron powder
Claims (1)
ロム硫酸鉄溶液中のフリー硫酸を中和してｐＨを２〜４
にする第１工程と、第１工程で処理された溶液に更に金
属粒を添加してｐＨを４〜６となした脱クロム溶液に前
記第１工程の溶液を適下すると共に鉄粉を添加しｐＨを
４〜６に調整してＣｒ（ＯＨ）＿３を生成させる第２工
程と、第２工程で中和処理された溶液からＣｒ（ＯＨ）
＿３を沈降分離させる第３工程と、第３工程で流出した
溶液を濾過する第４工程と、第４工程で流出した溶液か
ら酸化鉄を得ることを特徴とする含クロム硫酸鉄溶液を
用いた高純度酸化鉄粉の製造方法。 ２、一側が上広がり状に拡径した反応槽本体の内部で上
記拡径側の手前に、底部に間隙を有する仕切板を設け、
該仕切板よりも内側を反応槽、同外側を沈降槽となし、
しかも上記仕切板の中央付近には所要数の貫通孔が設け
られ、かつ反応槽内底部には攪伴翼が、又沈降槽上部に
はオーバーフロー液排出口がそれぞれ設けられたことを
特徴とする中和反応装置。[Claims] 1. Adding metal iron powder to a chromium-containing iron sulfate solution to neutralize free sulfuric acid in the chromium-containing iron sulfate solution and adjusting the pH to 2 to 4.
The first step is to add metal particles to the solution treated in the first step to adjust the pH to 4 to 6, then drop the solution in the first step into the dechromized solution and add iron powder. The second step is to adjust the pH to 4 to 6 to generate Cr(OH)_3, and to generate Cr(OH) from the solution neutralized in the second step.
A chromium-containing iron sulfate solution is used, which is characterized by a third step in which _3 is sedimented and separated, a fourth step in which the solution flowing out in the third step is filtered, and iron oxide is obtained from the solution flowing out in the fourth step. A method for producing high-purity iron oxide powder. 2. A partition plate having a gap at the bottom is provided in front of the expanded diameter side inside the reaction tank main body whose diameter is expanded upward on one side,
The inner side of the partition plate is a reaction tank, and the outer side is a settling tank,
Moreover, a required number of through holes are provided near the center of the partition plate, stirring blades are provided at the bottom of the reaction tank, and an overflow liquid discharge port is provided at the top of the settling tank. Neutralization reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28643089A JPH03146422A (en) | 1989-11-01 | 1989-11-01 | Method and apparatus for producing high purity iron oxide powder with chromium-containing iron sulfate solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28643089A JPH03146422A (en) | 1989-11-01 | 1989-11-01 | Method and apparatus for producing high purity iron oxide powder with chromium-containing iron sulfate solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03146422A true JPH03146422A (en) | 1991-06-21 |
Family
ID=17704286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28643089A Pending JPH03146422A (en) | 1989-11-01 | 1989-11-01 | Method and apparatus for producing high purity iron oxide powder with chromium-containing iron sulfate solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03146422A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2012374201B2 (en) * | 2012-03-23 | 2015-09-03 | Amtpacific Co.,Ltd. | Liquid dispensing device |
-
1989
- 1989-11-01 JP JP28643089A patent/JPH03146422A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2012374201B2 (en) * | 2012-03-23 | 2015-09-03 | Amtpacific Co.,Ltd. | Liquid dispensing device |
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