JP4308215B2 - Method for wet classification of powder and granular material of metal and / or metal compound - Google Patents
Method for wet classification of powder and granular material of metal and / or metal compound Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 33
- 239000000843 powder Substances 0.000 title claims description 12
- 238000010333 wet classification Methods 0.000 title claims description 10
- 229910052751 metal Inorganic materials 0.000 title claims description 9
- 239000002184 metal Substances 0.000 title claims description 9
- 150000002736 metal compounds Chemical class 0.000 title claims description 9
- 239000008187 granular material Substances 0.000 title claims description 6
- 239000007788 liquid Substances 0.000 claims description 31
- 238000004140 cleaning Methods 0.000 claims description 10
- 230000005484 gravity Effects 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 description 15
- 239000010949 copper Substances 0.000 description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- 229910052802 copper Inorganic materials 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 7
- 238000002386 leaching Methods 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 229910000380 bismuth sulfate Inorganic materials 0.000 description 4
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 238000009854 hydrometallurgy Methods 0.000 description 4
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 239000011362 coarse particle Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004071 soot Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
本発明は、重量による沈降を利用して液体中で金属及び又は金属化合物の粉状物と粒状物を分級する方法に関する。特に本発明は上昇液流により連続的に粉粒体を分級する方法に関するものである。 The present invention relates to a method for classifying powders and particulates of metals and / or metal compounds in a liquid using sedimentation by weight. In particular, the present invention relates to a method for continuously classifying powder particles by a rising liquid flow.
湿式分級のプロセスには、上昇流を利用するもの、水平流を利用するもの、単なる静置によるものなどがあり、特に分離の精度において優れているのは上昇流を利用するものである。 Wet classification processes include those using an upflow, those using a horizontal flow, and those by mere standing, and those that are superior in separation accuracy are those using an upflow.
上昇流を利用する湿式分級プロセスには連続式とバッチ式があり、金属及び金属化合物のような沈降速度が比較的大である粗い粒子に適用する場合、小さな装置で大量の粒子を処理できるという点で連続式のほうが優れており、その一例として特公昭47-33571号（出願人：信越化学工業株式会社）（特許文献1）の公告がある。 There are two types of wet classification processes that use upflow: continuous and batch processes, and when applied to coarse particles with relatively high settling rates, such as metals and metal compounds, a large amount of particles can be processed with a small device. The continuous type is superior in this respect, and an example is the publication of Japanese Patent Publication No. 47-33571 (Applicant: Shin-Etsu Chemical Co., Ltd.) (Patent Document 1).
しかし従来の連続式プロセスでは一般に装置下部の流出口から流出する粗い粒子のスラリーの中に、細粒子の一部が混入しやすいといった問題がある。
この原因の一つとしては、給液口から装置本体内に流入する高濃度のスラリーが作る部分的な下降流や、細粒子が凝集したまま速やかに沈降することなどによるショートパスが考えられる。
However, the conventional continuous process generally has a problem that some of the fine particles are likely to be mixed into the coarse particle slurry flowing out from the outlet at the bottom of the apparatus.
One of the causes is considered to be a partial downward flow created by a high-concentration slurry flowing into the apparatus main body from the liquid supply port, or a short path due to rapid settling while fine particles are aggregated.
また、特許文献１に示されている方法では底部へ給液スラリー以外の液を吹き込む必要があり、一般には水が使用されると考えられるが、湿式製錬工程で特許文献1の方法を実施する場合に水を使用すると、工程内での処理液量が増加するため、分級処理後工程での処理能力を増強する必要が生じる。 In addition, in the method shown in Patent Document 1, it is necessary to blow a liquid other than the feed slurry to the bottom, and it is generally considered that water is used, but the method of Patent Document 1 is carried out in a hydrometallurgical process. When water is used in this case, the amount of the processing liquid in the process increases, so that it is necessary to enhance the processing capacity in the post-classification process.
本発明は、金属及び又は金属化合物の粉状物と粒状物を簡単な構造で、連続的に分級することのでき、上記したような問題を解決することができる湿式分級方法を提供することを目的としている。 It is an object of the present invention to provide a wet classification method capable of continuously classifying powders and particulates of metals and / or metal compounds with a simple structure and solving the above-mentioned problems. It is aimed.
本発明者らは、上記の問題を解決すべく、以下の発明を成した。
即ち本発明は、
（１）重力による沈降を利用した湿式の分級装置であって、上部は直立する筒状であり、下部は逆円錐状の装置であり、該装置下部に流入口があり、前記筒状部の上端付近および装置底部に排出口を設けた装置において、
下部逆円錐部から装置底部排出口方向に清浄液を前記排出口の排出流量と同量から１．２倍をになるように流入する金属及び金属化合物の粉状物と粒状物の湿式分級方法。
In order to solve the above problems, the present inventors made the following invention.
That is, the present invention
(1) A wet classifier using gravity sedimentation, the upper part is an upright cylinder, the lower part is an inverted conical unit, the lower part of the apparatus has an inlet, In a device with a discharge port near the top and bottom of the device,
Method for wet classification of metal and metal compound powders and particulates in which the cleaning liquid flows from the lower inverted conical part toward the outlet of the bottom of the apparatus in an amount equal to 1.2 times the discharge flow rate of the discharge port .
（２）上記（１）の分級方法において給液口を上方に向けることにより、軽く小な粉状物のショートパスによる底部からの排出を抑制する湿式分級方法。 (2) A wet classification method that suppresses discharge of a light and small powdery substance from the bottom by a short pass by directing the liquid supply port upward in the classification method of (1).
（３）上記（１）或いは上記（２）の何れかの清浄液として
製錬工程内の工程液を利用することにより製錬工程内の処理液量を増加させずに分級できる湿式分級方法。
(3) A wet classification method that enables classification without increasing the amount of processing liquid in the smelting process by using the process liquid in the smelting process as the cleaning liquid of either (1) or (2).
本発明によれば、
（１）本発明によってスラリー状にした金属及び金属化合物の粒状物と粉状物を連続的に高い精度のもとに分級できる。
（２）本発明を湿式製錬工程で実施する場合、工程内の液量を増加させずに高い精度のもとに分級できる。
According to the present invention,
(1) Granular and powdery metal and metal compounds made into a slurry according to the present invention can be classified continuously with high accuracy.
(2) When carrying out the present invention in a hydrometallurgical process, classification can be performed with high accuracy without increasing the amount of liquid in the process.
以下本発明に関して、詳細に説明する。
本発明に関する対象物は、金属および金属化合物の粉状物と粒状物である。金属及び金属化合物の粉状物と粒状物とは例えば、銅転炉ダストの湿式処理において、銅転炉ダストを希硫酸浸出した後に発生する浸出残渣がある。
Hereinafter, the present invention will be described in detail.
The objects related to the present invention are powders and granules of metals and metal compounds. For example, in the wet processing of copper converter dust, there is a leaching residue generated after leaching the copper converter dust with dilute sulfuric acid in the wet processing of copper converter dust.
この浸出残渣には主に硫酸鉛、硫酸ビスマス、金属銅、硫化銅等が含まれる。硫酸鉛（比重6.2）、硫酸ビスマス（比重5.08）は粒径が非常に細かく、数μm程度の粉状物であり、
金属銅（比重8.96）、硫化銅（比重CuS:4.64、Cu2S：5.6）は10〜250μmと粗大な粒状物である。
This leaching residue mainly contains lead sulfate, bismuth sulfate, metallic copper, copper sulfide and the like. Lead sulfate (specific gravity 6.2) and bismuth sulfate (specific gravity 5.08) are very fine in particle size and are a powdery substance of about several μm.
Metallic copper (specific gravity 8.96) and copper sulfide (specific gravity CuS: 4.64, Cu 2 S: 5.6) are coarse particles of 10 to 250 μm.
このような金属および金属化合物の粉状物と粒状物を含んだスラリーを例えば図１に示す設備を用いて連続的に湿式分級する。図１に示す湿式分級装置は被分級粉粒体スラリーを所定の流量を給液しながら底部からも所定の液量を抜き出すが、その際に装置底部に湿式製錬工程内で発生する清浄な工程液を底部からの抜出流量と同量から１．２倍になるように流入する。
上記の流量より少ない場合は、粒子の細かいものに多く含むＢｉ，Ｐｂが、底部に沈降し好ましくなく、
上記より多い流量であると上昇流が変化し、粒子の粗いものに多く含む沈降すべき硫化銅等が沈降しなくなるためである。。
A slurry containing such a metal and metal compound powder and granule is continuously wet-classified using, for example, the equipment shown in FIG. The wet classifier shown in FIG. 1 draws a predetermined amount of liquid from the bottom while supplying a predetermined granular powder slurry at a predetermined flow rate. At this time, the clean powder generated in the hydrometallurgical process at the bottom of the apparatus. The process liquid is introduced so that the flow rate is 1.2 times the same as the flow rate from the bottom.
When the flow rate is lower than the above, Bi and Pb, which are contained in a large amount of fine particles, are settled at the bottom and are not preferable.
This is because the upward flow changes when the flow rate is higher than the above, and copper sulfide and the like to be precipitated, which are contained in a large amount of particles, do not settle. .
一般に湿式製錬工程は浸出、中和、硫化等の数工程に分かれており、それぞれの工程の反応槽で発生する残渣は濾過して分離し、濾液を次工程へ送液することが多い。 In general, the hydrometallurgical process is divided into several processes such as leaching, neutralization, and sulfidation, and the residue generated in the reaction tank of each process is often separated by filtration, and the filtrate is often sent to the next process.
本発明の底部吹き込み清浄液として被分級粉粒体が処理される工程の濾液を使用することで工程内の液量を増加させることなく連続的に分級可能となる。 By using the filtrate of the process in which the classified powder is treated as the bottom blowing cleaning liquid of the present invention, it is possible to continuously classify without increasing the liquid amount in the process.
本発明で使用する湿式分級装置は以下のような条件が望ましい。
給液口は筒状部最下端より高い位置に設置することが望ましい。これより低い下部逆円錐状部分に設置すると、沈降する粒状物が上昇流の影響を受けて沈降速度が遅くなり逆円錐状部分に堆積しやすいと考えられるからである。
The following conditions are desirable for the wet classifier used in the present invention.
It is desirable to install the liquid supply port at a position higher than the lowermost end of the cylindrical portion. This is because if it is installed in a lower inverted conical portion lower than this, it is considered that the settled particulate matter is affected by the upward flow, and the sedimentation speed becomes slow and is easily deposited on the inverted conical portion.
装置上部の直立する筒状部の内径に対する、給液口から装置上部オーバフローレベルまでの高さの比率はできるだけ大きい方が望ましい。被分級粉粒状物スラリーが装置に給液され装置上部からオーバーフローするまでに液の上昇流を水平方向に均一な流速にするためである。 The ratio of the height from the liquid supply port to the apparatus upper overflow level with respect to the inner diameter of the upright cylindrical part at the upper part of the apparatus is desirably as large as possible. This is to make the upward flow of the liquid uniform in the horizontal direction before the classified granular slurry is supplied to the apparatus and overflows from the upper part of the apparatus.
下部逆円錐状部分はできるだけ鋭角な方が良い。沈降した粒状物を逆円錐状部分に堆積させないためである。 The lower inverted conical part should be as sharp as possible. This is because the settled particulate matter is not deposited on the inverted conical portion.
給液流量は分級する粉粒体についてそれぞれ以下のストークスの式
V＝
V:固体粒子の終末沈降速度、d：粒径、μ：流体の粘度、ρs：固体粒子の密度、ρ：流体密度、g：重力加速度
を用いて終末沈降速度を計算し、適切な流体の上昇速度を決定し、分級装置断面積を掛けて求める。
The liquid supply flow rate is the following Stokes' formula for each granular material to be classified:
V =
V: terminal settling velocity of the solid particles, d: particle diameter, mu: viscosity of the fluid, [rho s: density of solid particles, [rho: fluid density, g: with gravitational acceleration to calculate the terminal settling velocity, suitable fluid Is determined by multiplying the cross-sectional area of the classifier.
底部への清浄液は鉛直下向きに吹き込み、底部からの抜出流量と同じかやや多い程度が良い。清浄液吹き込み流量が抜出流量より少ない場合、装置内部で部分的な下降流が生じ、細粒子が底部へショートパスするからである。 The cleaning liquid to the bottom is blown vertically downward, and it is good that the flow rate is the same as or slightly larger than the flow rate from the bottom. This is because when the flow rate of the cleaning liquid blown is smaller than the withdrawal flow rate, a partial downward flow is generated inside the apparatus, and the fine particles are short-passed to the bottom.
図1に示す湿式分級装置を作製した。装置寸法は以下のとおりである。
H1：1000mm
H2：1300mm
H3：500mm
H4：150mm
給液配管内径：50mm
底部抜き出し配管内径：50mm
底部清浄液吹き込み配管内径：20mm
A wet classifier shown in FIG. 1 was produced. The device dimensions are as follows.
H1: 1000mm
H2: 1300mm
H3: 500mm
H4: 150mm
Supply pipe inner diameter: 50mm
Bottom extraction piping inner diameter: 50mm
Bottom cleaning liquid blower piping inner diameter: 20mm
図１の装置を用いて銅転炉ダスト処理工程において希硫酸浸出工程で発生する鉛滓（主成分は硫酸鉛（比重6.2、粒径 数μm程度）、硫酸ビスマス（比重5.08、粒径
数μm程度）であり、鉛電気炉にて原料とする）に不純物として混入している金属銅（比重8.96 粒径 10〜250μm）および硫化銅（比重CuS:4.64、Cu2S：5.6
粒径は10〜250μm）を分級し除去するために図２に示す一連の設備を設置し運転した。
Lead soot generated in the dilute sulfuric acid leaching process in the copper converter dust treatment process using the equipment shown in Fig. 1 (main components are lead sulfate (specific gravity 6.2, particle size around several μm), bismuth sulfate (specific gravity 5.08, particle size several μm) Copper) (specific gravity 8.96 particle size 10 to 250 μm) and copper sulfide (specific gravity CuS: 4.64, Cu 2 S: 5.6)
In order to classify and remove the particle size (10 to 250 μm), a series of equipment shown in FIG. 2 was installed and operated.
希硫酸浸出工程の次の工程は銅、鉄等の濾液中のあらゆる重金属を除去する工程であるため、給液する鉛滓スラリー中の硫酸鉛、硫酸ビスマスはオーバーフローさせ濾過し鉛滓として回収し、いっぽう、金属銅及び硫化銅は底部より抜き出しながら次の工程へ送液した。 Since the next step of the dilute sulfuric acid leaching step is to remove all heavy metals in the filtrate such as copper and iron, lead sulfate and bismuth sulfate in the supplied lead lees slurry are overflowed, filtered and recovered as lead lees On the other hand, metallic copper and copper sulfide were fed to the next step while being extracted from the bottom.
以下の操業条件で運転を1日間実施した。
スラリー濃度：70〜150g/L
硫酸濃度：10〜20g/L
スラリー温度：35〜45℃
分級装置給液流量Q1、オーバーフロー流量：45〜50 L/min
分級装置底部抜出流量Q2：45〜50 L/min
分級装置底部清浄液吹き込み流量Q3：50 L/min
Operation was carried out for one day under the following operating conditions.
Slurry concentration: 70-150g / L
Sulfuric acid concentration: 10-20g / L
Slurry temperature: 35-45 ° C
Classifier supply liquid flow rate Q1, overflow flow rate: 45-50 L / min
Flow rate Q2 at the bottom of the classifier: 45 to 50 L / min
Cleaner flow rate at the bottom of the classifier Q3: 50 L / min
湿式分級装置の効果として、銅、鉛、ビスマスの分配を表５に示す。
特にオーバーフロー残渣は、銅品位が大幅に低下し、鉛が高品位で維持されているため鉛製錬において、良好に処理が成された。
また底部抜き出し残渣の鉛、ビスマスの品位を低く抑えられたので鉛滓として回収すべき鉛、ビスマスのロスもかなり低く抑えることができた。
In particular, the overflow residue was processed well in lead smelting because the copper quality was significantly reduced and lead was maintained at a high quality.
In addition, since the quality of lead and bismuth from the bottom extraction residue was kept low, the loss of lead and bismuth that should be recovered as lead soot could be kept quite low.
比較例としてオーバーフロー流量を変えずに分級装置下部への清浄液吹込みを実施しなかった場合の結果を示す。
以下の操業条件で運転を1日間実施した。
スラリー濃度：70〜150g/L
硫酸濃度：10〜20g/L
スラリー温度：35〜45℃
分級装置給液流量Q1：90〜100 L/min
オーバーフロー流量：45〜50 L/min
分級装置底部抜出流量Q2：45〜50 L/min
分級装置底部清浄液吹き込み流量Q3：０ L/min
Operation was carried out for one day under the following operating conditions.
Slurry concentration: 70-150g / L
Sulfuric acid concentration: 10-20g / L
Slurry temperature: 35-45 ° C
Classifier supply liquid flow rate Q1: 90-100 L / min
Overflow rate: 45-50 L / min
Flow rate Q2 at the bottom of the classifier: 45 to 50 L / min
Classifier bottom cleaning liquid injection flow rate Q3: 0 L / min
前記表2のように銅についてはオーバーフロー側と底部抜き出し側の移行率がそれほど変わらないが、鉛、ビスマスについては底部抜き出し側への移行率が増加し、分級性能が悪化した。 As shown in Table 2, the transfer rate on the overflow side and the bottom extraction side was not so different for copper, but the transfer rate to the bottom extraction side was increased for lead and bismuth, and the classification performance deteriorated.
１ 本体筒状部
２ 本体逆円錐部
３ 非分級粉粒体スラリー給液配管
４ オーバーフロー排出口
５ 底部抜き出し口
６ 底部清浄液吹き込み配管
DESCRIPTION OF SYMBOLS 1 Main body cylindrical part 2 Main body reverse cone part 3 Non-classified granular material slurry supply piping 4 Overflow discharge port 5 Bottom extraction port 6 Bottom clean liquid blowing piping
７ 鉛滓スラリー貯液槽
８ 分級装置給液ポンプ
９ 湿式分級装置
１０ 流量測定用計量ポット
１１ 次工程反応槽
１２ 鉛滓スラリー濾液槽
１３ 分級装置底部吹き込みポンプ
１４ 流量計
１５ 流量調整自動弁
7 Lead tank slurry storage tank 8 Classifier feed pump 9 Wet classifier 10 Flow rate measuring pot 11 Next process reactor 12 Lead tank slurry filtrate tank 13 Classifier bottom blowing pump 14 Flow meter 15 Flow control automatic valve
Claims (3)
下部逆円錐部から装置底部排出口方向に清浄液を前記排出口の排出流量と同量から１．２倍になるように流入することを特徴とする金属及び金属化合物の粉状物と粒状物の湿式分級方法。 It is a wet classifier using gravity sedimentation, the upper part is an upright cylinder, the lower part is an inverted conical apparatus, there is an inlet at the lower part of the apparatus, near the upper end of the cylindrical part and In a device with a discharge port at the bottom of the device,
Powder and granular material of metal and metal compound, wherein the cleaning liquid flows in from the lower inverted conical portion toward the apparatus bottom discharge port so as to be 1.2 times as large as the discharge flow rate of the discharge port. Wet classification method.
製錬工程内の工程液を利用することにより製錬工程内の処理液量を増加させずに分級できることを特徴とする湿式分級方法。 Wet classification method characterized by be classified without increasing the amount of treatment liquid in the smelting process by utilizing the process liquid in the smelting process as one of the cleaning solution of claim 1 or claim 2.
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| CN102319620B (en) * | 2011-06-02 | 2013-08-07 | 江苏大阳光辅股份有限公司 | Fully-automatic micro powder screening method with feedback function |
| CN103394407B (en) * | 2013-08-08 | 2015-07-15 | 连云港海蓝研磨材料有限公司 | Precise and efficient overflow classifying technology |
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