JP6738560B2 - Calibration method of level meter of closed MS reaction tank, detection method of liquid level fluctuation, and monitoring system using them - Google Patents
Calibration method of level meter of closed MS reaction tank, detection method of liquid level fluctuation, and monitoring system using them Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims description 171
- 238000006243 chemical reaction Methods 0.000 title claims description 88
- 238000000034 method Methods 0.000 title claims description 48
- 238000001514 detection method Methods 0.000 title claims description 15
- 238000012544 monitoring process Methods 0.000 title claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 13
- 238000005486 sulfidation Methods 0.000 claims description 13
- IPRPPFIAVHPVJH-UHFFFAOYSA-N (4-hydroxyphenyl)acetaldehyde Chemical compound OC1=CC=C(CC=O)C=C1 IPRPPFIAVHPVJH-UHFFFAOYSA-N 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 10
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005987 sulfurization reaction Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000005856 abnormality Effects 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 12
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 12
- 239000007789 gas Substances 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000717 retained effect Effects 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Description
ＨＰＡＬの硫化工程において撹拌機の電流値を基に、密閉反応槽の液位を監視して、当該反応槽に取り付けられているレベル計を校正する方法に関する。 The present invention relates to a method of calibrating a level meter attached to a reaction tank by monitoring the liquid level in a closed reaction tank based on the current value of a stirrer in the HPAL sulfurization step.
図１に、その製錬フローの概略を示すＨＰＡＬ技術を用いたニッケル酸化鉱の製錬では、製造工程中の硫化工程（１０６）で硫化水素ガス（図示せず）とニッケル水溶液の反応でＭＳ（ミックスサルファイド：混合硫化物：Ｎｉ・Ｃｏ混合硫化物）を製造する。
ＭＳ反応槽は、マイクロウェーブ式レベル計と攪拌機を備えた容器で、硫化水素ガスを密閉できる構造であり、一度運転を始めると定期休転迄の連続運転となる。反応槽は槽底部に底抜き管を備え、底抜き管は次工程の容器の上部に接続されているが、反応槽内の圧力を次工程の容器内の圧力よりも高く保つことによって、反応槽内のスラリーを次工程の容器へ常時送り出すことができる。このＭＳ反応槽では、反応時間を適度に確保するために液位を安定させる必要があり、そのために、圧力の調節によってスラリーの送り出し量を増減させる。圧力の調節は、硫化水素ガスを吹き込むことによって高めることができる一方、圧力を下げるには硫化水素が反応によって消費されるのを待つしかない。このため、圧力の調節は、小幅かつ早期に調節することによって液位を安定させることが試みられている。すると、圧力の調節に先立って、液位を早期に検出する必要が生じ、レベル計（以下、液面レベル計とも称す）は、槽内部での反応の管理や撹拌機保護の観点から信頼性が求められる。
ところが、ＭＳ反応槽には次のような２つの困難がある。
In the smelting of nickel oxide ore using the HPAL technology, which shows the outline of the smelting flow in FIG. 1, in the sulfiding step (106) in the manufacturing process, hydrogen sulfide gas (not shown) reacts with the nickel aqueous solution to produce MS. (Mixed sulfide: mixed sulfide: Ni/Co mixed sulfide) is produced.
The MS reaction tank is a container equipped with a microwave type level meter and a stirrer, and has a structure capable of sealing hydrogen sulfide gas, and once the operation is started, it will be continuously operated until a periodic shutdown. The reaction tank is equipped with a bottom vent pipe at the bottom of the tank, and the bottom vent pipe is connected to the upper part of the container for the next step, but by maintaining the pressure in the reaction tank higher than the pressure in the container for the next step, the reaction The slurry in the tank can be constantly sent to the container for the next step. In this MS reaction tank, it is necessary to stabilize the liquid level in order to secure an appropriate reaction time, and therefore the amount of slurry to be fed is increased or decreased by adjusting the pressure. Control of the pressure can be increased by blowing in hydrogen sulfide gas, while lowering the pressure requires waiting for hydrogen sulfide to be consumed by the reaction. For this reason, it has been attempted to stabilize the liquid level by adjusting the pressure to a small extent and at an early stage. Then, before adjusting the pressure, it is necessary to detect the liquid level early, and the level meter (hereinafter also referred to as the liquid level meter) is reliable from the viewpoint of reaction management inside the tank and protection of the agitator. Is required.
However, the MS reaction tank has the following two difficulties.
１．レベル計指示不良時における点検、補修が困難な点
この困難は、ＭＳ反応槽が密閉型の反応容器であり、その内部には硫化水素が常に吹き込まれ充満しているために生じる。このＭＳ反応槽を構成する反応容器に設置されたレベル計に点検・補修が必要な場合、反応容器の開放作業を伴う。この際、硫化水素が漏れないように、硫化工程を停止し、容器内部のガスを窒素で置換する必要があり、作業の手間がかかり、生産量が低下し、窒素などの資材を要し、硫化水素が無駄になる。
1. Difficulties in inspection and repair when the level meter is not correctly indicated This difficulty occurs because the MS reaction tank is a closed reaction vessel, and hydrogen sulfide is constantly blown into and filled with it. When the level meter installed in the reaction vessel constituting the MS reaction tank needs to be inspected and repaired, the reaction vessel is opened. At this time, in order to prevent hydrogen sulfide from leaking, it is necessary to stop the sulfiding process and replace the gas inside the container with nitrogen, which takes time and labor, reduces the production amount, requires materials such as nitrogen, Hydrogen sulfide is wasted.
２．運転中の液位の監視ができなくなる点
運転中は、ＭＳ反応槽には硫化水素が吹き込まれており、液面が泡立ちやすくなっている。ＭＳ反応槽にはマイクロウェーブ式のレベル計が１台取り付けられているが、泡立った液面を測定してしまう恐れがある。また、飛び散った液に含まれていたＭＳがレベル計に付着しやすく、付着位置によってはレベル計が故障し、反応槽内のレベル下限が検知できなくなる。
2. Point where liquid level cannot be monitored during operation During operation, hydrogen sulfide is blown into the MS reaction tank, and the liquid surface is prone to foaming. One microwave type level meter is attached to the MS reaction tank, but there is a risk of measuring a bubbling liquid level. Further, the MS contained in the scattered liquid easily adheres to the level meter, and the level meter may fail depending on the adhesion position, and the lower limit of the level in the reaction tank cannot be detected.
本発明は、このような状況を解決するために成されたものであり、反応槽を開放することなくレベル計の点検、校正を実施して、密閉反応槽のレベル計の信頼性を向上させ、さらにマイクロウェーブ式のレベル計の故障時に、これに替わって液位を監視する方法である。 The present invention has been made to solve such a situation, and performs inspection and calibration of the level meter without opening the reaction tank to improve the reliability of the level meter in the closed reaction tank. Moreover, when the microwave type level meter fails, it is a method of monitoring the liquid level instead of this.
本発明は、ＭＳ反応槽の液位変動による撹拌機の電流値の変化に着目し上記課題を解決できることを見出し、本発明を完成したものである。 The present invention has completed the present invention by finding that the above problems can be solved by paying attention to the change in the current value of the stirrer due to the fluctuation of the liquid level in the MS reaction tank.
すなわち、本発明の第１の発明は、ＨＰＡＬ技術を用いてニッケル酸化鉱から得られたＮｉを含む浸出液を硫化処理する硫化工程で、前記硫化処理に使用される密閉型ＭＳ反応槽に貯留された処理液の液面レベルを計測するレベル計の運転中における校正方法であって、そのＭＳ反応槽が反応槽の底部方向から数えてｎカ所以上の羽根車Ｐｉ（ｉ＝１〜ｎ；ｎ≧２）を備え、定回転数で槽内に貯留された処理液を攪拌する電動攪拌機と、その処理液の槽内の液面レベルを計測するレベル計を有し、準備過程として、予め電動攪拌機の駆動電流値とレベル計の液面レベル値の時系列変化を計測して求めた、駆動電流値と液面レベル値との相関データの準備と、ＭＳ反応槽の運転において、電動攪拌機の羽根車Ｐｎ−１又はＰｎの上部が前記処理液の液面下から現出する時点の液面レベルを校正基準レベルＳ０ ｎ−１又はＳ０ ｎとする設定を行い、レベル計校正の実施は、第一に相関データから校正基準レベルＳ０ ｎ−１又はＳ０ ｎに対応する駆動電流値Ｉ０ ｎ−１又はＩ０ ｎを求め、第二にＭＳ反応槽の運転において、電動攪拌機の駆動電流値がＩ０ ｎ−１のときのレベル計が指示する計測液面レベルＬｎ−１と前記校正基準レベルＳ０ ｎ−１、又は駆動電流値がＩ０ ｎのときのレベル計が指示する計測液面レベルＬｎと前記校正基準レベルＳ０ ｎを用いて前記レベル計を校正することを特徴とするレベル計の校正方法である。 That is, the first invention of the present invention is a sulfidation step of sulfidizing a Ni-containing leachate obtained from nickel oxide ore by using HPAL technology, and is stored in a closed MS reaction tank used for the sulfidation. A method for calibrating a level meter for measuring the liquid level of the treatment liquid during operation, wherein the MS reaction tank has n or more impellers P i (i=1 to n ; counting from the bottom direction of the reaction tank) . n≧2 ) and has an electric stirrer for stirring the processing liquid stored in the tank at a constant rotation speed and a level meter for measuring the liquid level in the tank of the processing liquid. In preparation of the correlation data between the driving current value and the liquid level value obtained by measuring the time series change of the driving current value of the electric stirrer and the liquid level value of the level meter, and the operation of the MS reaction tank, the electric stirrer Of the impeller P n-1 or P n of the processing liquid is set to be the calibration reference level S 0 n-1 or S 0 n , and the level meter is set. The calibration is performed by first obtaining the drive current value I 0 n-1 or I 0 n corresponding to the calibration reference level S 0 n-1 or S 0 n from the correlation data, and secondly in the operation of the MS reaction tank. When the drive current value of the electric stirrer is I 0 n-1 , the measured liquid level L n-1 indicated by the level meter and the calibration reference level S 0 n-1 , or when the drive current value is I 0 n The calibration method for a level meter is characterized in that the level meter is calibrated using the measured liquid surface level L n indicated by the level meter and the calibration reference level S 0 n .
本発明の第２の発明は、第１の発明における相関データが、ＭＳ反応槽内の液レベルと電動攪拌機の駆動電流値から構成される近似式であることを特徴とするレベル計の校正方法である。 A second invention of the present invention is a calibration method for a level meter, wherein the correlation data in the first invention is an approximate expression composed of a liquid level in an MS reaction tank and a driving current value of an electric stirrer. Is.
本発明の第３の発明は、第１及び第２の発明における電動攪拌機が、ｎ＝３のＰ１、Ｐ２及びＰ３の３段の羽根車を備えることを特徴とするレベル計の校正方法である。 A third invention of the present invention is a calibration of a level meter, characterized in that the electric stirrer according to the first and second inventions is equipped with three-stage impellers of P 1 , P 2 and P 3 of n=3. Is the way.
本発明の第４の発明は、ＨＰＡＬ技術を用いてニッケル酸化鉱から得られたＮｉを含む浸出液を硫化処理する硫化工程で、前記硫化処理に使用される密閉型ＭＳ反応槽に貯留された処理液の液面レベル変動の検出方法であって、ＭＳ反応槽が反応槽の底部方向から数えて２カ所以上の羽根車Ｐ ｉ （ｉ＝１〜ｎ）を備え、定回転数で槽内に貯留された液体を攪拌する電動攪拌機を有し、予め求めていた反応槽内の液レベルの変化と電動攪拌機の駆動電流値の変化の関係から電動攪拌機の駆動電流の計測値に対応するＭＳ反応槽に貯留される処理液の液面レベルを求めて液面レベル変動を検出することを特徴とする液面レベル変動の検出方法である。 A fourth invention of the present invention is a sulfidation step of sulfidizing a Ni-containing leachate obtained from nickel oxide ore using HPAL technology, which is a treatment stored in a closed MS reaction tank used for the sulfidation treatment. A method for detecting a liquid level fluctuation of a liquid, wherein the MS reaction tank is equipped with two or more impellers P i (i=1 to n) counting from the bottom direction of the reaction tank, and the MS reaction tank is placed in the tank at a constant rotation speed. It has an electric stirrer that stirs the stored liquid, and the MS reaction corresponding to the measured value of the drive current of the electric stirrer from the relationship between the change in the liquid level in the reaction tank and the change in the drive current value of the electric stirrer that was obtained in advance. A liquid level fluctuation detecting method is characterized in that a liquid level fluctuation of a processing liquid stored in a bath is obtained to detect a liquid level fluctuation.
本発明の第５の発明は、ＨＰＡＬ技術を用いてニッケル酸化鉱から得られたＮｉを含む浸出液を硫化処理する硫化工程で、前記硫化処理に使用される液面レベル計を備えた密閉型ＭＳ反応槽に貯留された処理液の液面レベルの監視システムであって、下記（１）の液面レベル計の校正方法、或いは（２）の液面レベル監視方法が実行可能で、ＭＳ反応槽に設置された液面レベル計が、正常に稼働している場合には、（１）の校正方法を用いてレベル計の校正を行い、校正された液面レベル計を使用して硫化処理を継続し、液面レベル計に異常が発生した場合には、（２）の検出方法による液面レベルの検出に切り替えて液面レベルを監視して硫化処理を継続することを特徴とする液面レベルの監視システムである。 A fifth aspect of the present invention is a sulphiding step of sulphating a Ni-containing leachate obtained from nickel oxide ore using HPAL technology, which is a closed MS equipped with a liquid level gauge used for the sulphating treatment. A system for monitoring a liquid level of a processing liquid stored in a reaction tank, which is capable of executing the following liquid level level calibration method (1) or liquid level monitoring method (2). If the liquid level meter installed in the unit is operating normally, calibrate the level meter using the calibration method in (1) and perform the sulfurization treatment using the calibrated liquid level meter. If the liquid level meter continues to operate abnormally, the liquid level is detected by the detection method of (2), the liquid level is monitored, and the sulfidation process is continued. It is a level monitoring system.
（１）第１の発明に記載の液面レベル計の校正方法を用いて使用中の液面レベル計の校正を行う液面レベル計の校正方法。
（２）第４の発明に記載の液面レベル変動の検出方法を用いて稼働中におけるＭＳ反応槽に貯留される処理液の液面レベル検出を行う液面レベル検出方法。
(1) A liquid level meter calibration method for calibrating a liquid level meter in use using the liquid level meter calibration method according to the first invention.
(2) A liquid level detecting method for detecting the liquid level of the treatment liquid stored in the MS reaction tank during operation using the liquid level fluctuation detecting method according to the fourth aspect of the invention.
本発明のレベル構成及びレベルコントロールシステムでシステムの２重化によって不具合の発生を防止することができるので、その工業的価値は極めて大きい。 With the level configuration and level control system of the present invention, it is possible to prevent the occurrence of defects due to the duplication of the system, and therefore its industrial value is extremely large.
以上説明してきたとおり、ＭＳ反応槽は２４時間連続で運転されている。即ち使用しているレベル計の保守、整備、修理は、休転毎に行うことになり、運転時にはできない。そのため、レベル計に不具合が生じた場合、その解決にはＭＳ反応槽の運転を停止しなければならなかった。その際、不具合のあった槽の前段や後段にある多数の槽を逐次停止する必要があった。
このような状況のなかで、本発明はＭＳ反応槽を連続運転するために、ＭＳ反応槽のレベルコントロールシステムの不具合の発生を予防すると共に、発生してしまった場合でもＭＳ反応槽の運転を停止せずに、レベルコントロールシステムの不具合、特に液面レベル計の不具合を解消する、以下のような特徴を備えている。
As described above, the MS reaction tank is operated continuously for 24 hours. That is, the maintenance, maintenance, and repair of the level meter being used must be performed every time the machine is stopped, and cannot be performed during operation. Therefore, when a problem occurs in the level meter, the operation of the MS reaction tank has to be stopped to solve the problem. At that time, it was necessary to sequentially stop a large number of tanks at the front and rear of the defective tank.
Under such circumstances, since the present invention continuously operates the MS reaction tank, it prevents the occurrence of a malfunction of the level control system of the MS reaction tank, and even if it occurs, the operation of the MS reaction tank is prevented. It has the following features to solve the problems of the level control system, especially the problems of the liquid level meter without stopping.
即ち、ＭＳ反応槽内の被攪拌物を攪拌する電動攪拌機に備えられている複数段の羽根車の一つ一つが、被攪拌物に浸漬されて全没する毎に、定回転数で攪拌している攪拌機の駆動電流値が大きく変わる事を利用して、運転中の反応槽に設置、稼働状態の液面レベル計を校正する方法を可能とするものである。 That is, each of the multi-stage impellers provided in the electric stirrer that stirs the object to be stirred in the MS reaction tank is stirred at a constant rotation number every time it is completely immersed in the object to be stirred. By utilizing the fact that the driving current value of the agitator is greatly changed, it is possible to install a method in a reaction tank during operation to calibrate a liquid level meter in operation.
また、このレベル計が故障した場合、予め導き出しておいた電動攪拌機の駆動電流値と同期した反応槽内の被攪拌物レベル値の両者間における相関関係から、計測した電動攪拌機の駆動電流値を用いて反応槽内の被攪拌物レベル値が算出される、この算出した推定レベル値によって、レベル計が不具合時でも反応槽の被攪拌物レベルを検出することができる検出方法が利用可能となる。 In addition, if the level meter fails, the measured drive current value of the electric stirrer can be calculated from the correlation between the level value of the object to be stirred in the reaction tank synchronized with the drive current value of the electric stirrer that is derived in advance. The level value of the object to be stirred in the reaction tank is calculated by using the estimated level value thus calculated, and the detection method capable of detecting the level of the object to be stirred in the reaction tank even when the level meter fails ..
さらに、本発明に係る液面レベルの監視システムは、上記２つの特徴を備えたシステムである。
即ち、ＭＳ反応槽に設置されたレベル計が、正常に稼働している場合には、本発明に係る液面レベル計の校正方法を用いて稼働中のレベル計の校正を行い、その校正されたレベル計を使用して硫化処理を継続する。一方、レベル計に異常が発生した場合には、本発明に係る液面レベル変動の検出方法による液面レベルの検出に切り替えて液面レベルを監視して硫化処理を継続する。
Further, the liquid level monitoring system according to the present invention is a system having the above two features.
That is, when the level meter installed in the MS reaction tank is operating normally, the level meter in operation is calibrated using the calibration method of the liquid level meter according to the present invention, and the calibration is performed. Continue the sulfurization process using a level meter. On the other hand, when an abnormality occurs in the level meter, the liquid level is detected by the liquid level fluctuation detection method according to the present invention, the liquid level is monitored, and the sulfurating treatment is continued.
以下、図面を参照しながら、各々説明する。
［レベル計の校正方法］
図２は、ＭＳ反応槽筐体２に電動攪拌機１０、レベル計２０を設置した組立状態のＭＳ反応槽１の縦断面を示す図で、本発明で使用する電動攪拌機１０は、ＭＳ反応槽筐体の底部に備えつけられる据付型攪拌機、若しくは上部から筐体内に装入される懸吊形攪拌機のいずれであっても良く、被攪拌物を攪拌する少なくとも２段以上の羽根車Ｐｉ（ｉ＝１〜ｎ：ｎ≧２）を備えるものである。さらに、この２段以上の羽根車は、ＭＳ反応槽底部側から、Ｐ１、Ｐ２・・・Ｐｎ−１、Ｐｎと番号付けされる。なお、図２において、１１は攪拌機の駆動部、１２は攪拌機モーターで、Ｓ０ ３はＭＳ反応槽底部から３段目の羽根車Ｐ３上部までの距離で、校正基準レベルとして用いられる。
Each will be described below with reference to the drawings.
[Calibration method of level meter]
FIG. 2 is a view showing a longitudinal section of the MS reaction tank 1 in an assembled state in which the electric stirrer 10 and the level meter 20 are installed in the MS reaction tank housing 2. The electric stirrer 10 used in the present invention is the MS reaction tank housing. It may be either a stationary stirrer provided at the bottom of the body or a suspension stirrer loaded into the housing from the top, and at least two stages of impellers P i (i= 1 to n: n≧2). Further, the two or more stages of impellers are numbered P 1 , P 2 ... P n-1 , P n from the bottom of the MS reaction tank. In FIG. 2, 11 is a drive unit of the stirrer, 12 is a stirrer motor, S 0 3 is the distance from the bottom of the MS reaction tank to the upper part of the third-stage impeller P 3 , and is used as a calibration reference level.
このような電動攪拌機を用い、定回転数で羽根車を回転させて被攪拌物の処理液を攪拌した場合、攪拌に伴い羽根車の回転への抵抗が生じ、その大きさは羽根車が処理液の液面下から姿を現すにつれて小さくなり、攪拌機の羽根車の駆動電流値も少なくなる。また、羽根車から離れた位置に液面がある場合も、液面が上昇または下降すると、羽根車によって力を受けるスラリーの総量（質量）と駆動電流値が増加または減少する。
そこで、上記駆動電流値の変化を確認する予備実験を行い、図３に示す結果を得た。図３は、３段の羽根車（ｎ＝３、Ｐ１、Ｐ２、Ｐ３）を備える電動攪拌機を使用中における液面レベル（単位：％）の経時変化と駆動電流値（単位：Ａ ただし、縦軸に数値は表示していない。）の経時変化を捉えた一例を示す。
When such an electric stirrer is used to rotate the impeller at a constant rotation speed to stir the treatment liquid of the object to be stirred, the stirring causes resistance to the rotation of the impeller, and the size of the impeller is processed by the impeller. The liquid becomes smaller as it appears from below the liquid surface, and the driving current value of the impeller of the stirrer also becomes smaller. Further, even when the liquid surface is at a position away from the impeller, when the liquid surface rises or falls, the total amount (mass) of the slurry and the driving current value which receive the force of the impeller increase or decrease.
Therefore, a preliminary experiment for confirming the change in the drive current value was conducted, and the results shown in FIG. 3 were obtained. FIG. 3 shows the change over time of the liquid level (unit: %) and the drive current value (unit: A) when an electric stirrer equipped with a three-stage impeller (n=3, P 1 , P 2 , P 3 ) was used. However, numerical values are not shown on the vertical axis.) is shown as an example.
図３において、ＭＳ反応槽内の処理液の液面は、羽根車Ｐ３を全没するレベルの約８０％で反応が行われており、処理液は圧力に応じた流量で常に排出されている状態である。その状態から処理液の供給ポンプを低速にし、液面レベルを緩慢に低下させて羽根車Ｐ３の上部が液面に出現した時点（図３、「○」表示）から駆動電流は大きく減少を始めた。その時点で液量（液面レベル）に対して硫化水素量が過剰となり、気相部の圧力が高くなったために、液面レベルは急激に低下しはじめ、伴って駆動電流も、より急激な減少を示していく。硫化水素ガスの吹き込み量を減少させたところ、羽根車Ｐ３の全体が露出した後（液面レベル、駆動電流値共に極小値を示す時点）で、処理液の排出量が減少に転じ、液面レベルの増加に伴い駆動電流値も上昇するが、再度、硫化水素ガスの吹き込み量を増加させると液面レベル、駆動電流値共に低下していく。その後処理液の供給ポンプを増速すると、液面レベルの上昇に伴って駆動電流値も上昇して液面レベルが羽根車Ｐ３が全没した時点（図３、「●」表示）以降、駆動電流は、その変動幅を狭めて一定の値を維持している様子が図３から見て取れる。 In FIG. 3, the liquid level of the treatment liquid in the MS reaction tank is about 80% of the level at which the impeller P 3 is completely submerged, and the treatment liquid is constantly discharged at a flow rate according to the pressure. It is in a state of being. From that state, the supply pump of the processing liquid is slowed down, the liquid level is slowly lowered, and the drive current is greatly reduced from the time when the upper part of the impeller P 3 appears on the liquid surface (indicated by “◯” in FIG. 3). I started. At that time, the amount of hydrogen sulfide became excessive with respect to the liquid amount (liquid surface level), and the pressure in the gas phase became high, so the liquid surface level began to drop sharply, and the driving current also drastically increased. Show a decrease. When the blowing amount of hydrogen sulfide gas was reduced, after the entire impeller P 3 was exposed (at the time when both the liquid level and the driving current value reached their minimum values), the discharge amount of the treatment liquid started to decrease, and The drive current value also rises as the surface level increases, but both the liquid level and the drive current value decrease when the amount of hydrogen sulfide gas blown in is increased again. After that, when the supply pump of the processing liquid is accelerated, the driving current value is also increased with the increase of the liquid level, and the liquid level is completely immersed in the impeller P 3 (FIG. 3, “●” is displayed). It can be seen from FIG. 3 that the drive current maintains a constant value by narrowing its fluctuation range.
そこで、レベル計の校正は、校正実施の準備過程として、その校正基準液面レベル（Ｓ０ ｎ：図４の場合ではＳ０ ３）を、電動攪拌機の３段目の羽根車Ｐ３の上部が処理液の液面に現出する時点（図４、上矢印表示）の液面レベルを以って設定する。なお、図４において下矢印で示されたＳ１ ３は羽根車Ｐ３の下部が処理液の液面に現出する時点を指し示している。
具体的にはＭＳ反応槽に配置された電動攪拌機におけるＭＳ槽内面底部から羽根車Ｐ３の上部までの距離を実測して求めた値とする。なお、第２段目の羽根車を校正に使用する場合も、３段目の羽根車の場合と同様に設定する。
Therefore, in the calibration of the level meter, the calibration reference liquid level (S 0 n : S 0 3 in the case of FIG. 4) is set to the upper part of the third-stage impeller P 3 of the electric stirrer as a preparation process for the calibration. Is set on the liquid level of the processing liquid (FIG. 4, upper arrow mark). Incidentally, S 1 3 indicated by the down arrow in FIG. 4 points to the time when the lower portion of the impeller P 3 is emerge on the liquid surface of the treatment liquid.
Specifically, the distance from the bottom of the inner surface of the MS tank to the upper portion of the impeller P 3 in the electric stirrer arranged in the MS reaction tank is set to a value obtained by actual measurement. In addition, when the second-stage impeller is used for calibration, the same setting is performed as in the case of the third-stage impeller.
さらに、予め、電動攪拌機の駆動電流値と、レベル計の液面レベルの時系列変化の計測値から求めた、「駆動電流値と液面レベル値との相関データ」を準備する。
この相関データは、図４のようなグラフ、又は表として示すものや、計測値から求めた近似式で表したものであっても良い。この近似式は、一つの線形近似式、範囲を限定した複数の線形近似式の組合せ、非線形近似式などを、得られた計測データとレベル計の精度に合わせて適宜選択、利用できる。
Furthermore, “correlation data between the drive current value and the liquid level value” obtained from the drive current value of the electric stirrer and the measured value of the time series change of the liquid level of the level meter are prepared.
This correlation data may be represented as a graph or a table as shown in FIG. 4, or may be represented by an approximate expression obtained from measured values. As this approximation formula, one linear approximation formula, a combination of a plurality of linear approximation formulas with a limited range, a non-linear approximation formula and the like can be appropriately selected and used according to the obtained measurement data and the accuracy of the level meter.
レベル計校正の実施は、第一に、相関データから校正基準レベルＳ０ ｎ−１、又はＳ０ ｎに対応する駆動電流値Ｉ０ ｎ−１又はＩ０ ｎを求める。ここで、添え字ｎは、基準とする羽根車の番号で、３段目の羽根車を基準とする場合、ｎ＝３となる。
第二に、ＭＳ反応槽の運転において、電動攪拌機の駆動電流値がＩ０ ｎ−１のときのレベル計が指示する計測液面レベルＬｎ−１、或いは駆動電流値がＩ０ ｎのときのレベル計が指示する計測液面レベルＬｎを記録する。
次に、記録した計測液面レベルＬｎ−１と校正基準レベルＳ０ ｎ−１、又は計測液面レベルＬｎと校正基準レベルＳ０ ｎを用いて校正度合を、「ＪＩＳ Ｚ ９０９０−１９９１の基準点校正」に則り把握してレベル計の校正、調整を実施する。
To perform the level meter calibration, first , the drive current value I 0 n-1 or I 0 n corresponding to the calibration reference level S 0 n−1 or S 0 n is obtained from the correlation data. Here, the subscript n is the number of the impeller used as the reference, and when the impeller of the third stage is used as the reference, n=3.
Secondly, in the operation of the MS reaction tank, when the drive current value of the electric stirrer is I 0 n-1 , the measured liquid level L n-1 indicated by the level meter, or when the drive current value is I 0 n Record the measured liquid level L n indicated by the level meter.
Next, using the recorded measurement liquid level L n-1 and the calibration reference level S 0 n-1 , or the measurement liquid level L n and the calibration reference level S 0 n , the calibration degree is determined according to “JIS Z 9090-1991”. Perform the calibration and adjustment of the level meter based on the "Reference point calibration" .
［液面レベル変動の検出方法］
次に、ＭＳ反応槽に貯留された処理液の液面レベル変動の検出方法を説明する。
本発明は、ＨＰＡＬ技術を用いてニッケル酸化鉱から得られたＮｉを含む浸出液を硫化処理する硫化工程で、前記硫化処理に使用されるＭＳ反応槽に貯留された処理液の液面レベル変動の検出方法で、ＭＳ反応槽に備付のレベル計を故障などで使用できない状態、或いは校正等のメンテナンスで利用できない状態のときに、反応槽内の処理液の液面レベルを検出するものである。
[Detection method of liquid level fluctuation]
Next, a method of detecting a liquid level fluctuation of the processing liquid stored in the MS reaction tank will be described.
The present invention is a sulfidation step of sulfiding a Ni-containing leachate obtained from nickel oxide ore using the HPAL technology, in which the fluctuation of the liquid level of the treatment liquid stored in the MS reaction tank used for the sulfidation treatment In the detection method, the liquid level of the processing liquid in the reaction tank is detected when the level meter provided in the MS reaction tank cannot be used due to a failure or the like and cannot be used for maintenance such as calibration.
本方法が使用されるＭＳ反応槽は、図２に示すような反応槽の底部方向から数えて２段以上の羽根車Ｐｉ（ｉ＝１〜ｎ）を備え、定回転数で槽内に貯留された処理液を攪拌する電動攪拌機を有するものである。 The MS reaction tank in which this method is used is equipped with two or more stages of impellers P i (i=1 to n) counted from the bottom direction of the reaction tank as shown in FIG. It has an electric stirrer that stirs the stored treatment liquid.
以下、その検出方法を説明する。
先ず、「レベル計の校正方法」と同様に準備過程として、予め、電動攪拌機の駆動電流値と、レベル計の液面レベルの時系列変化の計測値から求めた、「駆動電流値と液面レベル値との相関データ」を準備する。
この相関データは、図４のようなグラフ、又は表として示すものや、計測値から求めた近似式：推定液面レベル式、例えば、「Ｌ＝ａ＋ｂ＊Ｉ（Ｉ：駆動電流値）」で表したものであっても良く、この近似式は、一つの線形近似式、範囲を限定した複数の線形近似式の組合せ、非線形近似式などを、得られた計測データとレベル計の精度に合わせて適宜選択、利用できる。図４では、３領域に分けて近似式を適応するのが妥当と思われる。
The detection method will be described below.
First, as in the preparation process similar to the “level meter calibration method”, the “driving current value and liquid level” obtained in advance from the driving current value of the electric stirrer and the measured value of the time series change of the liquid level of the level meter Prepare "correlation data with level value".
This correlation data is represented by a graph as shown in FIG. 4, or as a table, or an approximate expression obtained from measured values: an estimated liquid level equation, for example, “L=a+b*I (I: drive current value)”. This approximation formula may be a linear approximation formula, a combination of a plurality of linear approximation formulas with a limited range, a non-linear approximation formula, etc., which are adjusted to the obtained measurement data and level meter accuracy. Can be appropriately selected and used. In FIG. 4, it seems appropriate to apply the approximate expression by dividing into three regions.
次に、電動攪拌機の駆動電流の計測値ＩＭに対応するＭＳ反応槽に貯留される処理液の液面レベルを、上記相関データから算出し、推定液面レベルＬＥとして検出するもので、この検出を時系列で行うことで、稼働中の「推定液面レベルＬＥ」により液面レベル変動を検出するものである。 Then, those of the liquid level of the process liquid reserved in the MS reactor corresponding to the measured value I M of the driving current of the electric stirrer, calculated from the correlation data is detected as the estimated liquid surface level L E, by performing the detection in time series, and detects the liquid level fluctuation by 'estimated fluid level L E "running.
推定液面レベルＬＥを求めるための近似式として、簡略的に図４の関係を一つの近似式で表し、その全測定領域において関係を直線で示す近似式に、「ｙ（反応槽レベル［％］）＝０．８１３×ｘ（攪拌機の駆動電流値［Ａ］）＋３２．０７」を用い、推定による推定液面レベルＬＥと、この（計算に使用した電動攪拌機の）駆動電流値計測に対応したレベル計による指示値ＬＲの時系列変化の比較結果を図５に示す。
最大５％程度の変動幅を有しているが、指示値ＬＲの時系列傾向を推定液面レベルＬＥがトレースしているのが判る。推定液面レベルＬＥと指示値ＬＲの差は、例えば、図４に示すような範囲毎の近似式を用いたり、ｘやｙとして移動平均を取った値を使用するなどの方法により小さくすることができる。
一方実操業では、使用するＭＳ反応槽が縦長の槽では、羽根車を大径化するよりも、羽根車の段数を増やす方が均一に攪拌できるもので、このように複数段の羽根車を備えた撹拌機を有す反応槽では、液面が高くても低くても精度よく液面レベルを推定することが可能である。
As an approximate expression for obtaining the estimated liquid surface level L E , the relationship of FIG. 4 is simply represented by one approximate expression, and the relationship is indicated by a straight line in the entire measurement region. %]) = 0.813 × x (drive current value of the stirrer [a]) + 32.07 "using the estimated liquid surface level L E by the estimation, the electric stirrer was used for this (calculated) drive current value measurement FIG. 5 shows the comparison result of the time series change of the indicated value L R by the level meter corresponding to.
It has the variation width of up to about 5%, it can be seen that the indicated value L estimated liquid surface level L E series trend when R is tracing. The difference between the estimated liquid level L E and the indicated value L R can be reduced by, for example, using an approximate expression for each range as shown in FIG. 4 or using a value obtained by taking a moving average as x and y. can do.
On the other hand, in actual operation, if the MS reaction tank used is a vertically long tank, it is possible to stir more uniformly by increasing the number of impellers than by increasing the diameter of the impeller. In a reaction tank having a stirrer provided, it is possible to accurately estimate the liquid level regardless of whether the liquid level is high or low.
こうして求めた推定液面レベルＬＥは、予め定めた目標液面レベル（たとえば、７０〜８０％）より高い場合はＭＳ反応槽内の保有液量を減らす操作を行い、低い場合はＭＳ反応槽内の保有液量を増やす操作を行うのに役立てることができる。保有液量を減らす操作とは、たとえば、硫化水素などのガスの供給量を増加させてＭＳ反応槽内の圧力を高める操作や、ＭＳ反応槽内への給液ポンプの送液量を減らす操作が該当する。保有液量を増やす操作としては、保有液量を減らす操作の逆の操作である。 Thus determined estimated fluid level L E is predetermined target liquid surface level (e.g., 70-80%) is higher than performs an operation of reducing the holdings fluid volume in the MS reactor, if low MS reactor It can be used to perform an operation to increase the amount of retained liquid inside. The operation of reducing the amount of retained liquid is, for example, an operation of increasing the supply amount of gas such as hydrogen sulfide to increase the pressure in the MS reaction tank, or an operation of reducing the liquid supply amount of the liquid supply pump into the MS reaction tank. Is applicable. The operation of increasing the retained liquid amount is the reverse operation of the operation of decreasing the retained liquid amount.
［監視システム］
本発明の更なる発明は、ＨＰＡＬ技術を用いてニッケル酸化鉱から得られたＮｉを含む浸出液を硫化処理する硫化工程で、その硫化処理に使用される密閉されたＭＳ反応槽に貯留された処理液の液面レベルの監視システムで、（１）液面レベル計の校正方法、及び（２）液面レベル検出方法を有するもので、このＭＳ反応槽に設置されたレベル計が、正常に稼働している場合には、（１）液面レベル計の校正方法を用いて稼働中にレベル計の校正を行い、その校正されたレベル計を使用して硫化処理を継続することを特徴とし、レベル計に異常が発生した場合には、（２）液面レベル検出方法による液面レベルの検出に切り替えて液面レベルを監視して硫化処理を継続することを特徴とする液面レベルの監視システムである。
[Monitoring system]
A further invention of the present invention is a sulfidation step of sulfiding a Ni-containing leachate obtained from nickel oxide ore using HPAL technology, which is a treatment stored in a sealed MS reaction tank used for the sulfiding treatment. A liquid level monitoring system that has (1) a liquid level meter calibration method and (2) a liquid level detection method, and the level meter installed in this MS reaction tank operates normally. If it is, (1) the level meter is calibrated during operation by using the liquid level meter calibration method, and the sulfurating treatment is continued using the calibrated level meter, When an abnormality occurs in the level meter, (2) the liquid level is detected by switching to the liquid level detection method, and the liquid level is monitored to continue the sulfidation treatment. System.
ここで、（１）の液面レベル計の校正方法は、ＭＳ反応槽に設置された電動攪拌機に付随する羽根車と反応槽内の処理液量と電動攪拌機の駆動電流値の関係を利用したＭＳ反応槽の稼働中のレベル計の校正方法で、具体的には先に述べた第１から第３の発明による「使用中の液面レベル計の校正を行う液面レベル計の校正方法」である。 Here, the method of calibrating the liquid level meter in (1) utilized the relationship between the impeller attached to the electric stirrer installed in the MS reaction tank, the amount of the processing liquid in the reaction tank, and the drive current value of the electric stirrer. A method of calibrating a level meter during operation of an MS reaction tank, specifically, "a method of calibrating a liquid level meter for calibrating a liquid level meter in use" according to the first to third inventions described above. Is.
一方、（２）の液面レベルの検出方法は、予め求めた液面レベル値と駆動電流値の相関関係から液面レベルを推定する液面レベルの検出方法で、具体的には先に述べた第４の発明による「液面レベル変動の検出方法」を用いて稼働中における反応槽の液面レベルの検出を行うものである。 On the other hand, the liquid level detection method (2) is a liquid level detection method that estimates the liquid level from the correlation between the liquid level value and the drive current value obtained in advance. Also, the liquid level of the reaction tank in operation is detected by using the "method for detecting liquid level fluctuation" according to the fourth aspect of the present invention.
この監視システムの利点は、攪拌機の駆動電流値を利用した液面レベルの検出に切り替える直前まで、液面レベル計の校正を集められることにある。よって、液面レベルをなんらかの方法で途切れることなく測定できるし、もし羽根車が腐食したり固着物で覆われていたりしていた場合であっても、直近の近似式を用いて正確に液面レベルを算出できる。 The advantage of this monitoring system is that the calibration of the liquid level meter can be collected until immediately before switching to the liquid level detection using the drive current value of the stirrer. Therefore, the liquid level can be measured without interruption by some method, and even if the impeller is corroded or covered with adhered matter, the liquid level can be accurately measured using the latest approximate expression. The level can be calculated.
１ ＭＳ反応槽（３段の羽根車を備える）
２ ＭＳ反応槽筐体
１０ 電動攪拌機
１１ 攪拌機の駆動部
１２ 攪拌機モーター
２０ レベル計
Ｐｉ 羽根車
1 MS reaction tank (equipped with three-stage impeller)
2 MS reactor driving portion of the housing 10 an electric stirrer 11 stirrer 12 stirrer motor 20 level meter P i impeller
Claims (5)
前記ＭＳ反応槽が反応槽の底部方向から数えてｎカ所以上の羽根車Ｐｉ（ｉ＝１〜ｎ；ｎ≧２）を備え、定回転数で槽内に貯留された処理液を攪拌する電動攪拌機と、前記レベル計を有し、
準備過程として、予め、前記電動攪拌機の駆動電流値と、レベル計の液面レベル値の時系列変化を計測して求めた、駆動電流値と液面レベル値との相関データの準備と、
ＭＳ反応槽の運転において、前記電動攪拌機の羽根車Ｐｎ−１又はＰｎの上部が前記処理液の液面下から現出する時点の液面レベルを校正基準レベルＳ０ ｎ−１又はＳ０ ｎとする設定を行い、
レベル計校正の実施は、第一に前記相関データから、前記校正基準レベルＳ０ ｎ−１、又はＳ０ ｎに対応する駆動電流値Ｉ０ ｎ−１又はＩ０ ｎを求め、
第二に、ＭＳ反応槽の運転において、電動攪拌機の駆動電流値がＩ０ ｎ−１のときのレベル計が指示する計測液面レベルＬｎ−１と前記校正基準レベルＳ０ ｎ−１、又は駆動電流値がＩ０ ｎのときのレベル計が指示する計測液面レベルＬｎと前記校正基準レベルＳ０ ｎを用いて前記レベル計を校正することを特徴とするレベル計の校正方法。 A level meter for measuring the liquid level of the treatment liquid stored in the closed MS reaction tank used for the sulfurization treatment in the sulfurization process of sulfiding the nickel-containing leachate obtained from nickel oxide ore using the HPAL technology. Calibration method during operation of
The MS reactor is counted from the bottom direction of the reaction vessel n places more impellers P i; includes a (i = 1~n n ≧ 2) , to agitate the process liquid stored in the tank at a constant rotational speed With an electric stirrer and the level meter,
As a preparatory process, in advance, the drive current value of the electric stirrer and the time-series change of the liquid level value of the level meter were obtained, and the preparation of the correlation data between the drive current value and the liquid level value,
In the operation of the MS reaction tank, the liquid level at the time when the upper part of the impeller P n-1 or P n of the electric stirrer appears below the liquid level of the processing liquid is the calibration reference level S 0 n-1 or S. Set to 0 n ,
To carry out the level meter calibration, first , the drive current value I 0 n-1 or I 0 n corresponding to the calibration reference level S 0 n−1 or S 0 n is obtained from the correlation data,
Secondly, in the operation of the MS reaction tank, when the drive current value of the electric stirrer is I 0 n-1 , the measured liquid level L n-1 indicated by the level meter and the calibration reference level S 0 n-1 , Alternatively, the level meter is calibrated using the measured liquid level L n indicated by the level meter when the drive current value is I 0 n and the calibration reference level S 0 n .
前記ＭＳ反応槽が、反応槽の底部方向から数えて２カ所以上の羽根車Ｐｉ（ｉ＝１〜ｎ）を備え、定回転数で槽内に貯留された液体を攪拌する電動攪拌機を有し、
予め求めていた反応槽内の液レベルの変化と電動攪拌機の駆動電流値の変化の関係から、前記電動攪拌機の駆動電流の計測値に対応する前記ＭＳ反応槽に貯留される処理液の液面レベルを求めて液面レベル変動を検出することを特徴とする液面レベル変動の検出方法。 A method for detecting a liquid level fluctuation of a treatment liquid stored in a closed MS reaction tank used for the sulfidation in a sulfidation step of sulfidizing a nickel-containing leachate obtained from nickel oxide ore using HPAL technology. And
The MS reaction tank has two or more impellers P i (i=1 to n) counted from the bottom of the reaction tank, and has an electric stirrer for stirring the liquid stored in the tank at a constant rotation speed. Then
From the relationship between the change in the liquid level in the reaction tank and the change in the drive current value of the electric stirrer that has been obtained in advance, the liquid level of the treatment liquid stored in the MS reaction tank corresponding to the measured value of the drive current of the electric stirrer A liquid level fluctuation detecting method characterized by detecting a liquid level fluctuation by obtaining a level.
下記（１）の液面レベル計の校正方法、或いは（２）の液面レベル監視方法が実行可能で、
前記ＭＳ反応槽に設置された液面レベル計が、正常に稼働している場合には、（１）の校正方法を用いて前記レベル計の校正を行い、校正された液面レベル計を使用して液面レベルを測定し、
前記液面レベル計に異常が発生した場合には、（２）の検出方法による液面レベルの検出に切り替えて液面レベルを監視する
ことを特徴とする液面レベルの監視システム。
記）
（１）請求項１に記載の液面レベル計の校正方法を用いて使用中の液面レベル計の校正を行う液面レベル計の校正方法。
（２）請求項４に記載の液面レベル変動の検出方法を用いて稼働中におけるＭＳ反応槽に貯留される処理液の液面レベル検出を行う液面レベル検出方法。 In a sulfidation process of sulfiding the nickel-containing leachate obtained from nickel oxide ore using HPAL technology, a system for monitoring the level of the treatment liquid stored in the closed MS reaction tank used for the sulfidation treatment. There
The following (1) liquid level meter calibration method or (2) liquid level monitoring method can be executed,
When the liquid level meter installed in the MS reaction tank is operating normally, the level meter is calibrated using the calibration method of (1), and the calibrated liquid level meter is used. And measure the liquid level,
When an abnormality occurs in the liquid level meter, the liquid level is monitored by switching to the liquid level detection by the detection method of (2).
Record)
(1) A method of calibrating a liquid level meter which is in use by using the method of calibrating a liquid level meter according to claim 1.
(2) A liquid level detecting method for detecting the liquid level of the processing liquid stored in the MS reaction tank during operation, using the liquid level fluctuation detecting method according to claim 4.
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