JP2018048970A5 - - Google Patents
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- JP2018048970A5 JP2018048970A5 JP2016185864A JP2016185864A JP2018048970A5 JP 2018048970 A5 JP2018048970 A5 JP 2018048970A5 JP 2016185864 A JP2016185864 A JP 2016185864A JP 2016185864 A JP2016185864 A JP 2016185864A JP 2018048970 A5 JP2018048970 A5 JP 2018048970A5
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- 239000007788 liquid Substances 0.000 claims description 167
- 238000006243 chemical reaction Methods 0.000 claims description 81
- 238000001514 detection method Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 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
- 238000005259 measurement Methods 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
- 238000005987 sulfurization reaction Methods 0.000 claims description 9
- 230000000875 corresponding Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 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
- 238000002386 leaching Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 150000003568 thioethers Chemical class 0.000 description 3
- 230000003247 decreasing Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001360 synchronised 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 the level meter attached to the reaction vessel by monitoring the liquid level of the closed reaction vessel based on the current value of the stirrer in the sulfidation step of HPAL.
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, the outline of the smelting flow is shown in FIG. 1, MS is obtained by the reaction of hydrogen sulfide gas (not shown) and an aqueous nickel solution in the sulfidation step (106) during the manufacturing process. (Mix sulfide: mixed sulfide: Ni · Co mixed sulfide) is produced.
The MS reaction vessel is a vessel equipped with a microwave type level meter and a stirrer, and has a structure capable of sealing hydrogen sulfide gas, and once it starts operation, it becomes a continuous operation of regular rest. The reaction vessel is equipped with a bottom removal pipe at the bottom of the vessel, and the bottom removal pipe is connected to the top of the vessel of the next step, but the reaction is performed by keeping the pressure in the reaction vessel higher than the pressure in the vessel of the next step The slurry in the tank can be constantly sent to the container of the next step. In this MS reaction tank, it is necessary to stabilize the liquid level in order to ensure a proper reaction time, and therefore, the amount of slurry delivery is increased or decreased by adjusting the pressure. The adjustment of pressure can be increased by blowing in hydrogen sulfide gas, while reducing the pressure can only wait 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 slightly and early. Then, it becomes necessary to detect the liquid level early prior to the adjustment of pressure, and the level meter (hereinafter also referred to as liquid level meter) is reliable from the viewpoint of reaction control inside the tank and agitator protection. Is required.
However, the MS reaction tank has the following two problems.
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. Difficulty in inspection and repair at the time of level meter indication failure This difficulty arises because the MS reaction vessel is a closed type reaction vessel and hydrogen sulfide is always blown and filled in the inside thereof. If the level meter installed in the reaction container that constitutes this MS reaction tank needs inspection / repair, it involves opening the reaction container. At this time, it is necessary to stop the sulfidation process and replace the gas inside the vessel with nitrogen so that hydrogen sulfide does not leak, which takes time and labor, reduces the production amount, and 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. The point where the liquid level can not be monitored during operation During the operation, hydrogen sulfide is blown into the MS reaction tank, and the liquid level tends to foam. Although one microwave type level meter is attached to the MS reaction tank, there is a risk of measuring the bubbly liquid level. In addition, MS contained in the spattered liquid tends to adhere to the level meter, and depending on the adhesion position, the level meter may be broken, and the level lower limit in the reaction tank can not 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 the check and calibration of the level meter are performed without opening the reaction tank to improve the reliability of the level meter of the closed reaction tank. Furthermore, it is a method of monitoring the liquid level instead of this at the time of failure of the microwave type level meter.
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 been found out that the above problems can be solved focusing on the change in the current value of the stirrer due to the liquid level fluctuation of the MS reaction tank, and the present invention has been completed.
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 process for sulfidizing a leaching solution containing Ni obtained from a nickel oxide ore using the HPAL technology, which is stored in the closed MS reaction tank used for the sulfidation process. It is a calibration method during operation of a level meter that measures the liquid level of the processing liquid, and the MS reaction tank is counted from the bottom of the reaction tank, and n or more impellers P i (i = 1 to n ; n 電動 2 ), and has a motor-driven agitator for stirring the processing solution stored in the tank at a constant rotational speed, and a level meter for measuring the liquid level in the tank of the processing solution, as a preparation process Preparation of correlation data between drive current value and liquid level value obtained by measuring time series change of drive current value of electric stirrer and liquid level level value of level meter, and operation of MS reaction tank, electric stirrer top said impeller P n-1 or P n Settings for the liquid level at which to emerge from the liquid surface of a physical mixture and the calibration reference level S 0 n-1 or S 0 n, the implementation of the level meter calibration, calibration reference level from the correlation data in the first The driving current value I 0 n-1 or I 0 n corresponding to S 0 n-1 or S 0 n is determined, and secondly, in the operation of the MS reaction tank, the driving current value of the electric stirrer is I 0 n-1 said level meter and the measurement liquid level L n-1 to instruct the calibration reference level S 0 n-1, or the drive current value and the measured liquid level L n the level meter to indicate when the I 0 n when A calibration method of a level meter characterized by calibrating the level meter using a 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。 According to a second aspect of the present invention, there is provided a calibration method of a level meter, wherein the correlation data in the first aspect is an approximate expression composed of the liquid level in the MS reaction tank and the driving current value of the motor stirrer. It 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。 According to a third aspect of the present invention, there is provided a calibration of a level meter characterized in that the motorized stirrer according to the first and second aspects of the present invention is provided with n = 3 P 1 , P 2 and P 3 three-stage impellers. It is a method.
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。 The fourth invention of the present invention is a sulfidation process for sulfidizing a leaching solution containing Ni obtained from a nickel oxide ore using the HPAL technology, wherein the treatment stored in the closed MS reaction tank used for the sulfidation process A method for detecting liquid level fluctuation of a liquid, wherein the MS reaction vessel is provided with two or more impellers P i (i = 1 to n) counted from the bottom direction of the reaction vessel, and is fixed in the vessel at a constant rotation number. The MS reaction corresponding to the measured value of the drive current of the electric stirrer based on the relationship between the change of the liquid level in the reaction tank and the change of the drive current value of the motor stirrer, which has the motorized stirrer for stirring the stored liquid. A method of detecting liquid level fluctuation, comprising detecting liquid level fluctuation by obtaining liquid level of the processing liquid stored in the tank.
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。 The fifth invention of the present invention is a sulfurizing step of sulfurizing a leaching solution containing Ni obtained from a nickel oxide ore using the HPAL technology, wherein the closed MS comprising the liquid level meter used for the sulfurizing treatment It is a monitoring system of the liquid level of processing liquid stored in the reaction tank, and the calibration method of the liquid level meter of the following (1) or the liquid level monitoring method of (2) can be executed, MS reaction tank If the liquid level meter installed in the unit is operating normally, calibrate the level meter using the calibration method of (1), and use the calibrated liquid level meter to perform sulfurization treatment. Continuously, when an abnormality occurs in the liquid level meter, it switches to the detection of the liquid level by the detection method of (2), monitors the liquid level and continues the sulfurization processing. 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 method of calibrating a liquid level meter that calibrates a liquid level meter in use using the method of calibrating a liquid level meter according to the first invention.
(2) A liquid level detection method for detecting the liquid level of the processing liquid stored in the MS reaction tank during operation using the liquid level fluctuation detection method according to the fourth 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。 Since the level configuration and level control system of the present invention can prevent the occurrence of a failure by duplicating the system, 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 vessel is operated continuously for 24 hours. That is, maintenance, maintenance, and repair of the level meter being used will be performed at each rest, and can not be performed at the time of operation. Therefore, in the case of failure of the level meter, it was necessary to stop the operation of the MS reactor. At that time, it was necessary to sequentially stop a large number of tanks at the front stage and the rear stage of the tank where the failure occurred.
Under such circumstances, in order to operate the MS reaction vessel continuously, the present invention prevents the occurrence of a failure in the level control system of the MS reaction vessel and operates the MS reaction vessel even if it has occurred. It has the following features to eliminate problems with the level control system, especially with the level meter, without stopping it.
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 time the plurality of stages of impellers provided in the motorized stirrer for stirring the substance to be stirred in the MS reaction vessel is immersed in the substance to be stirred and is totally submerged, it is stirred at a constant rotation number. By making use of the fact that the driving current value of the stirrer is largely changed, it is possible to calibrate the liquid level meter installed in the operating reaction tank and in the operating state.
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。 If the level meter breaks down, the measured drive current value of the motor stirrer is calculated from the correlation between both the level values of the object in the reaction tank synchronized with the drive current value of the motor stirrer derived in advance. The level value of the object in the reaction vessel is calculated using this estimated level value, which makes it possible to use a detection method that allows the level meter to detect the level of the object in the reaction vessel even when there is a problem .
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 provided with 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, it switches to the detection of the liquid level by the method of detecting the liquid level fluctuation according to the present invention, monitors the liquid level, and continues the sulfurization treatment.
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 of these will be described below with reference to the drawings.
[How to calibrate the level meter]
FIG. 2 is a view showing a vertical cross section of the MS reaction tank 1 in an assembled state in which the motor stirrer 10 and the level meter 20 are installed in the MS reaction tank casing 2. The motor stirrer 10 used in the present invention It may be either a stationary stirrer mounted on the bottom of the body or a suspended stirrer charged into the housing from the top, and at least two or more stages of impellers P i (i = 1 to n: n ≧ 2). Furthermore, the two or more stages of impellers are numbered P 1 , P 2 ... P n−1 , P n from the MS reaction vessel bottom side. In FIG. 2, 11 is the driving part of the stirrer, the 12 with a stirrer motor, S 0 3 is the distance from MS reactor bottom to the impeller P 3 top of the third stage, is used as the 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 the processing solution of the material to be stirred is stirred by rotating the impeller at a constant rotational speed using such an electric stirrer, resistance to the rotation of the impeller is generated along with the stirring, and the size is determined by the impeller It becomes smaller as it appears from below the surface of the liquid, and the driving current value of the impeller of the stirrer also decreases. Also, even when the liquid level is at a position away from the impeller, when the liquid level rises or falls, the total amount (mass) of the slurry subjected to the force by the impeller and the drive current value increase or decrease.
Therefore, a preliminary experiment was conducted to confirm the change in the drive current value, and the results shown in FIG. 3 were obtained. FIG. 3 shows the time course of the liquid level (unit:%) and the driving current value (unit: A) during use of the electric stirrer having three stages of impellers (n = 3, P 1 , P 2 , P 3 ) Note, however, that the vertical axis does not show numerical values.
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 surface of the treatment liquid in the MS reaction tank is reacted at about 80% of the level at which the impeller P 3 is totally submerged, and the treatment liquid is always discharged at a flow rate corresponding to the pressure. It is in the state of The feed pump of the processing liquid from that state to a low speed, when the upper appeared on the liquid surface of the impeller P 3 by slowly lowering the liquid level (Fig. 3, "○" Display) drive current is decreased significantly from I started. At that time, the amount of hydrogen sulfide becomes excessive with respect to the amount of liquid (liquid level), and the pressure in the gas phase increases, so the liquid level starts to fall sharply, and the drive current is also more rapid. We will show a decrease. When the blowing amount of hydrogen sulfide gas was reduced, the amount of discharge of the processing solution turned to decrease after the entire impeller P 3 was exposed (at the time when the liquid level and the driving current value both show local minimum values), Although the drive current value also increases with the increase of the surface level, when the blowing amount of hydrogen sulfide gas is increased again, both the liquid level and the drive current value decrease. Then when accelerating the feed pump of the processing liquid, when the drive current value with increasing liquid level even rises and the liquid level impeller P 3 died all (FIG. 3, "●" Display) and later, It can be seen from FIG. 3 that the drive current is maintained at 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, the calibration of the level meter is performed as a preparation process of calibration execution by setting the calibration reference liquid level (S 0 n : S 0 3 in the case of FIG. 4) to the upper portion of the third stage impeller P 3 of the motorized stirrer. Is set according to the liquid level at the point when it appears on the liquid surface of the treatment liquid (indicated by the arrow in FIG. 4). 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.
In particular with a value determined by measuring the distance from MS vessel inner surface bottom in the electric agitator disposed MS reactor to the top of the impeller P 3. When the second stage impeller is used for calibration, it is set in the same manner 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”, which is obtained in advance from the drive current value of the electric stirrer and the measurement value of the time series change of the liquid level of the level meter, is prepared.
The correlation data may be a graph as shown in FIG. 4 or a table, or may be represented by an approximate expression obtained from measurement 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, etc. 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。
The implementation of the level meter calibration first determines 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. Here, the subscript n is the reference number of the impeller, and when the third stage impeller is the reference, n = 3.
Secondly, in the operation of the MS reaction tank, when the driving liquid value L n-1 indicated by the level meter when the driving current value of the motor stirrer is I 0 n -1 or when the driving current value is I 0 n Record the measured liquid level L n indicated by the level meter.
Next, the calibration degree is measured 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 , “JIS Z 9090-1991. Perform calibration and adjustment of the level meter by grasping in accordance with “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。
[Method of detecting liquid level fluctuation]
Next, the detection method of the liquid level fluctuation of the processing liquid stored in the MS reaction tank will be described.
The present invention is a sulfidation process for sulfidizing a leachate containing Ni obtained from a nickel oxide ore using the HPAL technology, wherein the level level fluctuation of the processing solution stored in the MS reaction tank used for the sulfidation process According to 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 can not be used due to failure or can not 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。 MS reactor to which the present method is used, provided with a bottom impeller of two or more stages as counted from the direction P i of the reaction vessel as shown in FIG. 2 (i = 1 to n), the tank in a constant rotational speed It has an electric stirrer for stirring 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。
Hereinafter, the detection method will be described.
First, as in the preparation process of “level meter calibration method”, “drive current value and liquid level obtained in advance from the drive current value of the motor stirrer and the time series change of the liquid level of the level meter. Prepare “correlation data with level value”.
This correlation data is a graph as shown in FIG. 4 or shown as a table, or an approximate expression obtained from the measured value: estimated liquid level expression, 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., according to the obtained measurement data and the accuracy of the level meter. Can be selected and used appropriately. In FIG. 4, it seems reasonable to divide the three regions and apply the approximate expression.
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 this detection in time series, the liquid level fluctuation is detected by the "estimated liquid level L E " in operation.
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 level L E , the relationship in FIG. 4 is simply expressed by one approximate expression, and in the entire measurement region, the relationship is indicated by a straight line “y (reactor level [ %]) = 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 the comparison results of the time series change in the instruction value L R according to the corresponding level meter shown in FIG.
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 is small, for example, by using an approximate expression for each range as shown in FIG. 4 or using a value obtained by taking a moving average as x or y. can do.
On the other hand, in an actual operation, when the MS reaction tank to be used is a vertically long tank, it is possible to uniformly stir by increasing the number of stages of the impeller rather than increasing the diameter of the impeller, and thus multiple impellers In a reaction tank having a built-in stirrer, 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 useful to carry out an operation to increase the amount of liquid held inside. The operation of reducing the amount of liquid holding includes, for example, an operation of increasing the pressure in the MS reaction tank by increasing the supply amount of gas such as hydrogen sulfide, and an operation of reducing the amount of liquid feed from the liquid feed pump into the MS reaction tank. Is the case. The operation of increasing the amount of liquid holding is the reverse of the operation of reducing the amount of liquid holding.
［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 process for sulfidizing a leaching solution containing Ni obtained from a nickel oxide ore using the HPAL technology, which is stored in a sealed MS reactor used for the sulfidation process. A monitoring system of liquid level of liquid, (1) calibration method of liquid level meter, and (2) liquid level detection method, the level meter installed in this MS reaction tank operates normally If it does, (1) the level meter is calibrated during operation using the calibration method of the liquid level meter, and the sulfurization processing is continued using the calibrated level meter, When an abnormality occurs in the level meter, (2) It switches to the detection of the liquid level by the liquid level detection method, monitors the liquid level, and continues the sulfurization processing, monitoring the liquid level It is a 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 according to (1) utilizes the relationship between the amount of processing liquid in the reaction tank and the impeller attached to the motorized stirrer installed in the MS reaction tank and the driving current value of the motorized stirrer The calibration method of the level meter during operation of the MS reaction vessel, specifically, the calibration method of the liquid level meter for calibrating the liquid level meter in use according to the first to third inventions described above It 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 method of detecting the liquid level of (2) is a method of detecting the liquid level which estimates the liquid level from the correlation between the liquid level value obtained in advance and the driving current value, and specifically described above. The liquid level of the reaction tank in operation is detected using the “method of detecting liquid level fluctuation” according to the fourth 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 just before switching to detection of the liquid level using the driving current value of the stirrer. Therefore, the liquid level can be measured without interruption in any way, and even if the impeller has been corroded or covered with a solid, the liquid level can be accurately measured using the nearest approximation formula. You can calculate the level.
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 Reactor (with 3 stages of impellers)
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 in the above-mentioned sulfurization treatment in a sulfurization step of sulfurizing a leachate containing nickel obtained from nickel oxide ore using HPAL technology Calibration method during operation of
The MS reaction tank has n or more impellers P i (i = 1 to n ; n; 2 ) counted from the bottom direction of the reaction tank, and the processing solution stored in the tank is stirred at a constant rotation number It has an electric stirrer and the above-mentioned level meter,
In the preparation process, preparation of correlation data between the drive current value and the liquid level value obtained by measuring the time-series change of the drive current value of the electric stirrer and the liquid level level value of the level meter in advance.
In the operation of the MS reaction tank, the liquid level at the time when the upper portion of the impeller P n-1 or P n of the electric stirrer emerges from below the liquid surface of the processing liquid is corrected to the calibration reference level S 0 n-1 or S Set to 0 n ,
First, the level meter calibration is performed from the correlation data to obtain a 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 .
Secondly, in the operation of MS reactors, the calibration reference level level meter and the measurement liquid level L n-1 to instruct the time of the driving current value of the electric agitator I 0 n-1 S 0 n -1, Alternatively, the method of calibrating a level meter is characterized in that the level meter is calibrated using the measurement 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 of detecting fluctuation in liquid level of a processing solution stored in a sealed MS reaction tank used in the above-mentioned sulfurization treatment in a sulfurizing step of sulfurizing a leachate containing nickel obtained from nickel oxide ore using HPAL technology And
The MS reaction tank is provided with two or more impellers P i (i = 1 to n) counted from the bottom direction of the reaction tank, and has an electric stirrer for stirring the liquid stored in the tank at a constant rotational speed And
From the relationship between the change in liquid level in the reaction tank and the change in drive current value of the electric stirrer, the liquid level of the processing liquid stored in the MS reaction tank corresponding to the measured value of the drive current of the electric stirrer A method of detecting liquid level fluctuation, comprising detecting 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 the sulfidation process of sulfidizing a leachate containing nickel obtained from nickel oxide ore using HPAL technology, the system for monitoring the liquid level of the processing solution stored in the closed MS reaction tank used for the sulfidation process There,
The calibration method of the liquid level meter below (1) or the liquid level monitoring method of (2) 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 Measure the liquid level,
When a failure occurs in the liquid level meter, the liquid level monitoring system switches to detection of the liquid level by the detection method of (2) and monitors the liquid level.
Record)
(1) A method of calibrating a liquid level meter which performs calibration of a liquid level meter in use by using the method of calibrating a liquid level meter according to claim 1.
(2) A liquid level detection method for detecting the liquid level of the processing liquid stored in the MS reaction tank in operation using the liquid level fluctuation detection method according to claim 4.
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