JP2020065971A - Cleaning function-added agitation device - Google Patents

Cleaning function-added agitation device Download PDF

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JP2020065971A
JP2020065971A JP2018199752A JP2018199752A JP2020065971A JP 2020065971 A JP2020065971 A JP 2020065971A JP 2018199752 A JP2018199752 A JP 2018199752A JP 2018199752 A JP2018199752 A JP 2018199752A JP 2020065971 A JP2020065971 A JP 2020065971A
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container
stirring
scattering
funnel
liquid
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JP7183505B2 (en
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翔太 三條
Shota Sanjo
翔太 三條
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Sumitomo Metal Mining Co Ltd
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Abstract

To provide a cleaning function-added agitation device that allows the cleaning of the inside of the agitation vessel without turning off the motor of the agitator or breaking down the vessel.SOLUTION: Provided is an agitator device 10 comprising a rotation shaft 11 which is installed in a vessel 20 having rotation drive means 23 outside, and which has agitation blades 12 at its lower end part, the agitation blades being caused to rotate by rotation drive force of the rotation drive means 23 to agitate fluid to be agitated inside the vessel 20. The rotation shaft 11 is provided with a scattering part 13 for scattering a cleaning solution by centrifugal force of the rotation shaft 11, the scattering part being preferably made of a funnel-shaped member with the diameter becoming smaller toward the lower end part.SELECTED DRAWING: Figure 1

Description

本発明は、洗浄機能付き撹拌装置に関し、特に、混合槽や反応槽などの撹拌機を備えた撹拌容器の内壁面や測定機器表面に付着した物質を容易に除去することが可能な洗浄機能付き撹拌装置に関する。   The present invention relates to a stirrer with a cleaning function, and in particular, with a stirrer capable of easily removing substances adhering to the inner wall surface of a stirring container equipped with a stirrer such as a mixing tank or reaction tank or the surface of a measuring instrument. Regarding a stirring device.

プロセス液を取り扱うプラントの実操業においては、該プロセス液に対して液体状や固体状の添加物を混合して目的成分を浸出させたり沈殿物を生成させたりする様々な処理が行われている。このようなプロセス液の処理には攪拌装置を備えた撹拌容器が一般的に用いられている。撹拌容器には、例えば特許文献1に記載されているように、混合や沈殿物生成等の各種操作における最適な条件の範囲内に調整するため、例えば温度計、pH計、ORP計などの液相に浸漬して測定する測定端子が一般的に設けられている。   In the actual operation of a plant that handles process liquids, various treatments are performed in which liquid or solid additives are mixed with the process liquids to leach target components or form precipitates. . A stirring container equipped with a stirring device is generally used for the treatment of such a process liquid. For example, as described in Patent Document 1, a liquid such as a thermometer, a pH meter, and an ORP meter is used in the stirring container in order to adjust within a range of optimum conditions in various operations such as mixing and precipitate formation. A measuring terminal for immersing in a phase for measurement is generally provided.

一方、研究現場においては、実操業における運転条件のベースとなる適切な混合条件や沈殿物生成条件等を探索するため、温度範囲を様々に変更したり添加剤の種類や量を変更したりして繰り返し試験することが行われている。そのため、研究現場においても撹拌装置を備えた撹拌容器が一般的に用いられている。このような研究現場で用いる撹拌容器にも、混合や沈殿物生成等の各種操作における最適な条件を測定するため、温度計、pH計、ORP計などの液相に浸漬して測定する測定端子が設けられている。   On the other hand, at the research site, in order to search for appropriate mixing conditions and precipitate formation conditions that are the basis of operating conditions in actual operation, the temperature range can be changed variously and the type and amount of additives can be changed. It is being repeatedly tested. Therefore, a stirring container equipped with a stirring device is generally used also in a research site. Even in such a stirring container used in a research site, in order to measure the optimum conditions in various operations such as mixing and precipitate formation, a measuring terminal for immersing in a liquid phase such as a thermometer, a pH meter, and an ORP meter. Is provided.

上記の撹拌容器では、撹拌により飛散した液体が、撹拌容器の液位より上側の気相部分に露出する内壁だけでなく、撹拌容器の天井部分、測定端子及び撹拌軸において液体に浸漬していない部分などにも付着する場合があり、これをそのまま放置しておくと品質がばらついたり、正確な試験結果が得られなかったりするおそれがある。また、該撹拌容器を用いて回分式(バッチ式)で多品種少量生産を行うプラントでは、各バッチ処理ごとに取り扱うプロセス液が異なる場合があるので、収率の向上やコンタミネーション防止のためにバッチ処理が完了したときに該付着物を除去して回収することが望ましい。   In the above stirring container, the liquid scattered by stirring is not immersed in the liquid at the ceiling part of the stirring container, the measuring terminal and the stirring shaft as well as the inner wall exposed to the gas phase portion above the liquid level of the stirring container. If they are left as they are, the quality may vary and accurate test results may not be obtained. Further, in a batch type batch production plant that uses the stirring container, the process liquid handled may differ for each batch process, so to improve yield and prevent contamination. It is desirable to remove and collect the deposits when batch processing is completed.

回分式で毎回同じプロセス液を取り扱う場合は、付着物が常にプロセス液とほぼ同じであれば特に問題は生じないが、例えば添加物の混合を伴う回分式処理の場合、混合操作の初期に飛散したものが付着していると、この付着物が次バッチのプロセス液に混入した場合は所望の添加物濃度にならない恐れがある。また、沈殿物を生成する処理の場合、該沈殿物生成反応の初期に飛散したものが付着していると、この付着物が次バッチのプロセス液に混入した場合は、該付着物によって次バッチのプロセス液中の溶質濃度が増大するので、予定していた沈殿物生成反応条件で沈殿物を生成することができなくなる恐れがある。   When handling the same process liquid each time in a batch system, there is no particular problem if the deposits are almost the same as the process liquid.For example, in the case of a batch process involving mixing of additives, scattering occurs at the beginning of the mixing operation. If the deposits adhere, the deposits may not reach the desired additive concentration when the deposits are mixed in the process liquid of the next batch. Further, in the case of the treatment for producing a precipitate, if the scattered matter is attached at the initial stage of the precipitate producing reaction, and if the attached matter is mixed in the process liquid of the next batch, the next batch is caused by the attached matter. Since the solute concentration in the process liquid is increased, it may not be possible to generate a precipitate under the predetermined precipitate generation reaction conditions.

特開2017−159194号公報JP, 2017-159194, A

上記のように、撹拌容器を用いて回分式で多品種少量生産を行う場合や研究現場で適切な条件を探索する場合、あるいは撹拌容器を用いて連続式でプロセス液を処理する場合であっても、ロット切り替えなどにより取り扱うプロセス液を変更する場合は、バッチ処理完了後やロット切り替え時に上記付着物を除去するのが好ましい。しかしながら、例えば研究現場で使用する撹拌容器は、通常は実操業で使用するものよりもサイズが小さいため付着物を除去しにくいうえ、撹拌容器の気相部分には、撹拌軸や測定端子が存在しているため、内壁面や天井部分の付着物を除去するには大変手間がかかることが問題になっていた。   As described above, there are cases where batch production using a stirring container for multi-product small quantity production, when searching for suitable conditions at a research site, or when continuously processing process liquids using a stirring container. However, when the process liquid to be handled is changed by switching lots, it is preferable to remove the deposits after the batch processing is completed or when the lots are switched. However, for example, stirring vessels used in research sites are usually smaller in size than those used in actual operations, and it is difficult to remove deposits.In addition, stirring tubes and measuring terminals exist in the gas phase of stirring vessels. Therefore, it has been a problem that it takes a lot of time to remove the deposits on the inner wall surface and the ceiling portion.

研究現場で用いる撹拌容器は、一般に上部が開放した円筒容器と、該開放部分を覆う蓋部と、該円筒容器に受け入れた被撹拌流体を撹拌する役割を担う撹拌機とから構成されており、該蓋部には撹拌機の撹拌軸や測定端子を挿通するための複数の貫通孔が設けられている。この撹拌容器の蓋部には更に固体添加剤を投入するための貫通孔が設けられることもある。従って洗ビンの先端部をこれら貫通孔のいずれかから差し込んで洗浄水を吹き付けることである程度洗浄することは可能である。   The stirring container used at the research site is generally composed of a cylindrical container having an open upper portion, a lid portion covering the open portion, and a stirrer having a role of stirring the stirred fluid received in the cylindrical container, The lid portion is provided with a plurality of through holes for inserting the stirring shaft of the stirrer and the measuring terminals. The lid portion of this stirring container may be provided with a through hole for introducing a solid additive. Therefore, it is possible to perform cleaning to some extent by inserting the tip of the washing bottle from any of these through holes and spraying washing water.

しかしながら、このように洗ビンによる洗浄は洗浄作業を行う作業者によって個人差が生じるおそれがある。また、できるだけ個人差が生じないようにするには撹拌容器を分解して洗浄するのが好ましいが、この場合は撹拌機のモーターを停止し、必要に応じてこれら撹拌機や測定端子を取り外してから蓋部を上方に又は傾けて持ち上げて取り外す必要があり、極めて煩雑な手間を要していた。本発明は上記した実情に鑑みてなされたものであり、撹拌機のモーターを停止させたり容器を分解したりする必要なく撹拌容器の内側を洗浄することが可能な洗浄機能付き撹拌装置を提供することを目的とする。   However, such cleaning with the cleaning bottle may cause individual differences depending on the worker who performs the cleaning work. In addition, it is preferable to disassemble and wash the agitating container in order to avoid individual differences as much as possible, but in this case, stop the agitator motor and remove these agitators and measuring terminals as necessary. It is necessary to remove the lid part by lifting it up or tilting it, which is extremely troublesome. The present invention has been made in view of the above circumstances, and provides a stirring device with a cleaning function capable of cleaning the inside of a stirring container without having to stop the motor of the stirrer or disassemble the container. The purpose is to

上記目的を達成するため、本発明に係る撹拌装置は、下端部に撹拌翼を有する回転軸からなる撹拌装置であって、前記回転軸には洗浄液を該回転軸の遠心力により飛散させる飛散部が設けられていることを特徴としている。   In order to achieve the above-mentioned object, the stirring device according to the present invention is a stirring device including a rotating shaft having a stirring blade at a lower end thereof, wherein the rotating shaft scatters a cleaning liquid by a centrifugal force of the rotating shaft. Is provided.

本発明によれば、撹拌機のモーターを停止させたり容器を分解したりすることなく撹拌容器の内側を洗浄することができるので、その工業的価値は極めて大きい。   According to the present invention, the inside of the stirring container can be washed without stopping the motor of the stirrer or disassembling the container, so that its industrial value is extremely large.

本発明の一具体例の洗浄機能付き撹拌装置を具備した撹拌容器の縦断面図である。1 is a vertical cross-sectional view of a stirring container equipped with a stirring device with a cleaning function according to an embodiment of the present invention. 図1の洗浄機能付き撹拌装置の斜視図である。It is a perspective view of the stirring device with a cleaning function of FIG. 本発明の一具体例の攪拌装置が有する漏斗状部材の平面図である。It is a top view of the funnel-shaped member which the stirring device of one example of the present invention has.

以下、本発明の洗浄機能付き撹拌装置及びこれを備えた撹拌容器の実施形態について図面を参照しながら詳細に説明する。図1に示すように、本発明の一具体例の洗浄機能付き撹拌装置10は、フッ素樹脂、ステンレス鋼などからなる回転軸11と、該回転軸11の下端部に設けられたプロペラ型、タービン型、パドル型等の撹拌翼12とからなり、好適には円筒形状を有する容器20に取り付けられる。この容器20では、プロセス液や研究用試料などの液体やスラリーを所定の液位まで受け入れて、浸出や沈殿物生成などの化学反応、混合、培養などの各種の単位操作が行われる。その際、撹拌装置10によって被撹拌流体である上記液体やスラリーが撹拌される。   Hereinafter, embodiments of a stirrer with a cleaning function of the present invention and a stirrer equipped with the stirrer will be described in detail with reference to the drawings. As shown in FIG. 1, a stirrer 10 with a cleaning function according to one embodiment of the present invention includes a rotary shaft 11 made of fluororesin, stainless steel, etc., a propeller type turbine provided at a lower end of the rotary shaft 11, and a turbine. And a paddle type stirring blade 12, and is preferably attached to a container 20 having a cylindrical shape. In the container 20, liquids or slurries such as process liquids and research samples are received up to a predetermined liquid level, and various unit operations such as chemical reaction such as leaching and precipitate formation, mixing, and culturing are performed. At that time, the liquid or slurry as the fluid to be stirred is stirred by the stirring device 10.

この容器20は、例えば上部が開放した円筒胴部21と、該円筒胴部21の該開放部分を塞ぐ取り外し自在な蓋部22とからなる。この円筒胴部21には図示しない液排出ノズル、液供給ノズル、オーバーフローノズル等の各種ノズル、撹拌効率を高めるバッフル板、液温調整用の冷媒や熱媒が循環する蛇管やジャケット等が設けられる場合がある。   The container 20 is composed of, for example, a cylindrical body portion 21 having an open upper portion, and a removable lid portion 22 that closes the open portion of the cylindrical body portion 21. The cylindrical body portion 21 is provided with various nozzles such as a liquid discharge nozzle, a liquid supply nozzle, and an overflow nozzle (not shown), a baffle plate that enhances stirring efficiency, a flexible pipe for adjusting the liquid temperature and a heating medium, and a jacket. There are cases.

一方、蓋部22には、その略中央部の外側に上記撹拌装置10を回転駆動するモーターなどの回転駆動手段23が搭載されている。この回転駆動手段23の駆動軸に上記撹拌装置10の回転軸11が連結されるため、該蓋部22には該回転軸11を挿通させる貫通孔が設けられている。また、該蓋部22には温度計、pH計、ORP計、DO計などの測定端子24を挿通させる貫通孔も設けられている。この蓋部22には更に液体や粉体等の供給用のノズル又は開口部、サンプリング用のノズル又は開口部、メンテナンス用のハンドホール等が設けられる場合がある。   On the other hand, a rotation driving means 23 such as a motor for rotating the stirring device 10 is mounted outside the substantially central portion of the lid portion 22. Since the rotary shaft 11 of the stirring device 10 is connected to the drive shaft of the rotary drive means 23, the lid 22 is provided with a through hole through which the rotary shaft 11 is inserted. Further, the lid portion 22 is also provided with a through hole through which a measuring terminal 24 such as a thermometer, a pH meter, an ORP meter, and a DO meter is inserted. The lid 22 may be further provided with a nozzle or opening for supplying liquid or powder, a sampling nozzle or opening, a handhole for maintenance, and the like.

上記のような構造を有する容器20に所定の液位まで液体を受け入れて上記の回転駆動手段23の回転駆動力による撹拌装置10の回転で撹拌を行った場合、該円筒胴部21の内壁面のうち該液位よりも上方の気相部に曝される部分、蓋部22の下面、撹拌装置10の回転軸11や測定端子24において該気相部に曝される部分には、撹拌により飛散した液体が付着する。なお、一般的には上記液位の高さは、円筒胴部21の直胴部の高さの20〜80%程度である。   When the liquid is received up to a predetermined liquid level in the container 20 having the above structure and the stirring is performed by the rotation of the stirring device 10 by the rotation driving force of the rotation driving means 23, the inner wall surface of the cylindrical body portion 21 Of the portion exposed to the gas phase portion above the liquid level, the lower surface of the lid portion 22, the rotating shaft 11 of the stirrer 10 and the portion exposed to the gas phase portion at the measurement terminal 24 by stirring, The scattered liquid adheres. The height of the liquid level is generally about 20 to 80% of the height of the straight body portion of the cylindrical body portion 21.

上記の内壁面等に付着した液体や該液体由来の付着物を洗浄液で除去するため、該撹拌装置10の回転軸11には該回転軸11の回転により生じる遠心力により洗浄液を周囲に飛散させる飛散部13が設けられている。この飛散部13は、容器20の外部から供給される水などの洗浄液を、撹拌装置10の回転軸11の遠心力で少なくとも容器20の胴部21の内壁面にまで到達させることができるものであれば特に限定はないが、撹拌翼12の安定的な回転が維持されるように回転軸11に対して回転対称な形状を有しているのが好ましく、図2に示すような漏斗形状を有しているのが好ましい。   In order to remove the liquid adhering to the inner wall surface or the like and the deposits derived from the liquid with a cleaning liquid, the cleaning liquid is scattered around the rotating shaft 11 of the stirring device 10 by the centrifugal force generated by the rotation of the rotating shaft 11. A scattering unit 13 is provided. The scattering unit 13 is capable of causing a cleaning liquid such as water supplied from the outside of the container 20 to reach at least the inner wall surface of the body portion 21 of the container 20 by the centrifugal force of the rotating shaft 11 of the stirring device 10. If there is no particular limitation as long as it is, it is preferable that it has a shape rotationally symmetric with respect to the rotating shaft 11 so as to maintain stable rotation of the stirring blade 12, and a funnel shape as shown in FIG. It is preferable to have.

以下、この図2に示す漏斗形状の飛散部13について具体的に説明する。この図2の飛散部13は、上端部から下端部に向かって徐々に縮径する漏斗部13aと、該漏斗部13aの下端部から下方に同心円状に延在する円筒部13bとからなり、この円筒部13bを上記回転軸11に外嵌させることで該回転軸11に取り付けられている。この漏斗部13aの材質は特に限定はないが、フッ素樹脂、ステンレス鋼等の耐食性材料で形成されるのが好ましい。一方、円筒部13bは漏斗部13aと同じ材質で一体成型してもよいが、上記回転軸11の外周面に摺接自在に外嵌されるように、可撓性部材で形成してもよい。   Hereinafter, the funnel-shaped scattering portion 13 shown in FIG. 2 will be specifically described. The scattering portion 13 in FIG. 2 is composed of a funnel portion 13a whose diameter gradually decreases from the upper end portion to the lower end portion, and a cylindrical portion 13b which extends concentrically downward from the lower end portion of the funnel portion 13a, The cylindrical portion 13b is attached to the rotary shaft 11 by fitting it onto the rotary shaft 11. The material of the funnel portion 13a is not particularly limited, but it is preferable that the funnel portion 13a is formed of a corrosion resistant material such as fluororesin or stainless steel. On the other hand, the cylindrical portion 13b may be integrally formed of the same material as the funnel portion 13a, but may be formed of a flexible member so as to be slidably fitted onto the outer peripheral surface of the rotating shaft 11. .

上記飛散部13は、この円筒部13bにおいて回転軸11にネジ留め、接着、溶接、ロウ付けなどにより固定するのが好ましく、これらの固定法の中では、ネジ留め等により取り外し自在に取り付けるのが、洗浄部位を適宜調整できるのでより好ましい。なお、この回転軸11において円筒部13bが外嵌される部分にシールテープを巻き付けてもよく、これにより取り外し自在に固定できるうえ、洗浄水が漏斗部13aの下端部から漏れるのを防ぐことができる。   The scattering portion 13 is preferably fixed to the rotary shaft 11 in the cylindrical portion 13b by screwing, bonding, welding, brazing or the like. Among these fixing methods, it is detachably attached by screwing or the like. It is more preferable because the washing site can be adjusted appropriately. In addition, a seal tape may be wound around a portion of the rotary shaft 11 where the cylindrical portion 13b is fitted, so that the cleaning tape can be detachably fixed and the wash water can be prevented from leaking from the lower end portion of the funnel portion 13a. it can.

上記飛散部13に容器20の外部から洗浄液を供給する方法としては、使用していない貫通孔やノズル、あるいは回転軸11の挿通用の蓋部22の貫通孔の隙間から洗ビンなどの注水器Sの注水部を差し込んで、漏斗部13aの上部開口部から洗浄水を直接流し込めばよい。なお、回転軸11の回転が比較的低速の場合は、回転軸11のうち蓋部22の上方に突出する部分に洗浄水を注水し、回転軸11の外周面を伝って洗浄水を流下させて漏斗部13aに注ぎ込むようにしてもよい。あるいは、容器20の外部の洗浄液供給源に接続した洗浄液供給配管を蓋部22を挿通させて回転軸11に沿って延在させ、その先端部から漏斗部13aに洗浄液を供給してもよい。   As a method of supplying the cleaning liquid from the outside of the container 20 to the scattering portion 13, a water injector such as a washing bottle is used from a gap between the through hole and the nozzle which are not used, or the through hole of the lid portion 22 for inserting the rotary shaft 11. It suffices to insert the water injection portion of S and directly inject the washing water from the upper opening portion of the funnel portion 13a. When the rotation shaft 11 rotates at a relatively low speed, cleaning water is poured into a portion of the rotation shaft 11 that protrudes above the lid portion 22, and the cleaning water flows down along the outer peripheral surface of the rotation shaft 11. Alternatively, it may be poured into the funnel portion 13a. Alternatively, the cleaning liquid supply pipe connected to the cleaning liquid supply source outside the container 20 may be inserted through the lid portion 22 to extend along the rotary shaft 11, and the cleaning liquid may be supplied from the tip end portion thereof to the funnel portion 13a.

上記の漏斗部13aの高さやその上端部の外径、その傾斜面の傾斜角度は、回転軸11の回転数や飛散部13の取り付け位置等を考慮したうえで、遠心力で飛散した洗浄液が容器20内の飛散部13から最も遠い部位まで到達するように設計するのが好ましい。特に、複数の測定端子が設けられる場合は、それらによって洗浄液の到達が阻害される部分にも洗浄液が行き渡るように、より勢いよく洗浄液を飛散させるのが好ましい。   The height of the funnel portion 13a, the outer diameter of the upper end portion thereof, and the inclination angle of the inclined surface of the funnel portion 13a are determined in consideration of the number of revolutions of the rotary shaft 11, the attachment position of the scattering portion 13, and the like. It is preferable to design so as to reach the farthest portion from the scattering portion 13 in the container 20. In particular, when a plurality of measuring terminals are provided, it is preferable that the cleaning liquid is spattered more vigorously so that the cleaning liquid reaches the portion where the arrival of the cleaning liquid is obstructed by them.

一般的には、漏斗部13aの上端部の外径は、容器20の内径の1/10〜1/3程度が好ましく、1/8〜1/5程度がより好ましい。この場合、漏斗部13aの上端部の外径は、回転軸11の直径の2倍以上であるのが好ましく、5倍以上であるのがより好ましい。また、漏斗部13aの傾斜面は、回転軸11に対して15〜60°傾斜しているのが好ましく、30°傾斜しているのがより好ましい。更に、漏斗部の上端部と蓋部22の下面との間は、少なくとも漏斗部の深さの10%で離間するように取り付けるのが好ましい。   Generally, the outer diameter of the upper end of the funnel portion 13a is preferably about 1/10 to 1/3 of the inner diameter of the container 20, and more preferably about 1/8 to 1/5. In this case, the outer diameter of the upper end of the funnel portion 13a is preferably twice or more the diameter of the rotating shaft 11, and more preferably 5 times or more. Further, the inclined surface of the funnel portion 13a is preferably inclined by 15 to 60 ° with respect to the rotating shaft 11, and more preferably inclined by 30 °. Further, it is preferable that the upper end portion of the funnel portion and the lower surface of the lid portion 22 are attached so as to be separated by at least 10% of the depth of the funnel portion.

かかる構成により、モーターなどの回転駆動手段23を停止させることなく、また蓋部22の取り外しなどの容器20の分解を行うことなく、容器20の内壁面や測定端子24等において付着物が残留しやすい部分を容易に洗浄することができる。なお、洗浄液の混入により容器20内のプロセス液の濃度が薄まることが懸念される場合は、例えばプロセス液の溶媒と同じ液を洗浄液に用い、該洗浄液の混入量に見合うようにあらかじめプロセス液の濃度を高めに調製しておけばよい。   With this configuration, the adhered matter remains on the inner wall surface of the container 20 and the measurement terminals 24 without stopping the rotation driving means 23 such as a motor and without disassembling the container 20 such as removing the lid 22. Easy parts can be easily washed. When it is feared that the concentration of the process liquid in the container 20 will be diminished due to the mixing of the cleaning liquid, for example, the same liquid as the solvent of the process liquid is used as the cleaning liquid, and the process liquid is mixed in advance so as to correspond to the mixing amount of the cleaning liquid. The concentration should be adjusted to a high level.

上記漏斗部13aの内側の傾斜面の形状には特に限定はないが、図3(a)に示すように、内壁面に放射状に延在する複数本の溝部13cを、周方向に均等な間隔をあけて設けるのが好ましい。これにより、洗浄液に遠心力を及ぼしやすくなり、該洗浄液をより勢いよく飛散させることが可能になる。上記の複数本の溝部は、図3(b)に示すように、各々半径方向に対して矢印で示す回転方向の後方側に傾斜させてもよい。これにより、より一層勢いよく洗浄液を飛散させることができる。なお、本発明の実施形態の撹拌装置10を処理前又は処理後の液体がない状態の容器20の洗浄用として用いてもよく、この場合は容器20の内壁全面に加えて底部や撹拌翼など撹拌容器の内側全体を洗浄することになる。   The shape of the inclined surface on the inner side of the funnel portion 13a is not particularly limited, but as shown in FIG. 3 (a), a plurality of groove portions 13c extending radially on the inner wall surface are provided at equal intervals in the circumferential direction. It is preferable to provide the opening. As a result, centrifugal force is easily exerted on the cleaning liquid, and the cleaning liquid can be more vigorously scattered. As shown in FIG. 3B, the plurality of groove portions may be inclined to the rear side in the rotational direction indicated by the arrow with respect to the radial direction. As a result, the cleaning liquid can be scattered more vigorously. The stirring device 10 according to the embodiment of the present invention may be used for cleaning the container 20 in a liquid-free state before or after the treatment. In this case, in addition to the entire inner wall of the container 20, the bottom portion, the stirring blade, etc. The entire inside of the stirring container will be washed.

図1に示すように、漏斗部13a及び円筒部13bからなる飛散部13を有する撹拌装置10を備えた円筒容器20を用意し、その内部にスラリーを受け入れて撹拌装置10で撹拌することで、該スラリーに含まれる固形分の浸出処理を行った。具体的には、容器20の円筒胴部21には外径約70mmの250mLビーカーを採用し、蓋部22はシリコン樹脂製の円板を用いた。この円板の中央部に撹拌装置10の回転軸11の挿通用の最も小さな孔径の第1貫通孔を穿孔した。この第1貫通孔の周りに、該第1貫通孔より大きな孔径を有する温度計端子挿通用の2個の第2貫通孔と、該第2貫通孔より大きな孔径を有するORP計端子挿通用の2個の第3貫通孔と、最も大きい孔径のpH計端子挿通用の2個の第4貫通孔とを穿孔した。   As shown in FIG. 1, a cylindrical container 20 provided with a stirring device 10 having a scattering part 13 composed of a funnel part 13a and a cylindrical part 13b is prepared, and the slurry is received inside and stirred by the stirring device 10, The leaching process of the solid content contained in the slurry was performed. Specifically, a 250 mL beaker with an outer diameter of about 70 mm was adopted as the cylindrical body portion 21 of the container 20, and a silicon resin disk was used as the lid portion 22. A first through hole having the smallest hole diameter for inserting the rotary shaft 11 of the stirring device 10 was bored in the center of the disc. Around the first through hole, two second through holes for inserting a thermometer terminal having a larger diameter than the first through hole and an ORP meter terminal for inserting a larger diameter than the second through hole. Two third through holes and two fourth through holes for inserting the pH meter terminal having the largest hole diameter were punched.

この第1貫通孔に、下端部に4枚の撹拌翼12を有する回転軸11を下側から挿通し、その上端部を上記ビーカーの上方に設けた支持具で支持されているモーターの回転駆動軸に連結した。また、第2貫通孔〜第4貫通孔に、それぞれ温度計、ORP計及びpH計を1本ずつ上方から挿入して液に浸漬する深さにセットした。漏斗部13a及び円筒部13bはフッ素樹脂製で一体成形されており、漏斗部13aは、高さ24mm、上端部の外径20mm、傾斜面の回転軸11に対する傾斜角30°であった。漏斗部13aの内面は図3(b)に示すように半径方向に対して回転方向の後方側に傾斜した4本の溝13cを設けた。   The rotary shaft 11 having four stirring blades 12 at the lower end is inserted into the first through hole from the lower side, and the upper end of the rotary shaft 11 is driven to rotate by a supporting tool provided above the beaker. Connected to the shaft. In addition, a thermometer, an ORP meter and a pH meter were inserted from above into the second through hole to the fourth through hole, respectively, and the depth was set so as to be immersed in the liquid. The funnel portion 13a and the cylindrical portion 13b were integrally formed of fluororesin, and the funnel portion 13a had a height of 24 mm, an outer diameter of the upper end portion of 20 mm, and an inclination angle of 30 ° with respect to the rotating shaft 11 of the inclined surface. As shown in FIG. 3B, the inner surface of the funnel portion 13a is provided with four grooves 13c that are inclined rearward in the rotational direction with respect to the radial direction.

上記の円筒部13bを回転軸11に外嵌させ、漏斗部13aの上端部と蓋部22の下面とが10mm離間するように位置を調整した。その際、回転軸11において該円筒部13bが外嵌される部分にPTFE製のシールテープを巻き付けて飛散部13を固定すると共に、漏斗部13a内の洗浄液が下端部から容易に漏れないようにした。このようにして組み立てた攪拌容器を、約70℃の一定の温度に保持されている温水バス内に浸漬させた。そして、容器20内に液体試料としての純水と、固体試料としてのNi含有物とをそれぞれ秤量して装入した。そして撹拌装置10を約650rpmで回転させながら、浸出用添加剤として濃度64質量%の硫酸を添加した。これにより、pHを1.5、ORPを約100mVとなるように調整し、終点のORP値275mVに落ち着いてから更に10分間保持した。   The cylindrical portion 13b was fitted onto the rotating shaft 11, and the position was adjusted so that the upper end of the funnel portion 13a and the lower surface of the lid portion 22 were separated by 10 mm. At that time, a PTFE sealing tape is wound around the portion of the rotary shaft 11 where the cylindrical portion 13b is fitted to fix the scattering portion 13, and the cleaning liquid in the funnel portion 13a is prevented from easily leaking from the lower end portion. did. The stirring container thus assembled was dipped in a hot water bath maintained at a constant temperature of about 70 ° C. Then, pure water as a liquid sample and Ni-containing material as a solid sample were weighed and placed in the container 20, respectively. Then, while rotating the stirring device 10 at about 650 rpm, sulfuric acid having a concentration of 64% by mass was added as a leaching additive. As a result, the pH was adjusted to 1.5 and the ORP was adjusted to about 100 mV, and the ORP value at the end point was settled at 275 mV, and the temperature was maintained for 10 minutes.

この10分の保持時間経過後、洗浄操作として撹拌装置10のモーターの回転を止めることなく撹拌を継続しながら回転軸11が挿通されている蓋部22の第1貫通孔の隙間から洗ビンSの先端部を差し込んで、純水10ccを該飛散部13の漏斗部13aに直接注入したところ、洗浄水は洗ビンSで注水するや否や一瞬で飛散し、1回の浸出処理に対して合計10回の洗浄を行っても、所要時間は合計数秒程度だった。処理後に容器20内を目視にて確認したところ、容器20の壁面の上縁部、蓋部22の下面、及び温度計等の測定端子24に付着していた付着物は良好に洗浄除去されていた。   After the lapse of the holding time of 10 minutes, the washing bottle S is washed from the gap of the first through hole of the lid 22 through which the rotating shaft 11 is inserted while continuing the stirring without stopping the rotation of the motor of the stirring device 10 as the washing operation. When 10 cc of pure water was directly injected into the funnel portion 13a of the spattering section 13 by inserting the tip of the washing water, the washing water was scattered in an instant as soon as the washing water was poured into the washing bottle S, and a total amount was obtained for one leaching process. Even after washing 10 times, the total time was about several seconds. When the inside of the container 20 was visually confirmed after the treatment, the adhered matters adhered to the upper edge portion of the wall surface of the container 20, the lower surface of the lid 22 and the measurement terminals 24 such as a thermometer were satisfactorily washed and removed. It was

その後、容器20内で処理された浸出液及び残渣を回収し、浸出液をICP−OES装置(Agilent 5100SVDV)で分析したところNi濃度は20g/Lであり、また、残渣を化学分析したところ、残渣中のNi品位は0.25%であり、これらのデータから容器20に装入した試料に含まれていたNiのほぼ100%が回収されていることを確認できた。   Thereafter, the leachate and the residue treated in the container 20 were collected, and the leachate was analyzed by an ICP-OES apparatus (Agilent 5100SVDV) to find that the Ni concentration was 20 g / L. The Ni quality of No. 2 was 0.25%, and it was confirmed from these data that almost 100% of Ni contained in the sample charged in the container 20 was recovered.

比較のため、飛散部13を用いた洗浄を行わなかった以外は上記と同様に浸出処理を行った。洗浄作業においては、撹拌容器10のモーターを停止してから該モーターを支持具ごと移動させた後、蓋部22を持ち上げて容器20の上端部や測定端子などに付着した液を洗ビンSを使用して洗浄水を吹き付けて除去する作業が必要となり、所要時間は1分程度を要した。1回の浸出処理に対して合計10回の洗浄を行ったため、合計10分程度の洗浄時間を要した。   For comparison, the leaching process was performed in the same manner as above except that the cleaning using the scattering part 13 was not performed. In the cleaning operation, after stopping the motor of the stirring container 10 and moving the motor together with the supporting tool, the lid 22 is lifted to wash the liquid adhering to the upper end portion of the container 20 and the measuring terminal into the washing bottle S. A work of spraying and removing the cleaning water was required, and the required time was about 1 minute. Since washing was performed 10 times in total for one leaching process, a washing time of about 10 minutes was required in total.

上記の結果から、本発明の要件を満たす飛散部を備えた撹拌装置を使用することにより、撹拌装置のモーターを停止することなく、また、蓋部を取り外すことなく容器内壁を洗浄でき、特に洗浄しにくい容器内壁の上端部や測定端子の裏側等を確実に洗浄できることが分かる。また、従来の分解洗浄に比べて洗浄時間を短縮できることも分かる。   From the above results, it is possible to wash the inner wall of the container without stopping the motor of the stirrer and without removing the lid, by using the stirrer provided with the scattering part satisfying the requirements of the present invention, and especially for washing. It can be seen that the upper end of the inner wall of the container, which is difficult to do, and the back side of the measuring terminals can be reliably washed. It is also found that the cleaning time can be shortened as compared with the conventional disassembly cleaning.

10 撹拌装置
11 回転軸
12 撹拌翼
13 飛散部
13a 漏斗部
13b 円筒部
13c 溝
20 容器
21 円筒胴部
22 蓋部
23 回転駆動手段
24 測定端子
S 洗ビン
DESCRIPTION OF SYMBOLS 10 Stirrer 11 Rotating shaft 12 Stirring blade 13 Scattering part 13a Funnel part 13b Cylindrical part 13c Groove 20 Container 21 Cylindrical body part 22 Lid part 23 Rotation drive means 24 Measuring terminal S Wash bottle

Claims (6)

下端部に撹拌翼を有する回転軸からなる撹拌装置であって、前記回転軸には洗浄液を該回転軸の遠心力により飛散させる飛散部が設けられていることを特徴とする撹拌装置。   A stirrer comprising a rotating shaft having a stirring blade at a lower end thereof, wherein the rotating shaft is provided with a scattering section for scattering the cleaning liquid by a centrifugal force of the rotating shaft. 前記飛散部は、上端部から下端部に向かって縮径する漏斗状部材からなり、該下端部において前記回転軸に外嵌されていることを特徴とする、請求項1に記載の撹拌装置。   The agitating device according to claim 1, wherein the scattering portion is formed of a funnel-shaped member whose diameter is reduced from an upper end portion toward a lower end portion, and is externally fitted to the rotary shaft at the lower end portion. 前記漏斗状部材は、その内壁面に放射状に延在する複数本の溝部が周方向に均等な間隔をあけて設けられていることを特徴とする、請求項2に記載の撹拌装置。   The stirrer according to claim 2, wherein the funnel-shaped member is provided with a plurality of radially extending groove portions on its inner wall surface at equal intervals in the circumferential direction. 前記複数本の溝部は、各々半径方向に対して回転方向の後方側に傾斜していることを特徴とする、請求項3に記載の撹拌装置。   The stirring device according to claim 3, wherein each of the plurality of groove portions is inclined to the rear side in the rotational direction with respect to the radial direction. 被撹拌流体が装入され、外側に回転駆動手段を備えた容器と、該回転駆動手段の回転駆動力によって回転して該被撹拌流体を撹拌する請求項1〜4のいずれか1項に記載の撹拌装置とからなる撹拌容器であって、前記飛散部が該容器内の液位より上方に位置していることを特徴とする撹拌容器。   5. The container in which the fluid to be stirred is charged and which is provided with rotation driving means on the outside, and the fluid to be stirred is rotated by the rotation driving force of the rotation driving means to stir the fluid to be stirred. An agitating container comprising the agitating device according to claim 1, wherein the scattering portion is located above the liquid level in the container. 前記容器は円筒形状を有し、前記漏斗状部材の上端部の外径は、前記円筒容器の内径の1/10〜1/5で且つ前記回転軸の直径の2倍以上であることを特徴とする、請求項5に記載の撹拌容器。   The container has a cylindrical shape, and the outer diameter of the upper end of the funnel-shaped member is 1/10 to 1/5 of the inner diameter of the cylindrical container and is twice or more the diameter of the rotating shaft. The stirring container according to claim 5.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4994579A (en) * 1973-01-13 1974-09-07
JPS59230652A (en) * 1983-06-14 1984-12-25 Nippon Ranzubaagu Kk Rotary spray apparatus
JPS63202328A (en) * 1987-02-17 1988-08-22 オリオン機械株式会社 Washing apparatus
JPH0570631U (en) * 1992-03-04 1993-09-24 三和機材株式会社 Cleaning device for stirring tank
JPH1015066A (en) * 1996-07-05 1998-01-20 Tiger Vacuum Bottle Co Ltd Negative ion generator
JPH11235522A (en) * 1997-11-14 1999-08-31 Kansai Kagaku Kikai Seisaku Kk Liquid jetting device and liquid jetting method
JP2004351361A (en) * 2003-05-30 2004-12-16 Fujifilm Arch Co Ltd Sprinkler

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4994579A (en) * 1973-01-13 1974-09-07
JPS59230652A (en) * 1983-06-14 1984-12-25 Nippon Ranzubaagu Kk Rotary spray apparatus
JPS63202328A (en) * 1987-02-17 1988-08-22 オリオン機械株式会社 Washing apparatus
JPH0570631U (en) * 1992-03-04 1993-09-24 三和機材株式会社 Cleaning device for stirring tank
JPH1015066A (en) * 1996-07-05 1998-01-20 Tiger Vacuum Bottle Co Ltd Negative ion generator
JPH11235522A (en) * 1997-11-14 1999-08-31 Kansai Kagaku Kikai Seisaku Kk Liquid jetting device and liquid jetting method
JP2004351361A (en) * 2003-05-30 2004-12-16 Fujifilm Arch Co Ltd Sprinkler

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