JPS60238427A - Reverse extraction apparatus of metal - Google Patents
Reverse extraction apparatus of metalInfo
- Publication number
- JPS60238427A JPS60238427A JP59094070A JP9407084A JPS60238427A JP S60238427 A JPS60238427 A JP S60238427A JP 59094070 A JP59094070 A JP 59094070A JP 9407084 A JP9407084 A JP 9407084A JP S60238427 A JPS60238427 A JP S60238427A
- Authority
- JP
- Japan
- Prior art keywords
- fluoride
- organic solvent
- crystals
- zone
- metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002184 metal Substances 0.000 title claims description 14
- 229910052751 metal Inorganic materials 0.000 title claims description 14
- 238000000605 extraction Methods 0.000 title claims description 13
- 239000013078 crystal Substances 0.000 claims description 60
- 239000003960 organic solvent Substances 0.000 claims description 51
- 238000002156 mixing Methods 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 229910021645 metal ion Inorganic materials 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 12
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 18
- 239000010419 fine particle Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 Fe3+ ions Chemical class 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
本発明は、金属イオンを抽出含有する有機溶媒と弗化物
系剥離液とを混合接触させることによ２金属イオンを逆
抽出（剥離）し、金属弗化物または弗化金属錯体結晶と
して析出させ、かつ逆抽出後の剥離液と有機溶媒とを分
離するための装置の改良に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention involves back-extracting (stripping) two metal ions by mixing and contacting an organic solvent containing metal ions with a fluoride-based stripping solution. The present invention relates to an improvement in an apparatus for precipitating metal complex crystals and separating a stripping solution and an organic solvent after back extraction.
溶媒抽出法において、金属イオンを抽出した有機溶媒か
ら弗化物系剥離液（ＨＦ、 Ｎ）１４ ＨＦ２ 。In the solvent extraction method, a fluoride stripping solution (HF, N) 14 HF2 is used from the organic solvent from which metal ions have been extracted.
ＮＨ４Ｆの１種または２種以上を含有する水溶液）を用
いて金属イオンを逆抽出し、弗化物または弗化金属錯体
結晶として析出させるための装置としては、従来、特開
昭５８−８１４０２号公報に示される逆円錐形の゛晶析
装置が開示されている。この晶析装置を使用して工業的
規模で金属の逆抽出を実施した場合、析出結晶の器壁へ
の付着や装置下部における堆積、固化あるいは結晶スラ
リーへの有機溶媒の取り込みなど、装置の連続運転に支
障を来たすような現象が発生し、これらの問題を解決す
るために改良発明されたのが５９年３月３０日出願しか
しながら、析出した結晶微粒子が有機溶媒中に混入し、
これが有機゛溶媒静置区域に連なる溢流せきに付着、堆
積し、せきを詰まらせるという問題は上記改良によって
も解決されず、本出願の有機溶媒剥離液混合槽および剥
離液冷却ゾーンに関する改良により解決をみた。Conventionally, an apparatus for back-extracting metal ions using an aqueous solution containing one or more types of NH4F and precipitating them as fluoride or metal fluoride complex crystals is disclosed in JP-A-58-81402. An inverted conical crystallizer shown in FIG. When back-extracting metals using this crystallizer on an industrial scale, there may be problems such as adhesion of precipitated crystals to the vessel walls, deposition at the bottom of the device, solidification, or incorporation of organic solvent into the crystal slurry. Phenomena that hindered operation occurred, and an improved invention was invented to solve these problems, which was filed on March 30, 1959. However, the precipitated crystal fine particles mixed into the organic solvent,
The problem of this adhering to and accumulating in the overflow weir connected to the organic solvent holding area and clogging the weir has not been solved by the above-mentioned improvements. I saw the solution.
本発明の目的は、従来装置の混合槽に起因する欠点を克
服し、器壁への結晶の付着を防ｄ−，するよう構成して
装置の連続運転を容易ならしめる金属逆抽出装置を提供
することにある。An object of the present invention is to provide a metal back-extraction device that overcomes the drawbacks caused by the mixing tank of conventional devices and is configured to prevent crystals from adhering to the vessel wall, thereby facilitating continuous operation of the device. It's about doing.
すなわち、本発明は、金属イオンを抽出含有する有機溶
媒と弗化物系剥離液との混合槽の下方に、結晶成長ゾー
ンまたは剥離液冷却ゾーンおよび結晶分離ゾーンを有し
、結晶が金属イオンを抽出含有する有機溶媒と加温され
た弗化物系Ｎ＃液とを前記混合槽において混合接触させ
て金属イオンを弗化物または弗化金属錯体として逆抽出
させ、前記弗化物または弗化金属錯体の結晶を前記結晶
成長ゾーンまたは剥離液冷却ゾーンにおいて成長させ、
結晶分離ゾーンにおいて結晶を分離するよう構成された
逆円錐系晶析装置において、前記混合槽に配設された下
降管内に、有機溶媒供給１１を剥離液供給口よりも下部
で前記下降管下端部よりも上部の位置に設け、これによ
り器壁への結晶の付着を防【］二したことを特徴とする
金属逆抽出装置を提供するものである。That is, the present invention has a crystal growth zone or a stripping solution cooling zone and a crystal separation zone below a mixing tank containing an organic solvent containing an extracted metal ion and a fluoride stripping solution, and the crystals extract metal ions. The contained organic solvent and the heated fluoride-based N# liquid are brought into mixed contact with each other in the mixing tank to back-extract the metal ions as fluoride or metal fluoride complex, thereby forming crystals of the fluoride or metal fluoride complex. grown in the crystal growth zone or stripping liquid cooling zone,
In an inverted conical crystallizer configured to separate crystals in a crystal separation zone, an organic solvent supply 11 is supplied to a downcomer pipe disposed in the mixing tank at a lower end of the downcomer pipe below a stripping liquid supply port. The object of the present invention is to provide a metal back-extraction device which is installed at a position above the container wall, thereby preventing crystals from adhering to the vessel wall.
本発明はまた、金属イオンを抽出含有する有機溶媒と弗
化物系剥離液との混合槽の下方に、結晶成長ゾーンまた
は剥離液冷却ゾーンおよび結晶分離ゾーンを有し、結晶
が金属イオンを抽出含有する有機溶媒と加温された弗化
物系剥離液とを前記混合槽において混合接触させて金属
イオンを弗化物または弗化金属錯体として逆抽出させ、
前記弗化物または弗化金属錯体の結晶を前記結晶成長ゾ
ーンまたは剥離液冷却ゾーンにおいて成長させ、結晶分
離ゾーンにおいて結晶を分離するよう構成された逆円錐
系晶析装置において、前記混合槽に配設された下降管内
に、有＃Ｉ溶鱒４＃鎖口ｔｆ―」一部の位置に設け、逆
円錐形装置本体下部に設けられ、外部の熱交換器と接続
された冷却ゾーンを具え、この冷却ゾーン中に設けられ
、その最下部に剥離液に旋回流を起させるよう、はぼ接
線方向に配向された少なくとも１個の吹き出しノズルを
有する強制循環ゾーンとを具え、これにより器壁への結
晶の付着を防ｆＦしたことを特徴とする金属逆抽出装置
を提供するものである。The present invention also has a crystal growth zone or a stripping solution cooling zone and a crystal separation zone below a mixing tank of an organic solvent containing an extracted metal ion and a fluoride stripping solution, and the crystals contain a crystal that extracts and contains metal ions. The organic solvent and the heated fluoride stripping solution are brought into mixed contact with each other in the mixing tank to back-extract metal ions as fluorides or metal fluoride complexes,
In an inverted conical crystallizer configured to grow crystals of the fluoride or metal fluoride complex in the crystal growth zone or stripping liquid cooling zone and separate the crystals in the crystal separation zone, disposed in the mixing tank. A cooling zone is installed at some positions in the downcomer pipe, which is connected to an external heat exchanger, and is installed at the bottom of the inverted conical device body. a forced circulation zone provided in the cooling zone and having at least one blowing nozzle oriented tangentially in the lowermost part of the cooling zone to generate a swirling flow in the stripping liquid, thereby causing a flow to the vessel wall. The object of the present invention is to provide a metal back-extraction device characterized in that fF is prevented from adhering to crystals.
本発明の詳細を図面に基づき詳細に説明するが、本発明
はこれに限定されるものではない。第１図が従来装置の
一例を示すのに対し、第２図および第３図は本発明の金
属逆抽出装置の例を示す。The details of the present invention will be explained in detail based on the drawings, but the present invention is not limited thereto. While FIG. 1 shows an example of a conventional device, FIGS. 2 and 3 show examples of the metal back-extraction device of the present invention.
金属イオンを抽出含有する有機溶媒２は供給口３を経て
、加温された弗化物系剥離液４は供給口５を経てそれぞ
れ混合槽または混合ゾーン６に導入され、ここで撹拌装
置７により混合されて有機相中の金属イオンは弗化物ま
たは弗化金属アンモニウム塩として水相中に逆抽出され
る。金屈イオ管１１中を有機溶媒を分離し、かつ溶解度
の比較的小さ・い弗化物または弗化金属アンモニウム塩
の結晶を析出しつつ下降する。下降管１１の下端部は、
第１図および第２図の装置では結晶成長ゾーン１２の、
第３図の装置では剥離液冷却ゾーン１３のそれぞ芥上限
よりさらに上部に位置しており、下降する剥離液や析出
結晶に附随して下降する有機溶媒の分離上昇を促進する
ように配慮されている。The organic solvent 2 containing extracted metal ions is introduced through a supply port 3 and the heated fluoride stripping solution 4 is introduced through a supply port 5 into a mixing tank or a mixing zone 6, where they are mixed by a stirring device 7. The metal ions in the organic phase are extracted back into the aqueous phase as fluoride or metal ammonium fluoride salts. The organic solvent is separated from the organic solvent in the ion tube 11, and crystals of fluoride or metal ammonium fluoride salt having relatively low solubility are precipitated while descending. The lower end of the downcomer pipe 11 is
In the apparatus of FIGS. 1 and 2, in the crystal growth zone 12,
In the apparatus shown in FIG. 3, each of the stripping liquid cooling zones 13 is located above the upper limit of the waste, and is designed to promote the separation and rise of the descending stripping solution and the organic solvent that descends with the precipitated crystals. ing.
有機溶媒は混合槽または混合ゾーン６から溢流して静置
区域８に分離され、溢流せき９を経て有機溶媒排出口ｌ
Ｏより排出される。下降管１１を下降した剥離液および
結晶は結晶成長ゾーン１２または剥離液冷却ゾーン１３
に導かれる。このゾーンは熱交換器１４と配管接続され
ており、混合槽６で加温状態にあった剥離液を冷却する
ことにより結晶の成長が促進されるとともに、一部結晶
の分級も行われる。The organic solvent overflows from the mixing tank or mixing zone 6 and is separated into a standing area 8, and then passes through an overflow weir 9 to an organic solvent outlet l.
It is discharged from O. The stripping solution and crystals descending down the downcomer pipe 11 are transferred to a crystal growth zone 12 or a stripping solution cooling zone 13.
guided by. This zone is connected via piping to a heat exchanger 14, and by cooling the stripping liquid heated in the mixing tank 6, the growth of crystals is promoted, and some of the crystals are also classified.
第３図は、第２図に示す装置の改良型であって、冷却ゾ
ーン１３の内部にさらに強制循環シーを与えつつ剥離液
の温度と濃度、組成とを均一に保つことにより、結晶の
器壁への付着や装置下部における堆積、固化を防奮卜す
るための配慮がなされている。第３ｂ図に示すように、
強制循環流は少なくとも１個の剥離液吹き出しノズル１
９により、はぼ接線方向流を強制的に生ぜしめるよう構
成する功が特に好適である。FIG. 3 shows an improved version of the apparatus shown in FIG. 2, which further provides a forced circulation sheet inside the cooling zone 13 while keeping the temperature, concentration, and composition of the stripping liquid uniform, thereby making it possible to maintain a uniform crystal vessel. Consideration has been taken to prevent adhesion to walls, accumulation and solidification at the bottom of the equipment. As shown in Figure 3b,
The forced circulation flow is caused by at least one stripping liquid blowout nozzle 1.
9, it is particularly advantageous to compulsorily generate a tangential flow.
剥離液４は、下降管１１を下降した後、最終的には結晶
分離ゾーン１６を上Ａし、排出口１７より装置外に排出
される。また、結晶は結晶排出管１８からスラリーとし
て適宜排出され、固液分離にかけられる。After the stripping liquid 4 descends through the downcomer pipe 11, it finally rises above the crystal separation zone 16 and is discharged from the apparatus through the discharge port 17. Further, the crystals are appropriately discharged as a slurry from the crystal discharge pipe 18 and subjected to solid-liquid separation.
本発明の金属逆抽出装置の主な′改良点である混合槽６
内における有機溶媒供給口３の位置の効果について説明
する。第１図に示す従来装置では、有機溶媒供給口３が
混合槽６の上部でかつ剥離液供給口５とほぼ同じ高さに
あるために有機溶媒の混合槽６内での滞留時間が短く、
また結晶粒子の発生が混合槽６の比較的上部で起こるた
め有機相に析出結晶の微粒子が取り込まれやすかった。Mixing tank 6 which is the main improvement of the metal back extraction device of the present invention
The effect of the position of the organic solvent supply port 3 in the interior will be explained. In the conventional apparatus shown in FIG. 1, since the organic solvent supply port 3 is located at the upper part of the mixing tank 6 and at approximately the same height as the stripping solution supply port 5, the residence time of the organic solvent in the mixing tank 6 is short.
In addition, since the generation of crystal particles occurred at a relatively upper portion of the mixing tank 6, fine particles of precipitated crystals were easily incorporated into the organic phase.
その結束、装置の運転開始後数日にして結晶微粒子の有
機溶媒溢流せき８への付着、堆積が起こって、せきを詰
まらせるという問題が繰り返し発生した。Several days after the bundling and the start of operation of the apparatus, crystal fine particles adhered to and accumulated on the organic solvent overflow weir 8, causing repeated problems of clogging the weir.
一方、本発明の装置では有機溶媒供給口３が混合槽６内
の剥離液供給口５より下部で下降管１１のド端部より一
１＝部に設けられており、そのため有機溶媒の混合槽６
内における滞留時間が従来装置に比へて長くなる。また
結晶粒子が混合槽６の比較的下部で発生し、かつ有機溶
媒供給口からの有機溶媒の流れは−に昇流であり、一方
、剥離液供給【１は混合槽の−Ｌ部にあるので剥離液お
よび結晶の流れはド降流であり、有機溶媒と剥離液およ
び結晶とは混合槽６内で向流接触することになる。その
結果、有機溶媒に伴って一ヒ舅する結晶微粒子は１−Ａ
するに従って除去され、最終的に有機相に取り込まれる
結晶微粒子は著しく減少し、実施例に示すように結晶微
粒子の有機溶媒溢流せき８への付着、堆積やせきの詰ま
りを防止することができるのである。On the other hand, in the apparatus of the present invention, the organic solvent supply port 3 is provided below the stripping liquid supply port 5 in the mixing tank 6 and at the 11= part from the do end of the downcomer pipe 11. 6
The residence time in the tank is longer than that of conventional equipment. In addition, crystal particles are generated at a relatively lower part of the mixing tank 6, and the flow of the organic solvent from the organic solvent supply port is upward to -, while the stripping liquid supply [1 is in the -L part of the mixing tank]. Therefore, the flow of the stripping solution and the crystals is a downward flow, and the organic solvent, the stripping solution and the crystals come into contact with each other in a countercurrent manner in the mixing tank 6. As a result, it was found that the crystalline fine particles that formed with the organic solvent were 1-A.
The number of crystalline particles that are removed and finally incorporated into the organic phase is significantly reduced, and as shown in the example, it is possible to prevent the crystalline particles from adhering to the organic solvent overflow weir 8, preventing it from accumulating and clogging the weir. It is.
以上に説明したとおり、本発明の目的は有機溶媒供給口
３が混合槽６内の剥離液供給口５より下部で、下降管１
１の下端部より上部に設けられておれば達成されるので
あるが、その効果は有機溶媒供給口３が下降管１１の下
端部の直近上部に設けられた装置において最も顕著とな
る。また、本発明の装置であって、装置下部の構造とし
て剥離液冷却ゾーン１３の内部に強制循環ゾーン１５を
有する型式の第３図に示す装置では、生成結晶への有機
溶媒の取り込みゃ結晶の器壁への付着を一層効果的に防
１トすることができ、装置の長期連続運転は一層容易と
なる。As explained above, the object of the present invention is to arrange the organic solvent supply port 3 below the stripping liquid supply port 5 in the mixing tank 6 and the downcomer pipe 1.
This effect can be achieved if the organic solvent supply port 3 is provided above the lower end of the downcomer pipe 11, but this effect is most noticeable in a device in which the organic solvent supply port 3 is provided immediately above the lower end of the downcomer pipe 11. In addition, in the apparatus of the present invention shown in FIG. 3, which has a forced circulation zone 15 inside the stripping liquid cooling zone 13 as a structure in the lower part of the apparatus, the incorporation of organic solvent into the formed crystals is difficult. Adhesion to the vessel wall can be more effectively prevented, and long-term continuous operation of the apparatus becomes easier.
さらに、有機溶媒供給口３の形状に関して、その実施態
様の変化したものも本発明の範囲内である。有機溶媒供
給口３の形状は、単一のノズル状のものでも本発明の目
的は達成されるのであるが、供給口３から上昇する有機
溶媒と下降する剥離液等との接触効率を高めるため、供
給口開口部の有効面積を大きくするなどの工夫がなされ
たものでは−・層効果的に達成される。その実施態様の
例を第４図および第５図に示すが、供給口３の形状はこ
れに限定されるものではない。Furthermore, variations in the shape of the organic solvent supply port 3 are also within the scope of the present invention. Although the purpose of the present invention can be achieved even if the organic solvent supply port 3 has a single nozzle shape, it is necessary to increase the contact efficiency between the organic solvent rising from the supply port 3 and the stripping liquid, etc. descending. This can be achieved effectively by increasing the effective area of the supply port opening. Examples of this embodiment are shown in FIGS. 4 and 5, but the shape of the supply port 3 is not limited thereto.
以１；で詳細に説明した通り、従来装置について有機溶
媒供給口を混合槽内の剥離液供給口より下部で一ト降管
下端部よりＬ部の位置に設けるという改良を施すことに
より、有機溶媒溢流せきの詰まりというトラブルを防ｌ
卜することができ、装置の連続渾転を容易に遂行するこ
とができる。As explained in detail in Section 1 below, an improvement was made to the conventional device in that the organic solvent supply port was provided in the mixing tank below the stripping solution supply port and at a position L from the bottom end of the downcomer tube. Prevents troubles such as clogging of solvent overflow drains
It is possible to easily rotate the device continuously.
３０ｖ／ｖ％Ｄ２ＥＨＰＡ ［ジー（２−エチルヘキシ
ル）りん酸］と７０７ハ％ｎ−パラフィンからなる有機
溶媒を用いてＦｅ３＋イオンを１８．３〜１８．４ｇ１
文抽出含有させた温度が２１〜２３℃の有機溶媒を、２
ｍ゛／時の割合で、第２図に示す本発明の装置の混合槽
５に導入した。この混合槽５内では、有機溶媒供給口３
は下降管１１の下端の直上にあり、剥離液供給口５は有
機溶媒供給口３の１８５ｃｍ上方に位置した。剥離液と
してＰｌｏｔ、 Ｉ（Ｉｉ２が１１８〜１３０ｇ／交、
）ＩＦが４〜９ｇ／愛で湿度が５に供給しながら連続運
転を行った。その結果、運転開始から３０日経過しても
、有機溶媒溢流せき８への結晶の付着はほとんどなく、
装置の連続運転には支障がなかった。Using an organic solvent consisting of 30v/v% D2EHPA [di(2-ethylhexyl) phosphoric acid] and 707% n-paraffin, 18.3 to 18.4 g of Fe3+ ions were extracted.
The organic solvent containing the organic solvent at a temperature of 21 to 23°C is
m/h into the mixing tank 5 of the apparatus of the invention shown in FIG. In this mixing tank 5, an organic solvent supply port 3
was located directly above the lower end of the downcomer pipe 11, and the stripping solution supply port 5 was located 185 cm above the organic solvent supply port 3. Plot, I (Ii2 is 118 to 130 g/cross,
) Continuous operation was performed while supplying an IF of 4 to 9 g/cm and a humidity of 5. As a result, even after 30 days had passed since the start of operation, almost no crystals were attached to the organic solvent overflow weir 8.
There was no problem with continuous operation of the device.
第１図は、従来装置の一例の線図的断面図、第２図およ
び第３ａ図は本発明の金属逆抽出装置の線図的断面図、
第３ｂ図は第３ａｌｌ！ＪのＸ−Ｙ線での断面図、第４
図および第５図は有機溶媒供給口３の形状の例を示す線
図的斜視図である。
符合の説明
ｌ・・・金属逆抽出装置本体、２用金属抽出有機溶奴、
３・・・有機溶媒供給口、４・・・剥離液（水相）。
５・・・剥離液供給口、６・・・混合槽、７・・・撹拌
装置。
８・・・有機溶媒静音区域、９・・・有機溶媒溢流せき
。
１０・・・有機溶媒排出口、ｌｌ・・・−ド降管、１２
・・・結晶成長ゾーン、１３・・・剥離液冷却ゾーン、
１４・・・熱交換器、１５−剥離液強制循環ゾーン、１
６・・・結晶分離ゾーン、１７・・・剥離液排出口、１
８・・・結晶排出管、１９・・・剥離液吹き出しノズル
特許出願人川崎製鉄株式会社
同 新技術開発事業団
株式会社西村渡辺抽出研究所
代理人 弁理士 渡 辺 望 稔□′
へ）
！、−８
、□゛
第１図FIG. 1 is a diagrammatic sectional view of an example of a conventional apparatus, FIGS. 2 and 3a are diagrammatic sectional views of a metal back-extraction apparatus of the present invention,
Figure 3b is the 3rd all! Cross-sectional view of J along the X-Y line, 4th
FIG. 5 and FIG. 5 are diagrammatic perspective views showing examples of the shape of the organic solvent supply port 3. Explanation of the code l...Metal back extraction device main body, metal extraction organic melt for 2,
3...Organic solvent supply port, 4...Removal liquid (aqueous phase). 5... Stripping liquid supply port, 6... Mixing tank, 7... Stirring device. 8...Organic solvent quiet area, 9...Organic solvent overflow weir. 10...Organic solvent outlet, ll...-downer tube, 12
...Crystal growth zone, 13... Stripping liquid cooling zone,
14... Heat exchanger, 15- Stripper liquid forced circulation zone, 1
6... Crystal separation zone, 17... Stripping liquid outlet, 1
8...Crystal discharge pipe, 19...Removal liquid blowout nozzle Patent applicant: Kawasaki Steel Corporation, New Technology Development Corporation, Nishimura Watanabe Extraction Research Institute, Patent attorney Nozomi Watanabe□')! , -8 , □゛Figure 1
Claims (1)
離液との混合槽の下方に、結晶成長ゾーンまたは剥離液
冷却ゾーンおよび結晶分離ゾーンを右し、結晶が金属イ
オンを抽出合奏する有機溶媒と加温された弗化物系剥離
液とを前記混合槽において混合接触させて金属イオンを
弗化物または弗化金属錯体として逆抽出させ、前記弗化
物または弗化金属錯体の結晶を前記結晶成長ゾーンまた
は剥離液冷却ゾーンにおいて成長させ、結晶分離ゾーン
において結晶を分離するよう構成された逆円錐系晶析装
置において、前記混合槽に配設されたド鋒管内に、有機
溶媒供給口を剥離液供給口よりも上部で前記ｒ降管下端
部よりも上部の位置に設け、これにより器壁への結晶の
付着を防止したことを特徴とする金属逆抽出装置。 物系剥離液との混合槽の下方に、結晶成長ゾーンまたは
剥離液冷却ゾーンおよび結晶分離ゾーンを有し、結晶が
金属イオンを抽出含有する有機溶媒と加温された弗化物
系剥離液とを前記混合槽において混合接触させて金属イ
オンを弗化物または弗化金属錯体として逆抽出させ、前
記弗化物または弗化金属錯体の結晶を前記結晶成長ゾー
ンまたは剥離液冷却ゾーンにおいて成長させ、結晶分離
ゾーンにおいて結晶を分離するよう構成された逆円錐系
晶析装置において、前記混合槽に配設されたド降管内に
、有機溶媒供給口を剥離液供給口よりもｔ゛部で前記下
降管Ｆ端部よりも上部の位置に設け、逆円錐形装置本体
下部に設けられ、外部の熱交換器と接続された冷却ゾー
ンを具え、この冷却ゾーン中に設けられ、その最Ｆ部に
剥離液に旋回流を起させるよう、はぼ接線方向に配向さ
れた少なくとも１個の吹き出しノズルを有する強制循環
ゾーンとを具え、これにより器壁への結晶の付着を防！
トシたことを特徴とする金属逆抽出装(1) A crystal growth zone or a stripping solution cooling zone and a crystal separation zone are placed below the mixing tank of an organic solvent containing an organic solvent containing metal ions and a fluoride stripping solution, and an organic A solvent and a heated fluoride-based stripping solution are mixed and contacted in the mixing tank to back-extract metal ions as a fluoride or metal fluoride complex, and the crystals of the fluoride or metal fluoride complex are grown as described above. In an inverted conical crystallizer configured to grow crystals in a cooling zone or a stripping liquid cooling zone and to separate crystals in a crystal separation zone, an organic solvent supply port is connected to a dowel tube disposed in the mixing tank to cool the stripping liquid. A metal back-extraction device, characterized in that it is provided above the supply port and above the lower end of the r downcomer tube, thereby preventing crystals from adhering to the vessel wall. Below the mixing tank with the physical stripping solution, there is a crystal growth zone or a stripping solution cooling zone and a crystal separation zone, in which the crystals extract metal ions from the organic solvent containing them and the heated fluoride stripping solution. Metal ions are back-extracted as a fluoride or metal fluoride complex by mixing and contacting in the mixing tank, crystals of the fluoride or metal fluoride complex are grown in the crystal growth zone or stripping liquid cooling zone, and a crystal separation zone is formed. In an inverted conical crystallizer configured to separate crystals in a downcomer pipe arranged in the mixing tank, an organic solvent supply port is connected to an F end of the downcomer pipe at a part t' from a stripping solution supply port. A cooling zone is provided in the lower part of the inverted conical device body and connected to an external heat exchanger. A forced circulation zone with at least one blowing nozzle oriented tangentially to create a flow, thereby preventing crystals from adhering to the vessel walls.
Metal reverse extraction equipment featuring a unique feature
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59094070A JPS60238427A (en) | 1984-05-11 | 1984-05-11 | Reverse extraction apparatus of metal |
| DE8585302030T DE3569201D1 (en) | 1984-03-30 | 1985-03-25 | Crystallization apparatus for metal stripping |
| EP85302030A EP0157562B1 (en) | 1984-03-30 | 1985-03-25 | Crystallization apparatus for metal stripping |
| CA000477477A CA1255073A (en) | 1984-03-30 | 1985-03-26 | Crystallization apparatus for metal stripping |
| KR1019850002120A KR890000166B1 (en) | 1984-03-30 | 1985-03-29 | Crystal Precipitator for Metal Stripping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59094070A JPS60238427A (en) | 1984-05-11 | 1984-05-11 | Reverse extraction apparatus of metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60238427A true JPS60238427A (en) | 1985-11-27 |
| JPH0121209B2 JPH0121209B2 (en) | 1989-04-20 |
Family
ID=14100240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59094070A Granted JPS60238427A (en) | 1984-03-30 | 1984-05-11 | Reverse extraction apparatus of metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60238427A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001058102A (en) * | 1999-08-23 | 2001-03-06 | Nishihara Environ Sanit Res Corp | Fluidized bed crystallization reactor |
| JPWO2004067139A1 (en) * | 2003-01-31 | 2006-05-18 | 株式会社荏原製作所 | Method and apparatus for removing ions in liquid by crystallization method |
| CN110280041A (en) * | 2019-07-01 | 2019-09-27 | 苏州乔发环保科技股份有限公司 | A kind of thickener |
-
1984
- 1984-05-11 JP JP59094070A patent/JPS60238427A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001058102A (en) * | 1999-08-23 | 2001-03-06 | Nishihara Environ Sanit Res Corp | Fluidized bed crystallization reactor |
| JPWO2004067139A1 (en) * | 2003-01-31 | 2006-05-18 | 株式会社荏原製作所 | Method and apparatus for removing ions in liquid by crystallization method |
| JP4748584B2 (en) * | 2003-01-31 | 2011-08-17 | 水ｉｎｇ株式会社 | Method and apparatus for removing ions in liquid by crystallization method |
| CN110280041A (en) * | 2019-07-01 | 2019-09-27 | 苏州乔发环保科技股份有限公司 | A kind of thickener |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0121209B2 (en) | 1989-04-20 |
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