EP0203076B1 - Separation et recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique - Google Patents

Separation et recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique Download PDF

Info

Publication number
EP0203076B1
EP0203076B1 EP85903006A EP85903006A EP0203076B1 EP 0203076 B1 EP0203076 B1 EP 0203076B1 EP 85903006 A EP85903006 A EP 85903006A EP 85903006 A EP85903006 A EP 85903006A EP 0203076 B1 EP0203076 B1 EP 0203076B1
Authority
EP
European Patent Office
Prior art keywords
solid
recovery
liquid
flotation
suspension
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.)
Expired
Application number
EP85903006A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0203076A1 (fr
Inventor
Marc 20 Route De Dhuilet Lebon
Michèle PREVOST
El Aid Jdid
Pierre Blazy
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Uranium Pechiney
Original Assignee
Institut de Recherches Chimiques et Biologiques Appliquees SARL IRCEBA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Institut de Recherches Chimiques et Biologiques Appliquees SARL IRCEBA filed Critical Institut de Recherches Chimiques et Biologiques Appliquees SARL IRCEBA
Publication of EP0203076A1 publication Critical patent/EP0203076A1/fr
Application granted granted Critical
Publication of EP0203076B1 publication Critical patent/EP0203076B1/fr
Expired legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/14Flotation machines
    • B03D1/1443Feed or discharge mechanisms for flotation tanks
    • B03D1/1475Flotation tanks having means for discharging the pulp, e.g. as a bleed stream
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/14Flotation machines
    • B03D1/24Pneumatic
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00Liquid purification or separation
    • Y10S210/902Materials removed
    • Y10S210/911Cumulative poison
    • Y10S210/912Heavy metal

Definitions

  • Ion flotation is a known technique aimed at eliminating certain ions, in particular metal cations, from a solution containing them.
  • This technique consists in introducing into the solution to be treated, a surfactant, called a collector, the role of which is to complex and insolubilize the ion which one wishes to separate and to entrain, within this liquid, in an upward movement, said complex on the surface of this liquid and to recover it on this surface.
  • the Applicant has unexpectedly found that by subjecting a fraction of the liquid to be treated containing the solid to be recovered to a process consisting in admitting this fraction in a device adapted to lower its pressure, in contacting the resulting flow with a gas admitted into this stream at very high speed and at low incidence, to cause the two fluids to converge under expansion conditions to produce a fine emulsion and to resume said emulsion by raising the pressure while maintaining the resulting pressure at a lower level to that corresponding to the initial pressure of the admitted liquid, and to inject said emulsion into a volume of the liquid to be treated, there was obtained on the surface of this volume, and in a quiet zone, an accumulation of the desired solid practically free of the liquid phase initial.
  • liquid to be treated is meant any suspension of the "collector-ion" precipitate in the liquid phase.
  • the Applicant has found that the system applies particularly well when the liquid to be treated is a concentrated solution of a mineral acid such as for example phosphoric acid; the yield expressed as a percentage of the quantity of solid separated in a single operation appears to be at least 90% in the case of the phosphoric medium.
  • a mineral acid such as for example phosphoric acid
  • the invention provides a recycling circuit in the system allowing total recovery of the desired solid.
  • a pre-treatment tank for the solution to be treated, this pre-treatment consisting in introducing into it a surfactant (collector) so as to form a suspension, this medium being maintained under stirring by means of an agitator 2 of any known type, and in 5 a flotation cell supplied with this suspension by any suitable means.
  • a surfactant collector
  • This cell is then made to pass through a non-turbulent rising current intended to convey the solid towards the surface of the suspension, this current being obtained in the following way: by means of a pump 3, the medium coming from the tank 1 in an apparatus 4 of the type which is the subject, for example, of French patent 2,484,862 and comprising from upstream to downstream, a converging conduit for supplying said medium, a gas injection stage produced so that this gas be admitted at very high speed under a relatively low incidence; this injection stage is immediately followed by an expansion stage constituted by an enclosure whose walls are non-convergent which opens into a clearly divergent zone in communication, possibly, with an enclosure for recovering and / or recycling the gas.
  • the device 4 is shown placed at the base of the cell 5.
  • the liquid medium is returned, by line 8, to the device 4 by the circuit designated by the references 9-10-11 , possibly using a pump 3a.
  • the liquid medium is recovered in the recovery tank 12.
  • the method and the device according to the invention are particularly advantageous for the recovery of elements such as uranium, zirconium, cadmium, arsenic, rare earths, etc., contained in wet phosphoric acid with minimum entrainment of said acid .
  • the method and the device according to the invention can be applied to a flotation cell of the type described in French patent 2,354,820 previously cited.
  • a flotation cell of the type described in French patent 2,354,820 previously cited.
  • Such a cell in which the original gas ejector is replaced by a device according to the invention can then operate under clearly different and more economical conditions than those for which it is designed.
  • the test is carried out on 2 liters of industrial wet phosphoric acid containing 75 mg / I of Cd.
  • the acid purification rate is greater than 99% (residual Cd 0.4 mg / I).
  • the precipitate, collector-cation, thus obtained is separated from the acid in a laboratory flotation cell fitted with a rotor and a stator in a squirrel cage. This cell makes it possible to float the precipitate but the entrainments of solution in the foams are significant (greater than 30%).
  • the percentage of cadmium removed from the acid by the implementation of the ion flotation process is thus greater than 90% for one passage and 98-99% after 5 minutes of recycling.
  • the collector used for uranium is a suitable dialkyl diphosphonic compound specific for the U +4 ion .
  • the precipitation is carried out as in Example 1 by carrying out a pre-reduction of the uranium (before the introduction of the collector into the acid).
  • Example 2 The conditions of flotation of the precipitate are the same as in Example 2 with an R ratio equal to 4.2.
  • the effectiveness of the device for the flotation of the precipitate is also excellent, of the order of 90% after one pass and 98% after recycling the acid solution for 5 minutes.
  • the uranium content eliminated by this implementation of the process is thus greater than 85% after one pass and equal to 95% after 5 minutes of recycling.
  • the acid treated is a wet industrial phosphoric acid containing 30% P 2 O 5 and containing approximately 40 mg / I in Cd and 115 mg / I in uranium.
  • the flotation equipment used is commercial pilot equipment (WEMCO Depurator type) with four in-line cells of approximately 30 liters each; the device (4) of the appended figure is then positioned vertically above the liquid phase loaded with solid circulating in the cell, the outlet of the device being located below the surface of the liquid; the tests were carried out with only two of the cells. These two cells were equipped with the device according to the invention to replace the original ejector.
  • WEMCO Depurator type commercial pilot equipment
  • the entrainment of acid in the floated precipitate is low, of the order of 5%.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Physical Water Treatments (AREA)
EP85903006A 1984-11-30 1985-06-19 Separation et recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique Expired EP0203076B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8418301 1984-11-30
FR8418301A FR2574002B1 (fr) 1984-11-30 1984-11-30 Perfectionnement apporte a la separation et a la recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique, et moyen pour la mise en oeuvre de ce perfectionnement

Publications (2)

Publication Number Publication Date
EP0203076A1 EP0203076A1 (fr) 1986-12-03
EP0203076B1 true EP0203076B1 (fr) 1989-08-30

Family

ID=9310119

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85903006A Expired EP0203076B1 (fr) 1984-11-30 1985-06-19 Separation et recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique

Country Status (8)

Country Link
US (1) US4844873A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
EP (1) EP0203076B1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
JP (1) JPS62500918A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
DE (1) DE3572604D1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
FR (1) FR2574002B1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
MA (1) MA20458A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
OA (1) OA08372A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
WO (1) WO1986003142A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3801905A1 (de) * 1988-01-23 1989-08-03 Allmineral Aufbereitungstech Pneumatische flotationszelle
US5281339A (en) * 1989-06-08 1994-01-25 Ici Australia Operations Proprietary Limited Removal of contaminants
US5320759A (en) * 1992-06-11 1994-06-14 Hazen Research, Inc. Selective recovery of heavy metals using xanthates
US5244492A (en) * 1992-06-26 1993-09-14 Ppg Industries, Inc. Process for recovery of metallic mercury from contaminated mercury-containing soil
US5820752A (en) * 1995-08-10 1998-10-13 Prestone Products Corporation Methods and apparatus for recycling used antifreeze/coolant
US6890431B1 (en) * 2000-02-18 2005-05-10 The F. B. Leopold Co., Inc. Buoyant media flotation
US6398968B1 (en) * 2000-02-25 2002-06-04 Watermark Technologies, Llc Methods for pressure stabilized removal of contaminants from solution
US6562241B1 (en) * 2000-11-10 2003-05-13 Watermark Technologies, Llc Methods for negative atmospheric pressure removal of arsenic and other metals
DE202010009140U1 (de) 2010-06-16 2010-10-21 Juan Valdivia Gmbh Anordnung zur Erzeugung von Luftblasen in Flüssigkeiten
FR3146604A1 (fr) * 2023-03-16 2024-09-20 Universite Mohammed VI Polytechnique Procédé de traitement de l’acide phosphorique par flottation ionique

Family Cites Families (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE342528C (de) * 1920-10-27 1921-10-19 Walter Ortmann Haekelschiffchen
US2793185A (en) * 1952-12-17 1957-05-21 Albrektsson John Oscar Georg Method and apparatus for introduction of gas into water to be treated by flotation
US3117082A (en) * 1958-08-21 1964-01-07 Pfaudler Permutit Inc Flotation system
US3179252A (en) * 1961-01-06 1965-04-20 Eimco Corp Apparatus for flotation
US3243046A (en) * 1962-12-01 1966-03-29 Ebara Infilco Floatation apparatus
US4160737A (en) * 1973-12-22 1979-07-10 Pielkenrood-Vinitex B.V. Flotation and plate separation device
US3966598A (en) * 1975-02-24 1976-06-29 Tenco Hydro/Aerosciences, Inc. Circular dissolved gas flotation system
JPS52116643A (en) * 1976-03-26 1977-09-30 Stanley Electric Co Ltd Process for producing pressure water generating fine foam
AT342528B (de) * 1976-09-01 1978-04-10 Envirotech Corp Flotationsverfahren
US4094783A (en) * 1977-09-29 1978-06-13 Jackson George F Centrifugal flotation separator
EP0004953B1 (de) * 1978-04-19 1982-03-03 Klaus Prof. Dr. Heckmann Verfahren und Vorrichtung zur selektiven Trennung des Urans von seinen Begleitmetallen und zu seiner Gewinnung
WO1980000423A1 (en) * 1978-08-21 1980-03-20 Feldmuehle Ag Method and device for cleaning suspension fibres
US4263148A (en) * 1979-04-09 1981-04-21 Earth Sciences, Inc. Process for removing humic matter from phosphoric acid solutions
DE3008476A1 (de) * 1980-03-05 1981-09-17 Bayer Ag, 5090 Leverkusen Verfahren zur flotation und verwendung von trichterduesen zur flotation
DE3011844A1 (de) * 1980-03-27 1981-10-01 Röhm GmbH, 6100 Darmstadt Verfahren und vorrichtung zur umwandlung und trennung von in einer traegerfluessigkeit enthaltenden oder eingebrachten geloesten bzw. loesbaren substanzen
EP0037513B1 (de) * 1980-04-09 1984-08-08 Feldmühle Aktiengesellschaft Flotationsvorrichtung zum Deinken von Faserstoffsuspensionen
FR2484862B1 (fr) * 1980-06-18 1984-09-14 Inst Nat Rech Chimique Procede et dispositif pour le transfert de gaz dans un liquide applicable en particulier au traitement des eaux, en biotechnologie et dans l'industrie chimique
DE3163266D1 (en) * 1981-02-26 1984-05-30 Agfa Gevaert Ag Flotation process for the continuous recovery of silver or silver compounds from solutions or dispersions
FR2530161A1 (fr) * 1982-07-16 1984-01-20 Inst Mondial Phosphate Perfectionnements apportes aux procedes de separation de metaux contenus dans des milieux hyperacides, par flottation ionique
FR2557090B1 (fr) * 1983-12-23 1986-04-11 Pechiney Uranium Procede de purification de l'acide phosphorique de voie humide par elimination du cadmium

Also Published As

Publication number Publication date
FR2574002B1 (fr) 1987-02-27
MA20458A1 (fr) 1985-12-31
JPS62500918A (ja) 1987-04-16
FR2574002A1 (fr) 1986-06-06
WO1986003142A1 (fr) 1986-06-05
EP0203076A1 (fr) 1986-12-03
OA08372A (fr) 1988-02-29
JPH0242545B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1990-09-25
US4844873A (en) 1989-07-04
DE3572604D1 (en) 1989-10-05

Similar Documents

Publication Publication Date Title
EP0203076B1 (fr) Separation et recuperation de solides a partir de liquides les contenant et faisant appel au procede de flottation ionique
US6355175B1 (en) Method for separating and isolating precious metals from non precious metals dissolved in solutions
CN1027500C (zh) 从水处理流中去除有机溶剂的方法和设备
CN105130087A (zh) 一种去除水中重金属的纳米量子点吸附及膜分离系统
CN108128939A (zh) 一种用集成膜技术处理稀土冶炼高氨氮废水的方法及装置
CN200950804Y (zh) 洗梗机
CN110002692B (zh) 一种工业清洗废水的零排放处理工艺
EP0925824B1 (fr) Procédé de séparation de métaux par ultrafiltration micellaire, utilisable pour le traitement d'effluents radioactifs
EP0279735B1 (fr) Procédé pour l'exploitation minière des océans
EP0099804B1 (fr) Perfectionnements apportés aux procédés de séparation de métaux contenus dans des milieux hyperacides, par flottation ionique
Hano et al. Continuous extraction of penicillin G with liquid surfactant membrane using Vibro Mixer®
CN103523864A (zh) 工业废水的处理方法及装置
CN1021811C (zh) 处理含氰废水的活性炭催化氧化法
CN1037127A (zh) 岩石风化土吸附型稀散贵金属的提取技术方案
CN212425660U (zh) 一种海水资源化利用的装置
WO1996006677A1 (fr) Procede pour abaisser la teneur en cations multivalents de solutions aqueuses
Valsaraj et al. Nonfoaming adsorptive bubble separation processes
CN208762281U (zh) 一种用集成膜技术处理稀土冶炼高氨氮废水的装置
CN117534269B (zh) 重金属废水资源化方法
CN103496717B (zh) 一种序批式硫铵溶液氧化及硫磺浮渣脱除方法
RU2162114C2 (ru) Способ очистки галлия от примесей
BE1000938A3 (fr) Melangeur-decanteur tubulaire a plusieurs etages, destine a etre mis en oeuvre dans l'extraction liquide-liquide a contre-courant.
CN113582427B (zh) 废水磁悬浮离心处理方法
CN115650365A (zh) 一种氰化镀银废水回收回用方法
CA1083062A (fr) Procede de traitement de sables asphaltiques

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19860724

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): BE CH DE GB IT LI NL SE

RBV Designated contracting states (corrected)

Designated state(s): BE CH DE GB LI NL SE

17Q First examination report despatched

Effective date: 19880128

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): BE CH DE GB LI NL SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19890830

Ref country code: GB

Effective date: 19890830

REF Corresponds to:

Ref document number: 3572604

Country of ref document: DE

Date of ref document: 19891005

GBV Gb: ep patent (uk) treated as always having been void in accordance with gb section 77(7)/1977 [no translation filed]
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Effective date: 19900630

Ref country code: CH

Effective date: 19900630

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

NLS Nl: assignments of ep-patents

Owner name: URANIUM PECHINEY TE PARIJS, FRANKRIJK.

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19930513

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 19930526

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 19930630

Year of fee payment: 9

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Effective date: 19940630

BERE Be: lapsed

Owner name: URANIUM PECHINEY

Effective date: 19940630

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Effective date: 19950101

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Effective date: 19950301