US20040136889A1 - Method for increasing the dry residue in processed cyclone dust - Google Patents

Method for increasing the dry residue in processed cyclone dust Download PDF

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Publication number
US20040136889A1
US20040136889A1 US10/467,905 US46790503A US2004136889A1 US 20040136889 A1 US20040136889 A1 US 20040136889A1 US 46790503 A US46790503 A US 46790503A US 2004136889 A1 US2004136889 A1 US 2004136889A1
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US
United States
Prior art keywords
flocculant
cyclone dust
sludge
value
flocculation
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.)
Abandoned
Application number
US10/467,905
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English (en)
Inventor
Hans-Jorg Bonath
Georg Bombeck
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Kronos International Inc
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Individual
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Assigned to KRONOS INTERNATIONAL INC. reassignment KRONOS INTERNATIONAL INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BOMBECK, GEORG, BONATH, HANS-JORG
Publication of US20040136889A1 publication Critical patent/US20040136889A1/en
Abandoned legal-status Critical Current

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    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
    • A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
    • C22B34/1222—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes using a halogen containing agent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/02—Working-up flue dust
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/40—Inorganic substances
    • A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
    • 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

Definitions

  • the invention relates to a method for processing, in a manner suitable for landfilling, heavy-metal chlorides obtained in the form of cyclone dust during the manufacture of titanium dioxide by the chloride process, where insoluble constituents are first separated from the cyclone dust slurried with water or acids, after which the pH value of the solution is raised to a pH ranging from 9 to 12 by adding a neutralising agent, the heavy metals are precipitated in the form of hydroxides, and the hydroxides are thickened in the form of sludge and further dewatered.
  • a method of this kind is known from DE 41 31 577 A1, which describes that the (heavy) metal chlorides—except iron chloride—inevitably occurring during the manufacture of titanium dioxide by the chloride process have to be converted into products suitable for landfilling and that a filter cake suitable for landfilling is obtained if the inert constituents also contained in the cyclone dust are not separated prior to neutralisation of the dust, thereby accepting that the volume for landfilling becomes substantially larger and the re-usable, inert components of the cyclone dust are dispensed with.
  • the object of the invention is a method for the economical, industrial-scale reprocessing of heavy-metal chlorides occurring during the chlorination of titanium ore; in particular, a product suitable for landfilling with a dry residue of more than 40% is to be obtained from the cyclone dust following separation of the inert constituents, regardless of the raw material used.
  • the object is solved in that a readily filterable floccule is produced in the course of the process, this being achieved by one—or preferably a combination—of the following process improvements: Rapid, homogeneous pre-neutralisation to a pH value in the range from 6 to 9 is carried out prior to adjusting the pH value to between 9 and 12 in the neutralisation stage.
  • a (preferably anionic) flocculant is mixed into the suspension containing the precipitated heavy-metal hydroxides prior to thickening.
  • a (preferably cationic) flocculant is mixed into the thickened sludge.
  • the invention is illustrated in the drawing, and an example is described in further detail below.
  • the Figure shows a diagram of the process for reprocessing cyclone dust.
  • the volatile metal chlorides ( 1 ) formed in the chlorinator are cooled to such an extent that, apart from titanium tetrachloride, they are all separated in a cyclone ( 2 ) in condensed form along with the inert constituents—mainly unreacted ore and coke particles.
  • the titanium tetrachloride ( 3 ) which is still gaseous at this temperature, is subsequently condensed (not shown here) and the remaining chlorinator off-gases are passed to a gas scrubber.
  • the solids mixture separated in the cyclone is referred to as cyclone dust ( 4 ).
  • the Figure outlines a method according to the invention, by which none of the heavy metals present in the solution ( 10 ) are to be selectively recovered; all heavy-metal ions are to be landfilled as unserviceable material. They are converted into metal hydroxides by neutralisation. It would be perfectly possible to selectively separate individual ions or ion groups (such as iron or vanadium) at this point and subject them to reprocessing. Process steps of this kind, which are familiar in themselves, do not disrupt or alter the method according to the invention and will therefore not be discussed further.
  • Rapid pre-neutralisation is performed in a stirred ( 11 ), small pre-mixing tank ( 12 ), this achieving a rapid and, above all, spatially and temporally uniform rise in the pH value, thereby ensuring that, even in the event of fluctuations in the operating cycle, no partial volumes occur in which nucleation and flocculation are spatially and temporally sub-optimum.
  • the pH value increases to between 6 and 9 during pre-neutralisation.
  • a second (larger) neutralisation tank ( 13 ) is provided for stabilisation and precision adjustment; the suspension ( 14 ) discharged from there has a uniform pH value of between 9 and 12, preferably in the region of 10. Neutralisation is preferably performed using milk of lime ( 15 ) from a tank ( 16 ).
  • a pH value controller ( 17 ) is indicated.
  • Sludge ( 19 ) settles from the suspension ( 14 ) in a thickener ( 18 ) and is conveyed to a filter press ( 21 ) by a pump ( 20 ), via a tank ( 24 ) and a pump ( 25 ).
  • a first flocculant ( 22 ), preferably an anionic flocculant, can be added upstream of the settling tank ( 18 ).
  • the anionic flocculants open to consideration include, for example, copolymers of acrylamide and sodium acrylate, the preferred quantity being in the range from 5 to 30 ppm, referred to the total quantity of suspension.
  • a second flocculant ( 23 ), preferably a cationic flocculant, can be added after thickening ( 18 ).
  • the cationic flocculants open to consideration include, for example, cationic acrylamide copolymers, the preferred quantity being in the range from 5 to 30 ppm, referred to the quantity of thickened sludge.
  • dewatering which is preferably performed using a membrane filter press ( 21 ).
  • the filter pressure should be greater than 4 bar, preferably 10 to 15 bar. Repressing of the sludge is preferably performed at 10 to 15 bar.
  • the dry residue in the filter cake can be increased to more than 45%. This value is achieved regardless of the raw material used. It has been found with the methods presented that the use of both natural and synthetic rutile as the ore to be chlorinated yields a non-thixotropic filter cake suitable for landfilling. With ilmenite or with slag/rutile blends as the starting material, either with or without selective reprocessing of the iron chloride, the advantage lies solely in the high dry solids content of the filter cake obtained during the neutralisation and reprocessing of the metal chlorides.
  • the filter cake When neutralising the original suspension without separation of the inert constituents, the filter cake is non-thixotropic; the dry residue reaches 46.5% and the quantity to be landfilled is 1,115 kg per metric ton TiO 2 .
  • the filter cake is thixotropic (not suitable for landfilling); the dry residue reaches only 26.9% and the quantity to be landfilled is 1,270 kg per metric ton TiO 2 .
  • the method according to the invention produces a non-thixotropic filter cake with 45% dry residue.
  • the quantity to be landfilled is only 538 kg per metric ton TiO 2 .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Toxicology (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Management (AREA)
  • Business, Economics & Management (AREA)
  • Treatment Of Sludge (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
US10/467,905 2001-03-13 2002-03-08 Method for increasing the dry residue in processed cyclone dust Abandoned US20040136889A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE2001111895 DE10111895A1 (de) 2001-03-13 2001-03-13 Verfahren zur Erhöhung des Trockenrückstandes bei aufgearbeitetem Zyklonstaub
DE10111895.3 2001-03-13
PCT/DE2002/000844 WO2002072205A2 (de) 2001-03-13 2002-03-08 Verfahren zur erhöhung des trockenrückstandes bei nass aufgearbeitetem zyklonstaub der chlorierung von titanerz

Publications (1)

Publication Number Publication Date
US20040136889A1 true US20040136889A1 (en) 2004-07-15

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ID=7677194

Family Applications (1)

Application Number Title Priority Date Filing Date
US10/467,905 Abandoned US20040136889A1 (en) 2001-03-13 2002-03-08 Method for increasing the dry residue in processed cyclone dust

Country Status (8)

Country Link
US (1) US20040136889A1 (de)
EP (1) EP1368503A2 (de)
JP (1) JP2004528162A (de)
CA (1) CA2438311A1 (de)
DE (1) DE10111895A1 (de)
MX (1) MXPA03007247A (de)
TW (1) TWI243697B (de)
WO (1) WO2002072205A2 (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060231493A1 (en) * 2005-04-18 2006-10-19 Jan Procida Method of producing pure halide salts of alkaline and/or alkaline earth metal resulting from hydrolytic treatment of halogenous organic waste material
US20070187330A1 (en) * 2004-03-12 2007-08-16 Tony Whittaker Dewatering process
US20070264178A1 (en) * 2006-04-27 2007-11-15 Tronox Llc Waste solids handling
CN115427163A (zh) * 2020-06-16 2022-12-02 雅苒国际集团 用于从含磷酸组合物中去除重金属的方法
US12508636B2 (en) 2020-06-16 2025-12-30 Yara International Asa Method for treating solid hazardous heavy metal-containing compositions
US12545582B2 (en) 2020-06-16 2026-02-10 Yara International Asa Process for the removal of heavy metals from a phosphoric acid containing composition using a flocculating agent
US12545584B2 (en) 2020-06-16 2026-02-10 Yara International Asa Process for the removal of heavy metals from a phosphoric acid containing composition using an ionic polymeric surfactant and use of said surfactant in the precipitation of heavy metals in a phosphoric acid containing composition

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2258752C2 (ru) * 2003-11-04 2005-08-20 ООО Научно-производственная экологическая фирма "ЭКО-технология" Способ комплексной переработки металлургических отходов
JP4811728B2 (ja) * 2006-11-02 2011-11-09 清水建設株式会社 スラリー脱水処理方法および装置、ならびに懸濁液処理システム
DE102011106864B4 (de) * 2011-06-28 2013-06-20 Kronos International, Inc. Verfahren zur selektiven Abtrennung von Vanadium aus Rückständen der Titandioxidherstellung (Chloridverfahren)
JP2016510255A (ja) * 2013-01-07 2016-04-07 サハトレーベン・ヒェミー・ゲーエムベーハー チタン含有骨材、その製造方法及びその使用
AU2017268041B2 (en) * 2016-05-19 2021-11-04 Iluka Resources Limited Agglomeration of fines of titanium bearing materials
CN108569797A (zh) * 2017-03-07 2018-09-25 夏燕 一种处理磷矿废水的装置

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3655344A (en) * 1969-09-02 1972-04-11 Ppg Industries Inc Treatment of titanium tetrachloride drier residue
US4889697A (en) * 1987-12-10 1989-12-26 Nkk Corporation Method of refining ferrous ion-containing acid solution
US5238579A (en) * 1990-09-12 1993-08-24 Falconbridge Limited Method for generating coarse precipitates from solutions or slurries containing ionic species
US5271910A (en) * 1989-03-30 1993-12-21 Shell Internationale Research Maatschappij B.V. Process of treating metal chloride wastes
US5282977A (en) * 1991-10-01 1994-02-01 Kronos, Inc. Separation of heavy metals from waste water of the titanium dioxide industry
US5334362A (en) * 1991-09-23 1994-08-02 Kronos, Inc. Process for the production of disposable products from metal chlorides in a titanium dioxide chloride process
US5393510A (en) * 1992-07-22 1995-02-28 Rheox, Inc. High solids content titanium dioxide suspension
US5882513A (en) * 1993-05-25 1999-03-16 Stevenson; Sanford M. Apparatus for removing metal compounds from waste water
US5976383A (en) * 1991-04-08 1999-11-02 Romar Technologies, Inc. Recycle process for removing dissolved heavy metals from water with aluminum particles
US6800260B2 (en) * 2002-02-11 2004-10-05 Millennium Inorganic Chemicals, Inc. Processes for treating iron-containing waste streams

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RO81184A2 (ro) * 1980-10-24 1983-02-01 Institutul De Cercetari Si Proiectari Pentru Epurarea Apelor Reziduale,Ro Procedeu de recuperare a zincului din apele reziduale
DE3305802A1 (de) * 1983-02-19 1984-08-23 Philipp Müller, Nachf. Eugen Bucher GmbH & Co., 7000 Stuttgart Abwasseraufbereitungsverfahren
DE4321168A1 (de) * 1992-07-22 1994-01-27 Kronos Titan Gmbh Verfahren zur Herstellung einer Titandioxidsuspension mit einem hohen Feststoffgehalt

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3655344A (en) * 1969-09-02 1972-04-11 Ppg Industries Inc Treatment of titanium tetrachloride drier residue
US4889697A (en) * 1987-12-10 1989-12-26 Nkk Corporation Method of refining ferrous ion-containing acid solution
US5271910A (en) * 1989-03-30 1993-12-21 Shell Internationale Research Maatschappij B.V. Process of treating metal chloride wastes
US5238579A (en) * 1990-09-12 1993-08-24 Falconbridge Limited Method for generating coarse precipitates from solutions or slurries containing ionic species
US5976383A (en) * 1991-04-08 1999-11-02 Romar Technologies, Inc. Recycle process for removing dissolved heavy metals from water with aluminum particles
US5334362A (en) * 1991-09-23 1994-08-02 Kronos, Inc. Process for the production of disposable products from metal chlorides in a titanium dioxide chloride process
US5282977A (en) * 1991-10-01 1994-02-01 Kronos, Inc. Separation of heavy metals from waste water of the titanium dioxide industry
US5393510A (en) * 1992-07-22 1995-02-28 Rheox, Inc. High solids content titanium dioxide suspension
US5882513A (en) * 1993-05-25 1999-03-16 Stevenson; Sanford M. Apparatus for removing metal compounds from waste water
US6800260B2 (en) * 2002-02-11 2004-10-05 Millennium Inorganic Chemicals, Inc. Processes for treating iron-containing waste streams

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7754086B2 (en) 2004-03-12 2010-07-13 Ciba Specialty Chemicals Water Treatments Ltd. Dewatering process
US20070187330A1 (en) * 2004-03-12 2007-08-16 Tony Whittaker Dewatering process
US20060231493A1 (en) * 2005-04-18 2006-10-19 Jan Procida Method of producing pure halide salts of alkaline and/or alkaline earth metal resulting from hydrolytic treatment of halogenous organic waste material
US7645386B2 (en) 2005-04-18 2010-01-12 Jan Procida Method of producing pure halide salts of alkaline and/or alkaline earth metal resulting from hydrolytic treatment of halogenous organic waste material
AU2007243591B2 (en) * 2006-04-27 2011-09-15 Tronox Llc Processing of waste or cyclone solids from the chlorination of titanium bearing ores
US7943103B2 (en) * 2006-04-27 2011-05-17 Tronox Llc Waste solids handling
US20070264178A1 (en) * 2006-04-27 2007-11-15 Tronox Llc Waste solids handling
AU2007243591C1 (en) * 2006-04-27 2012-02-23 Tronox Llc Processing of waste or cyclone solids from the chlorination of titanium bearing ores
CN115427163A (zh) * 2020-06-16 2022-12-02 雅苒国际集团 用于从含磷酸组合物中去除重金属的方法
US12508636B2 (en) 2020-06-16 2025-12-30 Yara International Asa Method for treating solid hazardous heavy metal-containing compositions
US12545582B2 (en) 2020-06-16 2026-02-10 Yara International Asa Process for the removal of heavy metals from a phosphoric acid containing composition using a flocculating agent
US12545583B2 (en) 2020-06-16 2026-02-10 Yara International Asa Process for the removal of heavy metals from a phosphoric acid containing composition
US12545584B2 (en) 2020-06-16 2026-02-10 Yara International Asa Process for the removal of heavy metals from a phosphoric acid containing composition using an ionic polymeric surfactant and use of said surfactant in the precipitation of heavy metals in a phosphoric acid containing composition

Also Published As

Publication number Publication date
CA2438311A1 (en) 2002-09-19
WO2002072205A2 (de) 2002-09-19
EP1368503A2 (de) 2003-12-10
MXPA03007247A (es) 2003-12-04
DE10111895A1 (de) 2002-09-19
JP2004528162A (ja) 2004-09-16
WO2002072205A3 (de) 2003-04-17
TWI243697B (en) 2005-11-21

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AS Assignment

Owner name: KRONOS INTERNATIONAL INC., GERMANY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:BONATH, HANS-JORG;BOMBECK, GEORG;REEL/FRAME:014153/0407

Effective date: 20030826

STCB Information on status: application discontinuation

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