EP1286780B1 - Mittel zur aufbereitung von phosphaterz - Google Patents
Mittel zur aufbereitung von phosphaterz Download PDFInfo
- Publication number
- EP1286780B1 EP1286780B1 EP01951475A EP01951475A EP1286780B1 EP 1286780 B1 EP1286780 B1 EP 1286780B1 EP 01951475 A EP01951475 A EP 01951475A EP 01951475 A EP01951475 A EP 01951475A EP 1286780 B1 EP1286780 B1 EP 1286780B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- flotation
- agent
- ethylene oxide
- flotation agent
- 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 - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/005—Dispersants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
Definitions
- the present invention relates to an improved flotation agent for Phosphate ore, which in addition to a fatty acid is a mixture of collectors includes ethoxylated alkylphenols.
- a dispersant such as, for example, a nonylphenol with 2-5 mol ethylene oxide (EO) and an aliphatic ethoxylated alcohol with the chain length C 11 -C 15 , which contains 2-4 moles of EO, is used.
- EO nonylphenol with 2-5 mol ethylene oxide
- a further improvement results if an alcohol with the chain length C 1 -C 15 is dissolved in the dispersant. This alcohol improves the emulsifiability of the dispersant.
- Another object of the invention is the use of a mixture of alkoxylated alkylphenols as described above as dispersants in the Flotation of phosphate ores.
- the Use with fatty acids as a collector is the use of a mixture of alkoxylated alkylphenols as described above as dispersants in the Flotation of phosphate ores.
- the Use with fatty acids as a collector is the use of a mixture of alkoxylated alkylphenols as described above as dispersants in the Flotation of phosphate ores.
- the dispersant preferably comprises 9 to 15, in particular 10 to 13% by weight of component a).
- the content of component b) results from the Difference to 100% by weight.
- the alkyl radicals are preferably linear or branched nonyl residues.
- ethylene oxide is between 2 and 4, in particular between 2.5 and 3.5 mol.
- the flotation agent according to the invention contains no alcohols.
- fatty acid which is the main component of the invention Flotation agent
- Flotation agent it is preferably a linear or branched monocarboxylic acid with 8 to 26 carbon atoms.
- Fatty acids known in the art can be used.
- the flotation agent according to the invention preferably contains between 1 and 30% by weight of the dispersant.
- the flotation agent according to the invention is preferably in amounts of 100 to 1,000 g / t solids for flotation of Phosphate ores used.
- the addition amount of the invention Dispersant with separate collector / dispersant metering preferably between 30 and 150 g / t, in particular between 40 and 60 g / t, based on the solids feed.
- the flotation agent according to the invention can, in addition to the above Ingredients fatty acid and dispersant, pusher or others from the Contain components known in the art. Such ingredients are for example foaming agents and aliphatic polyglycol ethers. You can also different pushers, e.g. Water glass, to be used separately.
- the flotation agent according to the invention is exemplified below:
- the reaction can be carried out in such a way that the phenol / nonene mixture is circulated over an acidic fixed bed catalyst.
- the following mixtures were obtained: Mole of phenol Moles of nons Proportion of dinonylphenol 1 0.9 9% by weight 1 1.0 11% by weight 1 1.1 13% by weight comparison 1 0.6 3% by weight
- the dosage can reduced from 81 g / t to 40 to 60 g / t compared to the reference product, without the concentrate quality or the yield deteriorating.
- composition of the raw ore apatite 22% by weight phlogopite 24% by weight calcite 25% by weight dolomite 3% by weight forsterite 7% by weight diopside 8% by weight
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Dental Preparations (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Paper (AREA)
- Materials For Medical Uses (AREA)
Description
- Phenol wird vorgelegt
- Zugabe 0,2 eq konz. Schwefelsäure
- Unter Rühren Zugabe von Nonen
- Innentemperatur steigt auf 30 bis 50°C, und es entwickelt sich Chlorwasserstoff
- Die Reaktion ist beendet, wenn die Chlorwasserstoffentwicklung aufhört
Mol Phenol | Mol Nonen | Anteil Dinonylphenol |
1 | 0,9 | 9 Gew.-% |
1 | 1,0 | 11 Gew.-% |
1 | 1,1 | 13 Gew.-% |
Vergleich | ||
1 | 0,6 | 3 Gew.-% |
- Nonylphenol in sauberen Kessel einfüllen.
- Rührer einschalten.
- Die angegebene Menge Natronlauge (als Katalysator) zugeben bzw. einsaugen.
- Kesselinhalt unter Rühren auf 85 - 90°C aufheizen, dann Vakuum anlegen.
- Vakuum mit Stickstoff aufheben und Kesselinhalt unter Rühren auf 140 - 145°C aufheizen.
- Bei dieser Temperatur Ethylenoxid zudosieren.
- Ethylenoxid bis zum Erreichen der berechneten Menge weiter zudosieren.
- Zur Ethylenoxid-Abreaktion ca. 1 Stunde bei einer Sumpftemperatur von 140 - 150°C nachrühren.
- Probe ziehen und OH-Zahl oder Trübungspunkt bestimmen und bis zum Gutbefund bei 140 - 150°C weiterrühren.
- Ist die Ziel-OH-Zahl bzw. Ziel-Trübungspunkt noch nicht erreicht, muss zum Kesselinhalt die berechnete Ethylenoxidmenge nachdosiert werden.
- Ist die Ziel-OH-Zahl erreicht, wird der Kesselinhalt abgekühlt auf 100 °C und unter Vakuum bei 100°C ausgegast.
- Es folgt die Neutralisation bei 50 - 70°C mit Essigsäure bis auf einen pH-Bereich von 6,0 - 8,0.
Ausgangsstoffe | ||
Rohstoff | Mol | Menge |
Nonyl-/Dinonylphenol | 1 | 231,3/233,9/236,4 kg |
Ethylenoxid | 3 | 132 kg |
NaOH (50 %ig) | 0,006 | 0,24 kg |
Essigsäure (techn. rein) | 0,006 | 0,36 kg |
erhaltene Substanzen | ||
Anteil Dinonylphenol | Molverhältnis Nonylphenol/Ethylenoxid | |
Beispiel 1 | 9 % | 1:3 |
2 | 11 % | 1:3 |
3 | 13 % | 1:3 |
Vergleich | 3 % | 1:4 |
Reagentien in g/t Feststoff | Aufgabe P2O5 in % | Konzentrat P2O5 in % | Ausbeute | ||
Fettsäure | Dispergiermittel | ||||
Vergleich | 430 | 81 | 7,2 | 38,1 | 89,8 |
Beispiel 1 | 430 | 65 | 6,2 | 38,5 | 87,2 |
Beispiel 2 | 430 | 54 | 6,0 | 38,1 | 89,8 |
Beispiel 3 | 430 | 43 | 5,7 | 37,7 | 92,4 |
Reagentien in g/t | Aufgabe P2O5 in % | Konzentrat P2O5 in % | Ausbeute | ||
Fettsäure | Dispergiermittel | ||||
Vergleich | 400 | 150 | 7,3 | 39,9 | 71,3 |
Beispiel 2 | 400 | 150 | 7,8 | 40,1 | 76,2 |
Beispiel 3 | 400 | 150 | 8,1 | 40,3 | 76,4 |
Apatit | 22 Gew.-% |
Phlogopit | 24 Gew.-% |
Calcit | 25 Gew.-% |
Dolomit | 3 Gew.-% |
Forsterit | 7 Gew.-% |
Diopsid | 8 Gew.-% |
Claims (7)
- Flotationsmittel für Phosphaterz, enthaltend eine Fettsäure als Sammler und alkoxylierte Alkylphenole als Dispergiermittel, dadurch gekennzeichnet, dass die Alkylphenole zusammengesetzt sind ausa) 8 bis 20 Gew.-% eines oder mehrerer Dialkylphenole mit Alkylresten von 8 bis 12 C-Atomenb) 80 bis 92 Gew.-% eines oder mehrerer Monoalkylphenole mit Alkylresten von 8 bis 12 C-Atomen,
- Flotationsmittel nach Anspruch 1, enthaltend Nonylphenolethoxilate als Dispergiermittel.
- Flotationsmittel nach Anspruch 1 und/oder 2, worin 9 bis 15 Gew.-% des Dispergiermittels aus einem oder mehreren Dialkylphenolethoxilaten bestehen.
- Flotationsmittel nach einem oder mehreren der Ansprüche 1 bis 3, worin der Ethylenoxidgehalt zwischen 2 und 4 mol liegt.
- Flotationsmittel nach einem oder mehreren der Ansprüche 1 bis 4, worin kein Alkohol enthalten ist.
- Verwendung eines Flotationsmittels gemäß den Ansprüchen 1 bis 5 in Mengen von 100 bis 1.000 g/t zur Flotation von Phosphaterz.
- Verwendung eines Dispergiermittels wie in den Ansprüchen 1 bis 5 definiert für die Phosphatflotation.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10024667 | 2000-05-18 | ||
DE10024667A DE10024667C2 (de) | 2000-05-18 | 2000-05-18 | Mittel zur Aufbereitung von Phosphaterz |
PCT/EP2001/004964 WO2001087490A1 (de) | 2000-05-18 | 2001-05-03 | Mittel zur aufbereitung von phosphaterz |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1286780A1 EP1286780A1 (de) | 2003-03-05 |
EP1286780B1 true EP1286780B1 (de) | 2004-08-04 |
Family
ID=7642710
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01951475A Expired - Lifetime EP1286780B1 (de) | 2000-05-18 | 2001-05-03 | Mittel zur aufbereitung von phosphaterz |
Country Status (10)
Country | Link |
---|---|
US (1) | US6712217B2 (de) |
EP (1) | EP1286780B1 (de) |
AT (1) | ATE272447T1 (de) |
AU (1) | AU7239001A (de) |
BR (1) | BR0110820A (de) |
DE (2) | DE10024667C2 (de) |
ES (1) | ES2225579T3 (de) |
MX (1) | MXPA02011316A (de) |
WO (1) | WO2001087490A1 (de) |
ZA (1) | ZA200208449B (de) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6799682B1 (en) | 2000-05-16 | 2004-10-05 | Roe-Hoan Yoon | Method of increasing flotation rate |
DE10024667C2 (de) | 2000-05-18 | 2002-02-28 | Clariant Gmbh | Mittel zur Aufbereitung von Phosphaterz |
CA2597176C (en) | 2005-02-04 | 2013-10-22 | Mineral And Coal Technologies, Inc. | Improving the separation of diamond from gangue minerals |
CN103265409B (zh) * | 2013-05-31 | 2016-05-11 | 滁州市润达溶剂有限公司 | 一种壬基酚的精制方法 |
CN103920596B (zh) * | 2014-04-25 | 2017-02-15 | 中蓝连海设计研究院 | 一种胶磷矿组合浮选捕收剂及其制法与用途 |
CN104307640B (zh) * | 2014-11-07 | 2016-08-17 | 中蓝连海设计研究院 | 一种磷矿反浮选方解石的捕收剂 |
CN107511268A (zh) * | 2017-09-08 | 2017-12-26 | 湖北富邦科技股份有限公司 | 一种制备高强捕收能力的磷矿石浮选药剂的方法 |
CN113600344B (zh) * | 2021-07-21 | 2022-12-02 | 宜都兴发化工有限公司 | 一种中间分级再处理的胶磷矿脱除倍半氧化物选矿工艺 |
US20230091787A1 (en) * | 2021-09-09 | 2023-03-23 | Clariant International, Ltd. | Composition And Method For Use Of 1-Alkyl-5-Oxopyrrolidine-3-Carboxylic Acids As Collectors For Phosphate And Lithium Flotation |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4110207A (en) * | 1976-01-05 | 1978-08-29 | American Cyanamid Company | Process for flotation of non-sulfide ores |
FR2366067A1 (fr) | 1976-09-29 | 1978-04-28 | Chem Y | Procede de flottation de minerais utilisant des esters d'acides dicarboxyliques comme constituants du collecteur |
US4200522A (en) * | 1976-09-29 | 1980-04-29 | Chem-Y, Fabriek Van Chemische Produkten B.V. | Process for the flotation of ores |
US4309282A (en) * | 1980-04-14 | 1982-01-05 | American Cyanamid Company | Process of phosphate ore beneficiation in the presence of residual organic polymeric flocculants |
US4690752A (en) * | 1983-08-19 | 1987-09-01 | Resource Technology Associates | Selective flocculation process for the recovery of phosphate |
IL80331A (en) * | 1985-10-25 | 1989-07-31 | Sentrachem Ltd | Recovering phosphate values by froth flotation |
DE4030160A1 (de) | 1990-09-24 | 1992-03-26 | Henkel Kgaa | Verfahren zur gewinnung von mineralien aus nichtsulfidischen erzen durch flotation |
DE4127151C2 (de) * | 1991-08-16 | 1996-08-29 | Hoechst Ag | Verfahren zur selektiven Flotation von Phosphormineralen |
US5962828A (en) * | 1997-10-15 | 1999-10-05 | Custom Chemicals Corporation | Enhanced flotation reagents for beneficiation of phosphate ores |
DE10024667C2 (de) | 2000-05-18 | 2002-02-28 | Clariant Gmbh | Mittel zur Aufbereitung von Phosphaterz |
-
2000
- 2000-05-18 DE DE10024667A patent/DE10024667C2/de not_active Expired - Fee Related
-
2001
- 2001-05-03 BR BR0110820-4A patent/BR0110820A/pt not_active Application Discontinuation
- 2001-05-03 AU AU72390/01A patent/AU7239001A/en not_active Abandoned
- 2001-05-03 WO PCT/EP2001/004964 patent/WO2001087490A1/de active IP Right Grant
- 2001-05-03 DE DE50103125T patent/DE50103125D1/de not_active Expired - Lifetime
- 2001-05-03 US US10/276,211 patent/US6712217B2/en not_active Expired - Fee Related
- 2001-05-03 AT AT01951475T patent/ATE272447T1/de active
- 2001-05-03 MX MXPA02011316A patent/MXPA02011316A/es active IP Right Grant
- 2001-05-03 EP EP01951475A patent/EP1286780B1/de not_active Expired - Lifetime
- 2001-05-03 ES ES01951475T patent/ES2225579T3/es not_active Expired - Lifetime
-
2002
- 2002-10-18 ZA ZA200208449A patent/ZA200208449B/en unknown
Also Published As
Publication number | Publication date |
---|---|
ATE272447T1 (de) | 2004-08-15 |
US20030146136A1 (en) | 2003-08-07 |
US6712217B2 (en) | 2004-03-30 |
MXPA02011316A (es) | 2004-09-06 |
DE10024667A1 (de) | 2001-11-29 |
ES2225579T3 (es) | 2005-03-16 |
AU7239001A (en) | 2001-11-26 |
EP1286780A1 (de) | 2003-03-05 |
DE50103125D1 (de) | 2004-09-09 |
BR0110820A (pt) | 2003-02-11 |
DE10024667C2 (de) | 2002-02-28 |
ZA200208449B (en) | 2003-05-12 |
WO2001087490A1 (de) | 2001-11-22 |
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