AU2013254846A1 - Magnetic separation of particles including one-step-conditioning of a pulp - Google Patents
Magnetic separation of particles including one-step-conditioning of a pulp Download PDFInfo
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- AU2013254846A1 AU2013254846A1 AU2013254846A AU2013254846A AU2013254846A1 AU 2013254846 A1 AU2013254846 A1 AU 2013254846A1 AU 2013254846 A AU2013254846 A AU 2013254846A AU 2013254846 A AU2013254846 A AU 2013254846A AU 2013254846 A1 AU2013254846 A1 AU 2013254846A1
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- Prior art keywords
- mixture
- magnetic
- process according
- magnetic particle
- group
- Prior art date
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Links
- 239000002245 particle Substances 0.000 title claims description 32
- 238000007885 magnetic separation Methods 0.000 title description 5
- 239000000463 material Substances 0.000 claims abstract description 108
- 238000000034 method Methods 0.000 claims abstract description 105
- 239000000203 mixture Substances 0.000 claims abstract description 101
- 230000008569 process Effects 0.000 claims abstract description 97
- 239000006249 magnetic particle Substances 0.000 claims abstract description 88
- 239000000126 substance Substances 0.000 claims abstract description 70
- 230000005291 magnetic effect Effects 0.000 claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims description 38
- 239000002612 dispersion medium Substances 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 25
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- 150000001875 compounds Chemical class 0.000 claims description 20
- 150000002736 metal compounds Chemical class 0.000 claims description 18
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003776 cleavage reaction Methods 0.000 claims description 11
- 230000007017 scission Effects 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
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- 150000002739 metals Chemical class 0.000 claims description 9
- 229910000510 noble metal Inorganic materials 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 6
- 229910000859 α-Fe Inorganic materials 0.000 claims description 6
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- 150000001340 alkali metals Chemical class 0.000 claims description 5
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
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- 125000000129 anionic group Chemical group 0.000 claims description 4
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- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 2
- 230000005294 ferromagnetic effect Effects 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
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- 125000004404 heteroalkyl group Chemical group 0.000 claims 1
- 235000013980 iron oxide Nutrition 0.000 claims 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 claims 1
- 239000010949 copper Substances 0.000 description 17
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- 125000004432 carbon atom Chemical group C* 0.000 description 9
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- 125000000217 alkyl group Chemical group 0.000 description 6
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- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 4
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
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- NJGCRMAPOWGWMW-UHFFFAOYSA-N octylphosphonic acid Chemical compound CCCCCCCCP(O)(O)=O NJGCRMAPOWGWMW-UHFFFAOYSA-N 0.000 description 3
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- 238000011084 recovery Methods 0.000 description 3
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- GWBUNZLLLLDXMD-UHFFFAOYSA-H tricopper;dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Cu+2].[Cu+2].[Cu+2].[O-]C([O-])=O.[O-]C([O-])=O GWBUNZLLLLDXMD-UHFFFAOYSA-H 0.000 description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
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- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 2
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- 239000012141 concentrate Substances 0.000 description 2
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- 150000004662 dithiols Chemical class 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
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- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- 239000005046 Chlorosilane Substances 0.000 description 1
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- 238000007869 Guerbet synthesis reaction Methods 0.000 description 1
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- 150000001412 amines Chemical class 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
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- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052948 bornite Inorganic materials 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
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- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
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- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- FYHQYEVHSYHJHO-UHFFFAOYSA-N octoxymethanedithioic acid Chemical compound CCCCCCCCOC(S)=S FYHQYEVHSYHJHO-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- QWENMOXLTHDKDL-UHFFFAOYSA-N pentoxymethanedithioic acid Chemical compound CCCCCOC(S)=S QWENMOXLTHDKDL-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
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- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- OMKVZYFAGQKILB-UHFFFAOYSA-M potassium;butoxymethanedithioate Chemical compound [K+].CCCCOC([S-])=S OMKVZYFAGQKILB-UHFFFAOYSA-M 0.000 description 1
- HRANSTGHZSEXRW-UHFFFAOYSA-M potassium;dioctyl-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [K+].CCCCCCCCP([S-])(=S)CCCCCCCC HRANSTGHZSEXRW-UHFFFAOYSA-M 0.000 description 1
- ABCMVVZRRCUIBB-UHFFFAOYSA-M potassium;n,n-dioctylcarbamodithioate Chemical class [K+].CCCCCCCCN(C([S-])=S)CCCCCCCC ABCMVVZRRCUIBB-UHFFFAOYSA-M 0.000 description 1
- YEEBCCODSASHMM-UHFFFAOYSA-M potassium;octoxymethanedithioate Chemical compound [K+].CCCCCCCCOC([S-])=S YEEBCCODSASHMM-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- RZFBEFUNINJXRQ-UHFFFAOYSA-M sodium ethyl xanthate Chemical compound [Na+].CCOC([S-])=S RZFBEFUNINJXRQ-UHFFFAOYSA-M 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- AAJRIJBGDLLRAE-UHFFFAOYSA-M sodium;butoxymethanedithioate Chemical compound [Na+].CCCCOC([S-])=S AAJRIJBGDLLRAE-UHFFFAOYSA-M 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- XIUROWKZWPIAIB-UHFFFAOYSA-N sulfotep Chemical compound CCOP(=S)(OCC)OP(=S)(OCC)OCC XIUROWKZWPIAIB-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
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- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/005—Pretreatment specially adapted for magnetic separation
- B03C1/01—Pretreatment specially adapted for magnetic separation by addition of magnetic adjuvants
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- 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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C2201/00—Details of magnetic or electrostatic separation
- B03C2201/18—Magnetic separation whereby the particles are suspended in a liquid
-
- 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
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C2201/00—Details of magnetic or electrostatic separation
- B03C2201/20—Magnetic separation whereby the particles to be separated are in solid form
Abstract
The present invention relates to a process for separating at least one first material from a mixture comprising this at least one first material and at least one second material, which comprises contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle, or contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle and at least one surface-modifying substance at the same time, contacting of the mixture from step (A) with at least one surface-modifying substance, if this has not been done in step (A), so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, and separation of the addition product by application of a magnetic field.
Description
WO 2013/160219 PCT/EP2013/058245 1 Magnetic separation of particles including one-step-conditioning of a pulp Description 5 The present invention relates to a process for separating at least one first material from a mixture comprising this at least one first material and at least one second material, which comprises the following steps (A) contacting of the mixture comprising at least one first material and at least one 10 second material with at least one magnetic particle, if appropriate in the presence of at least one dispersant, or 15 contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle and at least one surface modifying substance at the same time, so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, if appropriate in the presence of at least one 20 dispersant, (B) if appropriate, addition of at least one dispersant to the mixture obtained in step (A) to give a dispersion having a suitable concentration, 25 (C) contacting of the mixture from step (A) or (B) with at least one surface-modifying substance, if this has not been done in step (A), so that the at least one first ma terial, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, 30 (D) separation of the addition product from step (A), (B) or (C) from the mixture by application of a magnetic field, (E) if appropriate, cleavage of the addition product which has been separated off in step (D) to obtain the at least one first material and the at least one magnetic par 35 ticle separately. In particular, the present invention relates to a process for the enrichment of ores in the presence of the gangue. 40 Processes for separating ores from mixtures comprising these are already known from the prior art.
WO 2013/160219 PCT/EP2013/058245 2 WO 02/0066168 Al relates to a process for separating ores from mixtures comprising these, in which suspensions or slurries of these mixtures are treated with particles which are magnetic and/or capable of floating in aqueous solutions. After addition of 5 the magnetic particles and/or particles capable of floating, a magnetic field is applied so that the agglomerates are separated off from the mixture. However, the extent to which the magnetic particles are bound to the ore and the strength of the bond is not suffi cient for the process to be carried out with a satisfactorily high yield and effectiveness. 10 US 4,657,666 discloses a process for the enrichment of ores, in which the ore present in the gangue is treated with magnetic particles, as a result of which agglomerates are formed due to the hydrophobic interactions. The magnetic particles are hydrophobized on the surface by treatment with hydrophobic compounds, so that attachment to the ore occurs. The agglomerates are then separated off from the mixture by means of a 15 magnetic field. The cited document also discloses that the ores are treated with a sur face-activating solution of 1% sodium ethylxanthogenate before the magnetic particle is added. In this process, separation of ore and magnetic particle is effected by the de struction of the surface-activating substance which has been applied in the form of the surface-activating solution to the ore. Furthermore, in this process only C4 20 hydrophobising agents are used for the ore. US 4,834,898 discloses a process for separating off nonmagnetic materials by bringing them into contact with magnetic reagents which are enveloped by two layers of sur face-modifying substances. US 4,834,898 also discloses that the surface charge of the 25 nonmagnetic particles which are to be separated off can be influenced by various types and concentrations of electrolytes reagents. For example, the surface charge is altered by addition of multivalent anions, for example tripolyphosphate ions. S. R. Gray, D. Landberg, N. B. Gray, Extractive Metallurgy Conference, Perth, 2 - 4 30 October 1991, pages 223 - 226, disclose a process for recovering small gold particles by bringing the particles into contact with magnetite. Before contacting, the gold parti cles are treated with potassium amylxanthogenate. A process for separating the gold particles from at least one hydrophilic material is not disclosed in this document. 35 WO 2007/008322 Al discloses a magnetic particle which is hydrophobized on the sur face for separating impurities from mineral substances by magnetic separation pro cesses. According to WO 2007/008322 Al, a dispersant selected from among sodium silicate, sodium polyacrylate and sodium hexametaphosphate can be added to the so lution or dispersion. 40 WO 2013/160219 PCT/EP2013/058245 3 W02009/030669 Al discloses a process for separating at least one first material from a mixture comprising this at least one first material and at least one second material, in which the first material is firstly brought into contact with a surface-modifying substance to hydrophobize it, this mixture is then brought into contact with at least one magnetic 5 particle so that the magnetic particle and the hydrophobized first material become at tached to one another and this agglomerate is separated from the at least one second material by application of a magnetic field. The at least one first material is subsequent ly separated, preferably quantitatively, from the magnetic particle, with the magnetic particle preferably being able to be recirculated to the process. This document does not 10 disclose that the addition of magnetic particles prior to a surface-modifying substance or the addition of magnetic particles and a surface-modifying substance at the same time gives rise to certain advantages like accelerated agglomeration. It is an object of the present invention to provide a process by means of which at least 15 one first material can be efficiently separated from mixtures comprising at least one first material and at least one second material. A further object of the present invention is to treat the first particles to be separated off in such a way that the addition product of magnetic particle and first material is sufficiently stable to ensure a high yield of the first material in the separation. 20 A further object is to provide a process for separating particles from a mixture compris ing them and other particles, using magnetic particles to obtain magnetic agglomerates of particles to be separated and magnetic particles, wherein the agglomeration occurs faster and more evenly than in processes of the prior art. 25 These objects are achieved by a process for separating at least one first material from a mixture comprising this at least one first material and at least one second material, which comprises the following steps: 30 (A) contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle, if appropriate in the presence of at least one dispersant, or 35 contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle and at least one surface modifying substance at the same time, so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle 40 become attached to one another, if appropriate in the presence of at least one dispersant, WO 2013/160219 PCT/EP2013/058245 4 (B) if appropriate, addition of at least one dispersant to the mixture obtained in step (A) to give a dispersion having a suitable concentration, 5 (C) contacting of the mixture from step (A) or (B) with at least one surface-modifying substance, if this has not been done in step (A), so that the at least one first ma terial, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, 10 (D) separation of the addition product from step (A), (B) or (C) from the mixture by application of a magnetic field, (E) if appropriate, cleavage of the addition product which has been separated off in step (D) to obtain the at least one first material and the at least one magnetic par 15 ticle separately. The process of the invention is preferably employed for separating at least one first, hydrophobic material from a mixture comprising this at least one first, hydrophobic ma terial and at least one second, hydrophilic material. 20 For the purposes of the present invention, "hydrophobic" means that the corresponding particle can subsequently be hydrophobized by treatment with the at least one surface modifying substance. 25 It is also possible for a particle which is hydrophobic per se to be additionally hydro phobized by treatment with the at least one surface-modifying substance. Within the scope of the present invention, "hydrophobic" means that the surface of cor responding "hydrophobic substances", and, respectively, of a "hydrophobized sub 30 stance" has a contact angle with water against air of > 90'. In the scope of the present invention, "hydrophilic" means that the surface of corresponding "hydrophilic sub stance" has a contact angle with water against air of < 90'. In a preferred embodiment of the process of the invention, the at least one first material 35 is at least one hydrophobic metal compound or coal and the at least one second mate rial is preferably at least one hydrophilic metal compound. In a further preferred embodiment of the process according to the present invention, the at least one hydrophobic metal compound is selected from the group consisting of 40 sulfidic ores, oxidic ores, carbonate-comprising ores, noble metals in elemental form, compounds comprising noble metals and mixtures thereof.
WO 2013/160219 PCT/EP2013/058245 5 The present invention therefore preferably relates to the process according to the pre sent invention, wherein the at least one hydrophobic metal compound is selected from the group consisting of sulfidic ores, oxidic ores, carbonate-comprising ores, noble 5 metals in elemental form, compounds comprising noble metals and mixtures thereof. In a further preferred embodiment of the process according to the present invention, the at least one hydrophilic metal compound is selected from the group consisting of oxidic metal compounds, hydroxidic metal compounds and mixtures thereof. 10 The present invention therefore preferably relates to the process according to the pre sent invention, wherein the at least one hydrophilic metal compound is selected from the group consisting of oxidic metal compounds, hydroxidic metal compounds and mix tures thereof. 15 Examples of the at least one first material to be separated off are preferably metal compounds selected from the group consisting of sufidic ores, oxidic and/or carbonate comprising ores, for example azurite [Cu 3
(CO
3
)
2
(OH)
2 ] or malachite [Cu 2
[(OH)
2 1CO 3 ]], rare earth metals comprising ores like bastnaesite (Y, Ce, La)CO 3 F, monazite (RE)P0 4 20 (RE = rare earth metal) or chrysocolla (Cu,AI) 2
H
2 Si 2
O
5
(OH)
4 - n H 2 0, noble metals in elemental form and their compounds to which a surface-modifying compound can be come selectively attached to produce hydrophobic surface properties. Examples of noble metals that may be present as at least first material are Au, Pt, Pd, Rh, etc., preferably in the native state or as sulphides, phosphides, selenides, tellurides or as 25 alloys with bismuth, antimony and/or other metals. Examples of sulfidic ores which can be separated according to the invention are, for example, selected from the group of copper ores consisting of covellite CuS, molyb denum(IV) sulfide, chalcopyrite (cupriferous pyrite) CuFeS 2 , bornite Cu 5 FeS 4 , chalco 30 cite (copper glass) Cu 2 S, pendlandite (Fe,Ni) 9
S
8 , and mixtures thereof. Suitable oxidic metal compounds which may be present as at least one second materi al according to the invention are preferably selected from the group consisting of silicon dioxide SiO 2 , silicates, aluminosilicates, for example feldspars, for example albite 35 Na(Si 3 AI)0 8 , mica, for example muscovite KA1 2
[(OH,F)
2 AISi 3
O
1 0 ], garnets (Mg, Ca, Fe") 3 (AI, Fe"') 2 (SiO4) 3 and further related minerals and mixtures thereof. Accordingly, untreated ore mixtures obtained from mines are preferably used as mix ture comprising at least one first material and at least one second material in the pro 40 cess of the invention.
WO 2013/160219 PCT/EP2013/058245 6 In a preferred embodiment of the process of the invention, the mixture comprising at least one first material and at least one second material in step (A) is in the form of particles having a size of from 100 nm to 100 pm, see for example US 5,051,199. In a preferred embodiment, this particle size is obtained by milling. Suitable processes and 5 apparatuses are known to those skilled in the art, for example wet milling in a ball mill. The mixture comprising at least one first material and at least one second material is therefore milled to particles having a size of from 100 nm to 100 pm before or during step (A) in a preferred embodiment of the process of the invention. Preferred ore mix tures have a content of sulfidic minerals of at least 0.4% by weight, particularly prefera 10 bly at least 10% by weight. Examples of sulfidic minerals which are present in the mixtures which can be used ac cording to the invention are those mentioned above. In addition, sulfide of metals other than copper, for example, sulfides of iron, lead, zinc or molybdenum, i.e. FeS, FeS 2 , 15 PbS, ZnS or MoS 2 , can also be present in the mixtures. Furthermore, oxidic com pounds of metals and semimetals, for example silicates or borates or other salts of metals and semimetals, for example phosphates, sulfates or ox ides/hydroxides/carbonates, and further salts, for example azurite [Cu 3
(CO
3
)
2
(OH)
2 ], malachite [Cu 2
[(OH)
2
(CO
3 )]], barite (BaSO4), monazite ((La-Lu)P04), spinels (Mg, Ca, 20 Fe(Il))(Fe(Ill), Al, Cr) 2 0 4 , can be present in the ore mixtures to be treated according to the invention. A typical ore mixture which can be separated by means of the process of the invention has the following composition: about 30% by weight of Si0 2 as an example of a pre 25 ferred at least one second material, about 30% by weight of feldspar (e.g. Na(Si 3 AI)0 8 ), about 3% by weight of CuFeS 2 as an example of a preferred at least one first material, about 0,05% by weight of MoS 2 , balance chromium, iron, titanium and magnesium ox ides. 30 The individual steps of the process of the invention are described in detail below: Step (A): Step (A) of the process according to the present invention can be conducted according 35 to two alternative embodiments. According to the first embodiment of the process according to the present invention, step (A) comprises contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle, if appropriate in the 40 presence of at least one dispersant.
WO 2013/160219 PCT/EP2013/058245 7 According to this first embodiment only at least one magnetic particle is added in step (A), and at least one surface-modifying substance is added in step (C) of the process according to the present invention. 5 According to the second embodiment of the process according to the present invention, step (A) comprises contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle and at least one sur face-modifying substance at the same time, so that the at least one first material, the at 10 least one surface-modifying substance and the at least one magnetic particle become attached to one another, if appropriate in the presence of at least one dispersant. According to this second embodiment, both, at least one magnetic particle and at least one surface active substance are added in step (A). According to this embodiment, 15 step (C) of the process according to the present invention is not necessary and is pref erably not conducted. Suitable preferred first and second materials have been mentioned above. 20 According to the present invention at least one magnetic particle is added in step (A). In a preferred embodiment of the process according to the present invention, at least one hydrophobic magnetic particle is added in step (A). In a preferred embodiment of the present invention, the at least one magnetic particle is hydrophobized at the sur face. 25 In step (A) of the process of the invention, it is in general possible to use all magnetic substances and materials known to those skilled in the art. In a preferred embodiment, the at least one magnetic particle is selected from the group consisting of magnetic metals, for example iron, cobalt, nickel and mixtures thereof, ferromagnetic alloys of 30 magnetic metals, for example NdFeB, SmCo and mixtures thereof, magnetic iron ox ides, for example magnetite, maghemite, cubic ferrites of the general formula (II) M2+ xFe2+1.xFe3+204 (II) 35 where M is selected from among Co, Ni, Mn, Zn and mixtures thereof and x is 1, 40 hexagonal ferrites, for example barium or strontium ferrite MFe 6
O
1 9 where M = Ca, Sr, Ba, or a mixture thereof. The magnetic particles can additionally have an outer layer, for example of SiO 2
.
WO 2013/160219 PCT/EP2013/058245 8 In a particularly preferred embodiment of the present invention, the at least one mag netic particle is magnetite or cobalt ferrite Co2+Fe 2+1-Fe3+204 where x 5 1. Very prefer ably magnetite is used as at least one magnetic particle. 5 In a further preferred embodiment, in step (A) of the process according to the present invention, magnetic particles are present in the size of 100 nm to 100 pm, particularly preferred 1 to 50 pm. The magnetic particles may be brought into the adequate size by processes known to the skilled artisan, for example by milling. Furthermore, the parti 10 cles, obtained from precipitation reaction, can be brought to the adequate particle size by setting up the reaction parameters (for example pH, reaction time, temperature). In a further preferred embodiment, the at least one magnetic particle is hydrophobized at the surface by at least one hydrophobic compound. The hydrophobic compound is 15 preferably selected from among compounds of the general formula (Ill) B-Y (Ill), where 20 B is selected from among linear or branched C 3
-C
30 -alkyl, C 3
-C
30 -heteroalkyl, op tionally substituted C 6
-C
30 -aryl, optionally substituted C 6
-C
30 -heteroaryl, C6-C30 aralkyl, and 25 Y is a group by means of which the compound of the general formula (Ill) binds to the at least one magnetic particle. In a particularly preferred embodiment, B is a linear or branched C 6
-C
18 -alkyl, prefera bly linear C 8
-C
12 -alkyl, very particularly preferably a linear C 12 -alkyl. Heteroatoms which 30 may be present according to the invention are selected from among N, 0, P, S and halogens such as F, Cl, Br and I. In a further particularly preferred embodiment, Y is selected from the group consisting of -(X)n-SiHal 3 , -(X)n-SiHHal 2 , -(X)n-SiH 2 Hal where Hal is F, Cl, Br, I, -(X)n-Si(OR1)3-n 35 wherein n is 1, 2 or 3 and R 1 is C 1
-C
6 -alkyl, and anionic groups such as -(X)n-SiO 3 3 (X)n-CO2, -(X)n-PO 3 2 -, -(X)n-PO 2
S
2 -, -(X)n-POS 2 2-, -(X)n-PS 3 2-, -(X)n-PS2, -(X)n-POS, (X)n-PO2, -(X)n-CO2, -(X)n-CS2, -(X)n-COS-, -(X)n-C(S)NHOH, -(X)n-S- where X = 0, S, NH, CH 2 and n = 0, 1 or 2, and, if appropriate, cations selected from the group consist ing of hydrogen, NR 4 ' where the radicals R are each, independently of one another, 40 hydrogen or C 1
-C
8 -alkyl, an alkali metal, an alkaline earth metal or zinc, also -(X)n Si(OZ) 3 where n = 0, 1 or 2 and Z = charge, hydrogen or short-chain alkyl radical.
WO 2013/160219 PCT/EP2013/058245 9 If, in the mentioned formulas n = 2, two equal or different, preferably equal, groups B are attached to one group Y. 5 Very preferred hydrophobizing substances of general formula (Ill) are alkyltri chlorosilane (alkyl group having 1 to 12 carbon atoms), alkyldialkoxysilane (alkyl group having 1 to 12 carbon atoms and alkoxy group having 1 to 6 carbon atoms), for exam ple alkyldimethoxysilane (alkyl group having 1 to 12 carbon atoms), alkyltrialkoxysilane (alkyl group having 1 to 12 carbon atoms and alkoxy group having 1 to 6 carbon at 10 oms), for example alkyltrimethoxysilane (alkyl group having 6 to 12 carbon atoms), octylphosphonic acid, lauric acid, oleic acid, stearic acid or mixtures thereof. Using al kyltrialkoxysilanes as hydrophobizing substances of general formula (Ill), preferably a polymeric hydrophobic layer is obtained at the surface of the magnetic particle. 15 The at least one magnetic particle is in general added in an amount that is high enough to have the complete amount of at least one first material embedded in agglomerates, preferably the at least one magnetic particle is added in excess. For example, the at least one magnetic particle is added in an amount of 0.1 to 20% by weight, preferably 0.5 to 5% by weight, in each case based on the amount of the complete mixture to be 20 treated with the process according to the present invention. According to the second embodiment of step (A) of the process according to the pre sent invention, at least one surface-modifying substance is added. In general, all sur face-modifying substances can be used according to the present invention that are 25 able to modify the surface of the at least one first material in a way that agglomeration with at least one magnetic particle is possible. For the purposes of the present invention, a "surface-modifying substance" is a sub stance which is able to modify the surface of the particle to be separated off in the 30 presence of the other particles which are not to be separated off in such a way that attachment of a hydrophobic particle by means of hydrophobic interactions occurs. Surface-modifying substances which can be used according to the invention become attached to the at least one first material and thereby produce a suitable hydrophobicity of the first material. 35 In the process of the invention, preference is given to using a surface-modifying sub stance of the general formula (1) A-Z (1) 40 which becomes attached to the at least one first material, where WO 2013/160219 PCT/EP2013/058245 10 A is selected from among linear or branched C 2
-C
30 -alkyl, C 2
-C
30 -heteroalkyl, op tionally substituted C 6
-C
30 -aryl, optionally substituted C 6
-C
30 -heteroaryl, C6-C30 aralkyl, and 5 Z is a group by means of which the compound of the general formula (1) binds to the at least one hydrophobic material. In a particularly preferred embodiment, A is a linear or branched C 2
-C
14 -alkyl, very par 10 ticularly preferably a linear C4- or C 8 -alkyl. Heteroatoms which may be present accord ing to the invention are selected from among N, 0, P, S and halogens such as F, Cl, Br and I. In a further preferred embodiment, A is preferably a branched, C 2
-C
20 -alkyl, particularly 15 preferably a branched C 6
-C
14 -alkyl, wherein preferably the at least one substituent, preferably having 1 to 6 carbon atoms, is attached in 2-position, for example 2 ethylhexyl and/or 2-propylheptyl. Corresponding compounds being substituted in 2 position are, for example, obtained using the Guerbet reaction that is known to the skilled artisan as one reaction step. 20 In a further particularly preferred embodiment, X is selected from the group consisting of anionic groups -(X)n-PO 3 2 -, -(X)n-PO 2
S
2 -, -(X)n-POS 2 2-, -(X)n-PS 3 2-, -(X)n-PS2, -(X)n POS-, -(X)n-PO2-, -(X)n-PO3 2- -(X)n-CO2-, -(X)n-CS2 , -(X)n-COS-, -(X)n-C(S)NHOH, -(X)n S- where X is selected from the group consisting of 0, S, NH, CH 2 and n = 0, 1 or 2, 25 with, if appropriate, cations selected from the group consisting of hydrogen, NR 4 ' with R being independently of one another hydrogen and/or C 1
-C
8 -alkyl, hydroxy-substituted
C
1
-C
8 -alkyl or -heteroalkyl, like 2-hydroxy-ethyl HO-CH 2
CH
2 - or 2-hydroxy-ethoxy-ethyl
HO-CH
2
CH
2 -0-CH 2
CH
2 -, alkali- or earth alkali metals, preferably sodium or potassium, are present. The anions mentioned and the corresponding cations form, according to 30 the invention, uncharged compounds of the general formula (1). If, in the mentioned formulas n = 2, two equal or different, preferably equal, groups A are attached to one group Z. 35 In a further preferred embodiment, compounds are applied, selected from the group consisting of xanthates A-O-CS2, dialkyldithiophosphates (A-O) 2 -PS2, dialkyldithio phosphinates (A) 2 -PS2, dialkyldithiocarbamates, alkyltrithiocarbamates, dithiophos phates and mixtures thereof, wherein A independently of one another is a linear or branched, preferably linear, C 6
-C
2 0 -alkyl, for example n-octyl, or a branched C6-C14 40 alkyl, wherein the branch is preferably located in 2-position, for example 2-ethylhexyl WO 2013/160219 PCT/EP2013/058245 11 and/or 2-propylheptyl. As counterions, in these compounds preferably cations selected from the group consisting of hydrogen, NR 4 ' with R being independently of one another hydrogen and/or C 1
-C
8 -alkyl, hydroxy-substituted C 1
-C
8 -alkyl or -heteroalkyl, like 2 hydroxy-ethyl HO-CH 2
CH
2 - or 2-hydroxy-ethoxy-ethyl HO-CH 2
CH
2 -0-CH 2
CH
2 -, alkali 5 or earth alkali metals, preferably sodium or potassium, are present. Exceptionally preferred compounds of general formula (1) are selected from the group consisting of sodium- or potassium-n-octylxanthate, sodium- or potassium butylxanthate, sodium- or potassium-di-n-octyldithiophosphinate, sodium- or potassi 10 um-di-n-octyldithiophosphate, sodium- or potassium-di-n-octyldithiocarbamates and mixtures of these compounds. In the case of noble metals, for example Au, Pd, Rh, etc., particularly preferred surface modifying substances are monothiols, dithiols and trithiols, or 8-hydroxyquinolines, for 15 example as described in EP 1200408 B1. In the case of metal oxides, for example FeO(OH), Fe 3 0 4 , ZnO, etc., carbonates, for example azurite [Cu(C03)2(OH)2], malachite [Cu 2 [(OH)2CO3]], particularly preferred surface-modifying substances are octylphosphonic acid (OPS), (EtO) 3 Si-A, (MeO) 3 Si 20 A, with the abovementioned meanings of A. In the case of metal sulfides, for example Cu 2 S, MoS 2 , FeS 2 etc., particularly preferred surface-modifying substances are monothiols, dithiols and trithiols, xanthogenates or dithiophosphates. 25 Therefore, according to the above mentioned, in a further preferred embodiment of the process of the invention, Z is -(X)n-CS2, -(X)n-PS2 or -(X)n-S- where X is 0 and n is 0 or 1, and a cation is selected from among hydrogen, sodium, potassium and NHx(CH 2
CH
2 0H) 4 .x, wherein x is 0, 1, 2, 3, or 4. 30 The at least one surface-modifying substance is generally used in an amount which is sufficient to achieve the desired effect. In a preferred embodiment, the at least one surface-modifying substance is added in an amount of from 0.001 to 1% by weight, preferably 0.001 to 0.1% by weight in each case based on the total mixture to be treat 35 ed. According to the first embodiment of step (A) of the process according to the present invention, the contacting of the mixture with at least one magnetic particle in step (A) of the process of the invention can be carried out by all methods known to those skilled in 40 the art, for example in bulk or in dispersion, preferably in suspension. In a preferred WO 2013/160219 PCT/EP2013/058245 12 first embodiment, a dispersion of the at least one magnetic particle is added to the mix ture. In a preferred embodiment, the at least one magnetic particle is dispersed in a suitable 5 dispersion medium. Suitable dispersion media are all dispersion media in which the at least one magnetic particle is not completely soluble. Suitable dispersion media are for example selected from the group consisting of water, water-soluble organic com pounds, for example alcohols having from 1 to 4 carbon atoms, particularly preferably water. 10 According to the invention, the amount of dispersion medium for predispersing the magnetic particles can generally be selected so that a slurry or dispersion which is readily stirrable and/or conveyable is obtained. In a preferred embodiment, the amount of mixture to be treated based on the total slurry or dispersion is up to 100% by weight, 15 preferably up to 60% by weight, for example 0.5 to 60% by weight, preferably 0.5 to 20% by weight, particularly preferably 0.5 to 10% by weight. In one embodiment of the present invention, a high amount of mixture to be treated in the slurry or dispersion is preferred. Therefore, the present invention preferably relates 20 to the process according to the present invention, wherein the amount of mixture to be treated based on the total slurry or dispersion is up to 60% by weight, for example 20 to 60% by weight. According to the invention, the dispersion of the magnetic particles can be produced by 25 all methods known to those skilled in the art. In a preferred embodiment, the magnetic particles to be dispersed and the appropriate amount of dispersion medium or mixture of dispersion media are combined in a suitable reactor, for example a stirring tank, and stirred by means of devices known to those skilled in the art, for example in a stirring tank by means of a magnetically operated propeller stirrer, for example at a tempera 30 ture of from 1 to 80'C, preferably at room temperature. According to the second embodiment of step (A) of the process according to the pre sent invention, the contacting of the mixture with at least one magnetic particle and at least one surface-modifying substance at the same time is generally carried out by 35 combining the components by methods known to those skilled in the art. For example, this second embodiment of step (A) can be carried out in bulk or in dispersion, prefera bly in suspension. Suitable dispersion media are for example selected from the group consisting of water, water-soluble organic compounds, for example alcohols having from 1 to 4 carbon atoms, and mixtures thereof. In a particularly preferred embodiment, 40 the dispersion medium is water. In a preferred second embodiment, a dispersion of the WO 2013/160219 PCT/EP2013/058245 13 at least one magnetic particle and at least one surface-modifying substance is added to the mixture. The present invention therefore preferably relates to the process according to the pre 5 sent invention, wherein contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle or with at least one magnetic particle and at least one surface-modifying substance at the same time in step (A) is achieved by addition of a mixture, preferably a dispersion, of least one mag netic particle and at least one surface-modifying substance. 10 In a further embodiment of the process of the invention, both embodiments of step (A) can be carried out in bulk, i.e. in the absence of a dispersion medium. For example, the mixture to be treated and the at least one magnetic particle or at least 15 one magnetic particle and the at least one surface-modifying substance are combined and mixed in the appropriate amounts without a further dispersion medium. Suitable mixing apparatuses are known to those skilled in the art, for example mills such as ball mills. 20 Step (A) is generally carried out at a temperature of from 1 to 80 'C, preferably from 10 to 30 'C. According to the second embodiment of step (A), wherein at least one magnetic parti cle and at least one surface-modifying substance are added at the same time, the at 25 least one magnetic particle becomes attached to the at least one first material that is more hydrophobic than the at least one second material by nature and that is further hydrophobized at its surface by the at least one surface-modifying substance. The bond between the two components is based on hydrophobic interactions. There is generally no bonding interaction between the at least one magnetic particle and the 30 hydrophilic component of the mixture, so that these components do not become at tached to one another. Thus, addition products of the at least one first, hydrophobic material and the at least one magnetic particle are present alongside the at least one second, hydrophilic material in the mixture after the second embodiment of step (A) of the process according to the present invention. 35 40 WO 2013/160219 PCT/EP2013/058245 14 Step (B): The optional step (B) of the process of the invention comprises addition of at least one dispersion medium to the mixture obtained in step (A) to give a dispersion having a 5 suitable concentration. In one embodiment, if step (A) is carried out in bulk, the mixture obtained in step (A) comprises at least one first material and at least second material, at least one magnetic particle and optionally at least one surface-modifying substance. If step (A) is carried 10 out in bulk, step (B) of the process of the invention is preferably carried out, i.e. at least one suitable dispersion medium is added to the mixture obtained in step (A) in order to obtain a dispersion. In the embodiment in which step (A) of the process of the invention is carried out in dispersion, step (B) is preferably not carried out. However, in this embodiment, too, it is 15 possible to carry out step (B), i.e. to add further dispersion medium in order to obtain a dispersion having a lower concentration. Suitable dispersion media are all dispersion media which have been mentioned above in respect of step (A). In a particularly preferred embodiment, the dispersion medium in 20 step (B) is water. Thus, step (B) comprises either converting the mixture present in bulk from step (A) into a dispersion or converting the mixture which is already in dispersion from step (A) into a dispersion of lower concentration by addition of dispersion media. 25 According to the invention, the amount of dispersion medium added in step (A) and/or step (B) can generally be selected so that a dispersion is obtained which is readily stir rable and/or conveyable. In a preferred embodiment, the amount of mixture to be treat ed based on the total slurry or dispersion is up to 100% by weight, preferably up to 30 60% by weight, for example 0.5 to 60% by weight, preferably 0.5 to 20% by weight, particularly preferably 0.5 to 10% by weight. In one embodiment of the present invention, a high amount of mixture to be treated in the slurry or dispersion is preferred. Therefore, the present invention preferably relates 35 to the process according to the present invention, wherein the amount of mixture to be treated based on the total slurry or dispersion is up to 60% by weight, for example 20 to 60% by weight. In a preferred embodiment of the process of the invention, step (B) is not carried out 40 but instead step (A) is carried out in aqueous dispersion so that a mixture in aqueous WO 2013/160219 PCT/EP2013/058245 15 dispersion having the correct concentration for use in step (C) of the process of the invention is obtained directly in step (A). The addition of dispersion medium in step (B) of the process of the invention can, ac 5 cording to the invention, be carried out by all methods known to those skilled in the art. Step (C): Step (C) of the process of the invention comprises contacting of the mixture from step 10 (A) or (B) with at least one surface active substance, if this has not been done in step (A), so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another. Step (C) of the process according to the present invention is conducted, if at least one 15 surface-modifying active substance is not added in step (A) of the process according to the present invention. According to this first embodiment of the process according to the present invention, a mixture comprising the at least one first material, the at least one second material, the at least one magnetic particle and optionally at least one dis persion medium, that is obtained in step (A) or (B), is introduced in step (C). 20 The at least one surface-modifying substance that is added in step (C) of the process according to the present invention and preferred embodiments thereof can be selected from the group of compounds of general formula (1) as mentioned in respect of step (A) of the process according to the present invention. 25 According to step (C) of the process according to the present invention, the at least one surface-modifying substance is generally used in an amount which is sufficient to achieve the desired effect. In a preferred embodiment, the at least one surface modifying substance is added in step (C) of the process according to the present inven 30 tion in an amount of from 0.001 to 1% by weight, preferably 0.001 to 0.1% by weight in each case based on the total mixture to be treated. Step (C) of the process according to the present invention can in general be conducted according to all methods that are known to the skilled artisan. In particular, the addition 35 according to step (C) of the process according to the present invention can be con ducted as mentioned in respect of step (A) of this process. Step (D): 40 Step (D) of the process of the invention comprises separation of the addition product from step (A), (B) or (C) from the mixture by application of a magnetic field. According WO 2013/160219 PCT/EP2013/058245 16 to the present invention, the "addition product" in the sense of step (D) is the agglom erate that is obtained in step (A) or (C) containing at least one first material, at least one surface active substance and at least one magnetic particle. 5 In general, step (D) can be carried out with any magnetic equipment that is suitable to separate magnetic particles from dispersion, e. g. drum separators, high or low intensi ty magnetic separators, continuous belt type separators or others. Step (D) can be carried out by introducing a permanent magnet into the reactor in 10 which the mixture from step (A), (B) or (C) is present. In a preferred embodiment, a dividing wall composed of nonmagnetic material, for example the wall of the reactor, is present between permanent magnet and mixture to be treated. In a further preferred embodiment of the process of the invention, an electromagnet which is only magnetic when an electric current flows is used in step (D). Suitable apparatuses are known to 15 those skilled in the art. In a preferred embodiment, the magnetic separation equipment allows to wash the magnetic concentrate while the separation with a dispersant, preferably water. This washing preferably allows removing inert material from the magnetic concentrate lead 20 ing to higher grades of the valuables. In a preferred embodiment, step (D) is conducted continuously or semi-continuously, wherein preferably the mixture to be treated flows through a separator, preferably in dispersion. Flow velocities of the dispersion to be treated are in general adjusted to 25 obtain an advantageous yield of magnetic agglomerates separated. In a preferred em bodiment, flow velocities of the dispersion to be treated are 10 mm/sec. to 1000 mm/sec. The pH-value of the dispersion which is treated according to step (D) is in general neu 30 tral or weakly basic, being a pH-value of 6 to 13, preferably 8 to 12. In a preferred em bodiment, no adjustment of pH-value of the dispersion obtained in step (A) or (B) is necessary. Step (D) of the process of the invention can be carried out at any suitable temperature, 35 for example from 10 to 60 'C, preferably at ambient temperature. In a continuous or semi-continuous process the mixture is preferably mixed by turbu lent flow, and is preferably not additionally stirred.
WO 2013/160219 PCT/EP2013/058245 17 The magnetic agglomerates can be separated from the magnetic surface and/or the unit wherein magnetic separation is conducted according to the present invention by all methods known to those skilled in the art. 5 In a preferred embodiment the magnetic agglomerates are removed by flushing with a suitable dispersion medium. Suitable dispersion media have been mentioned above. In a preferred embodiment, water is used to flush the separated magnetic agglomerates. After step (D) of the process according to the present invention, the agglomerate of at 10 least one first material that is to be separated according to the present invention, at least one surface-modifying substance and at least one magnetic particle is separated from the at least one second material. Preferably both fractions that are obtained are present as dispersions in at least one dispersion medium, preferably in water. 15 Step (E): Optional step (E) of the process of the invention comprises cleavage of the addition product which has been separated off in step (D) to obtain the at least one first material 20 and the at least one magnetic particle separately. In a preferred embodiment of the process of the invention, the cleavage in step (E) is carried out in a nondestructive manner, i.e. the individual components present in the dispersion are not changed chemically. For example, the cleavage according to the 25 invention is preferably not affected by oxidation of the hydrophobizing agent, for exam ple to give the oxidation products or degradation products of the hydrophobizing agent. Cleavage can be carried out by all methods known to those skilled in the art which are suitable for cleaving the addition product in such a way that the at least one magnetic 30 particle can be recovered in reusable form. In a preferred embodiment, the magnetic particle which has been cleaved off is reused in step (A) of the process according to the present invention. In a preferred embodiment, the cleavage in step (E) of the process of the invention is 35 affected by treatment of the addition product with a substance selected from the group consisting of organic solvents, basic compounds, acidic compounds, oxidants, reducing agents, surface-active compounds and mixtures thereof. Examples of basic compounds which can be used according to the invention are aque 40 ous solutions of basic compounds, for example aqueous solutions of alkali metal and/or alkaline earth metal hydroxides, for example KOH, NaOH, lime water, aqueous ammo nia solutions, aqueous solutions of organic amines of the general formula R2N, where WO 2013/160219 PCT/EP2013/058245 18 the radicals R 2 are selected independently from the group consisting of C-C 8 -alkyl which may optionally be substituted by further functional groups. Examples of surface-active compounds which can be used according to the invention 5 are nonionic, anionic, cationic and/or zwitterionic surfactants. In a preferred embodi ment, the cleavage is made by the use of biodegradable, preferably nonionic, surfac tants with concentrations in the range of the critical micelle concentrations. In a pre ferred embodiment, the addition product of hydrophobic material and magnetic particle is cleaved by means of biodegradable nonionic surfactants, further preferably added in 10 an amount slightly, for example up o 5%, more preferably up to 3%, above the critical micelle concentration of the surfactant. After optional cleavage according to step (E), the at least one first material and the at least one magnetic particle are, according to the invention, present as dispersion in the 15 abovementioned cleavage reagent, preferably in a mixture of water and surfactant. For example, the at least one magnetic particle is separated from the dispersion com prising this at least one magnetic particle and the at least one first material by means of a permanent magnet or electromagnet. Details of the separation are analogous to step 20 (D) of the process of the invention. The first material to be separated off, preferably the metal compound to be separated off, is preferably separated from the dispersion medium by drying. 25 The process according to the present invention comprises steps (A) to (D), wherein particles or agglomerates are obtained comprising at least one magnetic particle and at least one metal. In a particularly preferred embodiment these particles or agglomerates are suitable for direct work-up without optional step (E) according to the present inven tion to obtain the at least one metal in pure form. 30 The present invention further relates to the process according to the present invention, wherein after step (D) or step (E) the following step (F) is conducted: (F) further processing of the particles or of the agglomerate from step (D) or (E) via 35 smelting, extracting and/or wet chemical refining. The magnetic particles or agglomerates obtained in step (D) preferably comprise iron comprising magnetic substances or magnetic particles in addition to at least one first material, being for example at least one precious metal. Because iron is essentially 40 necessary for melting and/or smelting processes to obtain the at least one first material WO 2013/160219 PCT/EP2013/058245 19 in pure or enriched form, the particles or agglomerates that are obtained in step (D) of the process according to the present invention can directly be treated in a smelting and/or melting process. 5 In the case that noble metals are used as first material in combination with iron com prising magnetic particles, no need for further addition of other iron containing com pounds may exist. Instead, the magnetic iron oxide particles loaded with precious met als are added to the furnace feed in place of iron oxide otherwise added to the process. 10 In a further embodiment of the process according to the present invention, step (F) is conducted according to the present invention after step (E). Smelting, extracting and/or wet chemical refining are conducted according to methods that are known to the skilled artisan. 15 Figures: Figure 1 shows a diagram, wherein a process for separating valuables from the gangue of an ore according to the prior art, wherein surface-modifying substance and magnet 20 ite are added in two steps (diamonds) is compared to the process according to the pre sent invention, wherein surface-modifying substance and magnetite are added in one step (square). The x-axis shows time in minutes, the y-axis shows a value that is corre sponding to the particle size in pm. 25 In the case of the process according to the present invention, both, surface-modifying substance and magnetite are added at t = 0 min. In the case of the process according to the prior art, surface-modifying substance is added at t = 0 min, and magnetite is added at t = about 37 min. (left vertical line). At about 72 min (right vertical line), a sur factant is added to separate the agglomerates, in both cases. 30 Examples A roughly premilled porhyric copper ore from south America (0.66 wt% Cu, 0.029 wt% Mo) is milled to d80 = about 40 pm without the addition of any additive. After milling, 35 the pulp having a solid content of 60 wt% is treated with octyl xanthate (400 g/t) and hydrophobic magnetite (3 wt%) in varying orders. Treatment is conducted in a beaker under stirring using an inertly coated paddle mixer. Subsequently, the pulp is diluted to a solid content of 15 wt% und is separated magnetically. Results in respect of recovery and grade of copper and molybdenum are shown in table 1. 40 WO 2013/160219 PCT/EP2013/058245 20 Table 1 Examples No. 1 2 3 4 5 6 Time of addition 15 15* of xanthate [min] 30 15 10 5 Time of addition of magnetite [min] 15 15* Cu Recovery 93 92 89 95 95 95 [wt%] Mo Recovery [wt%] 94 90 88 94 94 91 Cu Grade [%] 18.2 17.8 17.9 17.9 16.9 17.1 Mo Grade [%] 0.62 0.56 0.61 0.61 0.55 0.53 *reversed order 5 In examples 1 and 2 at t = 0 min, the first substance (xanthate or magnetite) is added, after 15 min the other substance (xanthate or magnetite) is added, then it is stirred for 15 min, before agglomerates are treated as mentioned above. 10 In examples 3 to 6 both substances (xanthate and magnetite) are added at t = 0 min, after stirring for the time as mentioned in table 1, the agglomerates are treated as men tioned above.
Claims (10)
1. A process for separating at least one first material from a mixture comprising this 5 at least one first material and at least one second material, which comprises the following steps: (A) contacting of the mixture comprising at least one first material and at least one second material with at least one magnetic particle, if appro 10 priate in the presence of at least one dispersant, or contacting of the mixture comprising at least one first material and at 15 least one second material with at least one magnetic particle and at least one surface-modifying substance at the same time, so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, if appro priate in the presence of at least one dispersant, 20 (B) if appropriate, addition of at least one dispersion medium to the mixture obtained in step (A) to give a dispersion having a suitable concentration, (C) contacting of the mixture from step (A) or (B) with at least one surface 25 modifying substance, if this has not been done in step (A), so that the at least one first material, the at least one surface-modifying substance and the at least one magnetic particle become attached to one another, (D) separation of the addition product from step (A), (B) or (C) from the mix 30 ture by application of a magnetic field, (E) if appropriate, cleavage of the addition product which has been separat ed off in step (D) to obtain the at least one first material and the at least one magnetic particle separately. 35
2. The process according to claim 1, wherein the first material is a hydrophobic metal compound or coal and the second material is a hydrophilic metal com pound. 40 WO 2013/160219 PCT/EP2013/058245 22
3. The process according to claim 1 or 2, wherein the surface-modifying substance is a substance of the general formula (1) A-Z (1) 5 where A is selected from among linear or branched C 2 -C 30 -alkyl, C3-C30 heteroalkyl, optionally substituted C 6 -C 3 0 -aryl, optionally substituted C6 10 C 30 -heteroaryl, C 6 -C 30 -aralkyl, and Z is a group by means of which the compound of the general formula (1) binds to the at least one hydrophobic material.. 15
4. The process according to claim 3, wherein Z is selected from the group consist ing of anionic groups -(X)n-PO 3 2 -, -(X)n-PO 2 S 2 -, -(X)n-POS 2 2-, -(X)n-PS 3 2-, -(X)n PS2 , -(X)n-POS-, -(X)n-PO2-, -(X)n-PO3 2- -(X)n-CO2-, -(X)n-CS2 , -(X)n-COS-, -(X)n C(S)NHOH, -(X)n-S- where X is selected from the group consisting of 0, S, NH, CH 2 and n = 0, 1 or 2, with, if appropriate, cations selected from the group con 20 sisting of hydrogen, NR 4 ' with R being independently of one another hydrogen and/or C 1 -C 8 -alkyl, hydroxy-substituted C 1 -C 8 -alkyl or -heteroalkyl, alkali- or earth alkali metals.
5. The process according to any of claims 2 to 4, wherein the at least one hydro 25 phobic metal compound is selected from the group consisting of sulfidic ores, oxidic ores, carbonate-comprising ores, noble metals in elemental form, com pounds comprising noble metals and mixtures thereof.
6. The process according to any of claims 2 to 5, wherein the at least one hydro 30 philic metal compound is selected from the group consisting of oxidic metal compounds, hydroxidic metal compounds and mixtures thereof.
7. The process according to any of claims 1 to 6, wherein the at least one magnet ic particle is selected from the group consisting of magnetic metals, for example 35 iron, cobalt, nickel and mixtures thereof, ferromagnetic alloys of magnetic met als, for example NdFeB, SmCo and mixtures thereof, magnetic iron oxides, for example magnetite, maghemite, cubic ferrites of the general formula (II) WO 2013/160219 PCT/EP2013/058245 23 M2+xFe2+1.xFe3+204(II) where 5 M is selected from among Co, Ni, Mn, Zn and mixtures thereof and x is 1, hexagonal ferrites and mixtures thereof. 10
8. The process according to any of claims 1 to 7, wherein the dispersion medium is water.
9. The process according to any of claims 1 to 8, wherein the mixture comprising at least one first material and at least one second material is milled to particles 15 having a size of from 100 nm to 100 pm before or during step (A).
10. The process according to any of claims 1 to 9, wherein contacting the mixture comprising at least one first material and at least one second material with at least one magnetic particle and at least one surface-modifying substance at the 20 same time in step (A) is achieved by addition of a mixture, preferably a disper sion, of least one magnetic particle and at least one surface-modifying sub stance.
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| EP12165162.4 | 2012-04-23 | ||
| PCT/EP2013/058245 WO2013160219A1 (en) | 2012-04-23 | 2013-04-22 | Magnetic separation of particles including one-step-conditioning of a pulp |
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| AU2013254846A1 true AU2013254846A1 (en) | 2014-10-23 |
| AU2013254846B2 AU2013254846B2 (en) | 2017-12-07 |
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| EP (1) | EP2841204B1 (en) |
| CN (1) | CN104271247B (en) |
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| ATE25595T1 (en) | 1981-10-26 | 1987-03-15 | Wsr Pty Ltd | MAGNETIC FLOTATION PROCESS. |
| GB8726857D0 (en) | 1987-11-17 | 1987-12-23 | Fospur Ltd | Froth floatation of mineral fines |
| US4834898A (en) | 1988-03-14 | 1989-05-30 | Board Of Control Of Michigan Technological University | Reagents for magnetizing nonmagnetic materials |
| DE19936472A1 (en) | 1999-08-03 | 2001-02-15 | Stn Atlas Elektronik Gmbh | Adhesion promoter |
| NO312373B1 (en) | 2000-06-29 | 2002-04-29 | Kjell Birkeland | Wall construction, especially for a valuables storage box, as well as the use of such a wall structure sometimes sidewalls in a storage box |
| ES2360232T3 (en) | 2005-06-29 | 2011-06-02 | Compumedics Limited | SENSOR ASSEMBLY WITH DRIVING BRIDGE. |
| UA97543C2 (en) * | 2007-09-03 | 2012-02-27 | Басф Се | Processing rich ores using magnetic particles |
| PE20120524A1 (en) * | 2008-12-11 | 2012-04-28 | Basf Se | ENRICHMENT OF MINERALS FROM MINING WASTE |
| EP2498913B8 (en) * | 2009-11-11 | 2014-10-08 | Basf Se | Method for increasing efficiency in the ore separating process by means of hydrophobic magnetic particles by applying targeted mechanical energy |
| AU2011335037A1 (en) * | 2010-11-29 | 2013-06-13 | Basf Corporation | Magnetic recovery of valuables from slag material |
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- 2013-04-22 AP AP2014008061A patent/AP2014008061A0/en unknown
- 2013-04-22 EA EA201491892A patent/EA201491892A1/en unknown
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| AU2013254846B2 (en) | 2017-12-07 |
| WO2013160219A1 (en) | 2013-10-31 |
| CN104271247A (en) | 2015-01-07 |
| PE20142381A1 (en) | 2015-01-30 |
| EA201491892A1 (en) | 2015-04-30 |
| CA2869226C (en) | 2020-03-10 |
| EP2841204A1 (en) | 2015-03-04 |
| CL2014002864A1 (en) | 2014-12-19 |
| CA2869226A1 (en) | 2013-10-31 |
| AP2014008061A0 (en) | 2014-11-30 |
| CN104271247B (en) | 2017-10-27 |
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