JP2015506896A - 塩化鉄(iii)含有塩酸溶液中の金属塩化物を濃縮し、かつこれを該溶液から分離する方法 - Google Patents
塩化鉄(iii)含有塩酸溶液中の金属塩化物を濃縮し、かつこれを該溶液から分離する方法 Download PDFInfo
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 455
- 238000000034 method Methods 0.000 title claims abstract description 130
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims abstract description 126
- 229910001510 metal chloride Inorganic materials 0.000 title claims abstract description 107
- 229910021578 Iron(III) chloride Inorganic materials 0.000 title claims abstract description 63
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 264
- 229910052742 iron Inorganic materials 0.000 claims abstract description 134
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000001914 filtration Methods 0.000 claims abstract description 29
- 239000000706 filtrate Substances 0.000 claims abstract description 28
- 239000011019 hematite Substances 0.000 claims abstract description 24
- 229910052595 hematite Inorganic materials 0.000 claims abstract description 24
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims abstract description 24
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 147
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 147
- 238000006460 hydrolysis reaction Methods 0.000 claims description 123
- 230000007062 hydrolysis Effects 0.000 claims description 118
- 238000002425 crystallisation Methods 0.000 claims description 46
- 230000008025 crystallization Effects 0.000 claims description 46
- 239000000047 product Substances 0.000 claims description 17
- 238000000638 solvent extraction Methods 0.000 claims description 17
- 239000012074 organic phase Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 185
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 58
- 229910001868 water Inorganic materials 0.000 description 58
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 30
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 30
- 238000009833 condensation Methods 0.000 description 24
- 230000005494 condensation Effects 0.000 description 24
- 238000004519 manufacturing process Methods 0.000 description 21
- 238000012360 testing method Methods 0.000 description 19
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- 238000009835 boiling Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- 238000011069 regeneration method Methods 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 239000012141 concentrate Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 230000008929 regeneration Effects 0.000 description 9
- 239000008346 aqueous phase Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 238000009834 vaporization Methods 0.000 description 7
- 230000008016 vaporization Effects 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 5
- 150000003841 chloride salts Chemical class 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 5
- 239000002826 coolant Substances 0.000 description 5
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- -1 ferrous metals Chemical class 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 239000011565 manganese chloride Substances 0.000 description 5
- 235000002867 manganese chloride Nutrition 0.000 description 5
- 229940099607 manganese chloride Drugs 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000011144 upstream manufacturing Methods 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000009854 hydrometallurgy Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000012492 regenerant Substances 0.000 description 2
- 238000010956 selective crystallization Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052781 Neptunium Inorganic materials 0.000 description 1
- 241000282372 Panthera onca Species 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 229910052767 actinium Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- YPLPZEKZDGQOOQ-UHFFFAOYSA-M iron oxychloride Chemical compound [O][Fe]Cl YPLPZEKZDGQOOQ-UHFFFAOYSA-M 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-N iron;hydrochloride Chemical compound Cl.[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910001710 laterite Inorganic materials 0.000 description 1
- 239000011504 laterite Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
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- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/02—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
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Abstract
Description
鉄含有塩酸溶液は、供給ライン(1)を介して、加水分解リアクター1にポンピングされ、ここで、加水分解反応が生じる。ここでは、溶液中の塩化鉄(III)が水と反応して、塩酸および酸化鉄、好ましくはヘマタイトを形成し、これが、溶液から沈殿する。従って、鉄含有塩酸溶液中の非加水分解性金属塩化物が濃縮される。溶液の一部は加水分解リアクター1から取り出され、循環ライン(4)を介して、例えば、蒸気または熱伝達オイルで作動される外部熱交換器4の中にポンピングされる。この溶液は、この熱交換器4の中で過熱され、水および塩化水素の気化によって加水分解リアクター1の中で除圧される。この加水分解蒸気は、加水分解リアクター1から排出ライン(2)を介して取り出され、凝縮器5の中で凝縮される。生成された再生物は、ドレイン(3)を介してこのプロセスから取り出され、次に、製造プラントで用いられて、これによって塩化物回路が完了する。
実施例1では、大気圧下の濃縮された塩化鉄(III)溶液中における、非加水分解性の要素としての塩化マンガンの気液平衡を決定するための試験を決定する。還流冷却器は、外部加熱されたガラスリアクター上に導入される。試験すべき溶液は、リアクターに入れられ、沸騰させられる。温度は連続して記録される。一旦、平衡に達してから、ガラスリアクター中および蒸留物中の濃縮された塩化鉄(III)溶液の組成を分析する。沸点はまた、サンプル取り出しの時点でも記録する。
さらなる試験において、塩化鉄(III)溶液中のニッケルの蒸気圧を決定した。この試験は、75重量%の総塩濃度に基づいて行った。
総塩濃度を増大することによって、蒸気相中の沸点および塩化水素濃度が増大される。72.8重量%の塩化鉄(III)および4.6重量%のニッケル濃度を有する濃縮された塩化鉄(III)水溶液は、184℃の沸点を有する。蒸気中の塩化水素の濃度は、27.6重量%である。
半連続加水分解を実施例4で行った。純粋な塩化鉄(III)合成溶液(75重量%)を、加熱されたガラスリアクターに入れる。蒸気は、蒸留器ブリッジを介して運ばれて、凝縮される。凝縮物は収集される。加水分解リアクター中の溶液は、沸騰される。一旦、沸点に達すれば、供給物を加水分解リアクター中に導入する。供給溶液の組成は、30重量%の塩化鉄(III)と2重量%の塩化ニッケルである。供給率を制御して、ガラスリアクター中の沸点を、170℃で一定に保持する。試験は3時間を超えて行われ、鉄含有塩酸加水分解溶液中の塩化ニッケルの濃度は、この試験の終わりにおいて1.1重量%である。全体的にみれば、約200gの酸化鉄が生成された。酸化鉄中のニッケル濃度は、GDMS(グロー放電質量分析)によって決定され、200ppmであった。この試験によって、ニッケルは加水分解せず、従って、加水分解リアクター中で濃縮され得ることが示される。
鉄含有塩酸溶液からの塩化ニッケルの沈殿のための結晶化試験を、実施例5で行った。塩化鉄(III)および塩化ニッケルの合成溶液を、結晶化リアクター中に入れた。試験の開始時点において、この溶液は、47重量%の塩化鉄(III)および11重量%の塩化ニッケルを含む。純粋な塩化水素をリアクター中に注入し、鉄含有塩酸溶液中に溶解する。試験は、60℃で行った。温度は、サーモスタットによって外部で制御した。
2つの非加水分解性金属塩化物である塩化ニッケルおよび塩化コバルトを含む塩化鉄(III)溶液を用いてさらなる結晶化試験を行った。
塩化セリウム(III)でのさらなる結晶化試験を行った。
実施例8では、本発明による方法の変形例のバランスが示され、図4に図示される。ここでは非加水分解金属塩化物、具体的には塩化ニッケルと混合された鉄含有塩酸溶液が処理される。鉄含有塩酸溶液中に含まれる塩化ニッケルは、最初に、加水分解リアクター中で濃縮され、当該塩化ニッケルは、さらなる方法工程において結晶化リアクター中の鉄含有塩酸溶液中の遊離の塩化水素の濃度を増加させることによって結晶化され、鉄から分離される。
1 加水分解リアクター
2 濾過装置
3 溶媒抽出用の装置
4 熱交換器
5 凝縮器
6 有機相のストリッピング用の装置
7 結晶化リアクター
8 金属塩化物の濾過用の装置
9 塩化水素の生成用の装置
10 プレエバポレーター
11 プレエバポレーター用の凝縮器
ライン
(1) 加水分解リアクターへの供給ライン
(2) 加水分解リアクターからの排出ライン
(3) 再生物用のドレイン
(4) 加水分解リアクター中の循環ライン
(5) 濾過装置への供給ライン
(6) 酸化鉄のドレイン
(7) 濾液の戻り
(8) 溶媒抽出用の装置への供給ライン
(9) 鉄含有塩酸溶液の戻り
(10) 有機相のストリッピング用の装置への供給ライン
(11) 有機相の戻りライン
(12) 水用の供給ライン
(13) 金属塩化物のドレイン
(14) 塩化水素の供給ライン
(15) 塩化水素濃縮用の装置への再生物用の供給ライン
(16) 水の戻り
(17) 金属塩化物の濾過用の装置への供給ライン
(18) 結晶化リアクターへの供給ライン
(19) プレエバポレーター用の循環ライン
(20) プレエバポレーター用の供給ライン
(21) プレエバポレーター用の放出ライン
Claims (6)
- 塩化鉄(III)含有塩酸溶液中の金属塩化物を濃縮し、かつ該溶液から前記金属塩化物を分離する方法であって、鉄を酸化鉄、好ましくはヘマタイトとして該溶液から沈殿させ、濾過装置中で濾別してから、それによりさらに濃縮された非加水分解性金属塩化物を塩酸濾液の少なくとも一部から取り出すことを特徴とする方法。
- 前記非加水分解性金属塩化物が、該鉄含有塩酸濾液の少なくとも一部からの溶媒抽出によって選択的に取り出され、かつ該金属塩化物がストリッピング法により有機相から逆抽出されることを特徴とする、請求項1に記載の方法。
- 抽出される各金属塩化物にあわせた溶媒抽出方法が順次行われることを特徴とする、請求項2に記載の方法。
- 該鉄含有塩酸濾液に含まれる塩化鉄(III)が、溶媒抽出によって直接的に抽出されることを特徴とする、請求項1〜3のいずれか1項に記載の方法。
- 前記濃縮された非加水分解性金属塩化物を、前記鉄含有塩酸溶液中の遊離の塩化水素の濃度を増加させることによって該溶液から沈殿させることを特徴とする、請求項1〜4のいずれか1項に記載の方法。
- 加水分解により得られる再生物の一部が取り出され、結晶化のための純粋な塩化水素が濃縮工程において前記再生物から得られることを特徴とする、請求項5に記載の方法。
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CN110467223A (zh) * | 2019-07-17 | 2019-11-19 | 李柏丛 | 钢厂酸洗液生产的氧化铁红制备高性能氧化铁用于软磁材料的新工艺 |
RU2725322C1 (ru) * | 2020-02-18 | 2020-07-02 | Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "Кольский научный центр Российской академии наук" (ФИЦ КНЦ РАН) | Способ очистки хлоридного раствора от железа |
RU2752352C1 (ru) * | 2020-09-16 | 2021-07-26 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Способ переработки отходов растворов хлоридов железа |
CN113479937B (zh) * | 2021-07-02 | 2023-01-03 | 内蒙古科技大学 | 一种制备类球形氧化铁的方法 |
CN113533629B (zh) * | 2021-07-20 | 2024-03-26 | 广东先导稀材股份有限公司 | 一种四氯化碲样品中游离盐酸含量的测定方法 |
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EP2791060B8 (de) | 2019-04-10 |
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CA2859207A1 (en) | 2013-06-20 |
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JP6468841B2 (ja) | 2019-02-13 |
BR112014014197B1 (pt) | 2020-12-08 |
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