WO2024138593A1 - Procédé de traitement pour la récupération d'étain, de fer et de manganèse par élution à l'acide sulfurique de laitier de tantale - Google Patents
Procédé de traitement pour la récupération d'étain, de fer et de manganèse par élution à l'acide sulfurique de laitier de tantale Download PDFInfo
- Publication number
- WO2024138593A1 WO2024138593A1 PCT/CN2022/143744 CN2022143744W WO2024138593A1 WO 2024138593 A1 WO2024138593 A1 WO 2024138593A1 CN 2022143744 W CN2022143744 W CN 2022143744W WO 2024138593 A1 WO2024138593 A1 WO 2024138593A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- manganese
- slag
- tin
- sulfuric acid
- iron
- Prior art date
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 74
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000011135 tin Substances 0.000 title claims abstract description 46
- 239000002893 slag Substances 0.000 title claims abstract description 44
- 229910052718 tin Inorganic materials 0.000 title claims abstract description 44
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 36
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000011572 manganese Substances 0.000 title claims abstract description 34
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 33
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000010828 elution Methods 0.000 title abstract 2
- 239000000706 filtrate Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 12
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 11
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 11
- 230000002378 acidificating effect Effects 0.000 claims abstract description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 7
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 7
- 235000006748 manganese carbonate Nutrition 0.000 claims abstract description 6
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 6
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 6
- 229940093474 manganese carbonate Drugs 0.000 claims abstract description 3
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 claims description 2
- 238000011085 pressure filtration Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003546 flue gas Substances 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 230000001698 pyrogenic effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000012065 filter cake Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- 239000007832 Na2SO4 Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 241001274216 Naso Species 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- -1 iron-manganese-tantalum Chemical compound 0.000 description 1
- IGSZZIUPCQHSQB-UHFFFAOYSA-N manganese tantalum Chemical compound [Mn][Ta] IGSZZIUPCQHSQB-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Definitions
- the invention belongs to the field of waste recovery and environmental protection, and specifically relates to a process for eluting sulfuric acid from tantalum slag containing tin, iron and manganese, and comprehensively recovering tin, iron and manganese.
- Tantalum is an important rare metal with a high melting point and has been widely used in many fields.
- the method of smelting tantalum ore by high-temperature roasting with concentrated sulfuric acid is to make tantalum soluble, extract it with water, and then recover it from the filtrate. If the tantalum ore contains tin, iron and manganese, the remaining tantalum slag contains 15% to 20% sulfuric acid, 7% to 8% Sn, 6% to 15% Fe, 6% to 10% Mn, and the rest is water and gangue.
- the tin contained in the tantalum slag is a high-value resource. It can generally be disposed of in a fuming furnace to recover high-grade tin-containing smoke.
- the raw materials contain a large amount of sulfuric acid, the environmental load of the smelting flue gas is huge, the operation is difficult, and sometimes the fuming furnace equipment is damaged; on the other hand, because of the high manganese content, the fuming furnace slag type is not suitable for smelting, which causes difficulties, so a large amount of filter residue inventory is accumulated, resulting in the difficulty of using resources and waste, and at the same time forming serious environmental safety hazards.
- the purpose of the present invention is to provide a process for eluting tantalum slag with sulfuric acid to recover tin, iron and manganese, so as to elute tantalum slag containing tin, iron and manganese with sulfuric acid and recover tin, iron and manganese at the same time.
- step C Add hydrogen peroxide to the acidic filtrate obtained in step A to oxidize Fe 2+ in the filtrate to Fe 3+ .
- the amount of hydrogen peroxide added depends on the amount of Fe 2+ in the tantalum slag. It is sufficient to oxidize all Fe 2+ to Fe 3+ .
- the filtrate is reserved for later use.
- the method of the present invention can leach and separate the residual sulfuric acid, ferrous sulfate and manganese sulfate in the tantalum slag, thereby reducing the improper influence on the slag type during the recovery of the pyro-fuming furnace and the adverse impact of a large amount of sulfuric acid-containing flue gas on the environment; at the same time, the tin grade is improved by 200%, which greatly improves the tin recovery index and increases the economic benefits; the iron and manganese recovered incidentally also have certain resources and economic benefits. This method enables the precious resources that cannot be directly used by the fuming furnace to achieve real environmental protection and harmless utilization.
Abstract
L'invention concerne un procédé de traitement pour la récupération d'étain, de fer et de manganèse par élution à l'acide sulfurique de laitier de tantale, ce procédé comprenant les opérations consistant à : ajouter de l'eau dans du laitier de tantale pour lixivier l'acide sulfurique soluble, le sulfate ferreux et le sulfate de manganèse dans le laitier de tantale, et effectuer une filtration-compression pour séparer un filtrat acide et des résidus de filtration contenant de l'étain ; et oxyder Fe2+dans le filtrat acide en Fe3+, effectuer une séparation par précipitation sur Fe3+, effectuer une filtration-compression pour obtenir du laitier de fer ; ajouter en continu du carbonate de sodium dans le filtrat pour générer un précipité de carbonate de manganèse, et effectuer une filtration-compression pour obtenir du laitier de manganèse. Selon le procédé, l'acide sulfurique résiduel, le sulfate ferreux résiduel et le sulfate de manganèse résiduel dans les scories de tantale sont lixiviés et séparés, de telle sorte que l'incidence indésirable sur le type de laitier et l'effet défavorable d'une grande quantité de gaz de combustion contenant de l'acide sulfurique sur l'environnement pendant la récupération par un four d'évaporation pyrogène peuvent être réduits ; et de plus, la qualité d'étain est améliorée, et le fer et le manganèse qui sont récupérés ont certaines ressources et avantages économiques. Selon le procédé, un recyclage respectueux de l'environnement réel et une utilisation sans danger de ressources de valeur qui ne peuvent pas être directement utilisées par le four d'évaporation sont réalisés.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2024138593A1 true WO2024138593A1 (fr) | 2024-07-04 |
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