HRP20171983T1 - POSTUPAK PRIPREME KRISTALA KOBALTOVOG NITRATA VISOKE ČISTOĆE IZ ISTROŠENIH KATALIZATORA Co/SiO2 - Google Patents
POSTUPAK PRIPREME KRISTALA KOBALTOVOG NITRATA VISOKE ČISTOĆE IZ ISTROŠENIH KATALIZATORA Co/SiO2 Download PDFInfo
- Publication number
- HRP20171983T1 HRP20171983T1 HRP20171983TT HRP20171983T HRP20171983T1 HR P20171983 T1 HRP20171983 T1 HR P20171983T1 HR P20171983T T HRP20171983T T HR P20171983TT HR P20171983 T HRP20171983 T HR P20171983T HR P20171983 T1 HRP20171983 T1 HR P20171983T1
- Authority
- HR
- Croatia
- Prior art keywords
- solution
- preheated
- temperature
- cobalt
- cobalt nitrate
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims 11
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 title claims 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 title claims 8
- 239000003054 catalyst Substances 0.000 title claims 5
- 239000013078 crystal Substances 0.000 title claims 3
- 239000002699 waste material Substances 0.000 title 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 19
- 239000000243 solution Substances 0.000 claims 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 6
- 235000006408 oxalic acid Nutrition 0.000 claims 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 5
- 239000008367 deionised water Substances 0.000 claims 5
- 229910021641 deionized water Inorganic materials 0.000 claims 5
- 229910017604 nitric acid Inorganic materials 0.000 claims 5
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims 3
- 229910052681 coesite Inorganic materials 0.000 claims 3
- 229910052906 cristobalite Inorganic materials 0.000 claims 3
- 239000000843 powder Substances 0.000 claims 3
- 239000002244 precipitate Substances 0.000 claims 3
- 239000000377 silicon dioxide Substances 0.000 claims 3
- 235000012239 silicon dioxide Nutrition 0.000 claims 3
- 229910052682 stishovite Inorganic materials 0.000 claims 3
- 229910052905 tridymite Inorganic materials 0.000 claims 3
- 239000012670 alkaline solution Substances 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 2
- 229910000428 cobalt oxide Inorganic materials 0.000 claims 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 239000000706 filtrate Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0438—Nitric acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/32—Carboxylic acids
- C22B3/322—Oxalic acids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Geochemistry & Mineralogy (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Removal Of Specific Substances (AREA)
- Manufacture And Refinement Of Metals (AREA)
Claims (9)
1. Postupak pripreme kristala kobaltovog nitrata iz istrošenog katalizatora Co/SiO2, naznačen time, da postupak obuhvaća sljedeće korake:
1) kalciniranje istrošenog katalizatora Co/SiO2 u prisutnosti zraka između 3 i 6 sati na temperaturi između 350 i 500°C, hlađenje na sobnu temperaturu, te mljevenje istrošenog katalizatora Co/SiO2 čime se dobije prašak;
2) uvođenje praha u reaktor s fluidiziranim slojem, ostavljanje da se prah reducira tijekom između 8 i 12 sati u prisutnosti mješavine plina H2 i N2, uz omjer volumena H2 i N2 mješavini plina koja je između 1: 1 i 4: 1;
3) dodavanje reduciranog potrošenog katalizatora u prekomjerno razrijeđenu otopinu dušične kiseline radi otapanja, filtriranja i sakupljanja otopine kobaltovog nitrata;
4) podešavanje pH vrijednosti otopine kobaltovog nitrata korištenjem alkalne otopine da bude 1.5, dodavanje prethodno zagrijane otopine oksalne kiseline koja ima temperaturu od između 25 i 80°C i pH vrijednost od 1.5 u otopinu kobalt nitrata u prisutnosti vodene kupelji od između 25 i 80°C, prilagođavanje pH vrijednosti dobivene otopine koristeći razrijeđenu alkalnu otopinu da bude 1.5, neposredno filtriranje dobivene otopine da se dobije talog kobalt oksalata, ispiranje taloga kobalt oksalata korištenjem deionizirane vode da se dobije neutralni filtrat, pri čemu se, molarni broj oksalne kiseline u otopini oksalne kiseline kontrolira da bude između 2 i 3 puta molarni broj kobalta u otopini kobalt nitrata;
5) sušenje taloga kobalt oksalata i kalciniranje između 4 i 8 sati na temperaturi od između 550 i 650°C, da se dobije kobaltov oksid;
6) otapanje kobaltovog oksida s razrijeđenom otopinom dušične kiseline da se dobije druga otopina kobaltovog nitrata; i
7) isparavanje i kristalizaciju druge otopine kobaltovog nitrata da se dobije kristal Co(NO3)2·6H2O.
2. Postupak prema zahtjevu 1, naznačen time da u koraku 2), brzina protoka miješanog plina iznosi između 1000 i 4000 h-1, tlak reaktora s fluidiziranim slojem je između 0.1 i 1 MPa, a temperatura reakcije je između 350 i 750°C.
3. Postupak prema zahtjevu 1 ili 2, naznačen time da u koraku 3), otopina razrijeđene dušične kiseline ima koncentraciju od 1 i 3 mol/L.
4. Postupak prema zahtjevu 1 ili 2, naznačen time da u koraku 6), otopina razrijeđene dušične kiseline ima koncentraciju od 1 i 3 mol/L.
5. Postupak prema zahtjevu 3, naznačen time da u koraku 6), otopina razrijeđene dušične kiseline ima koncentraciju od 1 i 3 mol/L.
6. Postupak prema zahtjevu 1 ili 2, naznačen time da u koraku 4), vodena kupelj ima temperaturu od 70°C, otopina oksalne kiseline se prethodno zagrijava na 70°C, a deionizirana voda se prethodno zagrijava na 70°C.
7. Postupak prema zahtjevu 3, naznačen time da u koraku 4), vodena kupelj ima temperaturu od 70°C, otopina oksalne kiseline se prethodno zagrijava na 70°C, a deionizirana voda se prethodno zagrijava na 70°C.
8. Postupak prema zahtjevu 4, naznačen time da u koraku 4), vodena kupelj ima temperaturu od 70°C, otopina oksalne kiseline se prethodno zagrijava na 70°C, a deionizirana voda se prethodno zagrijava na 70°C.
9. Postupak prema zahtjevu 5, naznačen time da u koraku 4), vodena kupelj ima temperaturu od 70°C, otopina oksalne kiseline se prethodno zagrijava na 70°C, a deionizirana voda se prethodno zagrijava na 70°C.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210055799.5A CN102583580B (zh) | 2012-03-05 | 2012-03-05 | 利用Co/SiO2废催化剂制备高纯硝酸钴晶体的方法 |
| EP13757151.9A EP2824075B1 (en) | 2012-03-05 | 2013-03-04 | Method for preparing high-purity cobalt nitrate crystals from co/sio2 waste catalysts |
| PCT/CN2013/072109 WO2013131452A1 (zh) | 2012-03-05 | 2013-03-04 | 利用Co/SiO2废催化剂制备高纯硝酸钴晶体的方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| HRP20171983T1 true HRP20171983T1 (hr) | 2018-02-23 |
Family
ID=46472943
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| HRP20171983TT HRP20171983T1 (hr) | 2012-03-05 | 2017-12-20 | POSTUPAK PRIPREME KRISTALA KOBALTOVOG NITRATA VISOKE ČISTOĆE IZ ISTROŠENIH KATALIZATORA Co/SiO2 |
Country Status (20)
| Country | Link |
|---|---|
| US (1) | US8986644B2 (hr) |
| EP (1) | EP2824075B1 (hr) |
| JP (1) | JP5837998B2 (hr) |
| KR (1) | KR101567589B1 (hr) |
| CN (1) | CN102583580B (hr) |
| AP (1) | AP2014007987A0 (hr) |
| AU (1) | AU2013230404B2 (hr) |
| BR (1) | BR112014021849B1 (hr) |
| CA (1) | CA2866188C (hr) |
| DK (1) | DK2824075T3 (hr) |
| HR (1) | HRP20171983T1 (hr) |
| HU (1) | HUE036070T2 (hr) |
| IN (1) | IN2014MN01922A (hr) |
| MX (1) | MX355250B (hr) |
| MY (1) | MY157636A (hr) |
| RU (1) | RU2580744C1 (hr) |
| SG (1) | SG11201405384YA (hr) |
| SI (1) | SI2824075T1 (hr) |
| WO (1) | WO2013131452A1 (hr) |
| ZA (1) | ZA201407150B (hr) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543496B (zh) * | 2015-12-29 | 2017-10-20 | 武汉凯迪工程技术研究总院有限公司 | 费托合成废催化剂Co‑Rh/Al2O3中金属钴、铑和铝的回收方法 |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125781C (zh) * | 2001-11-13 | 2003-10-29 | 山东大学 | 四氧化三钴纳米粉体的制备方法 |
| US7285188B2 (en) * | 2001-12-21 | 2007-10-23 | Georgia Tech Research Corporation | Oxynitride compounds, methods of preparation, and uses thereof |
| CN1190266C (zh) * | 2002-08-19 | 2005-02-23 | 中国科学院山西煤炭化学研究所 | 一种用于费托合成的含钴废催化剂的回收方法 |
| AU2005318130B2 (en) * | 2004-12-23 | 2009-04-30 | Shell Internationale Research Maatschappij B.V. | Method of preparing catalyst support from a waste catalyst |
| WO2008139407A2 (en) * | 2007-05-11 | 2008-11-20 | Sasol Technology (Proprietary) Limited | Catalysts |
| CN101270420A (zh) * | 2008-05-19 | 2008-09-24 | 中国科学院山西煤炭化学研究所 | 一种钴基费托合成催化剂中钴的回收方法 |
| CN101698152A (zh) * | 2009-10-20 | 2010-04-28 | 武汉凯迪科技发展研究院有限公司 | 一种钴基费托合成催化剂及其制备方法和应用 |
| CN101700913B (zh) * | 2009-11-17 | 2011-05-18 | 中南民族大学 | 利用费托合成用氧化铝负载钴基废催化剂制备高纯硝酸钴 |
| CN102796873B (zh) * | 2012-03-05 | 2014-02-26 | 阳光凯迪新能源集团有限公司 | 从费托合成废催化剂Co-Ru/Al2O3中综合回收金属钴、钌和铝的方法 |
-
2012
- 2012-03-05 CN CN201210055799.5A patent/CN102583580B/zh active Active
-
2013
- 2013-03-04 MY MYPI2014002570A patent/MY157636A/en unknown
- 2013-03-04 RU RU2014140152/05A patent/RU2580744C1/ru not_active IP Right Cessation
- 2013-03-04 DK DK13757151.9T patent/DK2824075T3/en active
- 2013-03-04 AU AU2013230404A patent/AU2013230404B2/en not_active Ceased
- 2013-03-04 EP EP13757151.9A patent/EP2824075B1/en not_active Not-in-force
- 2013-03-04 AP AP2014007987A patent/AP2014007987A0/xx unknown
- 2013-03-04 KR KR1020147027913A patent/KR101567589B1/ko active IP Right Grant
- 2013-03-04 IN IN1922MUN2014 patent/IN2014MN01922A/en unknown
- 2013-03-04 HU HUE13757151A patent/HUE036070T2/hu unknown
- 2013-03-04 WO PCT/CN2013/072109 patent/WO2013131452A1/zh active Application Filing
- 2013-03-04 SI SI201330896T patent/SI2824075T1/en unknown
- 2013-03-04 SG SG11201405384YA patent/SG11201405384YA/en unknown
- 2013-03-04 JP JP2014560229A patent/JP5837998B2/ja active Active
- 2013-03-04 MX MX2014010568A patent/MX355250B/es active IP Right Grant
- 2013-03-04 CA CA2866188A patent/CA2866188C/en not_active Expired - Fee Related
- 2013-03-04 BR BR112014021849-8A patent/BR112014021849B1/pt not_active IP Right Cessation
-
2014
- 2014-09-05 US US14/477,909 patent/US8986644B2/en active Active
- 2014-10-02 ZA ZA2014/07150A patent/ZA201407150B/en unknown
-
2017
- 2017-12-20 HR HRP20171983TT patent/HRP20171983T1/hr unknown
Also Published As
| Publication number | Publication date |
|---|---|
| EP2824075A1 (en) | 2015-01-14 |
| CA2866188C (en) | 2017-04-18 |
| WO2013131452A1 (zh) | 2013-09-12 |
| KR20140130748A (ko) | 2014-11-11 |
| IN2014MN01922A (hr) | 2015-07-10 |
| DK2824075T3 (en) | 2018-01-15 |
| US20140377153A1 (en) | 2014-12-25 |
| HUE036070T2 (hu) | 2018-06-28 |
| AU2013230404A1 (en) | 2014-10-16 |
| CN102583580A (zh) | 2012-07-18 |
| RU2580744C1 (ru) | 2016-04-10 |
| SG11201405384YA (en) | 2014-10-30 |
| EP2824075B1 (en) | 2017-10-11 |
| CA2866188A1 (en) | 2013-09-12 |
| CN102583580B (zh) | 2014-03-12 |
| AU2013230404B2 (en) | 2015-02-19 |
| ZA201407150B (en) | 2015-11-25 |
| JP5837998B2 (ja) | 2015-12-24 |
| KR101567589B1 (ko) | 2015-11-09 |
| BR112014021849B1 (pt) | 2020-12-15 |
| MX2014010568A (es) | 2014-12-08 |
| AP2014007987A0 (en) | 2014-10-31 |
| MY157636A (en) | 2016-07-15 |
| MX355250B (es) | 2018-04-11 |
| EP2824075A4 (en) | 2015-11-18 |
| US8986644B2 (en) | 2015-03-24 |
| SI2824075T1 (en) | 2018-05-31 |
| JP2015515362A (ja) | 2015-05-28 |
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