HRP20200081T1 - Proizvodnja fosfatnih spojeva od materijala koji sadrže fosfor i barem jedan odabran od željeza i aluminija - Google Patents
Proizvodnja fosfatnih spojeva od materijala koji sadrže fosfor i barem jedan odabran od željeza i aluminija Download PDFInfo
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- HRP20200081T1 HRP20200081T1 HRP20200081TT HRP20200081T HRP20200081T1 HR P20200081 T1 HRP20200081 T1 HR P20200081T1 HR P20200081T T HRP20200081T T HR P20200081TT HR P20200081 T HRP20200081 T HR P20200081T HR P20200081 T1 HRP20200081 T1 HR P20200081T1
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- Prior art keywords
- phosphate
- solution
- washing solution
- precipitated
- iron
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims 30
- 229910052742 iron Inorganic materials 0.000 title claims 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims 11
- 229910052698 phosphorus Inorganic materials 0.000 title claims 11
- 239000011574 phosphorus Substances 0.000 title claims 11
- 229910052782 aluminium Inorganic materials 0.000 title claims 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims 9
- 238000004519 manufacturing process Methods 0.000 title claims 3
- 239000004411 aluminium Substances 0.000 title 1
- 239000000463 material Substances 0.000 title 1
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 title 1
- 239000000243 solution Substances 0.000 claims 45
- 238000005406 washing Methods 0.000 claims 29
- 238000000034 method Methods 0.000 claims 25
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 22
- 239000003960 organic solvent Substances 0.000 claims 13
- 238000000926 separation method Methods 0.000 claims 13
- 238000001556 precipitation Methods 0.000 claims 11
- 239000007921 spray Substances 0.000 claims 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 8
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims 5
- 238000004064 recycling Methods 0.000 claims 5
- 239000012487 rinsing solution Substances 0.000 claims 5
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims 4
- 239000002253 acid Substances 0.000 claims 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 4
- 239000003085 diluting agent Substances 0.000 claims 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecanol group Chemical group C(CCCCCCCCCCC)O LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims 4
- 239000004571 lime Substances 0.000 claims 4
- 239000003607 modifier Substances 0.000 claims 4
- 239000002994 raw material Substances 0.000 claims 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 3
- 239000002904 solvent Substances 0.000 claims 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 2
- 239000001506 calcium phosphate Substances 0.000 claims 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims 2
- 235000011010 calcium phosphates Nutrition 0.000 claims 2
- 229960004887 ferric hydroxide Drugs 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 2
- 229910001385 heavy metal Inorganic materials 0.000 claims 2
- 235000014413 iron hydroxide Nutrition 0.000 claims 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims 2
- 239000003350 kerosene Substances 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 2
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims 2
- 238000011084 recovery Methods 0.000 claims 2
- 239000010802 sludge Substances 0.000 claims 2
- 238000005507 spraying Methods 0.000 claims 2
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 claims 1
- 125000001931 aliphatic group Chemical group 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 239000001569 carbon dioxide Substances 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 1
- 150000001768 cations Chemical class 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical class [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- 239000007800 oxidant agent Substances 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 235000021317 phosphate Nutrition 0.000 claims 1
- 150000003568 thioethers Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
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- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/2208—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with an acid or a mixture of acids other than sulfuric acid
- C01B25/2212—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with an acid or a mixture of acids other than sulfuric acid with hydrochloric acid or hydrogen chloride in aqueous medium
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- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
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- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
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- C05B—PHOSPHATIC FERTILISERS
- C05B1/00—Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
- C05B1/04—Double-superphosphate; Triple-superphosphate; Other fertilisers based essentially on monocalcium phosphate
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Claims (15)
1. Postupak za koncentriranje fosfatnih spojeva, koji sadrži korake:
- otapanje (205) sirovog materijala koji sadrži pepeo mulja, koji sadrži fosfor i barem jedan od željeza i aluminija, u tekućini koja sadrži barem klorovodičnu kiselinu;
- razdvajanje (210) netopivih ostataka iz spomenutog koraka otapanja, čime se dobiva prva otopina za ispiranje;
- kontroliranje (215) molarnog omjera fosfora naspram sume trovalentnog željeza i aluminija spomenute prve otopine za ispiranje kako bi bio veći od 1;
- dodavanje (220) baze u spomenutu prvu otopinu za ispiranje, nakon spomenutog koraka razdvajanja (210) netopivih ostataka, čime se izaziva taloženje fosfatnih spojeva koji sadrže barem jedan od željeza ili aluminija iz spomenute prve otopine za ispiranje;
- uklanjanje (225) spomenutih istaloženih fosfatnih spojeva iz spomenute prve otopine za ispiranje;
- dodavanje (240) sumporne kiseline u spomenutu prvu otopinu za ispiranje nakon spomenutog koraka uklanjanja (225) spomenutih istaloženih fosfatnih spojeva, čime se izaziva taloženje sulfatnih spojeva;
- razdvajanje (245) spomenutih istaloženih sulfatnih spojeva iz spomenute prve otopine za ispiranje; i
- recikliranje (248) barem dijela spomenute prve otopine za ispiranje nakon spomenutog koraka razdvajanja (245) spomenutih sulfatnih spojeva kao spomenute tekućine koja sadrži barem klorovodičnu kiselinu u spomenutom koraku otapanja (205) pepela mulja.
2. Postupak prema zahtjevu 1, naznačen time što spomenuti korak kontroliranja (215) spomenutog molarnog omjera sadrži barem jedno od:
- dodavanje fosfora u spomenutu prvu otopinu za ispiranje tijekom spomenutog koraka otapanja sirovog materijala;
- dodavanje fosfora u spomenutu prvu otopinu za ispiranje nakon spomenutog koraka otapanja sirovog materijala; i
- dodavanje fosfora u spomenuti sirovi materijal.
3. Postupak prema zahtjevu 1 ili 2, naznačen time što spomenuta baza sadrži vapno.
4. Postupak prema zahtjevu 1 ili 2, naznačen time što spomenuta baza sadrži željezni hidroksid.
5. Postupak prema bilo kojem od zahtjeva 1-4, naznačen daljnjim koracima:
- dodavanje (212, 232) sulfida u spomenutu prvu otopinu za ispiranje, čime se izaziva taloženje sulfida teških metala; i
- razdvajanje (213, 233) spomenutih istaloženih sulfida teških metala iz spomenute prve otopine za ispiranje.
6. Postupak prema bilo kojem od zahtjeva 1 do 5, naznačen daljnjim korakom:
- prilagođavanje (214) ionskog udjela u spomenutoj prvoj otopini za ispiranje dodavanjem (215) barem jednog od trovalentnog željeza i aluminija u spomenutu prvu otopinu za ispiranje prije spomenutog taloženja fosfatnih spojeva u spomenutom koraku dodavanja (220) baze u spomenutu prvu otopinu za ispiranje, pri čemu se povećava omjer između kationa koji se mogu istaložiti kao fosfatni spojevi i fosfatnih iona, kad je fosfatni molarni sadržaj u spomenutoj prvoj otopini za ispiranje viši nego molarna količina očekivana za taloženje u spomenutom koraku dodavanja baze u spomenutu prvu otopinu za ispiranje, održavajući spomenuti molarni omjer većim od 1.
7. Postupak prema zahtjevu 6, naznačen time što spomenuti korak prilagođavanja (214) ionskog udjela u spomenutoj prvoj otopini za ispiranje sadrži dodavanje oksidansa (216) u spomenutu prvu otopinu za ispiranje prije spomenutog taloženja fosfatnih spojeva u spomenutom koraku dodavanja (220) baze u spomenutu prvu otopinu za ispiranje, čime se dvovalentno željezo oksidira u trovalentno željezo.
8. Postupak za proizvodnju fosfatnih spojeva, koji sadrži:
postupak koncentriranja fosfatnih spojeva prema bilo kojem od zahtjeva 1 do 7;
i postupak obnavljanja fosfatnih spojeva;
spomenuti postupak obnavljanja fosfatnih spojeva sadrži korake:
- otapanje (261) spomenutih istaloženih fosfatnih spojeva u drugu otopinu za ispiranje, čime se pruža (260) otopina za raspršivanje koja sadrži željezne fosfate;
- ekstrahiranje (270) željeza iz spomenute otopine za raspršivanje s prvim organskim otapalom koje sadrži tributil fosfat, modifikator i razrjeđivač, čime se proizvodi otopina za raspršivanje osiromašena od željeza;
spomenuto prvo organsko otapalo ima prvi sadržaj tributil fosfata;
- uklanjanje (275) spomenutog ekstrahiranog željeza iz spomenutog prvog organskog otapala koristeći jedno od vode i razrijeđene kiseline;
- recikliranje (279) spomenutog prvog organskog otapala nakon spomenutog uklanjanja kako bi se koristilo za spomenuti korak ekstrahiranja željeza; te
- obnavljanje (280) spomenutih fosfatnih spojeva iz spomenute otopine za raspršivanje osiromašene od željeza;
spomenuto prvo organsko otapalo ima prvi sadržaj tributil fosfata između 5 i 60 % volumena, poželjno između 10 i 40 % volumena;
poželjno, spomenuti modifikator je dodekanol, poželjnije u koncentraciji između 10 i 40 % volumena;
poželjno, spomenuti razrjeđivač je alifatski kerozin.
9. Postupak prema zahtjevu 8, naznačen time što spomenuti korak obnavljanja (280) spomenutih fosfatnih spojeva iz spomenute otopine osiromašene od željeza sadrži korake:
- ekstrahiranje (281) fosforne kiseline iz spomenute otopine osiromašene od željeza s drugim organskim otapalom koje sadrži tributil fosfat, i poželjno modifikator i razrjeđivač, čime se proizvodi otopina za raspršivanje osiromašena od fosfora;
spomenuto drugo organsko otapalo ima višu koncentraciju tributil fosfata nego spomenuto prvo organsko otapalo;
- uklanjanje (283) spomenute ekstrahirane fosforne kiseline iz spomenutog drugog organskog otapala vodenom otopinom; i
- recikliranje (284) spomenutog drugog organskog otapala nakon spomenutog uklanjanja spomenute ekstrahirane fosforne kiseline kako bi se koristilo za spomenuti korak ekstrahiranja fosforne kiseline;
spomenuto drugo organsko otapalo ima koncentraciju tributil fosfata između 70 i 100 % volumena;
spomenuti modifikator u spomenutom drugom organskom otapalu je poželjno dodekanol;
spomenuti razrjeđivač u spomenutom drugom organskom otapalu je poželjno kerozin.
10. Postupak prema zahtjevu 8 ili 9, naznačen time što spomenuta otopina za raspršivanje nadalje sadrži aluminij, pri čemu postupak sadrži daljnje korake:
- dodavanje (290) baze u barem dio spomenute otopine za raspršivanje osiromašene od fosfora kako bi se dobio neutralni ili alkalni pH, čime se uzrokuje taloženje aluminij hidroksida;
- razdvajanje (291) istaloženog aluminij hidroksida iz spomenute otopine osiromašene od fosfora, kako bi se dobila otopina za raspršivanje osiromašena od aluminija.
11. Postupak prema zahtjevu 8 ili 9, naznačen time što spomenuta otopina za raspršivanje nadalje sadrži aluminij, pri čemu postupak sadrži daljnje korake:
- dodavanje (330) barem jednog od kalcij fosfata i baze u barem dio spomenute otopine za raspršivanje osiromašene od fosfora kako bi se dobio kiseli pH > 1,5, čime se uzrokuje taloženje aluminij fosfata;
- razdvajanje (332) istaloženog aluminij fosfata iz spomenute otopine osiromašene od fosfora, kako bi se dobila otopina za raspršivanje osiromašena od aluminija.
12. Postupak proizvodnje fosfatnih spojeva, koji sadrži:
postupak koncentriranja fosfatnih spojeva prema bilo kojem od zahtjeva 1 do 7;
i postupak obnavljanja fosfatnih spojeva;
spomenuti postupak obnavljanja fosfatnih spojeva sadrži korake:
- otapanje (302) barem dijela barem jednog od spomenutih istaloženih fosfatnih spojeva i spomenutog istaloženog aluminij fosfata alkalnim otapalom u drugu otopinu za ispiranje;
- dodavanje (306) vapna u spomenutu drugu otopinu za ispiranje čime se izaziva taloženje kalcij fosfata;
- razdvajanje (308) istaloženog kalcij fosfata iz spomenute druge otopine za ispiranje; te
- recikliranje (310) spomenute druge otopine za ispiranje nakon spomenutog koraka razdvajanja istaloženog kalcij fosfata kako bi se koristila u spomenutom koraku otapanja barem dijela barem jednog od spomenutih istaloženih fosfatnih spojeva i spomenutog istaloženog aluminij fosfata alkalnim otapalom.
13. Postupak prema zahtjevu 12, naznačen time što spomenuti dio barem jednog od spomenutih istaloženih fosfatnih spojeva i spomenutih istaloženih aluminij fosfata sadrži željezo, pri čemu spomenuti postupak sadrži daljnji korak filtriranja (304) željeznog hidroksida iz spomenute druge otopine za ispiranje prije spomenutog koraka dodavanja vapna;
spomenuti željezni hidroksid iz spomenutog koraka filtriranja (304) željeznog hidroksida iz spomenute druge otopine za ispiranje se koristi kao barem dio spomenute baze u spomenutom koraku dodavanja (220) baze u spomenutu prvu otopinu za ispiranje, u spomenutom koraku prilagođavanja (214) spomenutog ionskog udjela u spomenutoj prvoj otopini za ispiranje i/ili u spomenutom koraku kontroliranja (215) spomenutog molarnog omjera kako bi bio veći od 1.
14. Postupak prema zahtjevu 12 ili 13, naznačen daljnjim koracima:
- dodavanje (312) kiseline u barem izdvojeni dio spomenute druge otopine za ispiranje nakon spomenutog koraka razdvajanja (308) istaloženog kalcij fosfata, čime se izaziva taloženje aluminij hidroksida; te
- razdvajanje (314) spomenutog istaloženog aluminij hidroksida iz spomenutog izdvojenog dijela spomenute druge otopine za ispiranje.
15. Postupak prema zahtjevu 14, naznačen time što spomenuta kiselina korištena u spomenutom koraku dodavanja kiseline u spomenuti izdvojeni dio spomenute druge otopine za ispiranje sadrži ugljičnu kiselinu ili plinoviti ugljik dioksid, pri čemu spomenuti postupak sadrži daljnje korake:
- dodavanje (316) vapna u spomenuti izdvojeni dio spomenute druge otopine za ispiranje nakon spomenutog koraka razdvajanja spomenutog istaloženog aluminij hidroksida, čime se izaziva taloženje kalcij karbonata;
- razdvajanje (318) spomenutog istaloženog kalcij karbonata iz spomenutog izdvojenog dijela spomenute druge otopine za ispiranje; te
- recikliranje (320) spomenutog izdvojenog dijela spomenute druge otopine za ispiranje nakon spomenutog razdvajanja (318) spomenutog istaloženog kalcij karbonata kako bi se koristio u spomenutom koraku otapanja (302) barem dijela barem jednog od spomenutih istaloženih fosfatnih spojeva i spomenutog istaloženog aluminij fosfata alkalnim otapalom.
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| CH697083A5 (de) * | 2004-12-01 | 2008-04-30 | Eberhard Recycling Ag | Verfahren und Anlage zur Rückgewinnung von Phosphor aus phosphorhaltigen Verbrennungsaschen. |
| AT503073B1 (de) | 2006-05-03 | 2009-08-15 | Ash Dec Umwelt Ag | Verfahren zur abtrennung von schwermetallen und ascheagglomerat |
| AU2008227219B2 (en) * | 2007-03-19 | 2012-08-16 | Easymining Sweden Ab | Phosphorus recovery |
| RU2375334C1 (ru) * | 2008-05-27 | 2009-12-10 | Закрытое акционерное общество "Завод минеральных удобрений Кирово-Чепецкого химического комбината" (ЗАО "ЗМУ КЧХК") | Способ извлечения фосфора из железосодержащих отходов переработки вятско-камских фосфоритов |
| DE102009020745A1 (de) * | 2009-05-11 | 2010-11-25 | Chemische Fabrik Budenheim Kg | Phosphatgewinnung auf Klärschlamm |
| US8658117B2 (en) | 2009-05-27 | 2014-02-25 | Easymining Sweden Ab | Production of ammonium phosphates |
| SE534505C2 (sv) * | 2009-08-31 | 2011-09-13 | Easymining Sweden Ab | Återvinning av aluminium från fosforinnehållande material |
| CN101654238A (zh) * | 2009-09-11 | 2010-02-24 | 华东理工大学 | 从城市污水处理厂富磷剩余污泥中回收磷化合物的方法 |
| CN101774556B (zh) * | 2010-01-28 | 2011-12-07 | 四川大学 | 盐酸分解中低品位磷矿制备工业级和食品级磷酸的方法 |
| RU2456248C1 (ru) * | 2010-12-23 | 2012-07-20 | Учреждение Российской академии наук Институт катализа им. Г.К. Борескова Сибирского отделения РАН | Каталитический реактор для переработки осадков сточных вод и способ их переработки (варианты) |
| CN102320583B (zh) * | 2011-07-25 | 2013-04-03 | 南京林业大学 | 一种利用白云石回收城市污泥厌氧消化液中磷的方法 |
| CN102503060B (zh) * | 2011-11-23 | 2013-03-06 | 清华大学 | 一种于污泥中回收磷酸铁方法 |
| CN102815824B (zh) * | 2012-08-30 | 2013-11-06 | 北京世纪国瑞环境工程技术有限公司 | 一种从城市粪便中提取磷的方法 |
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