CA2552104A1 - Process for recovery of sulphate of potash - Google Patents
Process for recovery of sulphate of potash Download PDFInfo
- Publication number
- CA2552104A1 CA2552104A1 CA002552104A CA2552104A CA2552104A1 CA 2552104 A1 CA2552104 A1 CA 2552104A1 CA 002552104 A CA002552104 A CA 002552104A CA 2552104 A CA2552104 A CA 2552104A CA 2552104 A1 CA2552104 A1 CA 2552104A1
- Authority
- CA
- Canada
- Prior art keywords
- bittern
- carnallite
- nacl
- mgcl2
- kainite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract 29
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract 7
- 229940072033 potash Drugs 0.000 title claims abstract 7
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 title claims abstract 7
- 235000015320 potassium carbonate Nutrition 0.000 title claims abstract 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract 6
- 229910021653 sulphate ion Inorganic materials 0.000 title claims abstract 6
- 238000011084 recovery Methods 0.000 title claims abstract 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract 22
- 241001131796 Botaurus stellaris Species 0.000 claims abstract 20
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 claims abstract 12
- 239000011780 sodium chloride Substances 0.000 claims abstract 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 10
- GMLLYEDWRJDBIT-UHFFFAOYSA-J magnesium;dipotassium;disulfate Chemical compound [Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GMLLYEDWRJDBIT-UHFFFAOYSA-J 0.000 claims abstract 8
- BMQVDVJKPMGHDO-UHFFFAOYSA-K magnesium;potassium;chloride;sulfate;trihydrate Chemical compound O.O.O.[Mg+2].[Cl-].[K+].[O-]S([O-])(=O)=O BMQVDVJKPMGHDO-UHFFFAOYSA-K 0.000 claims abstract 8
- 150000003839 salts Chemical class 0.000 claims abstract 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract 5
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract 5
- 235000012254 magnesium hydroxide Nutrition 0.000 claims abstract 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract 5
- 238000006243 chemical reaction Methods 0.000 claims abstract 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract 2
- 239000000920 calcium hydroxide Substances 0.000 claims abstract 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract 2
- 238000001640 fractional crystallisation Methods 0.000 claims abstract 2
- 229910052602 gypsum Inorganic materials 0.000 claims abstract 2
- 239000010440 gypsum Substances 0.000 claims abstract 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims 20
- 229910001629 magnesium chloride Inorganic materials 0.000 claims 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims 6
- 239000000706 filtrate Substances 0.000 claims 6
- 238000001914 filtration Methods 0.000 claims 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims 4
- 239000001110 calcium chloride Substances 0.000 claims 4
- 235000011148 calcium chloride Nutrition 0.000 claims 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims 4
- 238000005406 washing Methods 0.000 claims 4
- 238000001704 evaporation Methods 0.000 claims 3
- 238000002386 leaching Methods 0.000 claims 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000008020 evaporation Effects 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 2
- 239000012452 mother liquor Substances 0.000 claims 2
- 229910052700 potassium Inorganic materials 0.000 claims 2
- 238000004064 recycling Methods 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 235000011941 Tilia x europaea Nutrition 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 239000004571 lime Substances 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims 1
- 229910052939 potassium sulfate Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 239000002699 waste material Substances 0.000 claims 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 1
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fertilizers (AREA)
Abstract
A novel integrated process for the recovery of sulphate of potash (SOP) from sulphate rich bittern is disclosed. The process requires only bittern and li me as raw materials. Kainite type mixed salt is obtained by fractional crystallization of the bittern. Kainite is converted to schoenite with simultaneous removal of NaCl by processing it with water and end liquor obtained from reaction of schoenite with MOP for its conversion to SOP. The end liquor from kainite to schoenite conversion (SEL) is used for the recove ry of MOP. SEL is desulphated and supplemented with MgC12using end bittern generated in the process of making carnallite. The carnallite is decomposed to get crude potash which in turn processed to get MOP. The carnallite decompos ed liquor produced in the decomposition of carnallite is reacted with hydrated lime for preparing CaC12 solution and high purity Mg(OH)2 having low boron content. The CaC12 solution is used for desulphatation of SEL producing high purity gypsum as a byproduct. It is shown that the liquid streams containing potash are recycled in the process, the recovery of potash in the form of SO P is quantitative.
Claims (21)
- Claims:
An integrated process for preparation of sulphate of potash (SOP) from bittern comprising:
(i) ~subjecting bittern to fractional crystallization to obtain kainite type mixed salt with high kainite content and MgCl2-rich end bittern, and subjecting the MgCl2 rich end bittern to desulphation;
(ii) treating the kainite type mixed salt with water and mother liquor obtained in step (xiii) below to leach out substantially all NaCl from the mixed salt and simultaneously convert kainite into schoenite;
(iii) filtering the schoenite and separating the filtrate;
(iv) desulphating the filtrate with aqueous CaCl2;
(v) ~filtering the gypsum produced in step (iv) and mixing the filtrate with the MgCl2-rich filtrate obtained in step (vii) below;
(vi) evaporating the resultant solution of step (v) and cooling to ambient temperature to crystallize crude carnallite;
(vii) centrifuging the crude carnallite and recycling the required quantity of filtrate to step (v);
(viii) decomposing the crude carnallite with appropriate quantity of water from step (vi) to yield crude KCl and carnallite decomposed liquor;
(ix) filtering the crude KCl, and washing with water to remove adhering MgCl2 and subjecting to hot leaching for production of MOP and NaCl;
(x) ~mixing the carnallite decomposed liquor from step (viii) and washing from step (ix) and treating with hydrated lime;
(xi) filtering the slurry and washing the cake to produce Mg(OH)2 and CaCl2-containing filtrate for the desulphatation process of step (iv);
(xii) treating by known method the schoenite produced in step (iii) with MOP
produced in step (ix) to produce SOP under ambient condition;
(xiii) filtering the SOP and collecting separately the mother liquor hereinafter referred to as KEL;
(xiv) recycling the KEL of step (xiii) in the process of step (ii). - 2. ~A process as claimed in Claim 1 wherein the bittern contains K, Mg and SO4 in concentrations that make it suitable for kainite production
- 3. ~A process as claimed in claim 2 wherein sand bittern is selected from sea bittern and sub-soil bittern, and preferably bittern with higher potassium content and which also requires the least evaporation to produce kainite-type mixed salt, and waste bittern sources such as debrominated bittern effluent.
- 4. ~A process as claimed in any one of claims 1 to 3 wherein said mixed salt contains KCl-15-22%, NaCl-15-22%, MgSO4-28-40%, MgCl2-5-10%.
- 5.~A process as claimed in any preceding claim wherein one part by weight of mixed salt is treated with 0.75-1.25 parts by volume of KEL and 0.3-0.7 parts by volume of water.
- 6. ~A process as claimed in any preceding claim wherein said KEL contains typically 15-17% KCl, 1-3% NaCl, 10-12% MgSO4, and 2-3% MgCl2.
- 7. ~A process as claimed in in any preceding claim wherein the SEL contains typically 8-10% KCl, 6-12% NaCl, 12-14% MgSO4 and 5-7% MgCl2.
- 8. ~A process as claimed in any preceding claim wherein the schoenite contains typically 40-45% K2SO4, 30-35% MgSO4 and 0.5-2.0% NaCl.
- 9. ~A process as claimed in any preceding claim wherein the stoichiometric ratio of CaCl2 to sulphate for the desulphatation reaction of step (iv) is 1.1:1 to 0.9:1, preferably 1:1.
- 10. ~A process as claimed in claim 7 wherein 1 part by volume of desulphated SEL was mixed with 0.5-1.5 parts by volume of MgCl2-rich end bittern of 36-38°Be'(s.g.
1.33-1.38), preferably, 0.7-0.9 parts of end bittern of 37°Be'(sp. gr.
1.342), and more preferably, MgCl2-rich end bittern containing no sulphate. - 11. ~A process as claimed in any one of claims 1 to 10 wherein the concentration of desulphated SEL to produce carnallite is carried out in a solar pan or in a multiple effect evaporator with simultaneous recovery of water.
- 12. ~A process as claimed in any preceding claim wherein evaporation is continued till the solution attained a temperature in the range of 120-128°C and more preferably,~
122-124°C. - 13. ~A process claimed in any preceding claim wherein the carnallite obtained has 15-20% KCl, 15-20% NaCl and 28-32% MgCl2.
- 14. ~A process claimed in any preceding claim wherein one part by weight of the carnallite is decomposed with 0.4-0.6 parts by volume of water, followed by washing of the cake with a small quantity of water.
- 15. ~A process claimed in any preceding claim wherein the molar ratio of active lime to MgCl2 for production of Mg(OH)2 and CaCl2 is in the range of 0.8-1.0, preferably, 0.90.
- 16. ~A process claimed in any preceding claim wherein said Mg(OH)2 obtained is calcined to produce MgO with 94-98 % purity and with 0.02-0.04% BaO3.
- 17. ~A process claimed in any preceding claim wherein the Mg(OH)2 is used without upgradation for neutralization of acidified de-brominated bittern where such bittern is used as potash source.
- 18. ~A process claimed in any preceding claim wherein the MOP obtained upon hot leaching of crude KCl has a purity in the range of 92-98% and NaCl content of % preferably >95% KCl and <2% NaCl.
- 19. ~A process as claimed in claims 1-3 wherein the NaCl obtained on hot leaching of crude KCl contains > 97% NaCl.
- 20. ~A process claimed in any preceding claim wherein one part by weight of schoenite is treated with 0.3-0.6 parts by weight of MOP and 1-2 parts by volume of water, and more preferably 0.4 parts by weight of MOP and 1.5 parts by volume of water, in the ambient temperature range of 20-45 degree C.
- 21. ~A process claimed in any preceding claim wherein the SOP produced has K2O
content in the range of 50-52% and chloride in the range of 0.5-2.0%.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/IN2003/000463 WO2005063626A1 (en) | 2003-12-31 | 2003-12-31 | Process for recovery of sulphate of potash |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2552104A1 true CA2552104A1 (en) | 2005-07-14 |
| CA2552104C CA2552104C (en) | 2009-11-24 |
Family
ID=34717580
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002552104A Expired - Lifetime CA2552104C (en) | 2003-12-31 | 2003-12-31 | Process for recovery of sulphate of potash |
Country Status (8)
| Country | Link |
|---|---|
| JP (1) | JP4516023B2 (en) |
| CN (1) | CN100439248C (en) |
| AU (1) | AU2003300719B2 (en) |
| BR (1) | BRPI0318666B1 (en) |
| CA (1) | CA2552104C (en) |
| GB (1) | GB2427190B8 (en) |
| IL (1) | IL176482A (en) |
| WO (1) | WO2005063626A1 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATE474815T1 (en) * | 2005-11-10 | 2010-08-15 | Council Scient Ind Res | IMPROVED PROCESS FOR OBTAINING POTASSIUM SULFATE (SOP, SULPHATE OF POTASH) FROM SULFATE-RICH MOTHER BRINE |
| CN100535389C (en) * | 2006-12-14 | 2009-09-02 | 国投新疆罗布泊钾盐有限责任公司 | Method for collecting kainite salt mine |
| CN102503619B (en) * | 2011-09-02 | 2013-11-06 | 天津科技大学 | Method for preparing compound fertilizer from salt manufacturing mother liquor |
| CN103397201B (en) * | 2013-07-26 | 2014-12-17 | 中国科学院青海盐湖研究所 | Method for statically leaching and extracting potassium from polyhalite and preparing potassium sulphate |
| WO2016059651A1 (en) * | 2014-10-16 | 2016-04-21 | Council Of Scientific And Industrial Research | A process of production of potassium ammonium sulfate compound fertilizer in cost-effective manner directly from concentrated sea bittern |
| CN104628017A (en) * | 2015-02-13 | 2015-05-20 | 中国科学院青海盐湖研究所 | Method for preparing kainite ore from sulfate-type brine |
| US10399861B2 (en) * | 2015-05-08 | 2019-09-03 | Yara Dallol Bv | Methods for the production of potassium sulphate from potassium-containing ores at high ambient temperatures |
| WO2017220709A1 (en) | 2016-06-24 | 2017-12-28 | Yara Dallol Bv | Method for the reduction of halite in the preparation of potassium sulphate from potassium-containing ores at high ambient temperatures |
| CN107285283B (en) * | 2017-06-01 | 2019-10-15 | 中国中轻国际工程有限公司 | A kind of akali sulphide black liquor, liquid caustic soda coproduction sodium bicarbonate, sodium chromate, akali sulphide technique |
| CA3076265C (en) | 2017-10-13 | 2021-05-25 | Novopro Projects Inc. | Systems and methods of producing potassium sulfate |
| CN107673372B (en) * | 2017-11-15 | 2023-09-08 | 河北工业大学 | Large-scale potassium-rich method and device based on coupling technology |
| CN114560480A (en) * | 2022-03-01 | 2022-05-31 | 天津长芦海晶集团有限公司 | Multi-element extraction method of bittern after desulfurization by calcium method |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3634041A (en) * | 1969-02-14 | 1972-01-11 | Great Salt Lake Minerals | Method for the production of potassium sulfate from potassium-containing double salts of magnesium sulfate |
| IL50873A (en) * | 1976-11-09 | 1979-11-30 | Sadan A | Process for the production of potassium chloride and magnesium chloride from carnallite |
| CN1035811C (en) * | 1992-09-12 | 1997-09-10 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing potassium sulfate from bittern and potassium chloride |
| CN1027883C (en) * | 1993-05-14 | 1995-03-15 | 中国石油天然气总公司工程技术研究所 | Pren. method of potassium sulfate from bittern and potassium chloride |
| CN1130152A (en) * | 1995-04-26 | 1996-09-04 | 国家海洋局天津海水淡化与综合利用研究所 | Process for producing potassium sulfate from bittern and potassium chloride |
| CN1057978C (en) * | 1997-04-10 | 2000-11-01 | 中国石油天然气总公司工程技术研究院 | Bittern comprehensive utilization method |
| CN1128760C (en) * | 2000-08-29 | 2003-11-26 | 化学工业部连云港设计研究院 | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern |
| CN1171794C (en) * | 2001-05-24 | 2004-10-20 | 化学工业部连云港设计研究院 | Preparation method of potassium sulfate with sulfate-type salt lake bittern containing potassium salt |
| EP1440036B1 (en) * | 2001-10-22 | 2007-03-21 | Council of Scientific and Industrial Research;an Indian Reg. body incorporated under Reg. of Societies Act (Act XXI of 1860) | Recovery of sodium chloride and other salts from brine |
| ATE490219T1 (en) * | 2003-12-31 | 2010-12-15 | Council Scient Ind Res | SIMULTANEOUS PRODUCTION OF POTASSIUM CHLORIDE AND KCL-enriched table salt |
-
2003
- 2003-12-31 GB GB0614762A patent/GB2427190B8/en not_active Expired - Lifetime
- 2003-12-31 CN CNB2003801109302A patent/CN100439248C/en not_active Expired - Lifetime
- 2003-12-31 JP JP2005512762A patent/JP4516023B2/en not_active Expired - Lifetime
- 2003-12-31 BR BRPI0318666A patent/BRPI0318666B1/en active IP Right Grant
- 2003-12-31 WO PCT/IN2003/000463 patent/WO2005063626A1/en active Application Filing
- 2003-12-31 AU AU2003300719A patent/AU2003300719B2/en not_active Expired
- 2003-12-31 CA CA002552104A patent/CA2552104C/en not_active Expired - Lifetime
-
2006
- 2006-06-21 IL IL176482A patent/IL176482A/en active IP Right Grant
Also Published As
| Publication number | Publication date |
|---|---|
| AU2003300719B2 (en) | 2008-06-12 |
| GB0614762D0 (en) | 2006-09-06 |
| GB2427190B (en) | 2009-04-15 |
| JP2007528333A (en) | 2007-10-11 |
| BR0318666A (en) | 2006-11-28 |
| CN1886339A (en) | 2006-12-27 |
| AU2003300719A1 (en) | 2005-07-21 |
| CN100439248C (en) | 2008-12-03 |
| GB2427190B8 (en) | 2009-07-22 |
| JP4516023B2 (en) | 2010-08-04 |
| CA2552104C (en) | 2009-11-24 |
| WO2005063626A1 (en) | 2005-07-14 |
| GB2427190A (en) | 2006-12-20 |
| IL176482A (en) | 2012-06-28 |
| IL176482A0 (en) | 2006-10-05 |
| BRPI0318666B1 (en) | 2015-12-15 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |
Effective date: 20201231 |
|
| MKLC | Lapsed (correction) |
Effective date: 20230711 |
|
| MKEX | Expiry |
Effective date: 20240102 |