WO2020016632A1 - Système et méthode de purification et de récupération de potasse - Google Patents

Système et méthode de purification et de récupération de potasse Download PDF

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Publication number
WO2020016632A1
WO2020016632A1 PCT/IB2018/055346 IB2018055346W WO2020016632A1 WO 2020016632 A1 WO2020016632 A1 WO 2020016632A1 IB 2018055346 W IB2018055346 W IB 2018055346W WO 2020016632 A1 WO2020016632 A1 WO 2020016632A1
Authority
WO
WIPO (PCT)
Prior art keywords
potash
solution
potassium bicarbonate
zone
carbon dioxide
Prior art date
Application number
PCT/IB2018/055346
Other languages
English (en)
Inventor
Graeme Norval
Original Assignee
Clearview Tci Ltd.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Clearview Tci Ltd. filed Critical Clearview Tci Ltd.
Priority to PCT/IB2018/055346 priority Critical patent/WO2020016632A1/fr
Publication of WO2020016632A1 publication Critical patent/WO2020016632A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/22—Purification
    • C01D7/24—Crystallisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/10—Preparation of bicarbonates from carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/12—Preparation of carbonates from bicarbonates or bicarbonate-containing product
    • C01D7/123—Preparation of carbonates from bicarbonates or bicarbonate-containing product by thermal decomposition of solids in the absence of a liquid medium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0018—Evaporation of components of the mixture to be separated
    • B01D9/0031—Evaporation of components of the mixture to be separated by heating
    • 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

Definitions

  • This invention relates to improved systems and methods for the
  • Potash is important for agriculture because it improves water retention, yield, nutritional value texture and disease resistance of food crops. It has wide application to fruits and vegetables, rice, wheat and other grains, sugar, corn, soybeans, palm oil and cotton, all of which benefit from the nutrient’s quality enhancing properties. Economic growth in Asia and Latin America has greatly contributed to the increased use of potash-based fertilizers.
  • potash is a fertilizer for the above-mentioned plants
  • agricultural plant wastes become a reservoir of potassium from which potash can be recovered by extraction from the residue (ashes) which are left from the burning of such agricultural plant wastes.
  • the agricultural plant wastes which are burned to ashes and from which potash is extracted preferably are cocoa pod husks, plantain (and banana) peels and cola nut husks.
  • potash may be recovered by extraction from the residue (ashes) left from the burning of the above preferred agricultural plant wastes.
  • bicarbonate is crystallized and the potassium bicarbonate crystals are filtered.
  • the filtrate is returned to the crystallizer.
  • a portion of the filtrate is used to regenerate the ion exchange column and a separate portion of the filtrate is added to the purge from the ion exchange column, thereby increasing the volume of the purge to keep the concentration of other impurities below the concentration at which they will precipitate in the crystallizer.
  • Potassium carbonate is then regenerated from the potassium bicarbonate crystals in a heating zone. Finally the potash is ground to provide ground potash
  • a method for the purification of impure potash comprising discharging the impure potash in an aqueous solution into a leaching zone, and leaching potash out of the impure potash, thereby producing leached potash slurry; passing the leached potash slurry through at least one thickener zone to provide a thickened potash solution; carbonating the concentrated thickened potash solution in a carbonization zone, thereby producing potassium bicarbonate; filtering the solution from the carbonization zone in a first filter zone; passing the filtered solution through an ion exchange column to remove bivalent cations; passing the product from the ion exchange column to an activated carbon bed; crystallizing the potassium
  • an interconnected system for the purification of impure potash comprising a leaching tank for containing impure potash to be purified; a solids inlet into the leaching tank for introducing impure potash to be purified; a water inlet line for introducing water into the leaching tank; a rinse water inlet line from a belt filter into the leaching tank; a thickener; a conduit for leading sludge of the impure potash from the leaching tank into the thickener; a carbonation column for converting the concentrated potash solution into potassium bicarbonate; a conduit for leading the concentrated potash solution from the thickener into the carbonation column; a first filter for filtering the potassium bicarbonate solution; a conduit leading from the carbonation column to the first filter; an ion exchange column to remove bivalent cations from solution of carbonization zone; a conduit for leading the potassium bicarbonate solution from the first filter into the ion exchange column; an
  • FIG. 1 is a block flow diagram of the system and method for the production of potash from agricultural waste ashes.
  • the system for the production and purification of potash preferably from the ashes of agricultural wastes, such as the ashes of cocoa pod husks, plantain (and banana) peels and cola nut husks, includes a leaching tank 500 (BLOCK A).
  • the leaching tank 500 includes an ash introduction line 501, a water inlet line 503 and a potash slurry outlet line 507 leading to a thickener 502 (BLOCK B).
  • Thickener 502 is provided with an overflow line 509 to lead a dilute potash solution to a carbonation column 508 (BLOCK C). A portion of the dilute potash solution from the Thickener 502 is returned to the Leaching Tank 501 through a return line 511.
  • a sludge outlet line 513 from the Thickener 502 sends the sludge to a device such as a belt filter 521 (BLOCK D).
  • a rinse water inlet line 523 introduces water to rinse the sludge before the rinsed sludge is disposed through disposal line 519, and the rinse water solution is returned to the leaching tank 500 through a rinse water return line 513.
  • the solution pH in the carbonation column 508 is reduced by providing a C02 stream 543 from both oven 526 (BLOCK J) and boiler 510 exhaust gas.
  • the potassium bicarbonate solution which is formed in carbonation column 508 exits carbonation column via bicarbonate feed line 545 and is fed into first Filter 513 (BLOCK E).
  • the filtered solution is sent through a filter outlet 516 to Ion Exchange Column 517 (BLOCK F).
  • the product from the ion exchange column 517 is sent via a column line 511 to an activated carbon bed 518 (BLOCK G).
  • the carbon bed line 512 leads the filtered clear solution from the activated carbon bed 518 to the Crystallizer 561 (BLOCK H).
  • a slurry of crystallized potassium bicarbonate then exits from crystallizer tank 561 and is fed into second filter 524 (BLOCK I) via slurry line 547.
  • the solid potassium bicarbonate exits second filter 524 and is conveyed by conveyor 549 into oven 526 (BLOCK J), wherein the potassium bicarbonate is converted to potassium carbonate.
  • a filtrate return line 548 leads from the second filter 524 to a crystallizer return line 549, to return filtrate back to the crystallizer 561.
  • Filtrate return line 548 also returns a portion of filtrate via line 551 to regenerate the ion exchange column 517.
  • Purge line 560 carries purge solution from the ion exchange column 517. Another portion of the filtrate solution from the filtrate return line 548 is directed by filtrate line 550 to mix with the ion exchange purge solution in purge line 560.
  • the potassium bicarbonate decomposes into crystalline potassium carbonate and effluent gases comprising carbon dioxide, nitrogen and steam are released.
  • these effluent gases exit oven 526 and are fed into condenser 558 (BLOCK K) via gas line 567.
  • Condenser 558 is fed with water from thickener return line 511 and rinse water return line 513 to condense the steam to water, thereby heating recycled clear solution from the thickener 502 and rinse water from the belt filter 521 to increase the leaching of potash in the leaching tank 500.
  • Nitrogen gas is vented through vent 541, and recovered gaseous carbon dioxide exits compressor 514 to add carbon dioxide into carbonation column 508 through carbon dioxide line 543.
  • the crystalline potassium carbonate (potash) from oven 526 exits onto oven conveyor 550 to be conveyed to grinders 528 (BLOCK P) where it is ground.
  • the ground potassium carbonate (potash) exits grinders 528 onto grinder conveyor 561 to be conveyed to packaging machine 530 (BLOCK Q).
  • the packages so formed may be supplied for local uses or may be sent to export 532 (BLOCK R) via export line 563.
  • a portion of the potash solution can be removed from the process and used for commercial processes as is.
  • the solution could be withdrawn prior to the carbonation stage and the commercial solution would be a potassium carbonate solution.
  • the solution could be withdrawn after the carbonation stage and the commercial solution would be a potassium bicarbonate solution.
  • the removal of solution prior to the crystallization step reduces the volume of high purity crystals produced, but may provide local benefits.
  • Boiler 510 (BLOCK L) is preferably fueled with a mixture of liquid petroleum gas and methane through fuel line 525. Steam effluent from boiler 510 exits through main steam line 527 to crystallizer 561. Flue gases, i.e., carbon dioxide, nitrogen and steam, pass from gas outlet of boiler 510 to condenser/economizer 558 (BLOCK K) through main gas line 533.
  • Condenser/economizer 558 is fed with water through return water line 511.
  • condenser/economizer 512 back to boiler 510 (not shown).
  • Effluent gases from condenser/economizer 558 exit condenser/economizer and are carried via second gas line 557 to compressor 514 (BLOCK L) for further use as described above, ie nitrogen gas is vented through vent 541, and recovered gaseous carbon dioxide exits compressor 514 to add carbon dioxide into carbonation column 508 through carbon dioxide line 543.
  • Water vapor from crystallizer 561 may be collected through water vapor line 571 and condensed using the water from the return line 511 and the rinse water return line 513, thereby heating the leaching solution to provide increased dissolution of the potash in the leaching tank 500.
  • extraction/purification of the potash which may be organic potash produced by controlled combustion of agricultural wastes, for example the ashes of cocoa pod husks, plantain (and banana) peels and cola nut husks, consists of discharging the ashes, containing typically about 77% potash, into water in preferably one or more stainless steel leaching tanks connected in series, which are of the CSTR type.
  • the leached slurry is sent through a thickener to remove un-dissolved matter and to form a clarified potash solution.
  • the ash waste is then thoroughly washed until it contains practically no potash.
  • the clarified potash solution is sent to a carbonation column, where the potash is carbonated to potassium bicarbonate.
  • the potassium bicarbonate solution is filtered and the filtered solution is sent to an ion exchange column to remove bivalent cations.
  • the resultant potassium bicarbonate solution is mixed, preferably in a stainless steel tank, with an adsorbent, preferably activated carbon.
  • the activated carbon adsorbs ferric ion complexes and clarifies the solution.
  • the potassium bicarbonate solution is sent into a crystallizer operating from a maximum of about 90°C down to a minimum of 30°C, from where it is sent to another filter to separate the crystals from the mother liquor.
  • the mother liquor is returned into the crystallizer while the bicarbonate crystals obtained are sent to an oven to regenerate the potash and to release carbon dioxide.
  • the carbon dioxide may be returned to the carbonation column for reuse.
  • the potash which is obtained is ground into powder for market. This final product potash is widely used in the fertilizer, soap, petrochemical, glass, food and pharmaceutical industries among others.
  • the purified potash may be of about 90% purity, or may be of about 99% purity.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

La présente invention concerne un système et une méthode de production de potasse à partir de déchets agricoles. La méthode comprend la décharge de potasse impure dans une zone de lixiviation, le passage de la potasse lixiviée à travers un épaississeur, la carbonatation, la filtration et le passage de la solution à travers une colonne échangeuse d'ions, le passage à un lit de charbon actif, la cristallisation du bicarbonate de potassium, la filtration des cristaux et la régénération du carbonate de potassium dans une zone de chauffage. Le système comprend un réservoir de lixiviation, un épaississeur, une colonne de carbonatation, un premier filtre, une colonne échangeuse d'ions, un lit de charbon actif, un cristalliseur, un second filtre et un four.
PCT/IB2018/055346 2018-07-18 2018-07-18 Système et méthode de purification et de récupération de potasse WO2020016632A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/IB2018/055346 WO2020016632A1 (fr) 2018-07-18 2018-07-18 Système et méthode de purification et de récupération de potasse

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/IB2018/055346 WO2020016632A1 (fr) 2018-07-18 2018-07-18 Système et méthode de purification et de récupération de potasse

Publications (1)

Publication Number Publication Date
WO2020016632A1 true WO2020016632A1 (fr) 2020-01-23

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112076494A (zh) * 2020-09-07 2020-12-15 衡阳百赛化工实业有限公司 一种硫酸锌晶体制备用蒸发结晶装置
CN113600010A (zh) * 2021-07-19 2021-11-05 陕西未来能源化工有限公司 费托合成尾气热钾碱溶液的净化再生方法及其装置和应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6207126B1 (en) * 1998-07-16 2001-03-27 Chemetall Foote Corporation Recovery of lithium compounds from brines
US20120189519A1 (en) * 2010-06-28 2012-07-26 Baoquan Zhang Flue-gas purification and reclamation system and method thereof
US9017426B2 (en) * 2011-11-17 2015-04-28 Gc Technology Limited Interconnected system and method for the purification and recovery of potash

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6207126B1 (en) * 1998-07-16 2001-03-27 Chemetall Foote Corporation Recovery of lithium compounds from brines
US20120189519A1 (en) * 2010-06-28 2012-07-26 Baoquan Zhang Flue-gas purification and reclamation system and method thereof
US9017426B2 (en) * 2011-11-17 2015-04-28 Gc Technology Limited Interconnected system and method for the purification and recovery of potash

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112076494A (zh) * 2020-09-07 2020-12-15 衡阳百赛化工实业有限公司 一种硫酸锌晶体制备用蒸发结晶装置
CN113600010A (zh) * 2021-07-19 2021-11-05 陕西未来能源化工有限公司 费托合成尾气热钾碱溶液的净化再生方法及其装置和应用
CN113600010B (zh) * 2021-07-19 2023-09-01 陕西未来能源化工有限公司 费托合成尾气热钾碱溶液的净化再生方法及其装置和应用

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