WO2023111784A1 - Nouveau procédé d'isolement de potasse à partir d'un produit de lavage épuisé - Google Patents
Nouveau procédé d'isolement de potasse à partir d'un produit de lavage épuisé Download PDFInfo
- Publication number
- WO2023111784A1 WO2023111784A1 PCT/IB2022/061928 IB2022061928W WO2023111784A1 WO 2023111784 A1 WO2023111784 A1 WO 2023111784A1 IB 2022061928 W IB2022061928 W IB 2022061928W WO 2023111784 A1 WO2023111784 A1 WO 2023111784A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- aluminium
- potassium
- spent wash
- potash
- lime
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 42
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract description 32
- 229940072033 potash Drugs 0.000 title claims abstract description 32
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 title claims abstract description 32
- 235000015320 potassium carbonate Nutrition 0.000 title claims abstract description 32
- 238000002955 isolation Methods 0.000 title claims description 28
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 43
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011591 potassium Substances 0.000 claims abstract description 42
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 34
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims abstract description 26
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 20
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 20
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 17
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 17
- 229910000160 potassium phosphate Inorganic materials 0.000 claims abstract description 12
- 235000011009 potassium phosphates Nutrition 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 52
- 239000004411 aluminium Substances 0.000 claims description 50
- 239000007788 liquid Substances 0.000 claims description 24
- 235000011126 aluminium potassium sulphate Nutrition 0.000 claims description 23
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 23
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 21
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 21
- 239000004571 lime Substances 0.000 claims description 21
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 17
- 235000011128 aluminium sulphate Nutrition 0.000 claims description 16
- 239000001120 potassium sulphate Substances 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 15
- 239000011541 reaction mixture Substances 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 13
- 239000001164 aluminium sulphate Substances 0.000 claims description 11
- 238000001704 evaporation Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 229910052602 gypsum Inorganic materials 0.000 claims description 8
- 239000010440 gypsum Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 17
- 235000013379 molasses Nutrition 0.000 abstract description 10
- 239000003337 fertilizer Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 6
- 235000011007 phosphoric acid Nutrition 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F5/00—Fertilisers from distillery wastes, molasses, vinasses, sugar plant or similar wastes or residues, e.g. from waste originating from industrial processing of raw material of agricultural origin or derived products thereof
- C05F5/004—Liquid waste from mechanical processing of material, e.g. wash-water, milling fluid, filtrate
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/02—Fertilisers containing other nitrates containing sodium or potassium nitrate
-
- 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
Definitions
- the present invention is relates to a novel isolation process of potash from spent wash (PFSW).
- PFSW potash from spent wash
- the present invention particularly relates to a novel isolation process of potassium from spent wash generated in sugar industry during molasses based alcohol distillery.
- the present invention also enables utilization of potassium resource from spent wash.
- BOD pollution load of all distilleries put together in India is more than 6 times the BOD load of the entire population of India.
- Molasses from the sugar factory is the major constituent in the sugar Industry. Molasses is the byproduct of sugar Industries. The effluent of distillery is known as spent wash. Spent wash is the approximately 13-16 times more by volume to that of the alcohol. It is highly organic and brown in color. Spent wash contains multi nutrients (potassium, nitrogen and phosphorus) and it is used in land applications, therefore potassium has been recovered from the spent wash for utilization of potassium source.
- the inventors of the present invention found that isolation of potassium from raw spent wash or biomethanated spent wash is an alternative technique in order to obtain potassium to overcome the problems as mentioned above. So, far it has been exploited to achieve the following objective.
- the present invention is to provide a novel isolation process for recovery of potassium from spent wash.
- the main object of the present invention is to provide a novel isolation process for recovery of potassium from spent wash which is green process.
- Yet another object of the present invention is to provide a novel isolation process for recovery of potassium from spent wash which avoids lengthy and complex processing steps.
- One other object of the present invention is to provide a novel isolation process for recovery of potassium from spent wash to produce multi-nutrient potassium fertilizers viz., potassium sulphate, potassium nitrate, mono potassium phosphate etc
- Yet another object of the present invention provide a novel isolation process for recovery of potassium from spent wash from sugar distillery and making ZLD (Zero Liquid Discharge) sugar distillery.
- Yet another object of the present invention provide a novel isolation process for recovery of potassium from spent wash to recover maximum water for reuse.
- the main aspect of the present invention is to provide a novel isolation process for recovery of potassium from spent wash comprises the steps of, a) concentrating a spent wash in multiple effect evaporator; b) reacting of concentrated spent wash of step (a) with aluminum sulphate for obtaining precipitation of potash alum and potash free spent wash(PFSW); c) clarifying precipitation of potash alum of step (b) to remove crystal of potash alum; d) reacting of potash alum crystal of step (c) with ingredient selected from lime, nitric acid and phosphoric acid; e) clarifying liquid of step (d) to get potassium sulphate, potassium nitrate , potassium sulfate solution and aluminium reach gypsum- 1; f) crystallizing of liquid from step (e) by cooling or evaporating the liquor to get potassium sulphate, potassium nitrate and potassium phosphate; and process for recovering aluminium sulfate comprises the steps; g) reacting the
- Figure 1 Flow chart of isolation Process for Recovery of Potash from Spent wash
- the main embodiment of the present invention is to provide a novel isolation process for recovery of potassium from spent wash.
- the present invention relates to a novel isolation process for recovery of potassium from spent wash.
- slurry means relating to mixture of solids denser than water suspended in liquid, usually water and a fine insoluble particulate substance.
- the term “clarifying” means removal of small amounts (usually less than 0.2%) of fine particulate solids from liquids (such as drinking water) by methods such as gravity sedimentation, centrifugal sedimentationn, filtration, and magnetic separation.
- crystallization means relating to the process by which a solid forms, where the atoms or molecules are highly organized into a structure known as a crystal.
- the term “supernatant liquid” means relating to clear liquid that lies above the solid residue after centrifugation, precipitation, crystallization or settling.
- the term "about” means plus or minus 10% of the numerical value of the number with which it is being used.
- the novel isolation process for recovery of potassium from spent wash comprises the steps of, a) concentrating a spent wash in multiple effect evaporator; b) reacting of concentrated spent wash of step (a) with aluminum sulphate for obtaining precipitation of potash alum and potash free spent wash(PFSW); c) clarifying precipitation of potash alum of step (b) to remove crystal of potash alum; d) reacting of potash alum crystal of step (c) with ingredient selected from lime, nitric acid and phosphoric acid; e) clarifying liquid of step (d) to get potassium sulphate, potassium nitrate , potassium sulfate solution and aluminium reach gypsum- 1; f) crystallizing of liquid from step (e) by cooling or evaporating the liquor to get potassium sulphate, potassium nitrate and potassium phosphate; and process for recovering aluminium sulfate comprises the steps; g) reacting the potash free spent wash of step (PFSW);
- the novel isolation process for recovery of potassium from spent wash comprises the steps of, a) concentrating potassium present in spent wash from 1.0. -2.0 % IIN to 4.5-5.0 % w/v in multiple effect evaporator; b) adding aluminium sulphate in concentrated spent wash of step (a) under stirring, to maintain aluminum concentration between 2.5-3% (w/w); c) clarifying reaction mixture of step (b) to get precipitation of potash alum having potassium concentration 6-8% w/v and aluminium concentration 4-5% (w/v) forming supernatant liquid; d) the resultant supernatant liquid from step (c) having potassium concentration 0.2-0.4% w/v and aluminium concentration 3-4% (w/v); e) adding ingredient selected from lime, nitric acid and phosphoric acid in precipitated potash alum of step (c) under stirring to maintain pH between 6.5 - 7.0 of reaction mixture; f) centrifuging the reaction mixture of step (e) to get liquid of potassium sulphide
- the present invention also provide potash free alcohol distillery spent wash which can be used for Animal (cattle) feed binder (replace the molasses in cattle feed plant).
- the present invention relates to recovery of water from sugar distillery spent wash effluent in each step after multiple effect evaporation.
- the invention also makes sugar distillery ZLD (Zero Liquid Discharge).
- potassium recovered from spent wash used to produce multi-nutrient potassium fertilizers viz., potassium sulphate, potassium nitrate, mono potassium phosphate etc.
- the invention is further illustrated by the following examples which are provided to be exemplary of the invention and do not limit the scope of the invention. While the present invention has been described in terms of its specific embodiments, certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention.
- Aluminium sulphate was added in to 100 Grams concentrated Spent Wash (K: 4.5-5.0%, pH: 3.5-4.5), under stirring to adjust pH of reaction mixer at 4.0-5.0 (Al +3 : 2.5-3%W/V).
- the resultant slurry was centrifuged at 10°C to obtain 70 Grams supernatant liquid Potash free spent wash (K + : 0.1-0.4 % W/V, Al +3 : 3-4 % W/V).
- the resultants Solid after centrifuge obtained 65 grams was the potash alum (K + : 6-8%, Al +3 : 4-6 % W/V).
- Example 1 teach us the method for isolation of potassium from spent wash.
- Example- 1 was repeated to obtain potash alum.
- Potassium sulphate/ Potassium Nitrate/ Potassium Phosphate solution crystallized by evaporation and cooling to produce crystals of potassium sulphate/ potassium nitrate/ potassium phosphate.
- Example-2 teach us the method of isolation of potash and aluminium from potash alum.
- Example- 1 was repeated and obtained potassium free spent wash , Lime was added in PFSW under stirring to adjust the pH at 5.0-6.5. The resultant slurry was centrifuged to obtain 12gm aluminium reach gypsum-2 (Al +3 : 7-8 % W/V) and remaining liquid would be the potash and aluminium free spent wash (Al +3 : 0.01- 0.03%, K + : 0.1-0.2 % W/V)
- Example- 3 teach us the method for recovery of aluminium from potassium free spent wash.
- Example-2 and Example-3 was repeated to obtain aluminium reach gypsum- 1, 2.
- H2SO4 was added in aluminium reach gypsum- 1, 2 under stirring to adjust the pH of reaction mixer at 0.8 -1.5.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
Le but de la présente invention vise à isoler du potassium d'un produit de lavage épuisé brut et d'un produit de lavage épuisé biométhanisé qui est généré durant les distillations d'alcool à base de mélasses. Le procédé implique la récupération du potassium à travers une technique de précipitation pour produire des engrais de potasse tels que du sulfate de potassium, du nitrate de potassium et du phosphate de potassium.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IN202121057901 | 2021-12-13 | ||
| IN202121057901 | 2021-12-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2023111784A1 true WO2023111784A1 (fr) | 2023-06-22 |
Family
ID=86773703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IB2022/061928 WO2023111784A1 (fr) | 2021-12-13 | 2022-12-08 | Nouveau procédé d'isolement de potasse à partir d'un produit de lavage épuisé |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2023111784A1 (fr) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3069230A (en) * | 1957-02-19 | 1962-12-18 | Montedison Spa | Process for extracting tartaric acid and potassium in form of pure potassium nitratein the cold form tartaric raw materials |
| CN101781138A (zh) * | 2010-03-19 | 2010-07-21 | 云南省轻工业科学研究院 | 用糖蜜酒精废醪液制取氮钾二元复混肥的方法 |
| WO2018154607A1 (fr) * | 2017-02-27 | 2018-08-30 | Council Of Scientific & Industrial Research | Processus de préparation d'engrais potassique à partir d'un effluent de distillerie d'alcool (lavage usé) |
| US10683211B2 (en) * | 2015-09-10 | 2020-06-16 | Council Of Scientific & Industrial Research | Process for potash recovery from biomethanated spent wash with concomitant environmental remediation of effluent |
-
2022
- 2022-12-08 WO PCT/IB2022/061928 patent/WO2023111784A1/fr unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3069230A (en) * | 1957-02-19 | 1962-12-18 | Montedison Spa | Process for extracting tartaric acid and potassium in form of pure potassium nitratein the cold form tartaric raw materials |
| CN101781138A (zh) * | 2010-03-19 | 2010-07-21 | 云南省轻工业科学研究院 | 用糖蜜酒精废醪液制取氮钾二元复混肥的方法 |
| US10683211B2 (en) * | 2015-09-10 | 2020-06-16 | Council Of Scientific & Industrial Research | Process for potash recovery from biomethanated spent wash with concomitant environmental remediation of effluent |
| WO2018154607A1 (fr) * | 2017-02-27 | 2018-08-30 | Council Of Scientific & Industrial Research | Processus de préparation d'engrais potassique à partir d'un effluent de distillerie d'alcool (lavage usé) |
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