CA2570565A1 - Method for extracting fulvic acid molecules - Google Patents
Method for extracting fulvic acid molecules Download PDFInfo
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- CA2570565A1 CA2570565A1 CA002570565A CA2570565A CA2570565A1 CA 2570565 A1 CA2570565 A1 CA 2570565A1 CA 002570565 A CA002570565 A CA 002570565A CA 2570565 A CA2570565 A CA 2570565A CA 2570565 A1 CA2570565 A1 CA 2570565A1
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- mixture
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- filtration apparatus
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- acid molecules
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
Abstract
Methods for extracting molecules of fulvic acid from a humus material such as oxidized lignite are disclosed. The humus material is mixed with water to solubilize at least some of the fulvic acid molecules. A first filtration apparatus (which may be an ultrafiltration apparatus) may be used to separate at least some of the solubilized fulvic acid molecules from the humin and at least some of the humic acid molecules. A second filtration apparatus (which may be an ultrafiltration apparatus or a nanfiltration apparatus) may be used to then separate the fulvic acid molecules from most of the water and any remaining impurities. A digestion step may also be carried out where microorganisms are brought into contact with the mixture in the presence of oxygen in order to oxidize any unoxidized organic compounds in the humus material. Iron and aluminum may be precipitated and removed by the addition of a phosphate to improve the purity of the end-product.
Claims (55)
1. A method for extracting molecules of fulvic acid from a humus material comprising molecules of humin, humic acid and fulvic acid, the method comprising the steps of: (a) mixing the humus material with water to solubilize at least some of the molecules of fulvic acid; and (b) separating at least some the solubilized fulvic acid molecules from the humin molecules and from at least some of the humic acid molecules by ultrafiltration
2. A method according to claim 1 further comprising, between steps (a) and (b), a digestion step comprising contacting microorganisms with the mixture in the presence of oxygen to oxidize any unoxidized organic compounds in the humus material.
3. A method according to claim 2 wherein the microorganisms are bacteria, protozoa, fungi or a mixture of two or more of bacteria, protozoa and fungi.
4. A method according to claim 2 or 3 wherein the microorganisms are contacted with the mixture by adding compost, compost tea, soil or manure to the mixture, the compost, compost tea, soil or manure comprising the microorgan-isms.
5. A method according to any one of claims 2 to 4 wherein air is bubbled through the mixture during the digestion step.
6. A method according to any one of claims 1 to 5 wherein at least some of the solubilized fulvic acid molecules are separated from at least some of the humic acid molecules by filtering the mixture through a first filtration appara-tus which retains at least some of the humic acid molecules while allowing at least some of the solubilized fulvic acid molecules to pass through, wherein at least some of the solubilized fulvic acid molecules are separated from the humin molecules before or during filtering the mixture through first filtration apparatus, wherein the first filtration apparatus is an ultrafiltration apparatus.
7. A method according to claim 6 wherein the first filtration apparatus retains particles or compounds having a molecular weight of at least about 2500 to 12,500 Daltons.
8. A method according to claim 7 wherein the first filtration apparatus retains particles or compounds having a molecular weight of at least about 8000 Daltons.
9. A method according to any one of claims 6 to 8 further comprising, after step (b), the step of (c) separating at least some of the solubilized fulvic acid molecules from part of the water by ultrafiltration or nanofiltration.
10. A method according to claim 9 wherein step (c) is carried out by filtering the mixture through a second filtration apparatus after being filtered through the first filtration apparatus, wherein the second filtration apparatus retains at least some of the solubilized fulvic acid molecules while allowing part of the water to pass through, wherein the second filtration apparatus is an ultrafiltration apparatus or a nanofiltration apparatus.
11. A method according to claim 10 wherein the second filtration apparatus retains all or substantially all of the fulvic acid molecules which have passed through the first filtration apparatus.
12. A method according to claim 10 or 11 wherein the second filtration apparatus retains particles or molecules having a molecular weight of at least about 250 to 1000 Daltons.
13. A method according to claim 14 wherein the second filtration apparatus retains particles or molecules having a molecular weight of at least about 600 Daltons.
14. A method according to any one of claims 10 to 13 wherein the second filtra-tion apparatus retains part of the water, thereby leaving the separated fulvic acid molecules from step (c) in a solution.
15. A method according to claim 14 further comprising the step of reducing the water content of the solution obtained from step (c) to concentrate the solution.
16. A method according to claim 14 further comprising the step of drying the solution obtained from step (c) to leave the fulvic acid in a powder.
17. A method according to any one of claims 6 to 16 wherein the first filtration apparatus allows all or substantially all of the solubilized fulvic acid molecules to pass through.
18. A method according to any one of claims 10 to 17 wherein the mixture is filtered through a third filtration apparatus before being filtered through the first filtration apparatus, wherein the third filtration apparatus retains the humin molecules and at least some of the humic acid molecules while allow-ing the solubilized fulvic acid molecules and at least some of the humic acid molecules to pass through, wherein the third filtration apparatus is an ultrafiltration apparatus.
19. A method according to claim 18 wherein the third filtration apparatus retains particles or molecules having a molecular weight of more than about 12,500 Daltons.
20. A method according to claim 19 wherein the third filtration apparatus retains particles or molecules having a molecular weight of at least about 25,000 Daltons.
21. A method according to any one of claims 6 to 17 wherein the first filtration apparatus retains all or substantially all of the humic acid molecules.
22. A method according to any one of claims 18 to 20 wherein all or substantially all of the humic acid molecules are retained by one or both of the first filtra-tion apparatus and the third filtration apparatus.
23. A method according to any one of claims 6 to 22 further comprising, after step (a) but before filtering the mixture through the first filtration apparatus, the steps of adjusting the pH of the mixture to about 5 to 8, adding a phosphate to the mixture to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate and separating any precipitated iron phosphate and aluminum phosphate from the fulvic acid molecules.
24. A method according to claim 23 wherein the phosphate is selected from the group consisting of monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate, magnesium phosphate, calcium phosphate, and mixtures of two or more of monopotassium phos-phate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate and calcium phosphate.
25. A method according to claim 23 or 24 wherein the phosphate is phosphoric acid.
26. A method according to any one of claims 23 to 25 wherein the addition of the phosphate to the mixture is sufficient to adjust the pH of the mixture to about to 8.
27. A method according to any one of claims 23 to 25 wherein an acid is added to the mixture to adjust the pH of the mixture to about 5 to 8.
28. A method according to claim 27 wherein the acid is selected from phosphoric acid, acetic acid, citric acid, hydrochloric acid and sulfuric acid and mixtures of two or more of phosphoric acid, acetic acid, citric acid, hydrochloric acid and sulfuric acid.
29. A method according to any one of claims 23 to 25 wherein an alkali is added to the mixture to adjust the pH of the mixture to about 5 to 8.
30. A method according to claim 29 wherein the alkali is selected from monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, calcium carbonate, calcium-magnesium carbonate, potassium hydroxide and sodium hydroxide and mixtures of two or more of monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate, magnesium phosphate, calcium phosphate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, calcium carbonate, calcium-magnesium carbonate, potassium hydroxide and sodium hydroxide.
31. A method according to any one of claims 18 to 20 and 22 further comprising, after filtering the mixture through the third filtration apparatus and before filtering through the first filtration apparatus, the steps of adjusting the pH of the mixture to about 5 to 8, adding a phosphate to the mixture to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate and separating any precipitated iron phosphate and aluminum phosphate from the fulvic acid molecules.
32. A method according to claim 31 wherein the phosphate is selected from the group consisting of monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate, magnesium phosphate, calcium phosphate, and mixtures of two or more of monopotassium phos-phate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate and calcium phosphate.
33. A method according to claim 31 or 32 wherein the phosphate is phosphoric acid.
34. A method according to any one of claims 31 to 33 wherein the pH of the mixture is adjusted to at least about 9.4 prior to filtering the mixture through the third filtration apparatus and wherein the pH of the mixture is adjusted, by the addition of an acid, to about 5 to 8 after filtering the mixture through the third filtration apparatus.
35. A method according to claim 34 wherein the acid is selected from phosphoric acid, acetic acid, citric acid, hydrochloric acid and sulfuric acid and mixtures of two or more of phosphoric acid, acetic acid, citric acid, hydrochloric acid and sulfuric acid.
36. A method according to any one of claims 31 to 35 wherein the pH of the mixture is adjusted to at least about 9.4 by the addition of an alkali.
37. A method according to claim 36 wherein the alkali is selected from monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, calcium carbonate, calcium-magnesium carbonate, potassium hydroxide and sodium hydroxide and mixtures of two or more of monopotassium phosphate, dipotassium phosphate, tripotassium phosphate, sodium pyrophosphate, magnesium phosphate, calcium phosphate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, calcium carbonate, calcium-magnesium carbonate, potassium hydroxide and sodium hydroxide.
38. A method according to any one of claims 1 to 37 wherein the humus material comprises one or more of peats, oxidized lignites, peat moss, composts, brown coals, soil, pond sediment and biosolids.
39. A method according to 38 wherein the humus material comprises oxidized lignite, and wherein the oxidized lignite is leonardite.
40. A method according to any one of claims 1 to 39 wherein the humus material is ground prior to being mixed with the water in step (a).
41. A method according to any one of claims 1 to 40 wherein the mixture in step (a) comprises from about 3% to about 35% by weight of the humus material.
42. A method according to any one of claims 1 to 41 further comprising the step of heating the mixture prior to step (b).
43. A method according to claim 42 wherein the mixture is heated at a tempera-ture from about 50 °C to 70 °C.
44. A method according to any one of claims 1 to 43 further comprising allowing the mixture to settle prior to step (b).
45. A method according to any one of claims 6 to 44 further comprising the step of filtering the mixture to remove particles of a chosen size prior to filtering the mixture through the first filtration apparatus.
46. A method according to any one of claims 1 to 45 wherein the water in step (a) is provided in an aqueous solution which is mixed with the humus material.
47. A method for producing an agricultural or horticultural solution comprising fulvic acid molecules, the method comprising:
(a) mixing a humus material comprising molecules of humin, humic acid and fulvic acid with water to solubilize at least some of the fulvic acid molecules;
(b) filtering the mixture through a first filtration apparatus which is configured to retain particles or molecules having a molecular weight of at least 2500 to 12,500 Daltons to separate at least some of the fulvic acid molecules from at least some of the humic acid molecules, the humin molecules being separated from the fulvic acid molecules prior to or during filtering the mixture through the first filtration apparatus; and (c) passing the filtrate from the first filtration apparatus through a second filtration apparatus, wherein the second filtration apparatus retains at least some of the solubilized fulvic acid molecules and some of the water, thereby producing the solution.
(a) mixing a humus material comprising molecules of humin, humic acid and fulvic acid with water to solubilize at least some of the fulvic acid molecules;
(b) filtering the mixture through a first filtration apparatus which is configured to retain particles or molecules having a molecular weight of at least 2500 to 12,500 Daltons to separate at least some of the fulvic acid molecules from at least some of the humic acid molecules, the humin molecules being separated from the fulvic acid molecules prior to or during filtering the mixture through the first filtration apparatus; and (c) passing the filtrate from the first filtration apparatus through a second filtration apparatus, wherein the second filtration apparatus retains at least some of the solubilized fulvic acid molecules and some of the water, thereby producing the solution.
48. A method according to claim 47 further comprising, between steps (a) and (b), a digestion step comprising contacting microorganisms with the mixture in the presence of oxygen to oxidize any unoxidized organic compounds in the humus material.
49. A method according to claim 47 or 48 wherein the second filtration appara-tus is configured to retain particles or molecules having a molecular weight of at least about 250 to 1000 Daltons.
50. A method according to any one of claims 47 to 49 wherein the mixture is filtered through a third filtration apparatus prior to being filtered through the first filtration apparatus, the third filtration apparatus retaining the humin molecules and at least some of the humic acid molecules while allowing the solubilized fulvic acid molecules to pass through, wherein the third filtration apparatus is configured to retain particles or molecules having a molecular weight of more than about 12,500 Daltons.
51. A method according to claim 50 further comprising, after filtering the mixture through the third filtration apparatus and before filtering the mixture through the first filtration apparatus, the steps of adjusting the pH of the mixture to about 5 to 8, adding a phosphate to the mixture to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate and separating any precipitated iron phosphate and aluminum phosphate from the fulvic acid molecules.
52. A solution produced according to a method according to any one of claims to 51.
53. A method for extracting molecules of fulvic acid from a humus material comprising molecules of humin, humic acid and fulvic acid, the method comprising the steps of:
(a) mixing ground humus material with water to solubilize at least some of the fulvic acid molecules;
(b) contacting microorganisms with the mixture in the presence of oxygen for a period of 1 to 7 days to oxidize any unoxidized organic com-pounds in the humus material;
(c) adding a phosphate to the mixture and adjusting the pH of the mixture to about 5 to 8 to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate, wherein any precipitated iron phosphate and aluminum phosphate is removed in one or more of steps (d), (g) and (h);
(d) passing the mixture through a first filter, the pores of the first filter being sized to retain particles have a size of at least 74 microns, the filtrate from the first filter comprising a mixture of a solution compris-ing fulvic acid molecules and solids having sizes smaller than about 74 microns;
(e) allowing the filtrate from the first filter to settle for a period of time;
(f) heating the filtrate from the first filter at temperature from about 50 °C
to 70 °C;
(g) passing the filtrate from the first filter through a second filter, the pores of the second filter being sized to retain particles having a size of at least about 5 to 30 microns, the filtrate from the second filter compris-ing a mixture of a solution comprising the solubilized fulvic acid molecules and particles having sizes smaller than about 5 to 30 mi-crons;
(h) passing the filtrate from the second filter through a first filtration apparatus, wherein the first filtration apparatus is an ultrafiltration apparatus which retains all or substantially all of the remaining humin and humic acid molecules while allowing the solution comprising the solubilized fulvic acid molecules to pass through;
(i) passing the filtrate from the first filtration apparatus through a second filtration apparatus, wherein the second filtration apparatus is an ultrafiltration apparatus or a nanofiltration apparatus, and wherein the second filtration apparatus retains all or substantially all of the fulvic acid molecules while allowing at least part of the water to pass through.
(a) mixing ground humus material with water to solubilize at least some of the fulvic acid molecules;
(b) contacting microorganisms with the mixture in the presence of oxygen for a period of 1 to 7 days to oxidize any unoxidized organic com-pounds in the humus material;
(c) adding a phosphate to the mixture and adjusting the pH of the mixture to about 5 to 8 to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate, wherein any precipitated iron phosphate and aluminum phosphate is removed in one or more of steps (d), (g) and (h);
(d) passing the mixture through a first filter, the pores of the first filter being sized to retain particles have a size of at least 74 microns, the filtrate from the first filter comprising a mixture of a solution compris-ing fulvic acid molecules and solids having sizes smaller than about 74 microns;
(e) allowing the filtrate from the first filter to settle for a period of time;
(f) heating the filtrate from the first filter at temperature from about 50 °C
to 70 °C;
(g) passing the filtrate from the first filter through a second filter, the pores of the second filter being sized to retain particles having a size of at least about 5 to 30 microns, the filtrate from the second filter compris-ing a mixture of a solution comprising the solubilized fulvic acid molecules and particles having sizes smaller than about 5 to 30 mi-crons;
(h) passing the filtrate from the second filter through a first filtration apparatus, wherein the first filtration apparatus is an ultrafiltration apparatus which retains all or substantially all of the remaining humin and humic acid molecules while allowing the solution comprising the solubilized fulvic acid molecules to pass through;
(i) passing the filtrate from the first filtration apparatus through a second filtration apparatus, wherein the second filtration apparatus is an ultrafiltration apparatus or a nanofiltration apparatus, and wherein the second filtration apparatus retains all or substantially all of the fulvic acid molecules while allowing at least part of the water to pass through.
54. A method for extracting molecules of fulvic acid from a humus material comprising molecules of humin, humic acid and fulvic acid, the method comprising the steps of:
(a) mixing ground humus material with water to solubilize at least some of the fulvic acid molecules;
(b) contacting microorganisms with the mixture in the presence of oxygen to oxidize any unoxidized organic compounds in the humus material;
(c) filtering the mixture through a first filtration apparatus, wherein the first filtration apparatus retains the humin molecules and at least some of the humic acid molecules while allowing the solubilized fulvic acid molecules to pass through the first filtration apparatus, wherein the first filtration apparatus is configured to retain particles or molecules having a molecular weight of more than about 12,500 Daltons.
d) adjusting the pH of the mixture to about 5 to 8;
(e) adding a phosphate to the mixture to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate;
(f) removing any precipitated iron phosphate and aluminum phosphate from the mixture;
(g) filtering the mixture through a second filtration apparatus to separate at least some of the fulvic acid molecules from at least some of the humic acid molecules, wherein the second filtration apparatus is configured to retain particles or molecules having a molecular weight of at least about 2500 to 12,500 Daltons; and (h) filtering the mixture through a third filtration apparatus, wherein the third filtration apparatus retains all or substantially all of the fulvic acid molecules which passed through the second filtration apparatus while allowing at least part of the water to pass through, wherein the third filtration apparatus is configured to retain particles or molecules having a molecular weight of at least about 250 to 1000 Daltons.
(a) mixing ground humus material with water to solubilize at least some of the fulvic acid molecules;
(b) contacting microorganisms with the mixture in the presence of oxygen to oxidize any unoxidized organic compounds in the humus material;
(c) filtering the mixture through a first filtration apparatus, wherein the first filtration apparatus retains the humin molecules and at least some of the humic acid molecules while allowing the solubilized fulvic acid molecules to pass through the first filtration apparatus, wherein the first filtration apparatus is configured to retain particles or molecules having a molecular weight of more than about 12,500 Daltons.
d) adjusting the pH of the mixture to about 5 to 8;
(e) adding a phosphate to the mixture to precipitate any iron and any aluminum in the humus material as iron phosphate and aluminum phosphate;
(f) removing any precipitated iron phosphate and aluminum phosphate from the mixture;
(g) filtering the mixture through a second filtration apparatus to separate at least some of the fulvic acid molecules from at least some of the humic acid molecules, wherein the second filtration apparatus is configured to retain particles or molecules having a molecular weight of at least about 2500 to 12,500 Daltons; and (h) filtering the mixture through a third filtration apparatus, wherein the third filtration apparatus retains all or substantially all of the fulvic acid molecules which passed through the second filtration apparatus while allowing at least part of the water to pass through, wherein the third filtration apparatus is configured to retain particles or molecules having a molecular weight of at least about 250 to 1000 Daltons.
55. A fulvic acid product comprising fulvic acid molecules extracted from a humus material according to a method according to any one of claims 1 to 46, 53 and 54.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CA2004/000935 WO2006000073A1 (en) | 2004-06-23 | 2004-06-23 | Method for extracting fulvic acid molecules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2570565A1 true CA2570565A1 (en) | 2006-01-05 |
| CA2570565C CA2570565C (en) | 2012-10-23 |
Family
ID=34957953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2570565A Active CA2570565C (en) | 2004-06-23 | 2004-06-23 | Method for extracting fulvic acid molecules |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US7896944B2 (en) |
| EP (1) | EP1797190B1 (en) |
| AU (1) | AU2004320919B2 (en) |
| CA (1) | CA2570565C (en) |
| DE (1) | DE602004029827D1 (en) |
| WO (1) | WO2006000073A1 (en) |
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