WO2017100507A1 - Compositions fertilisantes contenant un inhibiteur d'uréase résistant aux acides - Google Patents

Compositions fertilisantes contenant un inhibiteur d'uréase résistant aux acides Download PDF

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Publication number
WO2017100507A1
WO2017100507A1 PCT/US2016/065721 US2016065721W WO2017100507A1 WO 2017100507 A1 WO2017100507 A1 WO 2017100507A1 US 2016065721 W US2016065721 W US 2016065721W WO 2017100507 A1 WO2017100507 A1 WO 2017100507A1
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Prior art keywords
basic component
particulate
nbpt
fertilizer
substituted
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PCT/US2016/065721
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English (en)
Inventor
Drew BOBECK
Jessica GILES
Robert Kelly
Stuart STAPLES
Brian Wade
Stacey Wertz
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Koch Agromonic Services, Llc
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Publication of WO2017100507A1 publication Critical patent/WO2017100507A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C05C9/005—Post-treatment
    • 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
    • C05B—PHOSPHATIC FERTILISERS
    • C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • C05C3/005—Post-treatment
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C5/00—Fertilisers containing other nitrates
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/10—Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12—Granules or flakes

Definitions

  • the present disclosure relates to novel acid resistant fertilizer compositions that comprise a particulate urease inhibitor containing urea source, a particulate acidic fertilizer, and a basic component, and methods of making and using the acid resistant fertilizer compositions.
  • a urease inhibitor such as an N-alkyl phosphoric triamide or N-alkyl thiopho sphoric triamide (particularly N-(n-butyl) thiopho sphoric triamide, NBPT) can slow down the enzymatic breakdown of urea by inhibition of the urease enzyme. This provides an effective means of managing losses of nitrogen in the form of ammonia from surface-applied urea containing fertilizers.
  • N-alkyl phosphoric triamide or N-alkyl thiopho sphoric triamide urease inhibitor such as NBPT can be applied onto a granular fertilizer formulation by first blending the concentrated solution of the N-alkyl thiopho sphoric triamide that is dissolved in a solvent such as a glycol or glycol derivative or a mixed solvent of a glycol or glycol derivative and a liquid amide, (see U.S. Patent No. 5,698,003).
  • an N-alkyl phosphoric triamide or N-alkyl thiopho sphoric triamide urease inhibitor such as NBPT can be introduced into the urea melt to form an incorporated urea fertilizer (see WO 2015/027244).
  • NBPT N-alkyl phosphoric triamide or N-alkyl thiopho sphoric triamide urease inhibitor
  • a highly concentrated dry formulation of NBPT such as AGROTAIN® DRI-MAXX nitrogen stabilizer, which can adhere to the urea granules without adding additional moisture to the blend, can be used to treat urea granules to make a NBPT-containing urea as well, (see U.S. Patent No. 9,034,072).
  • N-alkyl phosphoric triamide or N-alkyl thiophosphoric triamide such as NBPT is reasonably stable under normal storage conditions such as room temperature and neutral pH, it is well known that acidic conditions may lead to rapid disappearance of NBPT. See, for example, Apparent persistence of N-(N -butyl) thiophosphoric triamide is greater in alkaline soils, Engel et al, Soil Science Society of America Journal (2013), 77(4), 1424-1429.
  • the primary objective of the present disclosure is to develop an economic and stable fertilizer composition that comprises a particulate urease inhibitor containing urea source, a particulate acidic fertilizer such as phosphate or sulfate fertilizer or a combination thereof, and a suitable basic component that is used to treat either the particulate urease inhibitor containing urea source or the particulate acidic fertilizer or both of them independently , wherein the impact of the acidic characteristics of the particulate acidic fertilizer to the urease inhibitor may be substantially mitigated to provide the improved storage life for the acid sensitive urease inhibitor such as NBPT.
  • Urease inhibitor containing urea based fertilizers and phosphate or sulfate based fertilizers can provide different nutrients to soils and/or plants to supply one or more nutrients essential to the growth of plants. Although fertilizers comprising different nutrients may be applied to soils or plants separately, it may be beneficial to prepare, package, transport, store and/or use a single fertilizer composition.
  • a urease inhibitor such as NBPT may decompose almost completely within 1-2 weeks after the blending of the NBPT-containing urea and one or more acidic fertilizers such as MAP.
  • certain basic components applied to the surface of particulate acidic fertilizers provide unexpected stability for NBPT when NBPT treated urea is blended with the basic component treated acidic fertilizers.
  • acidic fertilizers that can be treated include MAP, DAP, ammonium sulfate, rock phosphate, or Micro-Essentials® SZ (MESZ (12- 40-0-lOS-lZn).
  • MAP MAP
  • DAP ammonium sulfate
  • rock phosphate rock phosphate
  • Micro-Essentials® SZ MEZ (12- 40-0-lOS-lZn
  • the same surprising benefits are realized by treating the surface of the particulate urease inhibitor containing fertilizer with certain basic component.
  • This basic component treated composition may also provide unexpectedly longer NBPT storage life time when it is blended with an untreated acidic fertilizer.
  • the present disclosure provides novel economic and acid resistant urease inhibitor containing fertilizer compositions that may provide longer storage life for an acid sensitive urease inhibitor such as NBPT.
  • the present disclosure provides a particulate fertilizer composition
  • a particulate fertilizer composition comprising a basic component and a particulate acidic fertilizer having a surface, wherein the surface of the particulate acidic fertilizer is treated with the basic component.
  • the weight percentage range of the basic component can be 0.001% to 20 % by weight and the weight percentage range of the particulate acidic fertilizer can be 99.999 % to 80 % by weight.
  • the particulate acidic fertilizer that is treated with the basic component provides 14- 1500 days of half-life under accelerated NBPT stability lab test condition for a urease inhibitor when the basic component treated particulate acidic fertilizer is blended with a particulate urease inhibitor containing urea source.
  • the present disclosure provides a particulate fertilizer composition
  • a particulate fertilizer composition comprising a basic component and a particulate urease inhibitor containing urea source having a surface, wherein the surface of the particulate urease inhibitor containing urea source is treated with the basic component.
  • the particulate urease inhibitor containing urea source that is treated with the basic component provides 14-1500 days of half-life under accelerated NBPT stability lab test condition for the urease inhibitor when the basic component treated particulate urease inhibitor containing urea source is blended with a particulate acidic fertilizer.
  • the present disclosure provides an acid resistant fertilizer composition comprising
  • the acid resistant fertilizer composition provides 14-1500 days of half-life under accelerated NBPT stability lab test condition for the urease inhibitor.
  • Base component treated means that a suitable basic component is added and adhered onto the surface of either the particulate acidic fertilizer or the particulate urease inhibitor containing urea source to provide sufficient protection for the urease inhibitor such as NBPT.
  • the actual percentage of the covered surface of a particulate fertilizer may vary from 10% to 100%, 20% to 100%, 30% to 100%, 40% to 100%, 50% to 100%, 60% to 100%. 70% to 100%, 80% to 100%, 90% to 100%, or 95% to 100%.
  • the percentage of the covered surface in the present disclosure primarily means the percentage of the visible outer surface of the particulate fertilizer particles instead of the total surface area that may include the surface area of small pores within the particulate fertilizer particle.
  • Half-life storage time or "half-life" of a urease inhibitor such as NBPT in the present disclosure means the amount of time required for the amount of urease inhibitor such as NBPT to decrease to half of its initial value prior to the blending of the particulate acidic fertilizer and the particulate urease inhibitor containing urea source.
  • a fertilizer blend to be tested for the urease inhibitor half-life storage time is stored in sealed jar at ambient condition after the particulate acidic fertilizer is blended with the urease inhibitor containing urea source.
  • the urease inhibitor content is analyzed by high pressure liquid chromatography (HPLC), which is known to those skilled in the art. In some situations, the half-life storage time is long.
  • the urease inhibitor content is still above 50% of the original urease inhibitor content.
  • the actual urease inhibitor content and the days passed after the blending is recorded.
  • the NBPT content in Example 33 of the present disclosure reached half of the original content on day 91 (half-life). The half-life storage time of 91 days is thus recorded as the NBPT half-life.
  • the NBPT content in Example 34 of the present disclosure is 71% on day 28 when the data is collected. The value 71% is well above 50%.
  • the actual days after the blending (28 days) and the remaining NBPT (71%) content is provided.
  • NBPT is the most widely used urease inhibitor to mitigate the nitrogen losses due to the ammonia volatilization for urea or urea-based fertilizers.
  • NBPT is very sensitive to acidic conditions.
  • the most widely used phosphate and sulfate fertilizers are often very acidic and will decompose NBPT very quickly if they are blended with NBPT containing urea sources. It has been observed that NBPT may decompose almost completely within 1-2 weeks after the blending of the NBPT-containing urea and one or more acidic fertilizers such as MAP.
  • the present disclosure provides a particulate fertilizer composition
  • a particulate fertilizer composition comprising a basic component and a particulate acidic fertilizer having a surface, wherein the surface of the particulate acidic fertilizer is treated with the basic component.
  • the particulate acidic fertilizer that is treated with the basic component provides 14- 1500 days of half-life under accelerated NBPT stability lab test condition for a urease inhibitor when the basic component treated particulate acidic fertilizer is blended with a particulate urease inhibitor containing urea source.
  • the present disclosure provides a particulate fertilizer
  • composition comprising a basic component and a particulate urease inhibitor containing urea source having a surface, wherein the surface of the particulate urease inhibitor containing urea source is treated with the basic component.
  • the particulate urease inhibitor containing urea source that is treated with the basic component provides 14-1500 days of half-life under accelerated NBPT stability lab test condition for the urease inhibitor when the basic component treated particulate urease inhibitor containing urea source is blended with a particulate acidic fertilizer.
  • an acid resistant fertilizer composition comprising
  • the acid resistant fertilizer composition provides 14-1500 days of half-life under accelerated NBPT stability lab test condition for the urease inhibitor.
  • any particulate fertilizer may be treated with at least one additional layer of another material that may include but is not limited to a petroleum product, a wax, a paraffin oil, a bitumen, an asphalt, a lubricant, a coal product, an oil, canola oil, soybean oil, coconut oil, linseed oil, tung oil, vegetable wax, animal fat, animal wax, a forest product, tall oil, modified tall oil, tall oil pitch, pine tar, a synthetic oil, a synthetic wax, a synthetic lubricant, an ethylene- vinyl acetate copolymer, an ethyleneacrylic acid copolymer, an ethylene-ethyl acrylate copolymer, an ethylene-vinyl alcohol copolymer, ethylene-vinyl, alcohol- vinyl acetate terpolymers, polyurethane polymer, alkyd resin, a surfactant, soap or a combination thereof.
  • a petroleum product a wax, a paraffin oil, a bitumen, an
  • the at least one additional layer of another material may be applied prior to or after the treatment of a basic component to a particulate acidic realizer or a particulate urease inhibitor containing urea source.
  • the at least one additional layer of another material has a weight percentage range of 0.01% to 5 % by weight of the total weight of the particulate fertilizer that is treated by the at least one additional layer of another material.
  • the weight percentage range is 0.02% to 1.0 % by weight.
  • the weight percentage range is 0.04% to 0.5 % by weight.
  • the at least one additional layer of another material is a wax.
  • the particulate acidic fertilizer may be any acidic fertilizer or a fertilizer composition comprising an acidic component.
  • the particulate acidic fertilizer may provide a pH value lower than 7 when it is dissolved or partially dissolved in water.
  • a particulate acidic fertilizer in the present disclosure may include any material that comprises any form of phosphate or sulfate.
  • phosphate may include any material comprising any form of P0 4 3 ⁇ , HP0 4 2" , H 2 P0 4 2 ⁇ , H 3 P0 4 or any combination thereof.
  • Sulfate may include any material comprising any form of S0 4 2" , HS0 4 " , H 2 S0 4 , or any combination thereof.
  • a particulate acidic fertilizer in the present disclosure may be selected but is not limited to monoammonium phosphate (MAP), diammonium phosphate (DAP), ammonium sulfate, ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, NPSZ, Micro-Essentials SZ (MESZ ( 12-40-0- lOS- ⁇ ), triple super phosphate, struvite, or any combination thereof.
  • the particulate acidic fertilizer is selected from MAP, DAP or ammonium sulfate.
  • the particulate urea source may be urea or urea-formaldehyde polymers, or any combination thereof.
  • the solid form of a urea source may be pellets, prills, pastilles, flakes, granules, or a combination thereof.
  • a urea source is urea granules.
  • the urease inhibitors may be N-alkyl phosphoric triamides or N-alkyl thiophosphoric triamides according to Formula I:
  • X is oxygen or sulfur
  • R 1 and R 2 are independently hydrogen, 0-0 2 alkyl, C 3 -Ci 2 cycloalkyl, C 6 -Ci 4 aryl, C 2 -Ci 2 alkenyl, C 2 -Ci 2 alkynyl, C5-Ci 4 heteroaryl, 0-0 4 heteroalkyl, C 2 -Ci 4 heteroalkenyl, C 2 -Ci 4 heteroalkynyl, or C 3 -Ci 2 cycloheteroalkyl.
  • the urease inhibitor in the present disclosure is N-(n-butyl) thiophosphoric triamide (NBPT).
  • the particulate urease inhibitor containing urea source may be made by mixing a urease inhibitor such as NBPT with a urea source such as urea granules.
  • a urease inhibitor such as NBPT
  • a urea source such as urea granules.
  • NBPT may be applied onto urea granules by a concentrated solution of NBPT that is dissolved in a solvent such as a glycol or glycol derivative or a mixed solvent of a glycol or glycol derivative and a liquid amide, (see U.S. Patent No. 5,698,003).
  • a solvent such as a glycol or glycol derivative or a mixed solvent of a glycol or glycol derivative and a liquid amide, (see U.S. Patent No. 5,698,003).
  • Other solvents such as glycerol, glycol ethers, amines, and DMSO may also be used.
  • NBPT may be introduced into the
  • NBPT such as AGROTAIN DRI-MAXX® nitrogen stabilizer
  • AGROTAIN DRI-MAXX® nitrogen stabilizer which can adhere to the urea granules without adding additional moisture to the blend, can be used to treat urea granules to make a NBPT-containing urea as well, (see U.S. Patent No. 9,034,072).
  • a basic component may be any suitable substance that can accept hydrogen ions (protons) released from an acidic fertilizer.
  • a basic component may be an organic carboxylic or a sulfonic acid salt according to Formula (II):
  • R 1 is independently hydrogen, substituted or non-substituted C1-C30 straight or branched alkyl, substituted or non-substituted C1-C30 straight or branched alkenyl, substituted non-substituted C3-C8 cycloalkyl, or substituted or non-substituted C5-C6 aromatic carbon or heterocyclic ring
  • (X ) is a (COO ) or (SO3) "
  • M n+ is metal ion, wherein the metal is Li, Na, K, Rb, Cs, Mg, Ca, Sr, Ba, Ra, Al, Mn, Fe, Co, Cu, or Zn; n is 1, 2, 3, or 4.
  • the carboxylic acid or sulfonic acid salt has a structure according to Formula (II) wherein R 1 is independently hydrogen, substituted or non-substituted C8-C20 straight or branched alkyl, substituted or non-substituted C8-C20 straight or branched alkenyl, substituted or non-substituted C3-C6 cycloalkyl, or substituted or non-substituted benzene ring; M n+ is a metal ion, wherein the metal is Mg, Ca, or Al,; and n is 1, 2, or 3.
  • the carboxylic acid or sulfonic acid salt according to Formula (II) is a stearate, wherein the metal is Mg, Ca, or Al; and n is 2 or 3.
  • a basic component may be a metal oxide, metal hydroxide, metal alkoxide with C1-C30 straight or branched carbon chain, metal sulfate, metal bisulfate, metal carbonate, or metal bicarbonate, wherein the metal is Li, Na, K, Rb, Cs, Mg, Ca, Sr, Ba, Ra, Al, Mn, Fe, Co, Cu, or Zn.
  • the basic component is MgO, Mg(OH) 2 , CaO, Ca(OH) 2 , A1 2 0 3 , Al(OH) 3 , or lime (Lime is a calcium-containing inorganic material in which carbonates, oxides and hydroxides predominate).
  • a basic component may be an amine compound, which is a primary, secondary, or tertiary, straight or branched hydrocarbon amine.
  • the hydrocarbon is Ci-C 3 o straight or branched alkyl, Ci-C 3 o straight or branched alkenyl, C 3 -Cs cycloalkyl, or benzene ring, wherein the hydrocarbon is optionally substituted with hydroxyl, amino, or [(- NH)(CH 2 CH 2 )]xNH 2 , wherein x is 1, 2, 3, 3, or 4.
  • the amine compound is triethylenetetramine (TETA), trimethylamine (TEA), monoethanolamine (ME A),
  • the basic component is MgO.
  • the basic component in the present disclosure is a solid that can sufficiently adhere to the surface of a particulate fertilizer. In one aspect, the basic component in the present disclosure is a liquid that can provide a coating layer on the surface of a particulate fertilizer.
  • the fertilizer composition may further comprise a nitrification inhibitor.
  • the nitrification inhibitor may be selected from 2-chloro-6- trichloromethylpyridine, 5-ethoxy-3-trichloromethyl-l,2,4-thiadiazol, dicyandiamide (DCD), 2- amino-4-chloro-6-methyl-pyrimidine, l,3-benzothyiazole-2-thiol, 4-amino-N-l,3-thiazol-2- ylbenzene sulfonamide, thiourea, guanidine, 3,4-dimethylpyrazole phosphate, 2,4-diamino-6- trichloromethyl-5-triazine, poly etherionophores, 4-amino-l,2,4-triazole, 3-mercapto- 1,2,4- triazole, potassium azide, carbon bisulfide, sodium trithiocarbonate, ammonium dithiocarbamate, 2,3-
  • the nitrification inhibitor may be added as a separate particulate component at any time or be mixed with the urease inhibitor treated urea source prior to be treated with a basic component of the present disclosure.
  • a nitrification inhibitor is DCD or 2-chloro-6-trichloromethylpyridine.
  • the weight percentage of the nitrification inhibitor is 0.01% to 10% of the total weight of the final fertilizer composition blend. In one aspect, the weight percentage of the nitrification inhibitor is 1% to 5% of the total weight of the final fertilizer composition blend.
  • a particulate acidic fertilizer or a particulate urease inhibitor containing urea source with their surface treated with a suitable basic component may provide 14-1500, 28-1500, 60-1500, or 90-1500 days of NBPT half-life under accelerated NBPT stability lab test condition from the time when the particulate acidic fertilizer and the particulate urease inhibitor containing urea source are blended.
  • a particulate acidic fertilizer or a particulate urease inhibitor containing urea source with their surface treated with a suitable basic component may provide 14-1000, 28-1000, 60-1000, or 90-1000 days of NBPT half-life under accelerated NBPT stability lab test condition from the time when the particulate acidic fertilizer and the particulate urease inhibitor containing urea source are blended.
  • a particulate acidic fertilizer or a particulate urease inhibitor containing urea source with their surface treated with a suitable basic component may provide 14-500, 28-500, 60-500, or 90- 500 days of NBPT half-life under accelerated NBPT stability lab test condition from the time when the particulate acidic fertilizer and the particulate urease inhibitor containing urea source are blended.
  • a particulate acidic fertilizer or a particulate urease inhibitor containing urea source with their surface treated with a suitable basic component may provide 14-250, 28-250, 60-250, or 90-250 days of NBPT half-life under accelerated NBPT stability lab test condition from the time when the particulate acidic fertilizer and the particulate urease inhibitor containing urea source are blended.
  • a particulate acidic fertilizer or a particulate urease inhibitor containing urea source with their surface treated with a suitable basic component may provide 25% to 1000%, 50% to 1000%, 75% to 1000%, or 100%-1000% improvement of the NBPT half-life storage time compared to a particulate acidic fertilizer or a particulate urease inhibitor containing urea source that is not treated with a basic material.
  • the testing method used in the present disclosure is an accelerated NBPT stability lab testing method comparing to the standard real world storage condition.
  • the exact impact of the accelerated NBPT stability lab testing method to each example is not yet predictable. However, the impact may be very significant in certain blends.
  • NBPT has 12-18 months of half-life when ammonium sulfate is blended with ATU (AGROTAIN® stabilizer Treated Urea. AGROTAIN® stabilizer contains NBPT as its active ingredient) and stored under normal industrial storage condition.
  • ATU AGROTAIN® stabilizer Treated Urea.
  • AGROTAIN® stabilizer contains NBPT as its active ingredient
  • the NBPT half-life storage time results for the exemplified examples in the present disclosure may be obtained by the accelerated lab testing method wherein the blended particulate fertilizers are kept in a small sealed container with frequent opening and closing for sample collection and analysis.
  • the NBPT half-life storage time results for the exemplified examples in the present disclosure may also be obtained under standard real world storage conditions or normal industrial storage conditions in which the container/bag for the mixture is not repeatedly opened and closed as performed in the accelerated NBPT stability lab test.
  • Those skilled in the art will appreciate that different acidic fertilizers may have very different acidity. The stronger the acidity, the shorter the NBPT half-life storage may be observed.
  • the weight percentage range of the urease inhibitor in a particulate urease inhibitor containing urea source is 0.01% to 5 % by weight. In one aspect, the range is 0.02% to 1.0 % by weight. In another aspect, the range is 0.04% to 0.5 % by weight.
  • the urease inhibitor in the present disclosure is NBPT.
  • the weight percentage range of NBPT in the particulate NBPT containing urea source is 0.01% to 5 % by weight. In one aspect, the weight percentage range is 0.02% to 1.0 % by weight. In another aspect, the weight percentage range is 0.04% to 0.5 % by weight.
  • the weight percentage range of a basic component in a basic component treated particulate urease inhibitor containing urea source or a basic component treated particulate acidic fertilizer composition is 0.001% to 20 % by weight of the total weight of the basic component treated particulate urease inhibitor containing urea source or the basic component treated particulate acidic fertilizer. In one aspect, the weight percentage range is 0.1% to 5 % by weight. In one aspect, the weight percentage range is 0.2% to 2 % by weight. In another aspect, the weight percentage range is 0.25% to 1 % by weight.
  • the basic component in the present disclosure is MgO, Mg(OH) 2 , CaO, Ca(OH) 2 , A1 2 0 3 , Al(OH) 3 , or lime.
  • the weight percentage range of the basic component in a basic component treated particulate acidic fertilizer composition or in a basic component treated particulate urease inhibitor containing urea source is 0.001% to 20 % by weight and the weight percentage range of the particulate acidic fertilizer or the particulate urease inhibitor containing urea source is 99.999 % to 80 % by weight. In one aspect, the weight percentage range of the basic component is 0.1% to 5 % by weight and the weight percentage range of the particulate acidic fertilizer or the particulate urease inhibitor containing urea source is 99.9 % to 95 % by weight.
  • the weight percentage range of the basic component is 0.2% to 2 % by weight and the weight percentage range of the particulate acidic fertilizer or the particulate urease inhibitor containing urea source is 99.8 % to 98 % by weight. In another aspect, the weight percentage range of the basic component is 0.25% to 1 % by weight and the weight percentage of the particulate acidic fertilizer or the particulate urease inhibitor containing urea source is 99.75 % to 99 % by weight.
  • the present disclosure provides a particulate fertilizer composition
  • a particulate fertilizer composition comprising a basic component and a particulate acidic fertilizer having a surface, wherein the surface of the particulate acidic fertilizer is treated with the basic component, wherein the basic component is MgO and the acidic fertilizer is selected from the group consisting of MAP, DAP, ammonium sulfate, NPSZ, MESZ, and any combination thereof, wherein the weight percentage range of MgO is 0.001% to 20 % by weight and the weight percentage range of MAP, DAP, ammonium sulfate, NPSZ, MESZ, or any combination thereof is 80% to 99.999 % by weight.
  • the weight percentage range of MgO is 0.1 % to 5 % by weight and the weight percentage range of MAP, DAP, ammonium sulfate, NPSZ, MESZ, or any combination thereof is 99.9 % to 95 % by weight. In one aspect, the weight percentage range of MgO is 0.2 % to 2 % by weight and the weight percentage range of MAP, DAP, ammonium sulfate, NPSZ, MESZ, or any combination thereof 99.8 % to 98 % by weight.
  • the weight percentage range of MgO is 0.25 % to 1 % by weight and the weight percentage range of MAP, DAP, ammonium sulfate, NPSZ, MESZ, or any combination thereof is 99.75 % to 99 % by weight.
  • the present disclosure provides a particulate fertilizer composition
  • a particulate fertilizer composition comprising MgO and a particulate NBPT containing urea source having a surface, wherein the surface of the particulate NBPT containing urea source is treated with MgO, wherein the weight percentage range of MgO is 0.001% to 20 % by weight and the weight percentage range of the particulate NBPT containing urea source is 80% to 99.999 % by weight.
  • the weight percentage range of MgO is 0.1 % to 5 % by weight and the weight percentage range of the particulate NBPT containing urea source is 99.9 % to 95 % by weight.
  • the weight percentage range of MgO is 0.2 % to 2 % by weight and the weight percentage range of the particulate NBPT containing urea source is 99.8 % to 98 % by weight. In one aspect, the weight percentage range of MgO is 0.25 % to 1 % by weight and the weight percentage range of the particulate NBPT containing urea source is 99.75 % to 99 % by weight.
  • the diameter range of the particulate acid fertilizer particles or the particulate urease inhibitor containing urea source particles is 0.1 mm to 10 mm. In one aspect, the diameter range is 0.2 to 7.5 mm. In another aspect, the diameter range is 0.5 mm to 5 mm.
  • the diameter of basic component particles may be suitable in a very wide range as far as basic component particles can adhere to the surface of either the particulate acid fertilizer or the particulate urease inhibitor containing urea source.
  • a suitable basic component such as MgO may be as small as a
  • nanopowder which may have less than 50 nm diameter.
  • the present disclosure provides a method of making a basic component treated particulate acidic fertilizer compositions comprising providing a particulate acidic fertilizer having a surface; and contacting the basic component with the surface of the particulate acidic fertilizer.
  • the present disclosure also provides a method of making a basic component treated particulate urease inhibitor containing urea source compositions comprising providing a particulate urease inhibitor containing urea source having a surface; and contacting a basic component with the surface of the particulate urease inhibitor containing urea source.
  • the present disclosure also provides a method of making an acid resistant fertilizer composition
  • an acid resistant fertilizer composition comprising i) a particulate acidic fertilizer having a surface; ii) a particulate urease inhibitor containing urea source having a surface; and iii) a basic component, said method comprising contacting the basic component with the surface of i) and blending the basic component treated i) with ii); or contacting the basic component with the surface of ii) and blending the basic component treated ii) with i); or contacting the basic component with the surface of i) and the surface of ii) independently, and blending the basic component treated i) with the basic component treated ii).
  • the weight percentage range of a particulate urease inhibitor containing urea source is 1% to 99% of the total weight of the blend of the particulate urease inhibitor containing urea source and a particulate acidic fertilizer. In one aspect, the weight percentage range of the particulate urease inhibitor containing urea source is 20% to 80%. In one aspect, the weight percentage range of the particulate urease inhibitor containing urea source is 30% to 70%. In one aspect, the weight percentage range of the particulate urease inhibitor containing urea source is 40% to 60%. In another aspect, the weight percentage of the particulate urease inhibitor containing urea source range is 45% to 55%.
  • the weight percentage range of a particulate acidic fertilizer is 99% to 1% of the total weight of the blend of the particulate acidic fertilizer and a urease inhibitor containing urea source. In one aspect, the weight percentage range of the particulate acidic fertilizer is 80% to 20%. In one aspect, the weight percentage range of the particulate acidic fertilizer is 70% to 30%. In one aspect, the weight percentage range of the particulate acidic fertilizer is 60% to 40%. In another aspect, the weight percentage range of the particulate acidic fertilizer is 55% to 45%.
  • an inert fluorescent tracer may be applied after the treatment of a suitable basic component of the present disclosure.
  • An even distribution of the suitable basic component may be indicated when a UV black light is shined on the treated urea.
  • An inert fluorescent tracer may be but are not limited to 1,5-naphthalenedisulfonic acid disodium salt (1,5-NDSA), 2-amino-l-naphthalenesulfonic acid, 5-amino-2-naphthalenesulfonic acid, 4-amino-3-hydroxyl-l-naphthalenesulfonic acid, 6-amino-4-hydroxyl-2- naphthalenesulfonic acid, 7-amino-l,3-naphthalenedisulfonic acid, potassium salt, 4-amino-5- hydroxy-2,7-naphthalenedisulfonic acid, 5-dimethylamino-l-naphthalenesulfonic acid, 2,6- naphthalenedicarboxylic acid, dipotassium salt, 2-anthracenesulfonic acid, sodium salt, quinoline (CAS Registry No.
  • the present disclosure provides that the base treated acidic fertilizer has acceptable spreader test result according to European Standard EN13739-2 for solid fertilizer distributors. In one aspect, the base treated acidic fertilizer provides a coefficient of variation value of less than 15%.
  • the base treated acidic fertilizer provides a coefficient of variation value of less than 15%.
  • the base treated acidic fertilizer is MgO treated MAP, DAP, or a combination thereof.
  • the weight percentage of MgO in the MgO treated MAP or DAP is 0.1 to -2%. In one aspect, the weight percentage of MgO in the MgO treated MAP or DAP is 0.2 to - 1.5%.
  • Examples 1-43 are prepared for the NBPT stability testing.
  • Examples 44-90 are under "accelerated NBPT stability lab test” conditions.
  • magnesium oxide (MgO) powder to 75 g of diammonium phosphate
  • the lid is securely fastened and the jar is shaken until the powder is evenly distributed over DAP particles.
  • the MgO weight percentage of the MgO treated DAP is about 0.5% of the total weight.
  • Magnesium Oxide and Wax Treated Diammonium Phosphate Add 2000 g of DAP to a rotating drum coater and heat to 65 °C. At 65 °C, add 10 g of MgO to the rotating drum coater. After about 1 minute, add 3.3 g of AlphaPlus® C 26-28 wax and all components are mixed for 10 minutes then cooled down to room temperature.
  • the MgO weight percentage of the MgO and wax treated DAP is about 0.5% of the total weight.
  • the wax weight percentage is about 0.16%.
  • the calcium stearate weight percentage of the calcium stearate treated ATU is about 0.5% of the total weight. (In all examples, the NBPT concentration in the parenthesis for an ATU composition is the original NBPT concentration prior to the blend of a DAP composition and an ATU composition).
  • Example 34 in Table 3 is made essentially the same as Example 33.
  • MgO Treated AGROTAIN Stabilizer Treated Urea (ATU) Add 2000 g of AGROTAIN stabilizer treated urea (540 ppm NBPT) to a rotating drum coater and heat to 65 °C. At 65 °C, 10 g of MgO is added. After about 1 minute, 3.3 g of Alpha Plus C26-28 wax is added and all components are mixed for 10 minutes then cooled down to room temperature.
  • the MgO weight percentage of the MgO and wax treated ATU is about 0.5% of the total weight. The wax weight percentage is about 0.16%.
  • Example 36-43 in Table 4 are made essentially the same as Example 35.
  • the purpose of the NBPT stability test is to determine if certain basic component can provide NBPT an extended storage life after ATU is blended with a particulate acidic fertilizer, when at least one of ATU or the particulate acidic fertilizer is treated with the basic component.
  • One or more layers of variety of wax may be optionally applied.
  • the half-life of NBPT is used to show the performance of the NBPT stability. If the NBPT content is still above half of the original content on the day that the data is collected, the actual NBPT content and the days from the time that the blend is prepared is recorded. For example, if the NBPT content is 65% on day 50 from the blend of ATU and the particulate acidic fertilizer, the "65% at day 50" is used to show the performance.
  • an 8 oz. container (about 240 mL) may be used. If the ATU sample and the particulate acidic fertilizer sample are 150 g each, a 16 oz. container (about 240 mL) is used. The container is opened at regular intervals of 1 week, 2 weeks, 1 month, 2 months, 3 months, 6 months, 9 months, 12 months, or other time points as needed. The duration between each opening and closing is about 1-2 minutes. In real world situation, the "container" may be 600 kg or 1000 kg bulk bags with under plastic liner that is securely sealed until use.
  • the oxygen and moisture may have significant impact compared to the real world storage conditions.
  • the NBPT stability test in the present disclosure accelerates when is compared to the real world storage conditions. For example, when ammonium sulfate from UK blended with ATU and stored under the real world storage condition, the NBPT has 12-18 months half-life. When the exact same ammonium sulfate and ATU are blended under the NBPT stability testing conditions in a small container with frequent opening and closing, the NBPT half-life storage time is about 38 days. For this reason, the NBPT stability test in the present disclosure may be also referred as "accelerated NBPT stability lab test".
  • NBPT content of an ATU sample
  • about ten grams of the blend are removed from the container on the day of testing.
  • the green granules (ATU sample) are separated from the particulate acidic fertilizer.
  • the green granules (ATU sample) are then submitted for HPLC analysis for NBPT content (recorded as ppm of NBPT converted to % of the original NBPT).
  • HPLC testing is run using a standard C 18 column and 75 % water/ 25 % acetonitrile solution. The UV absorbance is measured at 214 nm.
  • Example 44-90 are tested based on the foregoing described method.
  • Fertilizer Composition of ATU and MgO Treated DAP, and NBPT Stability Performance Add Example 1 to a glass jar containing AGROTAIN stabilizer treated urea (ATU) (660 ppm NBPT, the original NBPT concentration prior to the blend with DAP) in 50:50 by weight ratio (75 g for each component). The lid is securely fastened and the blend is shaken in the jar until homogenous. The half-life storage time of NBPT is 140 days.
  • Examples 45- 75 in Table 5 are made essentially the same as Example 44.
  • Example 33 (470 ppm NBPT) to untreated DAP with 1: 1 ratio (75g: 75g). Securely fasten the lid and shake the blended mixture until visually homogenous.
  • the half-life storage time of NBPT is 94 days.
  • Examples 77- 90 in Table 6 are made essentially the same as Example 76.
  • ATU sample not blended with an acidic fertilizer provides the longest NBPT half-life storage time.
  • the half-life storage time significantly dropped.
  • the NBPT half-life dropped by about 96% from 214 days to 9 days when ATU sample is blended with MAP.
  • MAP is treated with a suitable basic component such as MgO in Example 56, the NBPT stability is significantly improved to 60% NBPT at day 91.
  • Same acidic fertilizer from different sources may provide very different NBPT half-life storage time.
  • ammonium sulfate from United Kingdom (UK) provides more than 100% longer NBPT half-life storage time (38 days) comparing with ammonium sulfate from Honeywell in the United States (18 days).
  • NBPT half-life time of NBPT
  • the basic component is not suitable for the treatment of the particulate fertilizers.
  • calcium stearate treated DAP in Example 50 only provides a NBPT half-life time of 12 days, conversely, the calcium stearate treated ATU in Example 77 provides an NBPT half-life time of 28 days.
  • the NBPT half-life time for KOH treated ATU in Example 85 is zero (decomposes more than one half on the first day), the NBPT half-life time for KOH treated DAP in Example 69 is 22 days.
  • Examples 91-98 are prepared for the NBPT stability testing.
  • Examples 99-106 are for examples stored under normal industrial storage condition, instead of under the "accelerated NBPT stability lab test" conditions.
  • DAP diammonium phosphate
  • MgO magnesium oxide
  • Examples 92-94 in Table 8 are made essentially the same as Example 91.
  • DAP diammonium phosphate
  • MgO magnesium oxide
  • Examples 96-98 in Table 9 are made essentially the same as Example 95.
  • NBPT stability test under normal industrial storage condition
  • the purpose of the NBPT stability test is to determine if certain basic component can provide NBPT an extended storage life after ATU is blended with a particulate acidic fertilizer, when at least one of ATU or the particulate acidic fertilizer is treated with the basic component.
  • One or more layers of variety of wax may be optionally applied.
  • the half-life of NBPT is used to show the performance of the NBPT stability. If the NBPT content is still above half of the original content on the day that the data is collected, the actual NBPT content and the days from the time that the blend is prepared is recorded. For example, if the NBPT content is 65% on day 50 from the blend of ATU and the particulate acidic fertilizer, the "65% at day 50" is used to show the performance.
  • Example 91 to a rotating vertical auger blender containing AGROTAIN stabilizer treated urea (ATU) (640 ppm NBPT, the original NBPT concentration prior to the blend with DAP) in 50:50 by weight ratio (3000 kg for each component). The components are blended for approximately 6 minutes at ambient temperature before being bagged off.
  • ATU AGROTAIN stabilizer treated urea
  • Examples 100- 106 in Table 10 are prepared and tested essentially the same as Example
  • the above values are based on analysis of the ATU samples and does not take into account NBPT transfer onto DAP.
  • the NBPT concentration in Examples 99-106 remains at least 70% of the original NBPT concentration at day 315 when the weight percentage of MgO in MgO treated DAP is 0.55% or higher.
  • the weight percentage of MgO in MgO treated DAP is 0.275% such as in Examples 99 and 103, the NBPT concentration are still more than 50% of the original NBPT concentration on day 217.
  • MgO treated DAP Examples 99-106 provided surprisingly high and extended NBPT stability at normal industrial storage condition.
  • the purpose of the spreader test is to evaluate if the MgO treated DAP fertilizer disclosed in the present disclosure may have significant variation comparing to the DAP that is not treated with MgO.
  • the value of coefficient of variation (CV) is used evaluate the variation. If the CV is more than 20%, it is unacceptable. The CV value between 15%-20% is considered poor performance. The CV value between 10%-15% is considered good performance. The CV value below 10% is considered excellent performance.
  • Production scale samples prepared according to the method for Example 98 are used for the spreader test.
  • Spreaders are checked for correct working condition.
  • Fertilizer is analyzed by Vicon grader box with compartments sized 0 to 2, 2 to 3.3, 3.3 to 4.75 and 4.75+ mm.
  • Bogballe strength tester is measured in kg of force to crush a granule/prill.
  • One liter measuring cylinder with digital scales are used for bulk density in kg/L. Collection trays 50cm by 50cm are spaced at one meter intervals across the spread width.
  • Fertilizer is transferred into tubes for visual assessment of the pattern.
  • the Maker/Model of the spreader is Amazone ZA-M.
  • the disc/vane type is OM 24-36.
  • the spreader width is 24 meter.
  • the spreader height is 80 cm from side of disc.
  • the tilt is zero degree.
  • the PTO/Disc speed is 540 rpm.
  • the application rate is 200 kg/Ha.
  • the forward speed is 10 km/h.
  • the MgO treated DAP disclosed in the present disclosure provides excellent spreader test result compared to the untreated DAP fertilizer.
  • the present invention provides an economic and acid resistant urease inhibitor containing fertilizer compositions that may provide multiple nutrients such as nitrogen, phosphate and sulfate to soil and/or plants.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Soil Sciences (AREA)
  • Fertilizers (AREA)

Abstract

La présente invention concerne de nouvelles compositions fertilisantes résistant aux acides qui comprennent une source d'urée contenant un inhibiteur d'uréase particulaire, un engrais acide particulaire, et un composant basique. Le composant basique est utilisé pour traiter la surface de la source d'urée contenant un inhibiteur d'uréase particulaire ou l'engrais acide particulaire, ou les deux indépendamment, pour prolonger la durée de stockage de l'inhibiteur d'uréase lorsque la source d'urée contenant un inhibiteur d'uréase particulaire est mélangée et stockée avec l'engrais acide particulaire. L'invention concerne également des procédés de fabrication et d'utilisation desdites compositions.
PCT/US2016/065721 2015-12-11 2016-12-09 Compositions fertilisantes contenant un inhibiteur d'uréase résistant aux acides WO2017100507A1 (fr)

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US10640430B2 (en) 2014-01-31 2020-05-05 Saudi Basic Industries Corporation Fertilizer capsule comprising one or more cores and method of making same
US10689306B2 (en) 2015-07-20 2020-06-23 Sabic Global Technologies B.V. Fertilizer composition and methods of making and using same
US10865159B2 (en) 2015-11-16 2020-12-15 Sabic Global Technologies B.V. Methods of manufacture for coated granular fertilizers
EP3822242A1 (fr) * 2019-11-15 2021-05-19 Yara International ASA Composition de mélange améliorée à base d'urée et son procédé de fabrication
US11021409B2 (en) 2017-08-09 2021-06-01 Sabic Global Technologies B.V. Extruded fertilizer granules with urease and/or nitrification inhibitors
US11104618B2 (en) 2015-07-20 2021-08-31 Sabic Global Technologies B.V. Fertilizer composition and methods of making and using same
WO2021171221A1 (fr) 2020-02-28 2021-09-02 Sabic Global Technologies B.V. Mélanges d'engrais contenant de l'urée stabilisée
US11124463B2 (en) 2015-11-16 2021-09-21 Sabic Global Technologies B.V. Coated granular fertilizers, methods of manufacture thereof, and uses thereof
US11306037B2 (en) 2017-04-19 2022-04-19 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with urease inhibitor and nitrification separated within the same particle
US11345645B2 (en) 2017-04-20 2022-05-31 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with embedded powder composition
US11358908B2 (en) 2017-04-19 2022-06-14 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with urease inhibitor and nitrification inhibitor in separate particles
US11401218B2 (en) 2014-05-05 2022-08-02 Sabic Global Technologies B.V. Coated granular fertilizers, methods of manufacture thereof, and uses
EP4067324A1 (fr) 2021-03-31 2022-10-05 SKW STICKSTOFFWERKE PIESTERITZ GmbH Engrais granulé au sulfate d'urée et d'ammonium au ph neutre comportant un inhibiteur d'urées
WO2022252173A1 (fr) * 2021-06-03 2022-12-08 Rhodia Operations Composition d'engrais à base de mélange d'urée et son procédé de préparation
US11806689B2 (en) 2016-02-08 2023-11-07 Sabic Global Technologies B.V. Method of making a fertilizer seed core
US11866383B1 (en) 2018-04-04 2024-01-09 Synsus Private Label Partners, Llc Nitrification inhibiting compositions and their use in agricultural applications

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Publication number Priority date Publication date Assignee Title
US10640430B2 (en) 2014-01-31 2020-05-05 Saudi Basic Industries Corporation Fertilizer capsule comprising one or more cores and method of making same
US11401218B2 (en) 2014-05-05 2022-08-02 Sabic Global Technologies B.V. Coated granular fertilizers, methods of manufacture thereof, and uses
US10689306B2 (en) 2015-07-20 2020-06-23 Sabic Global Technologies B.V. Fertilizer composition and methods of making and using same
US11104618B2 (en) 2015-07-20 2021-08-31 Sabic Global Technologies B.V. Fertilizer composition and methods of making and using same
US10865159B2 (en) 2015-11-16 2020-12-15 Sabic Global Technologies B.V. Methods of manufacture for coated granular fertilizers
US11124463B2 (en) 2015-11-16 2021-09-21 Sabic Global Technologies B.V. Coated granular fertilizers, methods of manufacture thereof, and uses thereof
US11806689B2 (en) 2016-02-08 2023-11-07 Sabic Global Technologies B.V. Method of making a fertilizer seed core
US12006273B2 (en) 2017-04-19 2024-06-11 SABIC Agri-Nutrients Company Enhanced efficiency fertilizer with urease inhibitor and nitrification inhibitor in separate particles
US11802097B2 (en) 2017-04-19 2023-10-31 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with urease inhibitor and nitrification separated within the same particle
US11306037B2 (en) 2017-04-19 2022-04-19 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with urease inhibitor and nitrification separated within the same particle
US11358908B2 (en) 2017-04-19 2022-06-14 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with urease inhibitor and nitrification inhibitor in separate particles
US11345645B2 (en) 2017-04-20 2022-05-31 Sabic Global Technologies B.V. Enhanced efficiency fertilizer with embedded powder composition
US11021409B2 (en) 2017-08-09 2021-06-01 Sabic Global Technologies B.V. Extruded fertilizer granules with urease and/or nitrification inhibitors
US11866383B1 (en) 2018-04-04 2024-01-09 Synsus Private Label Partners, Llc Nitrification inhibiting compositions and their use in agricultural applications
WO2021094512A1 (fr) * 2019-11-15 2021-05-20 Yara International Asa Composition de mélange à base d'urée améliorée et son procédé de fabrication
EP3822242A1 (fr) * 2019-11-15 2021-05-19 Yara International ASA Composition de mélange améliorée à base d'urée et son procédé de fabrication
WO2021171221A1 (fr) 2020-02-28 2021-09-02 Sabic Global Technologies B.V. Mélanges d'engrais contenant de l'urée stabilisée
EP4067324A1 (fr) 2021-03-31 2022-10-05 SKW STICKSTOFFWERKE PIESTERITZ GmbH Engrais granulé au sulfate d'urée et d'ammonium au ph neutre comportant un inhibiteur d'urées
DE102021108187A1 (de) 2021-03-31 2022-10-06 Skw Stickstoffwerke Piesteritz Gmbh Granuliertes pH-neutrales Harnstoff-Ammoniumsulfat-Düngemittel mit Ureaseinhibitor
WO2022252173A1 (fr) * 2021-06-03 2022-12-08 Rhodia Operations Composition d'engrais à base de mélange d'urée et son procédé de préparation

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