WO2022252173A1 - Urea blend fertilizer composition and the process for preparing the same - Google Patents

Urea blend fertilizer composition and the process for preparing the same Download PDF

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Publication number
WO2022252173A1
WO2022252173A1 PCT/CN2021/098086 CN2021098086W WO2022252173A1 WO 2022252173 A1 WO2022252173 A1 WO 2022252173A1 CN 2021098086 W CN2021098086 W CN 2021098086W WO 2022252173 A1 WO2022252173 A1 WO 2022252173A1
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Prior art keywords
urea
fertilizer composition
preparing
composition according
phosphate
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PCT/CN2021/098086
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French (fr)
Inventor
Ritu Ahuja
Zixian CHEN
Xiaobing Xi
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Rhodia Operations
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Priority to PCT/CN2021/098086 priority Critical patent/WO2022252173A1/en
Publication of WO2022252173A1 publication Critical patent/WO2022252173A1/en

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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
    • 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
    • C05G3/50—Surfactants; Emulsifiers
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

Definitions

  • the present invention relates to a process of preparing a urea blend fertilizer composition, comprising the steps of treating the urea granule coated with NBPT with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid.
  • the present invention further provide a bulk blending fertilizer composition comprising the urea blend fertilizer composition.
  • Urea is the most common nitrogen-containing fertilizer. Urea has the highest nitrogen content of all nitrogen-containing fertilizers in common use (46%) . Its consumption worldwide has been considerably increased, from about 20 million tons in the early seventies to about 100 million tons at the beginning of the twenty first century. Nitrogen is a basic element for any living system as a constituent of protein.
  • Urea is first hydrolyzed in the soil under the action of an enzyme, commonly called urease, to produce ammonia and carbon dioxide.
  • Ureases are found in numerous bacteria, fungi, algae, plants and some invertebrates, as well as in soils, as a soil enzyme.
  • Urea hydrolysis tends to increase the pH of its environment as the ammonia is dissolved into the water in the soil, and part of the ammonia can also be released into the atmosphere, a process called ammonia volatilization, thus becoming unavailable for the plant. About 50 weight%of nitrogen can sometimes be lost as a result of the volatilization of ammonia, all depending on the soil type, water content, pH, climate conditions, etc.
  • Urease inhibitors are compounds that are capable of temporarily reducing the activity of the enzyme and slow down the rate at which urea is hydrolyzed, avoiding peaks of ammonia concentration and therefore limiting the losses to the air.
  • N- (n-butyl) thiophosphoric triamide which will be referred to herein as NBPT.
  • This compound is actually the precursor for the active compound N- (n-butyl) phosphoric triamide (NBPT) , obtained through oxidation of the thio-compound, but it is the thio-compound that is commonly produced, sold and used.
  • phosphoric triamide compounds When combined with a urea-containing fertilizer, phosphoric triamide compounds reduce the rate at which urea is hydrolysed to ammonia in the soil.
  • the benefits that are realized as a result of the delayed urea hydrolysis include the following: (1) nutrient nitrogen is available to the plant over a longer period of time, (2) excessive build-up of ammonia in the soil following the application of the urea-containing fertilizer is avoided, (3) the potential for nitrogen loss through ammonia volatilization is reduced, (4) the potential for damage by high levels of ammonia to seedlings and young plants is reduced, (5) plant uptake of nitrogen is increased, and (6) an increase in crop yields is attained. While phosphoric triamide compounds do not directly influence the rate of ammonium nitrification, they do control the levels of ammonium which are subject to the nitrification process and thereby indirectly controls the levels of nitrate nitrogen in the soil.
  • the urease inhibitor of the type phosphoric triamide either applied as a liquid or as a solid, either applied on the urea granule or mixed in the urea granule is not stable over a prolonged period of time when in contact with urea blend fertilizer, despite the fact that a urease inhibitor of the type phosphoric triamide is generally disclosed for use with said urea blend fertilizers.
  • the urease inhibitor of the type phosphoric triamide is sensitive to acid, its decomposition process will speed up when mixed with some acidic fertilizers like ammonium sulfate.
  • US 2010/0206031 A1 (Whitehurst) describes a composition consisting of NBPT in a basic organic amine alcohol solvent, coated onto a blend of urea-particles and mono ammonium phosphate particles.
  • WO2017100507A1 (Koch) disclosed a method of treating urea particulate and NBPT with basic component, calcium oxide, zinc oxide, magnesium oxide, calcium carbonate and the like, wherein the basic component is incorporated into the mixture either by powder mixing or coating by means of wax.
  • urea granule treated with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid;
  • step ii) and iii) is proceeded simultaneously or successively.
  • the urease inhibitor of the type phosphoric triamide is a compound of formula:
  • X is oxygen or sulfur
  • R 1 is alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
  • R 2 is hydrogen, alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
  • R 3 , R 4 , R 5 and R 6 are independently hydrogen or alkyl having 1 to 6 carbon atoms.
  • the urease inhibitor is N- (n-butyl) thiophosphoric triamide (NBPT) .
  • the urea granule presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the urea blend fertilizer composition.
  • the basic component is selected from magnesium or calcium salt of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid.
  • the basic component is selected from magnesium stearate or calcium stearate or the mixture thereof.
  • a bulk blending fertilizer composition comprising:
  • the is acidic fertilizer selected from the group consisting of monoammonium phosphate (MAP) , diammonium phosphate (DAP) , ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, and the combination thereof.
  • MAP monoammonium phosphate
  • DAP diammonium phosphate
  • ammonium nitrate ammonium sulfate
  • ammonium hydrogensulfate rock phosphate
  • super phosphate super phosphate
  • serpentine super phosphate reactive phosphate rock
  • the urea blend fertilizer presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the bulk blending fertilizer composition.
  • any particular upper concentration, weight ratio or amount can be associated with any particular lower concentration, weight ratio or amount, respectively.
  • alkyl means a saturated hydrocarbon radical, which may be straight, branched or cyclic, such as, methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl, t-butyl, pentyl, n-hexyl, cyclohexyl.
  • urea granule treated with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid;
  • step ii) and iii) is proceeded simultaneously or successively.
  • the urea blend fertilizer composition refers to the fertilizer comprising solid urea as nitrogen source in an amount of ranging from 10 wt. %to 99 wt. %, based on the total weight of the urea blend fertilizer composition.
  • the urea granule is intended to cover all the solid form of urea, including but not limited to pellets, prills, pastilles, flakes, granules, or a combination thereof.
  • the urea fertilizer is in the form of granule.
  • urease inhibitors of the type phosphoric triamide when referring to urease inhibitors of the type phosphoric triamide, it is understood that this comprises all active compounds, active precursors and active conversion products, resulting from said phosphoric triamides.
  • the urease inhibitor is a compound of formula:
  • X is oxygen or sulfur
  • R 1 is alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
  • R 2 is hydrogen, alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
  • R 3 , R 4 , R 5 and R 6 are independently hydrogen or alkyl having 1 to 6 carbon atoms.
  • the urease inhibitor is N- (n-butyl) thiophosphoric triamide (NBPT) .
  • an aqueous solution or dispersion of a basic component is used to treat the urea granule which is coated with a urease inhibitor.
  • the basic component used in the present invention is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid.
  • the basic component is selected from magnesium or calcium salt of C 8 to C 50 fatty acid, preferably selected from magnesium or calcium salt of C 8 to C 32 fatty acid.
  • the basic component is selected from magnesium stearate or calcium stearate or the mixture thereof.
  • the step ii) that is to say coating at least part of the surface of the urea granule, is proceeded by mixing a urease inhibitor such as NBPT with urea granules.
  • a urease inhibitor such as NBPT
  • 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 urea melt to form an NBPT incorporated urea fertilizer (see WO 2015/027244) .
  • a highly concentrated dry formulation of NBPT 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) .
  • the urea granule was coated with a urease inhibitor solution.
  • the content of the urease inhibitor is in the range of 0.01 to 10 wt. %, preferably 0.01 to 5 wt. %, more preferably 0.01 to 2 wt. %, based on the total weight of the urease inhibitor solution.
  • the step iii) that is to say treating the urea granule with an aqueous solution or dispersion of a basic component, can be done by applying the dispersion onto the surface of the urea granules.
  • step ii) and iii) is proceeded simultaneously or successively.
  • the urease inhibitor is applied onto the surface of the urea granule at the same time of treating the urea granule with an aqueous solution or dispersion of a basic component.
  • the urease inhibitor and the aqueous dispersion can be premixed or added separately onto the surface of the urea granule.
  • the urea granule is coated with the urease inhibitor first and then the obtained granule is further treated with the aqueous dispersion or solution.t is surprisingly found that the stability of the urease inhibitor are not impaired by treating with the aqueous solution or dispersion of a basic component, which is on the contrary to the expectation of a person skilled in the art that water may result the decomposition of the urease inhibitors.
  • urea blend fertilizer composition prepared by the process as illustrated above.
  • the urea blend fertilizer composition has favorable urease inhibitor stability, even when mixing with other acidic fertilizers.
  • a bulk blending fertilizer composition comprising:
  • the acidic fertilizer may be any acidic fertilizer or a fertilizer composition comprising an acidic component.
  • the acidic fertilizer may provide a pH value lower than 7 when it is dissolved or partially dissolved in water.
  • An acidic fertilizer in the present invention may include any material that comprises any form of nitrate, phosphate or sulfate.
  • the acidic fertilizer which can be used is selected from monoammonium phosphate (MAP) , diammonium phosphate (DAP) , ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, and the combination thereof.
  • the acidic fertilizer is selected from ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, dihydrogen ammonium phosphate.
  • the urea blend fertilizer (a) presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the bulk blending fertilizer composition.
  • the NBPT solution (1.6L/ton) was added to urea granules in a rotary drum with the help of a syringe and was allowed to coat homogeneously in the rotary drum.
  • the aqueous dispersion of calcium stearate (4-6kg/ton) was added to NBPT coated urea granules in a rotary drum with the help of a syringe and was allowed to coat homogeneously in the rotary drum.
  • the NBPT solution and aqueous dispersion can be added simultaneously, the urea blend obtained as such is referred as one step coating.
  • the NBPT solution and aqueous dispersion can be added at a gap of 1-15 seconds between the two coatings
  • the urea blend fertilizer was obtained as such is referred as two steps coating.
  • the bulk blending fertilizer composition was prepared by physically blending the urea blend fertilizer composition with ammonium sulfate in a glass bottle in different weight ratio.
  • HPLC Agilent 1260 Infinity II; Column: XTERRA MS C18, 5.0 ⁇ m, 4.6mm ⁇ 250mm; Temp: 30°C; Detector wavelength: 205 nm; acetonitrile: water 2: 8; Inject Volume: 5 ⁇ L; Flow: 1.0mL/min; Run time: 15min) .

Abstract

The present invention relates to a process of preparing a urea blend fertilizer composition, comprising the steps of treating the urea granule coated with NBPT and an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid. The present invention further provide a bulk blending fertilizer composition comprising the urea blend fertilizer composition.

Description

Urea blend fertilizer Composition and the Process for Preparing the Same Field of the Invention
The present invention relates to a process of preparing a urea blend fertilizer composition, comprising the steps of treating the urea granule coated with NBPT with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid. The present invention further provide a bulk blending fertilizer composition comprising the urea blend fertilizer composition.
Background of the Invention
Urea is the most common nitrogen-containing fertilizer. Urea has the highest nitrogen content of all nitrogen-containing fertilizers in common use (46%) . Its consumption worldwide has been considerably increased, from about 20 million tons in the early seventies to about 100 million tons at the beginning of the twenty first century. Nitrogen is a basic element for any living system as a constituent of protein.
Unfortunately, urea nitrogen cannot be assimilated directly by the plants and needs to be converted through hydrolysis into ammonium and nitrification into nitrate. Urea is first hydrolyzed in the soil under the action of an enzyme, commonly called urease, to produce ammonia and carbon dioxide. Ureases are found in numerous bacteria, fungi, algae, plants and some invertebrates, as well as in soils, as a soil enzyme. Urea hydrolysis tends to increase the pH of its environment as the ammonia is dissolved into the water in the soil, and part of the ammonia can also be released into the atmosphere, a process called ammonia volatilization, thus becoming unavailable for the plant. About 50 weight%of nitrogen can sometimes be lost as a result of the volatilization of ammonia, all depending on the soil type, water content, pH, climate conditions, etc.
The availability of nitrogen, originating from urea, to the root system of plants can be improved by combining a urea-containing fertilizer (i.e. by incorporation or addition) with a urease inhibitor. Urease inhibitors are compounds that are capable of temporarily reducing the activity of the  enzyme and slow down the rate at which urea is hydrolyzed, avoiding peaks of ammonia concentration and therefore limiting the losses to the air. There are many compounds that can inhibit urease, but only a few that are non-toxic, effective at low concentrations, chemically stable enough and able to be combined with urea-containing fertilizers.
Among the most effective urease inhibitors known today are the phosphoric triamide compounds, first disclosed in US 4,530,714 (Allied Corporation, 1985) . An example of an effective urease inhibitor, disclosed in said patent is N- (n-butyl) thiophosphoric triamide, which will be referred to herein as NBPT. This compound is actually the precursor for the active compound N- (n-butyl) phosphoric triamide (NBPT) , obtained through oxidation of the thio-compound, but it is the thio-compound that is commonly produced, sold and used.
When combined with a urea-containing fertilizer, phosphoric triamide compounds reduce the rate at which urea is hydrolysed to ammonia in the soil. The benefits that are realized as a result of the delayed urea hydrolysis include the following: (1) nutrient nitrogen is available to the plant over a longer period of time, (2) excessive build-up of ammonia in the soil following the application of the urea-containing fertilizer is avoided, (3) the potential for nitrogen loss through ammonia volatilization is reduced, (4) the potential for damage by high levels of ammonia to seedlings and young plants is reduced, (5) plant uptake of nitrogen is increased, and (6) an increase in crop yields is attained. While phosphoric triamide compounds do not directly influence the rate of ammonium nitrification, they do control the levels of ammonium which are subject to the nitrification process and thereby indirectly controls the levels of nitrate nitrogen in the soil.
However, the urease inhibitor of the type phosphoric triamide, either applied as a liquid or as a solid, either applied on the urea granule or mixed in the urea granule is not stable over a prolonged period of time when in contact with urea blend fertilizer, despite the fact that a urease inhibitor of the type phosphoric triamide is generally disclosed for use with said urea blend fertilizers. Moreover, the urease inhibitor of the type  phosphoric triamide is sensitive to acid, its decomposition process will speed up when mixed with some acidic fertilizers like ammonium sulfate.
Several methods has been developed to deal with this problem. For example, US 2010/0206031 A1 (Whitehurst) describes a composition consisting of NBPT in a basic organic amine alcohol solvent, coated onto a blend of urea-particles and mono ammonium phosphate particles. WO2017100507A1 (Koch) disclosed a method of treating urea particulate and NBPT with basic component, calcium oxide, zinc oxide, magnesium oxide, calcium carbonate and the like, wherein the basic component is incorporated into the mixture either by powder mixing or coating by means of wax.
Summary of the Invention
It is well known that water will result the decomposition of the urease inhibitor of the type phosphoric triamide, so moisture shall be avoided which can be seen in Koch’s patent wherein the basic component is incorporated into the fertilizer mixture without using water. However, it is surprisingly found by the inventors that the use of water did not result in significant decomposition of the urease inhibitor. Furthermore, it is easier to handle (no powder dust) with the use of an environmental friendly liquid system (use of water) .
In one aspect of the present invention, it is provided a process of preparing a urea blend fertilizer, comprising the steps of
i) obtaining a urea granule;
ii) coating at least part of the surface of the urea granule with a urease inhibitor of the type phosphoric triamide; and
iii) treating the urea granule with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid;
wherein the step ii) and iii) is proceeded simultaneously or successively.
In one embodiment of the present invention, the urease inhibitor of the type phosphoric triamide is a compound of formula:
Figure PCTCN2021098086-appb-000001
wherein
X is oxygen or sulfur;
R 1 is alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
R 2 is hydrogen, alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl; and
R 3, R 4, R 5 and R 6 are independently hydrogen or alkyl having 1 to 6 carbon atoms.
In another embodiment of the present invention, the urease inhibitor is N- (n-butyl) thiophosphoric triamide (NBPT) .
In yet another embodiment of the present invention, the urea granule presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the urea blend fertilizer composition.
In still yet another embodiment of the present invention, the basic component is selected from magnesium or calcium salt of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid.
In still yet another embodiment of the present invention, the basic component is selected from magnesium stearate or calcium stearate or the mixture thereof.
In another aspect of the present invention, it is provided a urea blend fertilizer composition prepared according to the process as illustrated above.
In further another aspect of the present invention, it is provided a bulk blending fertilizer composition comprising:
a) the urea blend fertilizer composition as illustrated above; and
b) an acidic fertilizer.
In one embodiment of the present invention, the is acidic fertilizer selected from the group consisting of monoammonium phosphate (MAP) , diammonium phosphate (DAP) , ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, and the combination thereof.
In one embodiment of the present invention, the urea blend fertilizer presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the bulk blending fertilizer composition.
Detailed description of the Invention
Throughout the description, including the claims, the term "comprising one" or “comprising a" should be understood as being synonymous with the term "comprising at least one" , unless otherwise specified. The terms "between" and “from…to…” should be understood as being inclusive of the limits.
The articles “a” , “an” and “the” are used to refer to one or to more than one (i.e., to at least one) of the grammatical object of the article.
It should be noted that in specifying any range of concentration, weight ratio or amount, any particular upper concentration, weight ratio or amount can be associated with any particular lower concentration, weight ratio or amount, respectively.
As used herein, the term "alkyl" means a saturated hydrocarbon radical, which may be straight, branched or cyclic, such as, methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl, t-butyl, pentyl, n-hexyl, cyclohexyl.
As used herein, the terminology " (Cn to Cm) " in reference to an organic group, wherein n and m are each integers, indicates that the group may contain from n carbon atoms to m carbon atoms per group.
In one aspect of the present invention, it is provided a process of preparing a urea blend fertilizer, comprising the steps of
i) obtaining a urea granule;
ii) coating at least part of the surface of the urea granule with a urease inhibitor of the type phosphoric triamide; and
iii) treating the urea granule with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid;
wherein the step ii) and iii) is proceeded simultaneously or successively.
As used herein, the urea blend fertilizer composition refers to the fertilizer comprising solid urea as nitrogen source in an amount of ranging from 10 wt. %to 99 wt. %, based on the total weight of the urea blend fertilizer composition.
In the present invention, the urea granule is intended to cover all the solid form of urea, including but not limited to pellets, prills, pastilles, flakes, granules, or a combination thereof. In one embodiment of the present invention, the urea fertilizer is in the form of granule.
In the present invention, when referring to urease inhibitors of the type phosphoric triamide, it is understood that this comprises all active compounds, active precursors and active conversion products, resulting from said phosphoric triamides.
In one embodiment of the present invention, the urease inhibitor is a compound of formula:
Figure PCTCN2021098086-appb-000002
wherein
X is oxygen or sulfur;
R 1 is alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
R 2 is hydrogen, alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl; and
R 3, R 4, R 5 and R 6 are independently hydrogen or alkyl having 1 to 6 carbon atoms.
In one embodiment of the present invention, the urease inhibitor is N- (n-butyl) thiophosphoric triamide (NBPT) .
In the present invention, an aqueous solution or dispersion of a basic component is used to treat the urea granule which is coated with a urease inhibitor. The basic component used in the present invention is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid.
In one embodiment of the present invention, the basic component is selected from magnesium or calcium salt of C 8 to C 50 fatty acid, preferably selected from magnesium or calcium salt of C 8 to C 32 fatty acid.
In one embodiment of the present invention, the basic component is selected from magnesium stearate or calcium stearate or the mixture thereof.
In the present invention, the step ii) , that is to say coating at least part of the surface of the urea granule, is proceeded by mixing a urease inhibitor such as NBPT with urea granules. For example, 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) . Other solvents such as glycerol, glycol ethers, amines, and DMSO may also be used. Alternatively, NBPT may be introduced into the urea melt to form an NBPT incorporated urea fertilizer (see WO 2015/027244) . In addition, a highly concentrated dry formulation of NBPT 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) .
In one embodiment of the present invention, the urea granule was coated with a urease inhibitor solution. The content of the urease inhibitor is in the range of 0.01 to 10 wt. %, preferably 0.01 to 5 wt. %, more preferably 0.01 to 2 wt. %, based on the total weight of the urease inhibitor solution.
In the present invention, the step iii) , that is to say treating the urea granule with an aqueous solution or dispersion of a basic component, can be done by applying the dispersion onto the surface of the urea granules.
In the present invention, step ii) and iii) is proceeded simultaneously or successively.
In case of proceeded simultaneously, the urease inhibitor is applied onto the surface of the urea granule at the same time of treating the urea granule with an aqueous solution or dispersion of a basic component. The urease inhibitor and the aqueous dispersion can be premixed or added separately onto the surface of the urea granule.
In case of proceeded successively, the urea granule is coated with the urease inhibitor first and then the obtained granule is further treated with the aqueous dispersion or solution.t is surprisingly found that the stability of the urease inhibitor are not impaired by treating with the aqueous solution or dispersion of a basic component, which is on the contrary to the expectation of a person skilled in the art that water may result the decomposition of the urease inhibitors.
In another aspect of the present invention, it is provided a urea blend fertilizer composition prepared by the process as illustrated above. The urea blend fertilizer composition has favorable urease inhibitor stability, even when mixing with other acidic fertilizers.
In further another aspect of the present invention, it is provided a bulk blending fertilizer composition comprising:
a) a urea blend fertilizer as illustrated above; and
b) an acidic fertilizer.
In any embodiment of the present invention, the acidic fertilizer may be any acidic fertilizer or a fertilizer composition comprising an acidic component. The acidic fertilizer may provide a pH value lower than 7 when it is dissolved or partially dissolved in water. An acidic fertilizer in the present invention may include any material that comprises any form of nitrate, phosphate or sulfate. The acidic fertilizer which can be used is selected from monoammonium phosphate (MAP) , diammonium phosphate (DAP) , ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, and the combination thereof.
In one embodiment of the present invention, the acidic fertilizer is selected from ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, dihydrogen ammonium phosphate.
In one embodiment of the present invention, the urea blend fertilizer (a) presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the bulk blending fertilizer composition.
Examples
1. The preparation of the urea blend fertilizer composition.
The NBPT solution (1.6L/ton) was added to urea granules in a rotary drum with the help of a syringe and was allowed to coat homogeneously in the rotary drum. The aqueous dispersion of calcium stearate (4-6kg/ton) was added to NBPT coated urea granules in a rotary drum with the help of a syringe and was allowed to coat homogeneously in the rotary drum.
The NBPT solution and aqueous dispersion can be added simultaneously, the urea blend obtained as such is referred as one step coating. The NBPT solution and aqueous dispersion can be added at a gap of 1-15 seconds between the two coatings The urea blend fertilizer was obtained as such is referred as two steps coating.
2. The bulk blending fertilizer
The bulk blending fertilizer composition was prepared by physically blending the urea blend fertilizer composition with ammonium sulfate in a glass bottle in different weight ratio.
The obtained bulk blending was then stored under 30 deg C/45%relative humidity over a period of weeks. At regular intervals, colored urea granules were separated manually and tested for residual NBPT content by HPLC analyses. (HPLC: Agilent 1260 Infinity II; Column: XTERRA MS C18, 5.0 μm, 4.6mm×250mm; Temp: 30℃; Detector wavelength: 205 nm; acetonitrile: water 2: 8; Inject Volume: 5 μL; Flow: 1.0mL/min; Run time: 15min) .
The NBPT stability assessment results were listed in table 1, wherein “CS” refers to comparative samples, “S” refers to the example of the present invention.
Table 1: NBPT stability assessment results
Figure PCTCN2021098086-appb-000003
*0.3 wt. %water was added to the NBPT coated urea granule before mixing with AMS
As shown in table 1, a minor content of water resulted obvious loss of NBPT in the fertilizer composition (CS2 and CS4) . The examples of the present invention (S1 to S4) , both one step coating and two steps coating  showed significant improvement in NBPT content compared to non-treated comparative examples (CS1 and CS3) .

Claims (10)

  1. A process of preparing a urea blend fertilizer composition, comprising the steps of
    i) obtaining a urea granule;
    ii) coating at least part of the surface of the urea granule with a urease inhibitor of the type phosphoric triamide; and
    iii) treating the urea granule with an aqueous solution or dispersion of a basic component which is selected from alkaline or alkaline earth salts of C 8 to C 50 fatty acid, preferably C 8 to C 32 fatty acid;
    wherein the step ii) and iii) is proceeded simultaneously or successively.
  2. The process of preparing a urea blend fertilizer composition according to claim 1, wherein the urease inhibitor of the type phosphoric triamide is a compound of formula:
    Figure PCTCN2021098086-appb-100001
    wherein
    X is oxygen or sulfur;
    R 1 is alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl;
    R 2 is hydrogen, alkyl, cycloalkenyl, aralkyl, aryl, alkenyl, alkynyl, or cycloalkyl; and
    R 3, R 4, R 5 and R 6 are independently hydrogen or alkyl having 1 to 6 carbon atoms.
  3. The process of preparing a urea blend fertilizer composition according to claim 2, wherein the urease inhibitor is N- (n-butyl) thiophosphoric triamide (NBPT) .
  4. The process of preparing a urea blend fertilizer composition according to any one of claims 1 to 3, wherein the urea granule presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the urea blend fertilizer composition.
  5. The process of preparing a urea blend fertilizer composition according to any one of claims 1 to 4, wherein the basic component is selected from magnesium or calcium salt of C 8 to C 50 fatty acid, preferably selected from magnesium or calcium salt of C 8 to C 32 fatty acid.
  6. The process of preparing a urea blend fertilizer composition according to claim 5, wherein the basic component is selected from magnesium stearate or calcium stearate or the mixture thereof.
  7. A urea blend fertilizer composition prepared according to the process of any one of claims 1 to 6.
  8. A bulk blending fertilizer composition comprising:
    a) the urea blend fertilizer composition according to claim 7; and
    b) an acidic fertilizer.
  9. The bulk blending fertilizer composition according to claim 8, wherein the acidic fertilizer is selected from the group consisting of monoammonium phosphate (MAP) , diammonium phosphate (DAP) , ammonium nitrate, ammonium sulfate, and ammonium hydrogensulfate, rock phosphate, super phosphate, serpentine super phosphate, reactive phosphate rock, and the combination thereof.
  10. The bulk blending fertilizer composition according to claim 8, wherein the urea blend fertilizer presents in an amount ranging from 10 wt. %to 99 wt. %, based on the total weight of the bulk blending fertilizer composition.
PCT/CN2021/098086 2021-06-03 2021-06-03 Urea blend fertilizer composition and the process for preparing the same WO2022252173A1 (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017100507A1 (en) * 2015-12-11 2017-06-15 Koch Agromonic Services, Llc Acid resistant urease inhibitor containing fertilizer compositions
CN108349827A (en) * 2015-11-12 2018-07-31 雅苒国际集团 The improved blend compositions and preparation method thereof based on urea
EP3372576A1 (en) * 2017-03-07 2018-09-12 Yara International ASA Urea-based composition and method for the manufacture thereof
US20210070669A1 (en) * 2018-05-09 2021-03-11 Yara International Asa Improved urea-based blend composition and method for the manufacture thereof
EP3821716A1 (en) * 2019-11-15 2021-05-19 Yara International ASA Urea ammonium sulphate-based composition and method for the manufacture thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108349827A (en) * 2015-11-12 2018-07-31 雅苒国际集团 The improved blend compositions and preparation method thereof based on urea
WO2017100507A1 (en) * 2015-12-11 2017-06-15 Koch Agromonic Services, Llc Acid resistant urease inhibitor containing fertilizer compositions
EP3372576A1 (en) * 2017-03-07 2018-09-12 Yara International ASA Urea-based composition and method for the manufacture thereof
US20210070669A1 (en) * 2018-05-09 2021-03-11 Yara International Asa Improved urea-based blend composition and method for the manufacture thereof
EP3821716A1 (en) * 2019-11-15 2021-05-19 Yara International ASA Urea ammonium sulphate-based composition and method for the manufacture thereof

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