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WO2024184904A1 - Concentrated liquid fertilizer including nitrogen and chelated micronutrients for foliar application and preparation process thereof - Google Patents

Concentrated liquid fertilizer including nitrogen and chelated micronutrients for foliar application and preparation process thereof Download PDF

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Publication number
WO2024184904A1
WO2024184904A1 PCT/IN2023/050676 IN2023050676W WO2024184904A1 WO 2024184904 A1 WO2024184904 A1 WO 2024184904A1 IN 2023050676 W IN2023050676 W IN 2023050676W WO 2024184904 A1 WO2024184904 A1 WO 2024184904A1
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WIPO (PCT)
Prior art keywords
source
nitrogen
weight
metal
liquid fertilizer
Prior art date
Application number
PCT/IN2023/050676
Other languages
French (fr)
Inventor
Aniruddha Dattatray Kapadnis
Harshal Tambat
Original Assignee
Aniruddha Dattatray Kapadnis
Harshal Tambat
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Publication of WO2024184904A1 publication Critical patent/WO2024184904A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00Other inorganic fertilisers
    • C05D9/02Other inorganic fertilisers containing trace elements
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G1/00Mixtures of fertilisers belonging individually to different subclasses of C05
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/50Surfactants; Emulsifiers
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/20Liquid fertilisers
    • C05G5/23Solutions

Definitions

  • the present invention relates to a clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients. More preferably, the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops. Present invention also provides a process of preparation thereof. The present invention provides a liquid fertilizer having 100% water miscibility comprising of highest concentration of Nitrogen and micronutrient chelated fertilizer composition.
  • Plant nutrients are one of the environmental factors essential for crop growth and development. Nutrient management is crucial for optimal productivity in commercial crop production. Those nutrients in concentrations of 100 parts per million (ppm) in plant tissues are described as micronutrients and include iron (Fe), zinc (Zn), manganese (Mn), copper (Cu), boron (B), chlorine (Cl), molybdenum (Mo), and nickel (Ni). Micronutrients such as Fe, Mn, Zn, and Cu are easily oxidized or precipitated in soil, and their utilization is, therefore, not efficient. Therefore, chelated fertilizers have been developed to increase micronutrient utilization efficiency.
  • Foliar application is done with spraying a mist of fine water droplets through small spray nozzles.
  • foliar applied fertilizers should soluble in water or dispersed in a such a good way that the spraying nozzles are not blocked.
  • Powder formulation are not perfectly homogeneous in the spray solution as it is being manually prepared in the field. Moreover during the spraying process the homogeneity of the solution reduces hence such solution often weakly absorbed and assimilated in plant system. Thus, from advantage point of view, Powder formulation is always behind the liquid formulation. Irrespective of the use either as foliar application or soil application.
  • the nutritional source and concentration of each nutrients per weight basis is also important to provide a easy to use formulation or having single dilution with maximum possible concentration to avoid the multiple applications.
  • the power form of chelated fertilizer need a solubilizing tank for ensuring the uniform solubility before spraying. Hence higher dosage need to apply to provide full nutrition result to higher cost of treatment by the end users.
  • liquid fertilizer typically prepared by considering the saturation solubilities of salts/chelate present in powder form and one can not achieve the solutions having concentration above said solubility, may be not more than 0.1 to 60% solid dissolved in solution. However, such less concentrations in said solutions are not effective to load the more concentrated solute due to limitation of said solubility parameter, or have limited compatibility in different pH ranges.
  • the objective of the present invention is to provide a concentrated solution of metal chelated fertilizer composition.
  • the chelated liquid fertilizer which will be having 100% water soluble form is an essential part of fertilizer composition to provide an accurate concentration of deficient metal/Mineral. Because, they form clear solutions having highest concentration of micronutrients, nitrogen and potassium and content as compare to the other known liquid fertilizer. Additionally, the said composition of liquid fertilizer is devoid of sediments or precipitates even higher concentration of nutritional constituents are present. This guarantees a high level of effectiveness and stops the nozzle becoming blocked.
  • the present invention solving the problem of powder, suspension type or less soluble foliar application micronutrient chelated fertilizer composition of said prior art disclosure by providing a novel and effective completely water soluble micronutrient chelated liquid fertilizer having maximum concentration of nutrients as well as micronutrients.
  • Another specific objective of the invention is to provide a liquid fertilizer composition in the form of nano particle sized liquid without any precipitation or agglomeration of solid concentrate/solute present therein.
  • One of the objective of the invention to provide a fertilizer composition having neutral pH as it is very safe and provides a highest availability of Metal-Nitrogen with no risk of scorching to given crop and plant so that provides a highest benefits with maximum uptake.
  • the one more objective of the present invention it to provide liquid fertilizer comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Metal content that ensures lower dosages are required to fulfill plant’s nutrient need & is economically beneficial to the farmer.
  • the present invention provides a process for preparation of concentrated liquid fertilizer composition having source of Metal and Nitrogen for foliar application.
  • the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops.
  • the present invention provides a liquid fertilizer having 100% water miscibility comprising of highest concentration of Nitrogen and micronutrient chelated fertilizer composition.
  • a concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs; Charactered in that, the metal is fully chelated with ammonium based Ethylenediaminetetraacetic acid with clear and complete solubility in water without any settling.
  • the present invention provides a concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising of: a) 35% to 94.8% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid consisting 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.1% to 35% w/w of nanoparticle liquid Chelated complex of metal sodium based Ethylenediaminetetraacetic acid consisting 0.24-0.70 weight % of Metal source and 0.14-0.45 weight % of Sodium (Na) source and 0.15-0.30 weight % of Nitrogen (N) source with respective to total weight of Metal- Sodium-Nitrogen sources; c) 0.1% to 35% w/w of combination of nanoparticle liquid Chelated complex of metal potassium based
  • metals are selected from Zinc, Calcium, Manganese, Copper, Magnesium, Cobalt, Iron, Molybdenum, Boron and combination thereof and ammonium based selected from ammonium and diammonium.
  • Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof and excipients are selected from preservative Benzoate and Formaldehyde.
  • the present invention provides a concentrated liquid fertilizer composition having source of Zinc, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Zinc diammonium Ethylenediaminetetraacetic acid consisting 0.50-0.60 weight % of Zinc (Zn) source and 0.40-0.50 weight % of Nitrogen (N) source with respective to total weight of Zinc- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • Zinc Zinc
  • Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Zinc diammonium Ethylenediaminetetraacetic acid consisting 0.50-0.60 weight % of Zinc (Zn) source and 0.40-0.50 weight % of Nitrogen (N) source with respective to total weight of Zinc- Nitrogen sources;
  • the present invention provides a concentrated liquid fertilizer composition having source of Calcium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Calcium diammonium Ethylenediaminetetraacetic acid consisting 0.35-0.45 weight % of Calcium (Ca) source and 0.5-0.6 weight % of Nitrogen (N) source with respective to total weight of Calcium- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • the present invention provides a concentrated liquid fertilizer composition having source of Manganese, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Manganese diammonium Ethylenediaminetetraacetic acid consisting 0.4-0.5 weight % of Manganese (Mn) source & 0.45-0.55 weight % of Nitrogen (N) source with respective to total weight of Manganese- Nitrogen sources b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • Mn Manganese
  • N Nitrogen
  • the present invention provides a concentrated liquid fertilizer composition having source of Copper, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Copper and diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.6 weight % of Copper (Cu) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Copper- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • a concentrated liquid fertilizer composition having source of Copper, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Copper and diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.6 weight % of Copper (Cu) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Copper- Nitrogen sources; b)
  • the present invention provides a concentrated liquid fertilizer composition having source of Magnesium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Magnesium diammonium Ethylenediaminetetraacetic acid consisting 0.22-0.32 weight % of Magnesium (Mg) source & 0.6-0.7 weight % of Nitrogen (N) source with respective to total weight of Magnesium - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • the present invention provides a concentrated liquid fertilizer composition having source of Cobalt, Nitrogen comprising of: a) 70% to 90% w/w of nanoparticle liquid Chelated complex of Cobalt diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.52 weight % of Cobalt (Co) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Cobalt- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • the present invention provides a concentrated liquid fertilizer composition having source of Iron, Nitrogen comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of Iron ammonium Ethylenediaminetetraacetic acid consisting 0.49-0.72 weight % of Iron (Fe) source & 0.275-0.55 weight % of Nitrogen (N) source with respective to total weight of Iron- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • the present invention provides a concentrated liquid fertilizer composition having source of Molybdenum, Nitrogen comprising of: a) 80% to 95% w/w of nanoparticle liquid Chelated complex of Molybdenum diammonium Ethylenediaminetetraacetic acid consisting 0.55-0.65 weight % of Molybdenum (Mo) source & 0.3-0.4 weight % ofNitrogen (N) source with respective to total weight of Molybdenum - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
  • the present invention provides a process for preparation of concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen, comprising steps of:
  • Step 1 Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to l00 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0 weight % to 0.175 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from second alkali source and 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source; wherein weight ratio of first alkali source to second alkali source is selected between 1:0 to 1: 1.
  • Step 2 Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring.
  • Step 3 Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition.
  • Step 4 Packing the concentrated liquid fertilizer composition.
  • the present invention also provides a process for preparation of concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising steps of:
  • Step 1 Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to l00 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source; wherein weight ratio of first alkali source to second alkali source is selected between 1 :0 to 1: 1.
  • Step 2 Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring.
  • Step 2 Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition.
  • Step 3 Packing the concentrated liquid fertilizer composition.
  • the first alkali source selected from Monoethanolamine, Diethanolamine, Triethanolamine and combination thereof and the second alkali source selected from Ammonium Hydroxide, Liquor Ammonia, Ammonium Carbonate, Ammonium Chloride, Sodium Hydroxide, Sodium Carbonate, Sodium Chloride, Potassium Hydroxide, Potassium Carbonate, Potassium Chloride and combination thereof.
  • Metal source selected from Zinc Ash, Zinc Dust, Zinc Oxide, Zinc Carbonate, Zinc Carbonate Basic, Zinc Hydroxide, Zinc Chloride. Calcium Oxide, Calcium Carbonate, Calcium Hydroxide, Calcium Chloride, Manganese Oxide, Manganese Carbonate, Manganese Hydroxide, Manganese Chloride, Copper Ash, Copper Dust, Copper Oxide, Copper Carbonate, Copper Hydroxide, Copper Carbonate Basic, Copper Chloride, Copper Oxychloride.
  • chelating agent selected from Ethylenediaminetetraacetic acid; ammonium Ethylenediaminetetraacetic acid; diammonium Ethylenediaminetetraacetic acid; sodium Ethylenediaminetetraacetic acid; disodium Ethylenediaminetetraacetic acid; potassium
  • Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof and excipients selected from preservative Benzoate and Formaldehyde.
  • concentrated refers to liquid fertilizer having, at most, 5 to 40% water based on total weight of all of the components of the liquid fertilizer.
  • concentrated liquid fertilizer of any embodiment of the subject invention includes from 5 to 40 weight percent of water, based upon the total weight of all of the components of the liquid fertilizer.
  • the present invention relates to a clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients. More preferably, the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops.
  • the concentrated liquid is in the form of nano particle sized liquid without any precipitation or agglomeration of solid concentrate/solute present therein.
  • the liquid composition comprising of fully chelated complex of Metal diammonium EDTA with clear solubility without any precipitation or sedimentation and having dissolved solid concentration between 60% to 95% w/w and at the highest possible percentage of Metal, Nitrogen.
  • Non limiting examples of other nutrients that can be present in present invention composition are Sodium and Potassium.
  • the present liquid formulation of Metal Diammonium EDTA Chelate product is stronger (concentrated) than Sulfates, Nitrates & Market and any other EDTA Chelate product. Moreover it is highly soluble and stable in water between pH 1 to 11. Therefore, this being stable in alkaline and acidic conditions, that results to availability to the plants at a wider range of pH levels.
  • An important aspect of concentrated liquid fertilizer comprising a Metal Diammonium EDTA Chelate product is, it releases cations and that has a high affinity towards Lead, which plays an essential role in detoxification of Lead hence protect the plant from any the harmful effect due to this heavy metal.
  • the concentrated liquid fertilizer of the subject invention can find use in low water content formulations and applications for diluting small volume in large water tank for saving cost of storage, transportation and handling of bulky liquid formulations.
  • a concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % ofNitrogen (N) source with respective to total weight of Metal- Nitrogen sources; or in other words it comprises between 6-16 weight % of Metal source, 4.5-16 weight % of Nitrogen (N) source with respective total weight of product, a) 0.2 to 0.3% w/w Emulsifier, b) 0.01 to 0.3% w/w excipients, c) Water to qs;
  • the metal is fully chelated with ammonium based Ethylenediaminetetraacetic acid with clear and complete solubility in water without any settling.
  • the present invention provides a concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising of: a) 35% to 94.8% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid consisting 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % ofNitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.1% to 35% w/w of nanoparticle liquid Chelated complex of metal sodium based Ethylenediaminetetraacetic acid consisting 0.24-0.70 weight % of Metal source and 0.14-0.45 weight % of Sodium (Na) source and 0.15-0.30 weight % of Nitrogen (N) source with respective to total weight of Metal- Sodium-Nitrogen sources; c) 0.1% to 35% w/w of combination of nanoparticle liquid Chelated complex of metal potassium
  • fully chelated complex of metal-diammonium EDTA (Etheylene diamine tetra-acetic acid) is reaction product of combination of Metal source or Alkali + Base Metal Source, individual or combination of Alkali source or Alkali + Base Metal Source or Alkali + Chelating Acid Nitrogen Source & individual or combination of Chelating Acid Nitrogen Source or Alkali + Chelating Acid Nitrogen Source.
  • the present invention provides fertilizer comprising a chelate of diammonium salt of Etheylene diamine tetra-acetic acid and micronutrients.
  • said chelates are:Zinc- diammonium salt of Etheylene diamine tetra-acetic acid , Calcium- diammonium salt of Etheylene diamine tetra-acetic acid , Manganese- diammonium salt of Etheylene diamine tetra-acetic acid , Copper- diammonium salt of Etheylene diamine tetra- acetic acid , Magnesium- diammonium salt of Etheylene diamine tetra-acetic acid, Cobalt- diammonium salt of Etheylene diamine tetra-acetic Acid, Iron- ammonium salt of Etheylene diamine tetra-acetic acid, Molybdenum- diammonium salt of Etheylene diamine tetra-acetic acid or combination thereof.
  • the Preservative includes but not limiting to Benzoate, Formaldehyde.
  • Other optional excipients classified under emulsifier or humectant agent includes but not limiting Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof.
  • the present invention provides a process for preparation of concentrated liquid fertilizer comprising a chelate of diammonium salt of Etheylene diamine tetra-acetic acid and metal micronutrients, comprising of following steps:
  • Step 1 Mixing individual or combination of Metal source or Alkali + Base Metal Source, First Alkali source or combination of First Alkali source and Second Alkali source or Alkali + Base Metal Source or Alkali + Chelating Acid Nitrogen Source & individual or combination of Chelating Acid Nitrogen Source or Alkali + Chelating Acid Nitrogen Source are mixed together in water.
  • the reaction is an exothermic reaction having temperature between 40 to 100 °C and having solid concentration from 60% w/w to 95% w/w. Stirring the solution slowly so that all material will get dissolved completely and clear solution will obtain.
  • 50% w/w of total Nitrogen (N) is derived from EDTA and out of remaining 25 to 50% w/w of total Nitrogen (N) is derived from first alkali source and 0% to 25% w/w of total Nitrogen (N) optionally derived from second alkali source or any other nitrogen source agent.
  • Step 2 Adjust the resulting solution pH between 4 to 7 either by Alkali or by acid Source.
  • Step 3 Packing the liquid formulation.
  • the base Metal Sources are selected from following lists:
  • the First Alkali source is selected from Monoethanolamine (C2H7NO), Diethanolamine (C4H11NO2), Triethanolamine (C 6 HI 5 NO 3 ).
  • the second Alkali source is selected from Ammonium Hydroxide (NH4OH), Liquor Ammonia (NH3), Ammonium Carbonate ((NH4)2CO3), Ammonium Chloride (NH4CI).
  • the chelating Acid Nitrogen Source is selected from EDTA (C10H16N2O8), and Alkali based Chelating Acid Nitrogen Source is selected from Diammonium EDTA (C10H14N2O8 (NH4)2) Powder/liquid, and sodium source includes diammonium EDTA (CioHi4N20sNa2) and dipotassium EDTA (C10H14N2O8K2) as potassium source.
  • Non limiting examples of sources of Sodium(Na) are selected from Sodium Hydroxide (NaOH), Sodium Carbonate (Na2CC>3), Sodium Chloride (NaCl), preferably Sodium Hydroxide (NaOH) and sources of Potassium(K2O) selected from Potassium Hydroxide (KOH), Potassium Carbonate (K2CO3), Potassium Chloride (KC1), preferably Potassium Hydroxide (KOH).
  • the alkali +base metal source is selected from Ammonium Molybdate ((NH4)6Mo?O24), Sodium Molybdate (Na2MoO4), Potassium Molybdate (K2MOO4), Ammonium Borate ((NH4)2B4O?), Diammonium Octaborate ((NH4)2BsOi3), Boron Ethanolamine (C2H8BNO3 or C4H14BNO3 or CeHisBNOe), Sodium Borate (Na2B4O?), Disodium Octaborate (Na2BsOi3), Potassium Borate (K2B4O7) and Dipotassium Octaborate (K22B8O13).
  • Ammonium Molybdate ((NH4)6Mo?O24)
  • Na2MoO4 Sodium Molybdate
  • K2MOO4 Potassium Molybdate
  • Ammonium Borate ((NH4)2B4O?)
  • Diammonium Octaborate (
  • the second chelate known in the art that can be combined with Metal diammonium EDTA Chelate of the invention or combinations thereof.
  • the present invention of concentrated liquid fertilizer having 100% miscibility in water comprising of higher possible content of soluble Metal diammonium EDTA Chelate, Nitrogen and optionally Potassium and sodium.
  • Metal diammonium EDTA Chelate releases cations and has a high affinity with lead which plays an essential role in detoxification of lead in plants. This prevents plants from the toxic effects of lead.
  • Inventors of the present invention attempt to develop concentrated liquid formulations of Metal chelate with EDTA in combination with other ingredients led to solve the solubility, stability problems and issues like sedimentation, thickening and precipitation when chelated complex is prepared with concentration above 60% to 95 % w/v.
  • Step 1 Mixing Metal source, first Alkali source, second alkali source, Chelating agent, Emulsifier and excipients at temperature between 40 to 100 °C in water for solid concentration from 60% w/w to 95% w/w, under stirring,
  • Step 2 Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition
  • Step 3 Packing the liquid composition.
  • Sample 1 (Explain liquid preparation using 50% water): 0.500 kg of Zinc Diammonium EDTA complex was dissolved in 500 mL water. Solution was clear and Weight % concentration of Zinc (Zn) - 8.389: Nitrogen (N) - 7.189 was Sample 2 (Explain liquid preparation using 35% water): 0.650 kg of Zinc Diammonium EDTA complex was dissolved in 350 mL water. Solution was turbid.
  • Example 3 A concentrated nano particle sized liquid fertilizer composition consisting of Calcium Diammonium EDTA complex: Different formulation were developed using process disclosed in example no. 1.
  • Example 4 A concentrated nano particle sized liquid fertilizer composition consisting of Manganese Diammonium EDTA complex:
  • Example 5 A concentrated nano particle sized liquid fertilizer composition consisting of Copper Diammonium EDTA complex:
  • Example 6 A concentrated nano particle sized liquid fertilizer composition consisting of Magnesium Diammonium EDTA complex:
  • Example 7 A concentrated nano particle sized liquid fertilizer composition consisting of Cobalt Diammonium EDTA complex:
  • Example 8 A concentrated nano particle sized liquid fertilizer composition consisting of Iron ammonium EDTA complex:
  • Table no. 14 Analysis of liquid formulation having Iron metal
  • Example 9 A concentrated nano particle sized liquid fertilizer composition consisting of Molybdenum diammonium EDTA complex:
  • Example 10 Comparison of present invention and marketed formulation i) For Liquid concentrate comprising Metal Zinc diammonium EDTA Chelate
  • water is used to dilute the water soluble concentrate fertilizer compositions as per above disclosure to provide spray mixtures that can be used for foliar application without blockage in spray nozzle as the highly concentrated liquid fertilizer is completely water soluble .
  • the dilution of liquid concentrate in the spray mixtures of the disclosure can be varied from 0.001 to 10% v/v in water as per application.
  • the efficacy of liquid concentrate formulation is dependent on a number of factors, in particular the extent of pH stability of the formulation after adding to water.
  • the present invention is freely soluble in water form wide pH range between 1 to 12.
  • the present invention formulations have an average particle size of below 100 nm. As a result, a portion of the fertilizer active compounds applied using the formulation completely absorbed in to the crop without wasted into soil.
  • Trial 1 0.226 kg of Zinc oxide, 0.170 kg of first alkali source, 0.097 kg of second alkali source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 mb water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
  • Trial 2 0.226 kg of Zinc oxide, 0.340 kg of first alkali source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 m water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
  • Trial 3 0.226 kg of Zinc oxide, 0.166 kg of first alkali source, 0.0993 kg of Second Alkali Source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 mb water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
  • First and most important advantage of present invention is that the said invention is economic. Because the formulation is available in dilutable concentrated liquid form. Due to which 25% to 58% lower dosage are require as compare to normal liquid formulation and therefore are more economical.
  • the present invention of metal EDTA based chelated concentrated liquid fertilizer is it is stable in alkaline and acidic conditions meaning it is available for plants at a wider range of pH levels.
  • Metal Dialkali EDTA Chelate releases cations and has a high affinity with lead which plays an essential role in detoxification of lead in plants. This prevents plants from the toxic effects of lead.
  • the composition comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Nitrogen content than Metal Dialkali EDTA Chelate Liquid. That ensures lower dosages are required to fulfill plant’s nutrient need & is economically beneficial to the farmer.
  • composition comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Metal content on than Metal Dialkali EDTA Chelate liquid. It ensures lower dosages are required to fulfil plant’s nutrient need & is economically beneficial to the farmer.
  • composition comprising of Metal Dialkali EDTA Chelate concentrated liquid has 25% to 58% higher chelation value than Metal Dialkali EDTA Chelate liquid which makes present invention of Dialkali EDTA Chelate liquid more stable and easily available for plants.
  • Example 12 Comparison of Efficacy of Present invention fertilizer formulation prepared in example 1 or 2 (Zinc) and prior arts formulation::
  • TABLE NO. 25 Description of the treatment groups: Methodology of recording observations: For recording observations five plants were randomly selected and tagged from each net plot. The observations were recorded 4 days before spraying as apre-treatment and at 5 and 9 days after spraying as post treatment observations.

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Abstract

The present invention relates to a clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients. More preferably, the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops. Present invention also provides a process of preparation thereof. The present invention provides a liquid fertilizer having 100% water miscibility comprising of highest concentration of Nitrogen and micronutrient chelated fertilizer composition.

Description

TITLE OF THE INVENTION:
CONCENTRATED LIQUID FERTILIZER INCLUDING NITROGEN AND CHELATED MICRONUTRIENTS FOR FOLIAR APPLICATION AND PREPARATION PROCESS THEREOF
FIELD OF INVENTION:
The present invention relates to a clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients. More preferably, the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops. Present invention also provides a process of preparation thereof. The present invention provides a liquid fertilizer having 100% water miscibility comprising of highest concentration of Nitrogen and micronutrient chelated fertilizer composition.
BACKGROUND AND PRIOR ART OF THE INVENTION:
Plant nutrients are one of the environmental factors essential for crop growth and development. Nutrient management is crucial for optimal productivity in commercial crop production. Those nutrients in concentrations of 100 parts per million (ppm) in plant tissues are described as micronutrients and include iron (Fe), zinc (Zn), manganese (Mn), copper (Cu), boron (B), chlorine (Cl), molybdenum (Mo), and nickel (Ni). Micronutrients such as Fe, Mn, Zn, and Cu are easily oxidized or precipitated in soil, and their utilization is, therefore, not efficient. Therefore, chelated fertilizers have been developed to increase micronutrient utilization efficiency.
Foliar application is done with spraying a mist of fine water droplets through small spray nozzles. Typically, foliar applied fertilizers should soluble in water or dispersed in a such a good way that the spraying nozzles are not blocked.
There are several ways to categorize these fertilizers. One logical way to look at form is as “powder” and “liquids.” As powder formulation has a serious disadvantage due to non-uniformity of particles in-spite of any superior technology used to prepare the formulation. The macro particles remain at the top with micro particles subsiding below.
Additionally, manufacturing cost of powder formulation is always higher in comparison to the manufacturing of Liquid formulation. Preparation of the spray solution with powder formulation is a tedious and time-consuming process at a field situation. Moreover, calibration and miscibility in water at field situation are mostly inconvenient.
Powder formulation are not perfectly homogeneous in the spray solution as it is being manually prepared in the field. Moreover during the spraying process the homogeneity of the solution reduces hence such solution often weakly absorbed and assimilated in plant system. Thus, from advantage point of view, Powder formulation is always behind the liquid formulation. Irrespective of the use either as foliar application or soil application.
Considering the dose of application, the nutritional source and concentration of each nutrients per weight basis is also important to provide a easy to use formulation or having single dilution with maximum possible concentration to avoid the multiple applications. For that instance, the power form of chelated fertilizer need a solubilizing tank for ensuring the uniform solubility before spraying. Hence higher dosage need to apply to provide full nutrition result to higher cost of treatment by the end users.
The above problems of powder fertilizer formulation are considered to develop a suitable liquid fertilizer formulation specifically for foliar applications.
Therefore, the use of concentrated, liquid fertilizers are becoming increasingly popular for use in farms over standard solid (powder or granular) fertilizers and other suspension liquid fertilizer due to their ease of use and performance characteristics. The liquid fertilizer typically prepared by considering the saturation solubilities of salts/chelate present in powder form and one can not achieve the solutions having concentration above said solubility, may be not more than 0.1 to 60% solid dissolved in solution. However, such less concentrations in said solutions are not effective to load the more concentrated solute due to limitation of said solubility parameter, or have limited compatibility in different pH ranges.
Therefore, the objective of the present invention is to provide a concentrated solution of metal chelated fertilizer composition. Which includes providing a liquid fertilizer comprising a highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops.
As per present invention, the chelated liquid fertilizer which will be having 100% water soluble form is an essential part of fertilizer composition to provide an accurate concentration of deficient metal/Mineral. Because, they form clear solutions having highest concentration of micronutrients, nitrogen and potassium and content as compare to the other known liquid fertilizer. Additionally, the said composition of liquid fertilizer is devoid of sediments or precipitates even higher concentration of nutritional constituents are present. This guarantees a high level of effectiveness and stops the nozzle becoming blocked.
Therefore, the present invention solving the problem of powder, suspension type or less soluble foliar application micronutrient chelated fertilizer composition of said prior art disclosure by providing a novel and effective completely water soluble micronutrient chelated liquid fertilizer having maximum concentration of nutrients as well as micronutrients.
OBJECTIVE OF THE INVENTION:
It is an objective of the present invention to provide a concentrated clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients for reconstitution before foliar application.
Another specific objective of the invention is to provide a liquid fertilizer composition in the form of nano particle sized liquid without any precipitation or agglomeration of solid concentrate/solute present therein.
One of the objective of the invention to provide a fertilizer composition having neutral pH as it is very safe and provides a highest availability of Metal-Nitrogen with no risk of scorching to given crop and plant so that provides a highest benefits with maximum uptake.
The one more objective of the present invention it to provide liquid fertilizer comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Metal content that ensures lower dosages are required to fulfill plant’s nutrient need & is economically beneficial to the farmer.
In an aspect, the present invention provides a process for preparation of concentrated liquid fertilizer composition having source of Metal and Nitrogen for foliar application.
SUMMARY OF THE INVENTION:
The present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops. The present invention provides a liquid fertilizer having 100% water miscibility comprising of highest concentration of Nitrogen and micronutrient chelated fertilizer composition.
In accordance to present invention, it provides a concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen, comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs; Charactered in that, the metal is fully chelated with ammonium based Ethylenediaminetetraacetic acid with clear and complete solubility in water without any settling.
In accordance to second embodiment, the present invention provides a concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising of: a) 35% to 94.8% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid consisting 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.1% to 35% w/w of nanoparticle liquid Chelated complex of metal sodium based Ethylenediaminetetraacetic acid consisting 0.24-0.70 weight % of Metal source and 0.14-0.45 weight % of Sodium (Na) source and 0.15-0.30 weight % of Nitrogen (N) source with respective to total weight of Metal- Sodium-Nitrogen sources; c) 0.1% to 35% w/w of combination of nanoparticle liquid Chelated complex of metal potassium based Ethylenediaminetetraacetic acid consisting 0.15- 0.59 weight % of Metal source, 0.25-0.65 weight % of Potassium (K2O) source and 0.12-0.195 weight % ofNitrogen (N) source with respective to total weight of metal-Potassium-Nitrogen sources; d) 0.2 to 0.3% w/w Emulsifier, e) 0.01 to 0.3% w/w excipients, f) Water to qs;
Charactered in that the metal is fully chelated with Ethylenediaminetetraacetic acid with clear solubility in water without any settling. Wherein metals are selected from Zinc, Calcium, Manganese, Copper, Magnesium, Cobalt, Iron, Molybdenum, Boron and combination thereof and ammonium based selected from ammonium and diammonium.
The non-limiting examples of Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof and excipients are selected from preservative Benzoate and Formaldehyde.
More preferably, the present invention provides a concentrated liquid fertilizer composition having source of Zinc, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Zinc diammonium Ethylenediaminetetraacetic acid consisting 0.50-0.60 weight % of Zinc (Zn) source and 0.40-0.50 weight % of Nitrogen (N) source with respective to total weight of Zinc- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
Further, the present invention provides a concentrated liquid fertilizer composition having source of Calcium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Calcium diammonium Ethylenediaminetetraacetic acid consisting 0.35-0.45 weight % of Calcium (Ca) source and 0.5-0.6 weight % of Nitrogen (N) source with respective to total weight of Calcium- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs. Further, the present invention provides a concentrated liquid fertilizer composition having source of Manganese, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Manganese diammonium Ethylenediaminetetraacetic acid consisting 0.4-0.5 weight % of Manganese (Mn) source & 0.45-0.55 weight % of Nitrogen (N) source with respective to total weight of Manganese- Nitrogen sources b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
Further, the present invention provides a concentrated liquid fertilizer composition having source of Copper, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Copper and diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.6 weight % of Copper (Cu) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Copper- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
Further, the present invention provides a concentrated liquid fertilizer composition having source of Magnesium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Magnesium diammonium Ethylenediaminetetraacetic acid consisting 0.22-0.32 weight % of Magnesium (Mg) source & 0.6-0.7 weight % of Nitrogen (N) source with respective to total weight of Magnesium - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs. Further, the present invention provides a concentrated liquid fertilizer composition having source of Cobalt, Nitrogen comprising of: a) 70% to 90% w/w of nanoparticle liquid Chelated complex of Cobalt diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.52 weight % of Cobalt (Co) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Cobalt- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
Further, the present invention provides a concentrated liquid fertilizer composition having source of Iron, Nitrogen comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of Iron ammonium Ethylenediaminetetraacetic acid consisting 0.49-0.72 weight % of Iron (Fe) source & 0.275-0.55 weight % of Nitrogen (N) source with respective to total weight of Iron- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
Further, the present invention provides a concentrated liquid fertilizer composition having source of Molybdenum, Nitrogen comprising of: a) 80% to 95% w/w of nanoparticle liquid Chelated complex of Molybdenum diammonium Ethylenediaminetetraacetic acid consisting 0.55-0.65 weight % of Molybdenum (Mo) source & 0.3-0.4 weight % ofNitrogen (N) source with respective to total weight of Molybdenum - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs. In accordance to one more embodiments, the present invention provides a process for preparation of concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen, comprising steps of:
Step 1: Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to l00 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0 weight % to 0.175 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from second alkali source and 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source; wherein weight ratio of first alkali source to second alkali source is selected between 1:0 to 1: 1.
Step 2: Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring.
Step 3: Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition.
Step 4: Packing the concentrated liquid fertilizer composition.
Further, the present invention also provides a process for preparation of concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising steps of:
Step 1: Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to l00 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source; wherein weight ratio of first alkali source to second alkali source is selected between 1 :0 to 1: 1.
Step 2: Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring.
Step 2: Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition.
Step 3: Packing the concentrated liquid fertilizer composition.
Wherein, the first alkali source selected from Monoethanolamine, Diethanolamine, Triethanolamine and combination thereof and the second alkali source selected from Ammonium Hydroxide, Liquor Ammonia, Ammonium Carbonate, Ammonium Chloride, Sodium Hydroxide, Sodium Carbonate, Sodium Chloride, Potassium Hydroxide, Potassium Carbonate, Potassium Chloride and combination thereof.
The non-limiting examples of Metal source selected from Zinc Ash, Zinc Dust, Zinc Oxide, Zinc Carbonate, Zinc Carbonate Basic, Zinc Hydroxide, Zinc Chloride. Calcium Oxide, Calcium Carbonate, Calcium Hydroxide, Calcium Chloride, Manganese Oxide, Manganese Carbonate, Manganese Hydroxide, Manganese Chloride, Copper Ash, Copper Dust, Copper Oxide, Copper Carbonate, Copper Hydroxide, Copper Carbonate Basic, Copper Chloride, Copper Oxychloride. Magnesium Dust, Magnesium Ribbon, Magnesium Oxide, Magnesium Carbonate, Magnesium Hydroxide, Magnesium Carbonate Basic, Magnesium Chloride, Cobalt Ash, Cobalt Oxide, Cobalt Carbonate, Cobalt Hydroxide, Cobalt Carbonate Basic, Cobalt Chloride, Iron Sulphate, Iron Dust, Iron Red Oxide, Iron Yellow Oxide, Iron Sulphate, Iron Carbonate, Iron Hydroxide, Iron Chloride, Molybdenum Oxide, Molybdenum Disulphide, Molybdenum Chloride, Boric Acid, Ammonium Molybdate, Sodium Molybdate, Potassium Molybdate, Ammonium Borate, Diammonium Octaborate, Boron Ethanolamine, Sodium Borate, Disodium Octaborate, Potassium Borate, Dipotassium Octaborate and combination thereof.
The non-limiting examples of chelating agent selected from Ethylenediaminetetraacetic acid; ammonium Ethylenediaminetetraacetic acid; diammonium Ethylenediaminetetraacetic acid; sodium Ethylenediaminetetraacetic acid; disodium Ethylenediaminetetraacetic acid; potassium
Ethylenediaminetetraacetic acid and dipotassium Ethylenediaminetetraacetic acid and combination thereof.
The Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof and excipients selected from preservative Benzoate and Formaldehyde.
DETAILED DESCRIPTION OF THE INVENTION:
The foregoing summary, as well as the following detailed description of the invention will be better understood when read in conjunction with the appended examples. For the purpose of assisting in the explanation of the invention, the examples are presently preferred and considered illustrative.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art to which the invention(s) belong. As used herein, “100% water soluble”, “100% water soluble without any particle sedimentation after dissolving into a water”, which are be used interchangeably, refer to concentrate that is freely soluble form and fully chelated metal compound. The term “substantially fully chelated” meaning that a majority of the compounds have metals that are chelated and a minority of the compounds have metals that are not chelated. The term “fully chelated” meaning that all of the compounds have metals that are chelated with chelating agent. The term “concentrated”, as in “concentrated liquid fertilizer”, refers to liquid fertilizer having, at most, 5 to 40% water based on total weight of all of the components of the liquid fertilizer. Stated another way, the “concentrated liquid fertilizer” of any embodiment of the subject invention includes from 5 to 40 weight percent of water, based upon the total weight of all of the components of the liquid fertilizer.
The present invention relates to a clear liquid fertilizer for foliar application comprising of source of Nitrogen and Chelated micronutrients. More preferably, the present invention provides a concentrated liquid fertilizer composition comprising highest concentration of Nitrogen and Chelated micronutrients sources for foliar application on crops.
In accordance to present invention, the concentrated liquid is in the form of nano particle sized liquid without any precipitation or agglomeration of solid concentrate/solute present therein. The liquid composition comprising of fully chelated complex of Metal diammonium EDTA with clear solubility without any precipitation or sedimentation and having dissolved solid concentration between 60% to 95% w/w and at the highest possible percentage of Metal, Nitrogen. Non limiting examples of other nutrients that can be present in present invention composition are Sodium and Potassium.
The present liquid formulation of Metal Diammonium EDTA Chelate product is stronger (concentrated) than Sulfates, Nitrates & Market and any other EDTA Chelate product. Moreover it is highly soluble and stable in water between pH 1 to 11. Therefore, this being stable in alkaline and acidic conditions, that results to availability to the plants at a wider range of pH levels. An important aspect of concentrated liquid fertilizer comprising a Metal Diammonium EDTA Chelate product is, it releases cations and that has a high affinity towards Lead, which plays an essential role in detoxification of Lead hence protect the plant from any the harmful effect due to this heavy metal. The concentrated liquid fertilizer of the subject invention can find use in low water content formulations and applications for diluting small volume in large water tank for saving cost of storage, transportation and handling of bulky liquid formulations.
In accordance to present invention, it provides a concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen, comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % ofNitrogen (N) source with respective to total weight of Metal- Nitrogen sources; or in other words it comprises between 6-16 weight % of Metal source, 4.5-16 weight % of Nitrogen (N) source with respective total weight of product, a) 0.2 to 0.3% w/w Emulsifier, b) 0.01 to 0.3% w/w excipients, c) Water to qs;
Charactered in that, the metal is fully chelated with ammonium based Ethylenediaminetetraacetic acid with clear and complete solubility in water without any settling.
In accordance to second embodiment, the present invention provides a concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising of: a) 35% to 94.8% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid consisting 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % ofNitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.1% to 35% w/w of nanoparticle liquid Chelated complex of metal sodium based Ethylenediaminetetraacetic acid consisting 0.24-0.70 weight % of Metal source and 0.14-0.45 weight % of Sodium (Na) source and 0.15-0.30 weight % of Nitrogen (N) source with respective to total weight of Metal- Sodium-Nitrogen sources; c) 0.1% to 35% w/w of combination of nanoparticle liquid Chelated complex of metal potassium based Ethylenediaminetetraacetic acid consisting 0.15- 0.59 weight % of Metal source, 0.25-0.65 weight % of Potassium (K2O) source and 0.12-0.195 weight % ofNitrogen (N) source with respective to total weight of metal-Potassium-Nitrogen sources; d) 0.2 to 0.3% w/w Emulsifier, e) 0.01 to 0.3% w/w excipients, f) Water to qs;
Charactered in that the metal is fully chelated with Ethylenediaminetetraacetic acid with clear solubility in water without any settling.
In accordance to invention, fully chelated complex of metal-diammonium EDTA (Etheylene diamine tetra-acetic acid) is reaction product of combination of Metal source or Alkali + Base Metal Source, individual or combination of Alkali source or Alkali + Base Metal Source or Alkali + Chelating Acid Nitrogen Source & individual or combination of Chelating Acid Nitrogen Source or Alkali + Chelating Acid Nitrogen Source.
In accordance to present invention, the present invention provides fertilizer comprising a chelate of diammonium salt of Etheylene diamine tetra-acetic acid and micronutrients. Not limiting examples of said chelates are:Zinc- diammonium salt of Etheylene diamine tetra-acetic acid , Calcium- diammonium salt of Etheylene diamine tetra-acetic acid , Manganese- diammonium salt of Etheylene diamine tetra-acetic acid , Copper- diammonium salt of Etheylene diamine tetra- acetic acid , Magnesium- diammonium salt of Etheylene diamine tetra-acetic acid, Cobalt- diammonium salt of Etheylene diamine tetra-acetic Acid, Iron- ammonium salt of Etheylene diamine tetra-acetic acid, Molybdenum- diammonium salt of Etheylene diamine tetra-acetic acid or combination thereof. In certain instances of present invention, the composition may be mixture of above chelated compounds or any additional potassium or sodium based metal chelate compositions.
The Preservative includes but not limiting to Benzoate, Formaldehyde. Other optional excipients classified under emulsifier or humectant agent includes but not limiting Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof.
In accordance to one more embodiment, the present invention provides a process for preparation of concentrated liquid fertilizer comprising a chelate of diammonium salt of Etheylene diamine tetra-acetic acid and metal micronutrients, comprising of following steps:
Step 1 : Mixing individual or combination of Metal source or Alkali + Base Metal Source, First Alkali source or combination of First Alkali source and Second Alkali source or Alkali + Base Metal Source or Alkali + Chelating Acid Nitrogen Source & individual or combination of Chelating Acid Nitrogen Source or Alkali + Chelating Acid Nitrogen Source are mixed together in water. The reaction is an exothermic reaction having temperature between 40 to 100 °C and having solid concentration from 60% w/w to 95% w/w. Stirring the solution slowly so that all material will get dissolved completely and clear solution will obtain. Wherein, 50% w/w of total Nitrogen (N) is derived from EDTA and out of remaining 25 to 50% w/w of total Nitrogen (N) is derived from first alkali source and 0% to 25% w/w of total Nitrogen (N) optionally derived from second alkali source or any other nitrogen source agent.
Step 2: Adjust the resulting solution pH between 4 to 7 either by Alkali or by acid Source.
Step 3: Packing the liquid formulation.
Regarding final product form of this method of preparation, the introduction of the drying step to obtain dry powder in any suitable method can be performed. In accordance to present invention, the base Metal Sources are selected from following lists:
Zinc (Zn):- Zinc Ash (Zn), Zinc Dust (Zn), Zinc Oxide (ZnO), Zinc Carbonate (ZnCO3), Zinc Carbonate Basic (ZnCO3. Zn(0H)2), Zinc Hydroxide (Zn(0H)2), Zinc Chloride (ZnCh) preferably Zinc Oxide (ZnO).
Calcium (Ca):- Calcium Oxide (CaO), Calcium Carbonate (CaCO?). Calcium Hydroxide (Ca(0H)2), Calcium Chloride (CaCh) preferably Calcium Carbonate (CaCO3).
Manganese (Mn):- Manganese Oxide (Mn02), Manganese Carbonate (MnCO3), Manganese Hydroxide (Mn (OHh), Manganese Chloride (MnCh) preferably Manganese Carbonate (MnCO3).
Copper (Cu):- Copper Ash (Cu), Copper Dust (Cu), Copper Oxide ( 12O), Copper Carbonate (CuCO3), Copper Hydroxide (Cu(OH)3), Copper Carbonate Basic (CuCO3. CU(OH)3), Copper Chloride (CuCh), Copper Oxychloride (H3C1CU2O) preferably Copper Carbonate Basic (CuCO3. Cu(0H)2).
Magnesium (Mg):- Magnesium Dust (Mg), Magnesium Ribbon (Mg), Magnesium Oxide (MgO), Magnesium Carbonate (MgCO3), Magnesium Hydroxide (Mg(OH)3), Magnesium Carbonate Basic (MgCO3.Mg(OH)2), Magnesium Chloride (MgCh), preferably Magnesium Carbonate (MgCO3).
Cobalt (Co):- Cobalt Ash (Co), Cobalt Oxide (CoO), Cobalt Carbonate (CoCO3), Cobalt Hydroxide (Co(OH)2), Cobalt Carbonate Basic (CoCO3. Mg(OH)3), Cobalt Chloride (C0CI2), preferably Cobalt Carbonate (CoCO3).
Iron (Fe):- Iron Sulphate (FeSO4), Iron Dust (Fe), Iron Red Oxide (Fe3O3), Iron Yellow Oxide (Fe3O3), Iron Sulphate (FeSO4), Iron Carbonate (FeCO3), Iron Hydroxide (Fe(OH)3), Iron Chloride (FeCh or F2C13) preferably Iron Red Oxide (Fe2O3).
Molybdenum (Mo):- Molybdenum Oxide (MoO3), Molybdenum DiSulphide (M0S2), Molybdenum Chloride (M0CI5), preferably Molybdenum Oxide (MoO3). Boron (B):- Boric Acid (H3BO3).
In accordance to present invention, the First Alkali source is selected from Monoethanolamine (C2H7NO), Diethanolamine (C4H11NO2), Triethanolamine (C6HI5NO3).
In accordance to present invention, the second Alkali source is selected from Ammonium Hydroxide (NH4OH), Liquor Ammonia (NH3), Ammonium Carbonate ((NH4)2CO3), Ammonium Chloride (NH4CI).
In accordance to present invention, the chelating Acid Nitrogen Source is selected from EDTA (C10H16N2O8), and Alkali based Chelating Acid Nitrogen Source is selected from Diammonium EDTA (C10H14N2O8 (NH4)2) Powder/liquid, and sodium source includes diammonium EDTA (CioHi4N20sNa2) and dipotassium EDTA (C10H14N2O8K2) as potassium source.
Non limiting examples of sources of Sodium(Na) are selected from Sodium Hydroxide (NaOH), Sodium Carbonate (Na2CC>3), Sodium Chloride (NaCl), preferably Sodium Hydroxide (NaOH) and sources of Potassium(K2O) selected from Potassium Hydroxide (KOH), Potassium Carbonate (K2CO3), Potassium Chloride (KC1), preferably Potassium Hydroxide (KOH).
In a non-limiting examples, the alkali +base metal source is selected from Ammonium Molybdate ((NH4)6Mo?O24), Sodium Molybdate (Na2MoO4), Potassium Molybdate (K2MOO4), Ammonium Borate ((NH4)2B4O?), Diammonium Octaborate ((NH4)2BsOi3), Boron Ethanolamine (C2H8BNO3 or C4H14BNO3 or CeHisBNOe), Sodium Borate (Na2B4O?), Disodium Octaborate (Na2BsOi3), Potassium Borate (K2B4O7) and Dipotassium Octaborate (K22B8O13).
In an non-limiting embodiment, the second chelate known in the art that can be combined with Metal diammonium EDTA Chelate of the invention or combinations thereof.
Further, Therefore, the present invention of concentrated liquid fertilizer having 100% miscibility in water comprising of higher possible content of soluble Metal diammonium EDTA Chelate, Nitrogen and optionally Potassium and sodium. Wherein Metal diammonium EDTA Chelate releases cations and has a high affinity with lead which plays an essential role in detoxification of lead in plants. This prevents plants from the toxic effects of lead.
Dated this ....
It has been observed that water based formulations of metal chelated complex fertilizer for foliar application like Zinc -EDTA, Fe- EDTA which are insoluble or partially soluble in water at concentration above 50% w/w (Metal EDTA chelate has solubility between 0 to 50% w/w) and when concentrated solution tried to prepared then it suffer from a verities of problems such as crystal formation, agglomeration, settling formation, sedimentation, precipitation and the like. Such problem aggravates when the active metal chelated complex has the ability to precipitate out in acidic or basic pH medium or water content is less than 50% w/w.
Therefore, the chemical interconversion of chelated metal fertilizer from liquid to crystals, the drastic difference in their pH properties of diluting medium during spraying and their unpredictable properties of limited solubility below 60% w/w in water make it difficult to formulate concentrated liquid formulation of metal chelated composition for foliar application having desired physical (neutral pH/ freely soluble in wide pH range aqueous medium) and biological properties (quick absorption of nanoparticulate moieties by leaves stomata and electrical conductivity).
Inventors of the present invention attempt to develop concentrated liquid formulations of Metal chelate with EDTA in combination with other ingredients led to solve the solubility, stability problems and issues like sedimentation, thickening and precipitation when chelated complex is prepared with concentration above 60% to 95 % w/v.
It require additional efforts to obtain the nanoparticulate form of chelated complex having required uniform particle size and during such processes that led to maintain the stability of liquid fertilizer having highest concentration of metal and other nutrients like Nitrogen, Potassium, Sodium and Phosphorous content in liquid form.
The invention will now be further described with reference to the following examples:
Example 1 Preparation of concentrated nano particle sized liquid fertilizer composition as per present invention:
Procedure: Step 1: Mixing Metal source, first Alkali source, second alkali source, Chelating agent, Emulsifier and excipients at temperature between 40 to 100 °C in water for solid concentration from 60% w/w to 95% w/w, under stirring,
Step 2: Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition,
Step 3 Packing the liquid composition.
Example 2 (i): A concentrated nano particle sized liquid fertilizer composition consisting of Zinc Diammonium EDTA complex as per present invention:
226 kg ofZinc oxide, 288 kg of first alkali source, 33.48 kg of second alkali source and 821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 kg water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The weight of chemical agent in water was about 80% w/w . The resulting solution pH was 6 to7.
Liquid solution was clear and Weight % concentration of Zinc (Zn) - 12.94 : Nitrogen (N) was 11.08
Example 2(ii): Comparative liquid fertilizer composition consisting of Zinc Diammonium EDTA complex:
Sample 1 (Explain liquid preparation using 50% water): 0.500 kg of Zinc Diammonium EDTA complex was dissolved in 500 mL water. Solution was clear and Weight % concentration of Zinc (Zn) - 8.389: Nitrogen (N) - 7.189 was Sample 2 (Explain liquid preparation using 35% water): 0.650 kg of Zinc Diammonium EDTA complex was dissolved in 350 mL water. Solution was turbid.
Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table
Figure imgf000021_0001
Table no. 1: Different liquid formulation having Zinc metal
Figure imgf000021_0002
Table no. 2: Analysis of liquid formulation having Zinc metal
Example 3: A concentrated nano particle sized liquid fertilizer composition consisting of Calcium Diammonium EDTA complex: Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table
Figure imgf000022_0001
Table no. 3: Different liquid formulation having Calcium metal
Figure imgf000022_0002
Table no. 4: Analysis of liquid formulation having Calcium metal
Example 4: A concentrated nano particle sized liquid fertilizer composition consisting of Manganese Diammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table .
Figure imgf000022_0003
Table no. 5: Different liquid formulation having Manganese metal
Figure imgf000023_0001
Table no. 6: Analysis of liquid formulation having Manganese metal
Example 5: A concentrated nano particle sized liquid fertilizer composition consisting of Copper Diammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1. The formulations are disclosed in following table .
Figure imgf000023_0002
Table no. 5: Different liquid formulation having Copper metal
Figure imgf000024_0001
Example 6: A concentrated nano particle sized liquid fertilizer composition consisting of Magnesium Diammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1. The formulations are disclosed in following table.
Figure imgf000024_0002
Table no. 9: Different liquid formulation having Magnesium meta
Figure imgf000024_0003
Figure imgf000025_0001
Example 7: A concentrated nano particle sized liquid fertilizer composition consisting of Cobalt Diammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table.
Figure imgf000025_0002
Table no. 11: Different liquid formulation having Cobalt metal
Figure imgf000025_0003
Figure imgf000026_0001
Table no. 12: Analysis of liquid formulation having Cobalt metal
Example 8: A concentrated nano particle sized liquid fertilizer composition consisting of Iron ammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table.
Figure imgf000026_0002
Table no. 13: Different liquid formulation having Iron metal
Figure imgf000026_0003
Table no. 14: Analysis of liquid formulation having Iron metal Example 9: A concentrated nano particle sized liquid fertilizer composition consisting of Molybdenum diammonium EDTA complex:
Different formulation were developed using process disclosed in example no. 1.
The formulations are disclosed in following table.
Figure imgf000027_0001
Table no. 15: Different liquid formulation having Molybdenum metal
Figure imgf000027_0002
Table no. 16: Analysis of liquid formulation having Molybdenum metal
Example 10: Comparison of present invention and marketed formulation i) For Liquid concentrate comprising Metal Zinc diammonium EDTA Chelate
Figure imgf000028_0001
TABLE NO. 17: Comparison of Liquid composition comprising Zinc diammonium
EDTA Chelate ii) For Liquid concentrate comprising Metal Calcium diammonium EDTA
Chelate
Figure imgf000028_0002
Figure imgf000029_0001
TABLE NO. 18: Comparison of Liquid composition comprising Calcium diammonium EDTA Chelate iii) For Liquid concentrate comprising Metal Manganese diammonium EDTA Chelate
Figure imgf000029_0002
TABLE NO. 19: Comparison of Liquid composition comprising Manganese diammonium EDTA Chelate
iv) For Liquid concentrate comprising Metal Copper diammonium EDTA
Chelate
Figure imgf000030_0001
TABLE NO. 20: Comparison of Liquid composition comprising Copper diammonium EDTA Chelate v)For Liquid concentrate comprising Metal Magnesium diammonium EDTA Chelate
Figure imgf000030_0002
Figure imgf000031_0001
TABLE NO. 21: Comparison of Liquid composition comprising Magnesium diammonium EDTA Chelate vi) For Liquid concentrate comprising Metal Cobalt diammonium EDTA
Chelate
Figure imgf000031_0002
TABLE NO. 22: Comparison of Liquid composition comprising Cobalt diammonium EDTA Chelate vii) For Liquid concentrate comprising Metal Iron ammonium EDTA
Chelate
Figure imgf000032_0001
TABLE NO. 23: Comparison of Liquid composition comprising Iron ammonium
EDTA Chelate. viii) For Liquid concentrate comprising Metal Molybdenum diammonium EDTA Chelate
Figure imgf000032_0002
Figure imgf000033_0001
TABLE NO. 24: Comparison of Liquid composition comprising Molybdenum diammonium EDTA Chelate
In one embodiment, water is used to dilute the water soluble concentrate fertilizer compositions as per above disclosure to provide spray mixtures that can be used for foliar application without blockage in spray nozzle as the highly concentrated liquid fertilizer is completely water soluble . The dilution of liquid concentrate in the spray mixtures of the disclosure can be varied from 0.001 to 10% v/v in water as per application.
The efficacy of liquid concentrate formulation is dependent on a number of factors, in particular the extent of pH stability of the formulation after adding to water. The present invention is freely soluble in water form wide pH range between 1 to 12.
Further, the uniformity and size of droplets directly affect the permeability of the active micronutrients compounds and the final efficacy of the formulation. The present invention formulations have an average particle size of below 100 nm. As a result, a portion of the fertilizer active compounds applied using the formulation completely absorbed in to the crop without wasted into soil.
Example ll:Effect of First and second alkali source on formulation: (incorporate the examples for ethanolamine 50, 100, 49%), ammonia 50, 0 and 51%)%)
Trial 1: 0.226 kg of Zinc oxide, 0.170 kg of first alkali source, 0.097 kg of second alkali source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 mb water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
Observation of final Product: Solution is clear without any settling
Trial 2: 0.226 kg of Zinc oxide, 0.340 kg of first alkali source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 m water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
Observation of final Product: Solution is clear without any settling
Trial 3: 0.226 kg of Zinc oxide, 0.166 kg of first alkali source, 0.0993 kg of Second Alkali Source and 0.821 Kg of Ethylenediaminetetraacetic acid was dissolved in 500 mb water. The reaction mass was reacted at temperature between 90 to 100 °C. The temperature was maintained by jacketed vessel. The solid concentration of liquid was about 80% w/w . The resulting solution pH was 7.
Observation of final Product: Solution is turbid with settling.
Advantage of Present invention:
First and most important advantage of present invention is that the said invention is economic. Because the formulation is available in dilutable concentrated liquid form. Due to which 25% to 58% lower dosage are require as compare to normal liquid formulation and therefore are more economical.
The present invention of metal EDTA based chelated concentrated liquid fertilizer is it is stable in alkaline and acidic conditions meaning it is available for plants at a wider range of pH levels. As said Metal Dialkali EDTA Chelate releases cations and has a high affinity with lead which plays an essential role in detoxification of lead in plants. This prevents plants from the toxic effects of lead. The composition comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Nitrogen content than Metal Dialkali EDTA Chelate Liquid. That ensures lower dosages are required to fulfill plant’s nutrient need & is economically beneficial to the farmer.
The composition comprising of Metal Dialkali EDTA Chelate concentrated liquid contains 25% to 58% higher amount of Metal content on than Metal Dialkali EDTA Chelate liquid. It ensures lower dosages are required to fulfil plant’s nutrient need & is economically beneficial to the farmer.
The composition comprising of Metal Dialkali EDTA Chelate concentrated liquid has 25% to 58% higher chelation value than Metal Dialkali EDTA Chelate liquid which makes present invention of Dialkali EDTA Chelate liquid more stable and easily available for plants.
Example 12: Comparison of Efficacy of Present invention fertilizer formulation prepared in example 1 or 2 (Zinc) and prior arts formulation::
Field trials were carried out in order to assess the efficacy of the water soluble concentrated fertilizer having highest percentage of micronutrients for reconstitution composition described above in present invention when foliar sprayed on to a crop.
The trials were carried out using Chili (Capsicum) crop grown in open field of Western region of Maharashtra. Details of treatments are listed below:
Figure imgf000035_0001
TABLE NO. 25 : Description of the treatment groups: Methodology of recording observations: For recording observations five plants were randomly selected and tagged from each net plot. The observations were recorded 4 days before spraying as apre-treatment and at 5 and 9 days after spraying as post treatment observations.
Time of spray ing--> 1st spraying 30 days after transplanting and 2nd spraying 45 days after first spraying.
Figure imgf000036_0001
TABLE NO. 26: Effect of concentrated liquid fertilizer on plant height (cm).
DAS: Days after sowing
Data of plant height four days after first spray was found to be non significant indicating uniform plant height in all treatments. Data of plant height at 5 and 9 days after first spray and second spray showed that the spraying of (T2)was found to be the best treatment for producing taller plant and both the treatments were significantly superior over treatment T i and Treatment T3 without fertilizer.

Claims

CLAIMS We Claim,
1. A concentrated liquid fertilizer composition for foliar application having source of Metal and Nitrogen, comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3 % w/w excipients , d) Water to qs;
Charactered in that, the metal is fully chelated with ammonium based Ethylenediaminetetraacetic acid with clear and complete solubility in water without any settling.
2. A concentrated liquid fertilizer composition for foliar application having source of Metal, Potassium, Sodium, Nitrogen comprising of: a) 35% to 94.8% w/w of nanoparticle liquid Chelated complex of metal ammonium based Ethylenediaminetetraacetic acid consisting 0.22-0.72 weight % of Metal source and 0.30-0.70 weight % of Nitrogen (N) source with respective to total weight of Metal- Nitrogen sources; b) 0. 1% to 35% w/w of nanoparticle liquid Chelated complex of metal sodium based Ethylenediaminetetraacetic acid consisting 0.24-0.70 weight % of Metal source and 0.14-0.45 weight % of Sodium (Na) source and 0.15-0.30 weight % of Nitrogen (N) source with respective to total weight of Metal- Sodium-Nitrogen sources; c) 0.1% to 35% w/w of combination of nanoparticle liquid Chelated complex of metal potassium based Ethylenediaminetetraacetic acid consisting 0.15-0.59 weight % of Metal source, 0.25-0.65 weight % of Potassium (K2O) source and 0. 12-0. 195 weight % ofNitrogen (N) source with respective to total weight of metal-Potassium- Nitrogen sources; d) 0.2 to 0.3% w/w Emulsifier, e) 0.01 to 0.3% w/w excipients , f) Water to qs;
Charactered in that the metal is fully chelated with Ethylenediaminetetraacetic acid with clear solubility in water without any settling.
3. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1 and 2, wherein metals are selected from Zinc, Calcium, Manganese, Copper, Magnesium, Cobalt, Iron, Molybdenum, Boron and combination thereof.
4. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein ammonium based selected from ammonium and diammonium.
5. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1 and 2, wherein Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof.
6. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1 and 2, wherein excipients are selected from preservative Benzoate and Formaldehyde.
7. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Zinc, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Zinc diammonium Ethylenediaminetetraacetic acid consisting 0.50-0.60 weight % of Zinc (Zn) source and 0.40-0.50 weight % of Nitrogen (N) source with respective to total weight of Zinc- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
8. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Calcium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Calcium diammonium Ethylenediaminetetraacetic acid consisting 0.35-0.45 weight % of Calcium (Ca) source and 0.5-0.6 weight % of Nitrogen (N) source with respective to total weight of Calcium- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
9. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Manganese, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Manganese diammonium Ethylenediaminetetraacetic acid consisting 0.4-0.5 weight % of Manganese (Mn) source & 0.45- 0.55 weight % of Nitrogen (N) source with respective to total weight of Manganese- Nitrogen sources b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
10. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Copper, Nitrogen comprising of: a) 75% to 90% w/w of nanoparticle liquid Chelated complex of Copper and diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.6 weight % of Copper (Cu) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Copper- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
11. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Magnesium, Nitrogen comprising of: a) 85% to 95% w/w of nanoparticle liquid Chelated complex of Magnesium diammonium Ethylenediaminetetraacetic acid consisting 0.22-0.32 weight % of Magnesium (Mg) source & 0.6- 0.7 weight % of Nitrogen (N) source with respective to total weight of Magnesium - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
12. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Cobalt, Nitrogen comprising of: a) 70% to 90% w/w of nanoparticle liquid Chelated complex of Cobalt diammonium Ethylenediaminetetraacetic acid consisting 0.5-0.52 weight % of Cobalt (Co) source & 0.4-0.5 weight % of Nitrogen (N) source with respective to total weight of Cobalt- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
13. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Iron, Nitrogen comprising of: a) 70% to 95% w/w of nanoparticle liquid Chelated complex of Iron ammonium Ethylenediaminetetraacetic acid consisting 0.49-0.72 weight % of Iron (Fe) source & 0.275-0.55 weight % of Nitrogen (N) source with respective to total weight of Iron- Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
14. The concentrated liquid fertilizer composition for foliar application as claimed in claim 1, wherein composition having source of Molybdenum, Nitrogen comprising of: a) 80% to 95% w/w of nanoparticle liquid Chelated complex of Molybdenum diammonium Ethylenediaminetetraacetic acid consisting 0.55-0.65 weight % of Molybdenum (Mo) source & 0.3- 0.4 weight % ofNitrogen (N) source with respective to total weight of Molybdenum - Nitrogen sources; b) 0.2 to 0.3% w/w Emulsifier, c) 0.01 to 0.3% w/w excipients, d) Water to qs.
15. A process for preparation of concentrated liquid fertilizer composition for foliar application as claimed in claim 1, comprising steps of:
Step 1: Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0 weight % to 0. 175 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from second alkali source and 0 weight % to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source;
Step 2: Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring;
Step 3: Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition,
Step 4:Packing the concentrated liquid fertilizer composition.
16. A process for preparation of concentrated liquid fertilizer composition for foliar application as claimed in claim 2, comprising steps of:
Step 1: Reacting Metal source, first Alkali source, second alkali source, Ethylenediaminetetraacetic acid based chelating agent at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring, wherein 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen sources is derived from first alkali source; 0.075 to 0.35 weight % Nitrogen (N) with respective to total weight of Metal- Nitrogen- sources is derived from chelating agent source; Step 2: Addition of Emulsifier and excipients at temperature between 40 to 100 °C in water having solid concentration between 70% w/w to 95% w/w under stirring;
Step 3: Adjust the resulting solution pH between 4 to 7 to obtain a concentrated liquid fertilizer composition,
Step 4:Packing the concentrated liquid fertilizer composition.
17. The process for preparation of concentrated liquid fertilizer composition for foliar application as claimed in claim 15 and 16, wherein weight ratio of first alkali source to second alkali source is selected between 1:0 to 1: 1.
18. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein Metal source selected from Zinc Ash, Zinc Dust, Zinc Oxide, Zinc Carbonate, Zinc Carbonate Basic, Zinc Hydroxide, Zinc Chloride. Calcium Oxide, Calcium Carbonate, Calcium Hydroxide, Calcium Chloride, Manganese Oxide, Manganese Carbonate, Manganese Hydroxide, Manganese Chloride, Copper Ash, Copper Dust, Copper Oxide, Copper Carbonate, Copper Hydroxide, Copper Carbonate Basic, Copper Chloride, Copper Oxychloride. Magnesium Dust, Magnesium Ribbon, Magnesium Oxide, Magnesium Carbonate, Magnesium Hydroxide, Magnesium Carbonate Basic, Magnesium Chloride, Cobalt Ash, Cobalt Oxide, Cobalt Carbonate, Cobalt Hydroxide, Cobalt Carbonate Basic, Cobalt Chloride, Iron Sulphate, Iron Dust, Iron Red Oxide, Iron Y ellow Oxide, Iron Sulphate, Iron Carbonate, Iron Hydroxide, Iron Chloride, Molybdenum Oxide, Molybdenum Disulphide, Molybdenum Chloride, Boric Acid, Ammonium Molybdate, Sodium Molybdate, Potassium Molybdate, Ammonium Borate, Diammonium Octaborate, Boron Ethanolamine, Sodium Borate, Disodium Octaborate, Potassium Borate, Dipotassium Octaborate and combination thereof.
19. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein chelating agent selected from Ethylenediaminetetraacetic acid; ammonium Ethylenediaminetetraacetic acid; diammonium Ethylenediaminetetraacetic acid; sodium Ethylenediaminetetraacetic acid; disodium Ethylenediaminetetraacetic acid; potassium Ethylenediaminetetraacetic acid and dipotassium Ethylenediaminetetraacetic acid and combination thereof.
20. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein the first alkali source selected from Monoethanolamine, Diethanolamine, Triethanolamine and combination thereof.
21. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein the second alkali source selected from Ammonium Hydroxide, Liquor Ammonia, Ammonium Carbonate, Ammonium Chloride, Sodium Hydroxide, Sodium Carbonate, Sodium Chloride, Potassium Hydroxide, Potassium Carbonate, Potassium Chloride and combination thereof.
22. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein Emulsifier selected from Glycol, Glycerine, Ethylene glycol, Ethanolamine, Tween 80, Tween 20, Sorbitol, Propionic acid, Acetic acid and combination thereof .
23. The process for preparation of concentrated liquid fertilizer composition as claimed in claim 15, wherein excipients selected from preservative Benzoate and Formaldehyde.
PCT/IN2023/050676 2023-03-07 2023-07-10 Concentrated liquid fertilizer including nitrogen and chelated micronutrients for foliar application and preparation process thereof WO2024184904A1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108249994A (en) * 2018-02-14 2018-07-06 安徽辉隆集团五禾生态肥业有限公司 A great number of elements liquid Water soluble fertilizer containing Zn-ef ficiency and preparation method thereof
CN108440146A (en) * 2018-05-30 2018-08-24 云南云天化股份有限公司 A kind of full trophic function type suspension liquid fertilizer of high concentration and preparation method thereof
IN202121040874A (en) * 2021-09-09 2022-10-14

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108249994A (en) * 2018-02-14 2018-07-06 安徽辉隆集团五禾生态肥业有限公司 A great number of elements liquid Water soluble fertilizer containing Zn-ef ficiency and preparation method thereof
CN108440146A (en) * 2018-05-30 2018-08-24 云南云天化股份有限公司 A kind of full trophic function type suspension liquid fertilizer of high concentration and preparation method thereof
IN202121040874A (en) * 2021-09-09 2022-10-14

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