WO2013035106A1 - A process for manufacturing a composite fertilizer - Google Patents
A process for manufacturing a composite fertilizer Download PDFInfo
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- WO2013035106A1 WO2013035106A1 PCT/IN2012/000038 IN2012000038W WO2013035106A1 WO 2013035106 A1 WO2013035106 A1 WO 2013035106A1 IN 2012000038 W IN2012000038 W IN 2012000038W WO 2013035106 A1 WO2013035106 A1 WO 2013035106A1
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- Prior art keywords
- urea
- ammonium
- phosphate
- minutes
- composite fertilizer
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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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
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
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- 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
- C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
A method for manufacturing a customized, compound or composite fertilizer, which uses high shear mixing to combine two or more active ingredients, to provide NK, NS, PK, PS, NP, NKS, NPK, NPS, and NPKS fertilizer or a fortified composite fertilizer having micronutrients like Zn, Mg, Ca, B, and the like. The method is simple and cost-effective and provides a granular fertilizer having uniform granule composition.
Description
A PROCESS FOR MANUFACTURING A COMPOSITE
FERTILIZER
FIELD OF DISCLOSURE
The present disclosure relates to a process for manufacturing a composite fertilizer. BACKGROUND
Composite fertilizers contain two or more primary nutrients and are produced by chemical reactions between the raw materials or intermediates; typically in the form of granules having a uniform granule composition. Generally, composite fertilizers comprise nitrogen (N), phosphorus (P), potassium (K), boron (B), magnesium (Mg), and sulfur (S) nutrients. These composite fertilizers are difficult to define because of the infinite possible ranges of nutrient ratios and the numerous manufacturing processes thereof. Generally, these fertilizers are manufactured by way of: i) mixed acid slurry process with digestion of rock phosphate, ii) phosphoric acid slurry process, and iii) agglomeration of solid raw materials.
Some of the typical methods for manufacturing composite fertilizers are disclosed in the following prior art.
US3993466 discloses a process for the production of a nitrogen-potassium, and phosphorus containing fertilizer having reduced chlorine and calcium content. Calcium- containing phosphate rock is first reacted with nitric acid to produce a mixture containing nitrogen, calcium, and phosphorus-containing solution. The mixture is then contacted with a potassium and ammonium ion-exchange resin so as to replace the potassium and ammonium ions with calcium ions. The calcium soaked resin is separated from the solution containing potassium, nitrogen and phosphorus and the solution is worked to yield a fertilizer.
US 4323386 discloses a method for manufacturing a NP or a NPK containing fertilizer from phosphate ore. The ore is subjected to digestion with nitric acid to remove calcium by crystallization and filtration thereof. The filtrate is then treated with sulfuric acid or sulfate to further reduce the calcium content. The filtrate having Ca/P ratio of 0.01 - 0.15 is subjected to neutralization with ammonia until the filtrate has an N/P2O5 ratio of 0.5 - 2. The neutralized filtrate is then sent through evaporation, prilling and granulation stages.
US 4398936 discloses a process for the preparation of granules of NPK fertilizer. The process comprises adding a solid potassium salt to a liquid melt or aqueous solution containing ammonium nitrate and ammonium phosphate, and granulating/prilling the resulting mixture. The potassium salt is in the form of particles having temperature between 5 - 40 °C and an average particles size of 55 microns with at most 1 % of particles over 150 microns. The granules so obtained are storage-stable.
The processes discussed in the prior art above require separate equipments for mixing, kneading, and granulating. Further, the processes are complex and require critical control of the process parameters. Also, typically, the raw materials are treated with an acid, thereby, generating large volumes of effluent whose disposal is a problem. Therefore, there is felt a need for a process to manufacture granular composite/customized fertilizer, which will overcome the above-listed drawbacks and which is simple, easy-to-control and cost-effective in terms of the capital costs and the operation costs.
OBJECTS OF THE INVENTION
An object of the present invention is to provide a simple process for manufacturing a customized, compound and composite fertilizer of NK, NS, PK, PS, NP, NKS, NPK, NPS, and NPKS.
Another object of the present invention is to provide a process for manufacturing a composite fertilizer which gives uniform granule composition.
One more object of the present invention is to provide a process for manufacturing a composite fertilizer which is cost-effective.
Yet one more object of the present invention is to provide a process for manufacturing a composite fertilizer which reduces CO emissions.
Still one more object of the present invention is to provide a process for manufacturing a composite fertilizer fortified with micronutrients such as zinc (Zn), magnesium (Mg), calcium (Ca), boron (B), and the like.
An additional object of the present invention is to provide a process for manufacturing a composite fertilizer that meets the Fertilizer Control Order (FCO) specifications.
SUMMARY
The present invention discloses a simple process for manufacturing a composite fertilizer as per the Fertilizer Control Order (FCO) specifications.
In accordance with the present invention, there is provided a process for manufacturing a composite fertilizer, said process comprising the steps of:
■ conglomerating active ingredients in a mixing device by agitating at a speed between 200 - 6500 rpm for a duration between 0.5 - 15 minutes, to obtain a heterogeneous mass;
■ homogenizing said heterogeneous mass by imparting high shear mixing in the mixing device at a speed between 2000 - 6500 rpm for a duration between 2 - 15 minutes, to obtain a homogenous mass;
■ blending said homogenous mass by adding at least one binding material in an amount in the range of 0.1 - 5 % of the homogenous mass, to obtain a blended mass;
■ granulating said blended mass in the mixing device by slow agitating at a speed between 200 - 1000 rpm for a duration between 1 - 5 minutes, to obtain uniform granules; and
■ drying said granules at a temperature between 80 - 120 °C for a duration between 2 - 30 minutes to obtain composite fertilizer granules having moisture content below 2 %.
Typically, in accordance with the present invention, said active ingredients are selected from a group of materials consisting of urea, oxamide, ammonium nitrate, ammonium sulfate, ammonium nitrate sulphate, ammonium chloride, ammonium polyphosphate, diammonium phosphate, calcium ammonium nitrate, calcium nitrate, potassium chloride, potassium nitrate, potassium sulfate, potassium hydroxide, zinc oxide, zinc nitrate, zinc sulfate, zinc ash, zinc EDTA, sulfur, Muriate of Potash, copper sulphate, bentonite, rock phosphate, mono amino phosphate, dolomite, felspar, kaolin, talc, meta kaolinite, montmorillnite, alum, gypsum, magnesite, kainite, folibore, kernite, rasorite, borax, calcium borate, colemanite, magnesium borate, boric acid, potassium polyborate, ammonia, phosphoric acid, triple sulfur phosphate, single super phosphate, calcium cyanamide, ammonium thiosulphate, oil, resin, phospholipid, ester, poly(ethyleneoxide)lauryl alcohol, triazine, urea-formaldehyde, methylene-urea, isobutylidene diurea, urea crotonaldehyde, octanol, decanol, cosanol, n-triacotanol, N-m- tolylphthalamic acid, N-(n-butyl) thiophosphoric triamide, dicyandiamide, phenyl phosphorodiamidate, 2, 4 - D(amine) glyphosate, glufosinate, quinine, hetrocyclic sulfur, humectant, biopotash, biophos, calcium, biozinc, biosulfur, biomagnesium, seed weed, seed weed extract, plant hormones, neem, neem oil, deoiled neem cake, and the like.
Preferably, in accordance with the present invention, the process includes the step of using water and at least one set of active ingredients selected from urea-ammonium nitrate, urea-ammonium phosphate, urea-ammonium sulphate and urea-phosphate.
Typically, in accordance with the present invention, said binding material is selected from a group of materials consisting of polyvinyl alcohol, carboxymethylcellulose, agar- agar, molasses, PVDC copolymers, sodium acrylate, acrylamide, polyacrylamide, starch, modified starches, polyethylene glycols, glutaraldehdye, polyolefin, urea formaldehyde resin and sulfur.
Preferably, in accordance with the present invention, the process includes the step of powdering the active ingredients prior to conglomerating in the mixing device.
Typically, in accordance with the present invention, the process includes the step of enhancing the surface of said composite fertilizer granules by treatment with acid, base, powder or gases.
Alternatively, in accordance with the present invention, the process includes the step of reducing the moisture content of said composite fertilizer granules by reacting with nitric acid and subsequently neutralizing the acid treated fertilizer granules with ammonia.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
The invention will now be described with the help of the accompanying drawings, in which:
FIGURE 1 illustrates the DSC-TGA analysis of urea (a), the NPK composite fertilizer in the pre-granulation stage (b), and the NPK composite fertilizer in the post-granulation stage (c), in accordance with the present invention;
FIGURE 2 illustrates the DSC-TGA analysis of diammonium phosphate (a), urea (b), mixture of diammonium phosphate and urea mixed for 5 minutes (d), granulated and dried sample of diammonium phosphate and urea having moisture content of 0.58% (c),
and granulated sample of diammonium phosphate and urea having moisture content of 0.02% (e), in accordance with the present invention; and
FIGURE 3 illustrates the DSC-TGA analysis of sulfur powder (a), Muriate of Potash (b), bentonite (c), diammonium phosphate (d), mixture of the afore-mentioned raw materials mixed and granulated with water and having a moisture content of 3.6 % (e), and the granules further dried to a moisture content of 0.2% (f), in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention envisages a simple method for manufacturing a customized, compound and composite fertilizer of NK, NS, PK, PS, NP, NKS, NPK, NPS, and NPKS. Further, the process of the present invention can be used to obtain a fortified composite fertilizer having micronutrients like Zn, Mg, Ca, B, and the like. The process of the present invention uses high shear mixing to combine two or more raw materials. Functional additives such as neem oil, deoiled neem cake, agrochemicals including plant growth promoters, pesticides, nitrification inhibitors and urease inhibitors, can also be added. Further, an organic supplement selected from humectant, biopotash, biophos, calcium, biozinc, biosulfur, biomagnesium, seed weed, seed weed extract, plant hormones, neem, neem oil, and deoiled neem cake, can also be added. High shear mixing is caused by a velocity gradient within the material, where, when two or more raw materials having different particle characteristics are subjected to high shear mixing the particles break into primary particle size. Also, inter and intra particle collision between different particles as well as the wall of the mixing device produces energy which is transferred to the particles as kinetic energy. The kinetic energy helps in breaking down the compounds and thereby homogenizes the mixture to give a uniform composition. This process is also called as dispersive mixing. Further, the high shear mixing provides intense friction between the particles increasing temperature on the surface of the particles. This increase in temperature results in: removal of moisture, homogenization,
melting of the surface particles, particularly particles having a low melting point, and a consequent coating of the melted particles on the surface of the solid particles, agglomeration of solid particles around the melted particles, and induced physical and chemical reactions in the surface particles.
The process of the present invention comprises an initial step of conglomerating the raw materials in a mixing device by agitating at a speed between 200 - 6500 rpm for a duration between 0.5 - 15 minutes to obtain a heterogeneous mass, and a prime step of homogenizing the heterogeneous mass by imparting high shear mixing in the mixing device at a speed between 2000 - 6500 rpm for a duration between 2 - 15 minutes to obtain a homogenous mass. The raw materials can be pre-powdered prior to combining in the mixing device. The homogenous mass, so obtained, is blended by adding one or more binding materials selected from polyvinyl alcohol, carboxymethylcellulose, agar-agar, molasses, PVDC copolymers, sodium acrylate, acrylamide, polyacrylamide, starch, modified starches, polyethylene glycols, glutaraldehdye, polyolefin, urea formaldehyde resin and sulfur. The quantity of binding material used is in the range of 0.01 - 4 % of the homogenous mass. The blended mass is granulated in the mixing device by agitating at a reduced speed of 200 - 1000 rpm for a duration between 1 - 5 minutes to obtain granules having uniform composition. These granules are finally dried at a temperature between 80 - 120 °C for a duration between 2 - 30 minutes to obtain composite fertilizer granules having moisture content below 2 %.
The mixing device so chosen must be suitable for dry mixing as well as wet mixing, and must provide macro-mixing and micro-mixing. Further, in the process of the present invention, mixing, agglomeration, kneading, and granulation is done in the single- equipment. As it is known that the rate of particle-to-particle collision or particle-to-wall collision and the impact thereof is dependent on the speed of the agitator, hence the agitator speed decides the amount of energy that will be transferred to the particles. It is also observed that when the mixer pan is rotatable an additional energy is added to the
particles. The present invention, therefore, explores the use of mixing devices manufactured by Maschinenfabrik Gustav Eirich GmbH (Germany), which provide rotatable mixer pans. The Eirich mixers are dynamic mixers which are widely used as high shear mixers to provide homogenization. An added benefit of using the Eirich mixer is that the rotor speed is controllable between a wide range of 2 - 40 m/s. Particularly, the present invention explores the use of a R-type Eirich Intensive Mixer for the manufacturing of the composite fertilizer. This mixer prevents any demixing effect and provides complete circulation of the mixer contents in every pan rotation. The Eirich Intensive Mixer comprises: inclined, rotating mixing pan, stationary bottom/wall scraper, and a fast-turning rotor positioned eccentrically at the centre of the pan.
The active ingredients are selected from a wide range including: urea ((NH2)2CO), oxamide (H2NCOC)NH2), ammonium nitrate (NH4NO3), ammonium sulfate ((NH4)2SO4), ammonium nitrate sulphate, ammonium chloride (NH4CI), ammonium polyphosphate (NH4P03)n, diammonium phosphate (NH4)2HPO4, calcium ammonium nitrate (CaNH4(N03)3), calcium nitrate (Ca(NO3)2, potassium chloride (KCl), potassium nitrate (KN03), potassium sulfate (K2S04), potassium hydroxide (KOH), zinc oxide (ZnO), zinc nitrate (Zn(N03)2), zinc sulfate (ZnS04), zinc ash, zinc EDTA, sulfur (S), Muriate of Potash (MOP), copper sulphate (CuSO4), bentonite, rock phosphate, mono amino phosphate, dolomite, felspar, kaolin, talc, meta kaolinite, montmorillnite, alum, gypsum, magnesite, kainite, folibore, kemite (Na2B O7.4H2O), rasorite (Na2B4O7.10H2O), borax (Na2B4O7.10H2O), calcium borate (Ca2B6Ou.5H2O), colemanite (Ca2B6On.5H2O), magnesium borate, boric acid, potassium polyborate, ammonia (NH3), phosphoric acid (H3PO ), triple sulfur phosphate (TSP), single super phosphate (SSP), calcium cyanamide (CaCN2), sulfur, and ammonium thiosulphate. Typically, a low melting point ingredient is incorporated to enhance the homogenization. For example: i) when urea having a melting point of 128 °C is combined with zinc nitrate having a melting point of 36 °C or zinc sulfate having a melting point of 100 °C, under high shear for 10 - 12 minutes in the Eirich Intensive Mixer, the material converts from
solid to a homogenized semi-liquid state; ii) when diammonium phosphate, urea, muriate of potash and zinc sulfate are combined under high shear in the Eirich Intensive Mixer, a semi-liquid flowable paste is obtained. For granulation, water is used with a set of compounds selected from urea-ammonium nitrate, urea-ammonium phosphate, urea- ammonium sulphate and urea-phosphate. A slow-release property is imparted by adding an ingredient selected from oil, resin, phospholipid, sulfur, ester, poly(ethyleneoxide)lauryl alcohol, triazine, urea-formaldehyde, methylene-urea, isobutylidene diurea (IBDU) and urea crotonaldehyde. Additionally, an additive selected from octanol, decanol, cosanol, n-triacotanol, N-m-tolylphthalamic acid can be added. Also, an urease inhibitor selected from N-(n-butyl) thiophosphoric triamide (NBPT), dicyandiamide (DCD), and phenyl phosphorodiamidate (PPD) can be added. Further, a compound selected from quinine and hetrocyclic sulfur can be added. An herbicide/pesticide selected from 2, 4 - D (amine) glyphosate, glufosinate, etc., can be added to enhance the fertilizer quality. Thus, a variety of compound and composite fertilizers, for both foliar and soil applications, can be formulated using the principle of the present invention.
The composite fertilizer granules are typically dried to a moisture content below 2% prior to packaging. To further reduce the moisture content, the composite fertilizer granules may be reacted with nitric acid. The reaction is exothermic and effects in release of the moisture due to the heat generated. The acid treated granules are then neutralized with ammonia to balance the pH. Further, surface of the composite fertilizer granules can be enhanced by treatment with an acid, a base, a powder or a gas. The process of the present invention can also be used to combine liquid raw materials such as ammonia and phosphoric acid. Where, when these liquids are mixed under high shear condition at an elevated temperature of 85 - 95 °C for 5 - 10 minutes, a homogenous mixture with increased viscosity is obtained. This mixture is then cooled and subsequently granulated under controlled conditions.
The process of the present invention is a batch process; however, the process can be advanced as a continuous process. The fertilizer granules from the mixing device can be received in a fixed tunnel drier adapted to convey the granules on a perforated wire mesh to reduce the moisture content between 1 - 2 %. The dried, hardened granules can be passed through a vibrating sieving device to separate the granules as per size. Additionally, the fertilizer granules can be further dried in a drum drier to reduce the moisture content to 0.2 % or the granules can be provided a surface treatment to enhance its properties. The NPK fertilizer granules obtained in accordance with the process of the present invention meet the specification and norms of the Fertilizer Control Order (FCO).
TEST RESULTS
The invention will now be described with respect to the following examples and the accompanying drawings, which do not limit the scope and ambit of the invention in anyway and only exemplify the invention.
EXAMPLE 1:
A composite fertilizer comprising 90 % elemental sulfur, 5 % bentonite, and 4.5 % dolomite with minor amounts of additives such as polyvinyl alcohol was prepared using the process of the present invention. Primarily, the raw materials including 0.9 kg elemental sulfur, 0.5 kg bentonite clay, and 0.45 kg dolomite, were added in a sequence, in a mixing device. Particularly, a pilot-scale Intensive mixer (Type R) manufactured by Maschinenfabrik Gustav Eirich GmbH (Germany) was used for this experiment. This particular type of mixer comprises an inclined, rotating mixing pan, a bottom scraper, and a fast-turning rotor whose speed can be varied between 2 - 40 m/s; these attributes made the Eirich Intensive Mixer most suitable for this application. The mixture of raw materials was homogenized for 2 minutes at an agitator speed of 2000 rpm. 6 gm of polyvinyl alcohol (PVA) was dissolved in 200 ml of water and the pH of the solution was adjusted to 8 by adding ammonia solution. This solution was added to the homogenized mixture in the Eirich Intensive Mixer and the resultant mixture was agitated for 2 minutes
at a speed of 2000 rpm. After two minutes, the agitator speed was reduced to 760 rpm and the mixture was agitated at this speed for 2 minutes to allow granulation. The granulated product was removed from the Eirich Intensive Mixer and loaded in a pan drier. Drying was done by means of hot air at 95 °C for 4 minutes. The resulting composite fertilizer granules had a moisture content of 0.2 %.
EXAMPLE 2:
A composite fertilizer comprising diammonium phosphate and urea with minor amounts of additives such as polyvinyl alcohol was prepared using the process of the present invention. The raw materials including 1.641 kg of diammonium phosphate and 1 kg of urea, were added in a sequence, in a pilot-scale Intensive Eirich Mixer (Type R). The raw materials were homogenized by agitating at a speed of 2500 rpm for 5 minutes. 8 gm of polyvinyl alcohol was dissolved in 50 ml of water and the pH of the solution was adjusted to 8.5 by adding ammonia solution. This solution was added to the homogenized raw materials and the resultant mixture was again agitated. The agitator speed was reduced to 450 rpm for 2 minutes to allow granulation. The mixing device was stopped and the granulated product there from was loaded on a drier. Drying was done at 85 °C for 4 minutes in a pan drier by means of hot air to obtain the composite fertilizer.
EXAMPLE 3:
A customized composite nitrogen-phosphorus-potassium fertilizer comprising diammonium phosphate, urea, bentonite, and sulfur was made using the process of the present invention. The raw materials including 0.3423 kg of diammonium phosphate, 0.2079 kg of urea, 0.05 kg of bentonite, and 0.04 kg of sulfur, were added in a sequence, in a pilot-scale Enrich Intensive Mixer (Type R). The raw materials were homogenized for 2 minutes at a speed of 6000 rpm. 0.16 gm of zinc sulfate and 0.165 kg of dolomite was added to the homogenous mixture and the resultant mixture was agitated for 2 minutes at 6000 rpm. To this mixture, 0.2625 kg of Muriate of Potash (MOP) was added and the resultant mixture was agitated for 3 minutes at 6000 rpm. 6 gm of polyvinyl
alcohol was dissolved in 25 ml of water and pH of the solution was adjusted to 8.5 by adding ammonia solution. The agitator speed was reduced to 450 rpm for 2 minutes and the mixture was allowed to granulate. The granulated product was dried by means of hot air at 95 °C in a pan drier for 4 minutes. The composite fertilizer granules so obtained had a moisture content of 0.2 %.
EXAMPLE 4:
A water-soluble grade nitrogen-phosphorus-potassium composite fertilizer comprising potassium nitrate, mono amino phosphate, potassium sulfate, and urea, was made using the process of the present invention. The raw materials including 0.440 kg of potassium nitrate, 0.488 kg of mono amino phosphate, 0.209 kg of potassium sulfate, and 0.3750 kg of urea, were added in a sequence, in a pilot-scale Eirich Intensive Mixer (Type R). The raw materials were conglomerated by agitating the mixture at a speed of 3500 rpm for 3 minutes. The mixture was then homogenized by mixing at a speed of 5500 rpm for 3 minutes. 6 gm of polyvinyl alcohol was dissolved in 40 ml of water and pH of the solution was adjusted to 8.5 by adding ammonia solution. This solution was added to the homogenized mixture and the resultant mixture was agitated at 3500 rpm for 2 minutes. The agitator speed was reduced to 750 rpm for 2 minutes to allow granulation. The granulated product was dried by passing hot air at 80 °C in a pan drier for 3 minutes. The composite fertilizer thus obtained had a moisture content of 0.05 %.
EXAMPLE 5:
A sulfur bentonite composite fertilizer was prepared using the process of the present invention. The raw materials including 346 kg elemental sulfur, 8.75 kg dolomite and 26.65 kg of bentonite clay, were added in a sequence, in an industrial-scale Eirich RV15 Intensive Mixer. The raw materials were mixed at a speed of 4500 rpm for 5 minutes. 30 gm of polyvinyl alcohol was dissolved in 25 liters of water and the pH of the solution was adjusted to 8.5. This solution was added to the homogenized mixture. The agitator speed was reduced to 750 rpm for 2 minutes to allow granulation. After granulation, the
product was conveyed to a drier where the granules where dried by means of hot air at 90 °C for 15 minutes. The composite fertilizer so obtained had a moisture content of 0.2%. The fertilizer granules, after sieving, were sent for packaging. Field trial showed a greener, healthier and faster growth when the sulfur bentonite fertilizer of EXAMPLE 5, prepared in accordance with the present invention, was used.
EXAMPLE 6:
A nitrogen-phosphorus-potassium composite fertilizer was prepared using the process of the present invention. The raw materials including 103 kg of powdered diammonium phosphate, 63 kg of urea, 5 kg of zinc sulfate, 27.3 kg of bentonite, 10 kg of sulfur, and 20 kg of dolomite, were added in a sequence, in an industrial-scale Eirich RV15 Intensive Mixer. The raw materials were agitated at a speed of 4500 rpm for 5 minutes. To this mixture, 90 kg of muriate of potash was added and the resultant mixture was further agitated for 4 minutes at the same speed. 30 gm of polyvinyl alcohol and 12 gm of carboxymethylcellulose were dissolved in 6 liters of water, and the pH of the solution was adjusted to 8.5. This solution was mixed in the homogenized mixture. The agitator speed was reduced to 450 rpm for 3 minutes to allow granulation. The granulated product was then dried in a drier by means of hot air at 85 °C for 30 minutes. The composite fertilizer granules so obtained had a moisture content of 0.2%. After passing through a sieve, the fertilizer was sent for packaging.
The DSC-TGA analysis of a plain urea sample, the DSC-TGA analysis of this particular fertilizer sample (example 6) in the pre-granulation stage and the DSC-TGA analysis of this particular fertilizer sample (example 6) in the post-granulation stage is shown in FIGURE 1 (a), FIGURE 1(b) and FIGURE 1(c) respectively.
EXAMPLE 7:
A water-soluble grade, nitrogen-phosphorus-potassium composite fertilizer was prepared using the process of the present invention. The raw materials including 83 kg potassium
nitrate, 93.4 kg of mono amino phosphate, 71 kg of urea, 38.1 kg of potassium sulfate, were added in a sequence, in an industrial-scale Eirich RV15 Intensive Mixer. The raw materials were agitated at a speed of 6000 rpm for 5 minutes. 30 gm of polyvinyl alcohol and 10 gm of carboxymethylcellulose were dissolved in 5 liters of water. This solution was added to the homogenized raw materials and the resulting mixture was agitated for 1 minute at the same speed. The agitator speed was reduced to 450 rpm for 4 minutes to allow granulation. The granulated product was dried in a pan drier by means of hot air. The composite fertilizer so obtained had a moisture content of 0.05%.
EXAMPLE 8:
A composite fertilizer comprising urea and diammonium phosphate was manufactured by using the process of the present invention. A DSC-TGA analysis was performed for the raw materials diammonium phosphate (as shown in Fig. 2(a)) and urea (as shown in Fig. 2(b)). The raw materials were mixed for 5 minutes and a DSC-TGA analysis was performed on the resultant sample (sample B) (as shown in Fig. 2(d)). The sample B was further mixed, granulated and dried to a moisture level of 0.58 % to obtain the sample A. A DSC-TGA analysis of the sample A was performed, which is illustrated in Fig. 2(c). The sample A was further dried to obtain a sample C having a moisture content of 0.02% The DSC-TGA analysis of the sample C is illustrated in Fig. 2(e).
EXAMPLE 9:
A composite fertilizer comprising diammonium phosphate, muriate of potash (MOP), elemental sulfur, bentonite clay, and urea was manufactured by using the process of the present invention. A DSC-TGA analysis was performed for the raw materials: diammonium phosphate (as shown in Fig. 3(d)), MOP (as shown in Fig. 3(b)), sulfur powder (as shown in Fig. 3(a)), bentonite clay (as shown in Fig. 3(c)) and urea (as shown in Fig. 2(b)). The afore-mentioned raw materials were mixed in a ratio of 15:15:15:0.05:7 (NPKZNS) and the mixture was granulated and dried to a moisture level of 3.6% to obtain the sample E. A DSC-TGA analysis was performed on the sample E, which is
illustrated in Fig. 3(e). The sample E was further dried to a moisture level of 0.2 % to obtain the sample F. A DSC-TGA analysis of the sample F was performed, which is illustrated in Fig. 3(f). Field trial showed a greener, more even and faster growth when the composite fertilizer of EXAMPLE 9, prepared in accordance with the present invention, was used.
EXAMPLE 10:
A superior-grade neem coated fertilizer was prepared using the process of the present invention. The raw materials comprising 250 Kg Urea and 200 gm dried neem cake were combined and stirred in the Eirich mixer at low RPM of 250 rpm to retain the shape and size of the urea prill. The stirring speed was subsequently increased to 400 rpm for 3 minutes to facilitate the removal of any moisture generated due to the centrifugal force. Neem oil emulsion was prepared by mixing 0.205 It. of neem oil and same amount of water and adding ammonia solution and emulsifier containing additive such as PVA 3 % to the mixture. The neem oil emulsion was combined in the Eirich Mixer and the resultant mixture was mixed at 400 rpm for 2 minutes for homogenization and uniform coating/adsorption/absorption. The resulting material was dried and subsequently packed. Field trial showed a greener, healthier and faster growth when the superior-grade neem coated fertilizer of EXAMPLE 10, prepared in accordance with the present invention, was used.
EXAMPLE 11:
A superior-grade neem coated fertilizer was prepared using the process of the present invention. The raw materials comprising 250 kg urea was added to the Eirich mixer and the agitator speed was gradually increased to 6000 rpm with pan in counter-clockwise motion for 10 minutes to obtain a fine powder. To this powder, 200 gm of dried neem cake powder was added and the mixture was further agitated for 3 minutes. A neem oil emulsion prepared by pre-dissolving 0.205 It. neem oil and same amount of water with few drops of ammonia solution and 10 It. of water containing 5 % PVA was added to the
mixer. The agitator speed was reduced to 250 rpm for 5 minutes to facilitate granulation. The granules were dried and subsequently packed.
TECHNICAL ADVANTAGES
A process for manufacturing a composite fertilizer by homogenizing the raw materials with high shear mixing, as described in the present invention has several technical advantages including but not limited to the realization of: the process of the present invention is simple and cost-effective, gives uniform granule composition, reduces C02 emissions, and provides a NPK composite granule fertilizer that meets the Fertilizer Control Order (FCO) specifications.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the invention, unless there is a statement in the specification specific to the contrary. Wherever a range of values is specified, a value up to 10% below and above the lowest and highest numerical value respectively, of the specified range, is included in the scope of the invention.
In view of the wide variety of embodiments to which the principles of the present invention can be applied, it should be understood that the illustrated embodiments are exemplary only. While considerable emphasis has been placed herein on the particular features of this invention, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiments without departing from the principle of the invention. These and other modifications in the nature of the invention or the preferred embodiments will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation.
Claims
1. A process for manufacturing a composite fertilizer, said process comprising the steps of:
■ conglomerating active ingredients in a mixing device by agitating at a speed between 200 - 6500 rpm for a duration between 0.5 - 15 minutes, to obtain a heterogeneous mass;
■ homogenizing said heterogeneous mass by imparting high shear mixing in the mixing device at a speed between 2000 - 6500 rpm for a duration between 2 - 15 minutes, to obtain a homogenous mass;
■ blending said homogenous mass by adding at least one binding material in an amount in the range of 0.1 - 5 % of the homogenous mass, to obtain a blended mass;
■ granulating said blended mass in the mixing device by slow agitating at a speed between 200 - 1000 rpm for a duration between 1 - 5 minutes, to obtain uniform granules; and
■ drying said granules at a temperature between 80 - 120 °C for a duration between 2 - 30 minutes to obtain composite fertilizer granules having moisture content below 2 %.
2. The process as claimed in claim 1, which includes the step of selecting said active ingredients from a group of materials consisting of urea, oxamide, ammonium nitrate, ammonium sulfate, ammonium nitrate sulphate, ammonium chloride, ammonium polyphosphate, diammonium phosphate, calcium ammonium nitrate, calcium nitrate, potassium chloride, potassium nitrate, potassium sulfate, potassium hydroxide, zinc oxide, zinc nitrate, zinc sulfate, zinc ash, zinc EDTA, sulfur, Muriate of Potash, copper sulphate, bentonite, rock phosphate, mono amino phosphate, dolomite, felspar, kaolin, talc, meta kaolinite, montmorillnite, alum, gypsum, magnesite, kainite, folibore, kernite, rasorite, borax, calcium borate, colemanite, magnesium borate, boric acid, potassium polyborate, ammonia, phosphoric acid, triple sulfur phosphate, single super phosphate, calcium cyanamide, ammonium thiosulphate, oil, resin, phospholipid, ester, poly(ethyleneoxide)lauryl alcohol, triazine, urea-formaldehyde, methylene-urea, isobutylidene diurea, urea crotonaldehyde, octanol, decanol, cosanol, n- triacotanol, N-m-tolylphthalamic acid, N-(n-butyl) thiophosphoric triamide, dicyandiamide, phenyl phosphorodiamidate, 2, 4 - D(amine) glyphosate, glufosinate, quinine, hetrocyclic sulfur, humectant, biopotash, biophos, calcium, biozinc, biosulfur, biomagnesium, seed weed, seed weed extract, plant hormones, neem, neem oil, deoiled neem cake, and the like.
3. The process as claimed in claim 2, which includes the step of using water and at least one set of active ingredients selected from urea-ammonium nitrate, urea- ammonium phosphate, urea-ammonium sulphate and urea-phosphate.
4. The process as claimed in claim 1, which includes the step of selecting said binding material from a group of materials consisting of polyvinyl alcohol, carboxymethylcellulose, agar-agar, molasses, PVDC copolymers, sodium acrylate, acrylamide, polyacrylamide, starch, modified starches, polyethylene glycols, glutaraldehdye, polyolefin, urea formaldehyde resin and sulfur.
5. The process as claimed in claim 1, which includes the step of powdering the active ingredients prior to conglomerating in the mixing device.
6. The process as claimed in claim 1, which includes the step of enhancing the surface of said composite fertilizer granules by treatment with acid, base, powder or gases.
7. The process as claimed in claim 1, which includes the step of reducing the moisture content of said composite fertilizer granules by reacting with nitric acid.
8. The process as claimed in claim 7, which includes the step of neutralizing the acid treated fertilizer granules with ammonia.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IN2498/MUM/2011 | 2011-09-07 | ||
| IN2498MU2011 | 2011-09-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2013035106A1 true WO2013035106A1 (en) | 2013-03-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IN2012/000038 WO2013035106A1 (en) | 2011-09-07 | 2012-01-13 | A process for manufacturing a composite fertilizer |
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| Country | Link |
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| WO (1) | WO2013035106A1 (en) |
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| CN103193549A (en) * | 2013-05-05 | 2013-07-10 | 付增传 | Degradable resin envelop slow-control fertilizer-releasing production process |
| CN103319256A (en) * | 2013-06-29 | 2013-09-25 | 四川省乐山市福华通达农药科技有限公司 | Glyphosate-dicamba mixed preparation and preparation method thereof |
| CN103351004A (en) * | 2013-06-19 | 2013-10-16 | 安徽省农望农业科技开发有限公司 | Monohydrate sodium zinc decaborate and preparation method therefor |
| CN103833468A (en) * | 2014-03-06 | 2014-06-04 | 王俊科 | Nitrogen fertilizer |
| CN104072311A (en) * | 2014-07-21 | 2014-10-01 | 方秀琴 | Compound fertilizer for vegetables |
| CN104140332A (en) * | 2014-08-08 | 2014-11-12 | 成都新柯力化工科技有限公司 | Water-soluble fertilizer synergist additive and preparation method thereof |
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| DE102015122070A1 (en) * | 2015-12-17 | 2017-06-22 | Thyssenkrupp Ag | Urea-containing fertilizers and process for their preparation |
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| CN104072311A (en) * | 2014-07-21 | 2014-10-01 | 方秀琴 | Compound fertilizer for vegetables |
| CN104140332A (en) * | 2014-08-08 | 2014-11-12 | 成都新柯力化工科技有限公司 | Water-soluble fertilizer synergist additive and preparation method thereof |
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