Title of Invention

A NOVEL GRANULAR NUTRIENT COATED NITROGENOUS FERTILIZER AND A METHOD TO PRODUCE THE SAME

Abstract The granular coated fertilizers offer nutrients at a controlled rate to the plants. However, there is a growing need for supplying the required growth regulating hormones etc., along with metal ions as micro nutrients through an integrated granular coated fertilizer. The invention is related to the process of coating the granulated nitrogenous fertilizer with the aqueous extract of Gracilaria edulis, a sea weed, in presence of additives such as gypsum and a polymeric material like aniline black as a protective cover for the inner core which is a nitrogenous fertilizer like urea. The outer layer contains the nutrients from the extract. The polymeric coating prevents the absorption of water by the inner core of nitrogenous fertilizer while the gypsum provides the medium that absorbs any moisture left in addition to calcium. The product provides plants with enough nitrogenous fertilizer along with other nutrients. The yield of a number of crops has been found to increase substantially by the application of this fertilizer.
Full Text



4. DESCRIPTION: 1. FIELD OF INVENTION:
The present invention relates to supplementing the nitrogenous granulated urea fertilizer with nutrients such as N, P, K and Mg, Ca, Fe, I, Cu, Al, Mn and Zn, plant growth hormone and alginic acid in the form of an aqueous extract of Gracilaria eduils (sea weed) through external coating and a method for the preparation of the granulated coated urea fertilizer.
More specifically, the present invention relates to the preparation of the extract of G. edulis, a sea weed and its coating on the granulated nitrogenous fertilizer, urea, along with such ingredients as gypsum and aniline black.
The nitrogenous granulated urea fertilizer is characterized for its ability, on application, to enhance the yield of plants such as brinjal, rice, wheat, beans, cotton, tobacco leaf, tomato, banana, potato, com, onion, okara, beet root, black gram and chillies. Further, the fertilizer-coated granules have shown increased number of root nodules, leaf area, content of chlorophyll a & b, xanthophylls, carbohydrate, total protein and lipid. Polyanilines can also serve as chelating agents to supply the metal ion nutrients effectively to the plants.
An outer coating of inorganic micronutrients on organic fertilizers has been used to release the core nutrient slowly. (US Pat. No: 5,849,060). Adhesive-coating on granules is known from US Pat No: 5,766,302. The US Pat.No: 5,733,355 relates to the introduction of bacteria through a suitable

carrier like zeolite, earth or greenstuff into the granules. Metal ions like Zn^'(Micronutriants) have been known to be introduced in the granules (U.S. Pat. No : 6,159,263). The US Pat No : 6,331,300 concerns with use of porous particles impregnated with various nutrients or micronutrients to effect their controlled release.
2. BACKGROUND OF INVENTION WITH REGARD TO THE DRAWBACK OF ASSOCIATED KNOWN ART:
The granular fertilizer, coated on the surface with a resin, sulfur etc., has found application as a controlled release fertilizer for many years. For instance, Japanese Patent Kokoku Publication numbers: 40-28927, 44-28457, 37-15382 and 42-13681 reveal the various coating materials and coating methods. Controlled or slow release fertilizers have been prepared according to Japanese patent publication number Sho-54-39298-B with an inner coating layer of wax and an outer layer of urethane resin. Granular fertilizer, coated with four layers of different resins, has been reported in US Pat. No: 7,018,440.
Description of materials and method of making effective controlled release fertilizers (100-200 days) is found in JP Sho-54-39298-B. Further references to coating by urethane and epoxy resins are found in US Pat. No. 3,264,089 and US Pat No: 3,264,088 respectively. Different techniques for making coated granular fertilizers are reported in Japanese Patent Kohyo Pubhcation Nos. 07-500560 & 1-500661. The wax coating prevents hygroscopic fertilizer products from adhering to each other. The dissolution rates of fertilizers have been different for different coating materials.
The preparation of a granular urea fertilizer coated with a thermosetting resin and a hydrophobic compound is reported in US Patent No. 6,231,633.

Further, production of biosolid granules coated with concentric layers has been reported in US Pat. No : 6, 841, 515. Outercoating of urea granules by clay containing sulphur has been described in US Patent No: HI, 085.
However, we have not come across a single patent that relates to the coating of a fertilizer on a granular fertilizer to supplement the nutrients. Further, there is a growing need for supplying the required growth regulating hormones etc., along with metal ions as micro nutrients through an integrated granular coated fertilizer.
The objective of the present invention is to provide a granular nitrogenous fertilizer coated with the nutritious aqueous extract of Gracilaria edulis that augments trace elements, N, P, K elements, alginic acid and humic acid, hormones etc., available from it.
3. OBJECTIVE OF THE INVENTION:
The objective of the present invention is related to the development of a method for coating the granulated nitrogenous fertilizer with supplementary nutrients of sea weed origin such as metal ions, plant-growth regulating hormones etc., gypsum and aniline black to obtain an integrated nutrient coated nitrogenous granulated fertilizer.
4. SUMMARY OF THE INVENTION:
The present fertilizer is a granular fertilizer coated with a material layer containing nutrients extracted from sea weed, Gracilaria edulis along with a dehydrating agent and a polymer.

The invention is as described below:
i) The granular coated fertilizer is coated with the contents of the aqueous extract of the sea weed, G. edulis, mixed with a dehydrating agent and a polymer that serves as a coating which prevents any interaction between the granules and moisture.
ii) The dehydrating agent referred to in (i) is gypsum.
iii) The polymer referred above in (i) is aniline black.
iv) The aqueous extract.

5. BRIEF DESCRIPTION OF ACCOMPANYING DRAWING:
Figure 1:
Figure 1 illustrates the washing tank set up. It consists of three tanks erected on the ground in series connected with each other. A pipline supplies water to tanks A and B. G.edulis (200 Kg) is kept in tank-1 (A) for the first wash with concentrated sulfuric acid (3 lit; 20 N). The washed materials are allowed to pass into tank-2 (B) for the subsequent washes with water. In tank B, two more water washes are given. The material is then led into tank-3(C), drained, removed and shade dried.
Figure 2:
The extractor employed in recovering the nutrients from the sea weed, G. edulis, is shown in figure 2. The arrangement has a steam generator (A) that produces steam for the extraction process. 250 ml of 5N sulfuric acid is sprayed on to the material kept in tank B for 30 minutes for further softening. Just before steam is passed, about 200 ml of 5N NaOH is added to make the material have a pH of 6.7-7.0. The steam flows through a connecting tube into the extractor tank, B, in which the thrice washed and softened G.edulis is taken. Steam, provides hot water or solvent extraction. The aqueous extract of G. edulis now enters the filter tank, C. The filter tank contains a wire mesh at the bottom that holds back the debris while clear extract emerges out into the collector tank, D.
Figure 3:
The figure shows the mixing and drying unit consisting of a separate mixer unit (A) and a drier unit (B).

The mixer unit contrains a feed inlet and a mixing chamber that has two axle rods rotating about the pivotal bottom. The feed contains the aqueous extract (20 liters), the additives (1 Kg of aniline black and 1 Kg of gypsum) and the nitrogenous granules (1000 Kg). The contents get mixed for 15 minutes at 30*^C. The coated ganules then flow into the drier drum (B). The granules are heated for about 30 minutes at 30-40°C. The final product is taken out and dried on a zinc metal sheet platform for 30 minutes.
6. DETAILED DESCRIPTION OF THE INVENTION : A. CORE:
The core of the granular fertilizer used in the present invention may be one of the conventional fertilizer granules such as N, P, K, Si, Mg, Ca, Mn, B, Fe & so on based for supplying nutrients to the cultivated crops. Typical examples include N-fertilizer such as urea, ammoium nitrate, ammonium magnesium nitrate, ammonium chloride, ammoniimi sulfate, ammonium phosphate, sodium nitrate, calcium nitrate, potassium nitrate, guanyl urea, phosphate fertilizer such as calcium superphosphate, humic acid P-fertilizer, magnesiimi superphosphate, ammonium polyphosphate, potassium meta phosphate, calcium meta phosphate, magnesium phosphate, ammonium sulfate phosphate; potash fertilizer such as KCl, K2SO4, K3PO4, silicate fertilizer such as calcium silicate, magnesium fertilizer such as MgS04 & MgCb; Ca fertilizer such as CaO, Ca(0H)2 of CaCOj, Mn fertilizer such as MnS04, Manganese sulfate magnesia and boron fertilizer such as boric acid and borates.
Typical examples include urea granules with diameter preferably in the range of 1-5 mm that is suitable for manufacture.

B. COATING INGREDIENTS:
The coating of the iimer core granules contains typically three ingredients, viz., i) A dehydrating moisture absorbing compound (ii) a bio fertilizer (extract of the sea-weed, G. edulis) and (iii) a coating material that protects the inner core and the outer coated nutrients.
The dehydrating agent should be a solid, capable of absorbing water readily and remain as a solid. It could have higher melting point above 50^C and can be one of the metal sulphates which can take up a lot of water of crystallisation.
Typical examples of dehydrating agents include gypsum, ammonium sulfates, magnesium sulfates or mixtures there of. Typical examples of Bio-fertilizer include aquous extract from sea weed (G. edulis).
Examples of coating material include a polymeric material that can effectively interact with the core as well as the bio-fertilizer.
Typical polymeric materials can include the polyaniline derivatives such as aniline black.
The amount of gypsum constitutes 0.1% by weight taking the weight of core urea as 100.
The amount of extract is in the range 2% . The ratio of extract: gypsum: urea granules is 2 : 0.1 : 100.

The water insoluble polymeric compound, aniline black, is used to the extent of 0.1% with the overall ratio of extract : gypsum : urea : polymer = 2:0.1 : 100:0.1.

C. PROCEDURE TO PREPARE THE EXTRACT FROM G. edulis:
Step 1 :
The dried G. edulis (200 Kg) is charged into the tank 1(A) of capacity 700 litres shown in figure 1. Enough water (500 litres) is added just sufficient to soak all the material. 3 litres of commercial concentrated sulfuric acid (25 N) is added with a view to soften it and stirred well. The contents are kept undisturbed for 6 to 8 hours. The acid is then drained out along with the impurities. The softened G.edulis is then forced into tank2 (B) of approximately the same size as that of tank 1. The material is washed with about 600 litres of water after keeping it for 30 minutes under stirred conditions. The process is repeated three times to remove the entire the acid. The material, finally, is removed into tank 3(C). The material is thoroughly drained, taken out and dried in open air.
Step 2:
The acid-treated and water washed G.eduUs material is then, fed into the extractor, shown in figure 2. The extractor tank B, holds the G.edulis that is softened. Now 250 ml of 5N H2SO4 is sprayed on to the material. It is kept for 15 minutes as such. About 200 ml of 5N KOH solution is added to the material and mixed so that the pH becomes 6.7 - 7.0. Steam generated in the steam generator A, is led into the tank B. The temperature is kept in the range of 25-30°C. The steam is passed for about 4 hours. The extract that collects at the bottom of the tank is about 4 litres. Thus, 20 litres can be collected per 1000 Kg of G.edulis.
The extract is then allowed to pass into the filter tank, C. It is filtered through the meshed filter kept at the bottom and goes into the collector tank, D.

D. PREPARATION OF THE COATED GRANULES:
The aqueous extract of G. edulis is employed in the coating of granular nitrogenous fertilizer along with other ingredients. The extract (20 Utres) was fed into the mixer, A (figure 3) along with 1000 Kg of urea granules, 1 Kg of aniline black and 1 Kg of gypsum. The granules of urea get mixed with the above ingrredients at ambient temperature (30-40^C) to give a paste-coated granular urea. The mixer, when switched on, mixes all the ingredients thoroughly to give uniformly coated granules within 15 minutes. The coated granules are then allowed to flow into the drier B, kept at 30°-40°C for 30 minutes. The dried granules are then removed and packed in polythene bags surrounded by gunny bags.
The mixing and drying processes could be accomplished vide an alternate procedure. About 20 litres of the extract is mixed with 1 Kg of aniline black to produce a paste. The urea granules (1000 Kg) are mixed with the above paste at room temperature (30-40^^C). The contents are then mixed with 1 Kg of gypsum to absorb the excess water on the coating. Drying is achieved by placing the granules in sun light to obtain the black granules of the product by spreading them on a zinc metal plate at ambient temperature (30-40°C).

7. EXAMPLES :
Example 1:
The available ingredients in the extract of G. edulis were evaluated. The results obtained are provided in table 1.


Example 2: ^ ^
The effect of the fertilizer on the chemical constituents of plants in terms of the increase in yield in comparision to the urea granules alone is shown in table 2.


Example 3:
The effect of the fertilizer on the yield of crops in relation to urea alone was evaluated and the results are presented below in table 3.
Table 3. The % increase in yield of various crops


V
The flowing examples illustrate the invention in further detail: The evaluation of the fertilizer was conducted as mentioned below :
The IR spectra of the raw materials were recorded in isolation and also for the coated finished fertilizer with urea in the central core. The spectra revealed the presence of carbonyl and N-H bands along with some H2O bands.
Example
The UV - visible spectra of the urea granules and the coated fertilizer were recorded in water as solvent. The peaks corresponded to the presence of urea, polyaniline, gypsum and the biofertilizer from G.edulis.





5. CLAIMS :
We claim:
1. A granular coated fertilizer comprising of a fertilizer central core and a coating of a mixture containing the aqueous extract from Gracilaria edulis, a dehydrating agent and a polymer that prevents the agglomeration of the moisture loving fertilizer core.
2. The granular coated fertilizer according to claim 1, wherein the core fertilizer in the granular form is any one of the diamides, salts containing N, Salts containing P, salts containing S, salts containing CI or Salts containing B.
3. The granular coated fertilizer according to claim 1 and 2 wherein the core fertilizer in the granular form is any one of the diamides.
4. The granular coated fertilizer according to claim 1, 2 and 3 wherein the core fertilizer in the granular form is urea.
5. The granular coated fertilizer according to claim 1 and 2 wherein the core fertilizer in the granular form is any one of the salts containing nitrogen.
6. The granular coated fertilizer according to claim 1, 2 and 5 wherein the core fertilizer in the granular form is an ammonium salt.
7. The granular coated fertilizer according to claim 1, 2, 5 and 6 wherein
the core fertilizer in the granular form is any one among ammonium
nitrate, ammonium chloride, ammonium sulfate or ammonium phosphate.
8. The granular coated fertilizer according to claim 1, 2 and 5 wherein the
core fertilizer in the granular form is any one of the salts containing
nitrate.

9. The granular coated fertilizer according to claim 1, 2, 5 and 8 wherein the core fertilizer in the granular form is any one among ammonium nitrate, sodium nitrate, calcium nitrate or potassium nitrate.
10. The granular coated fertilizer according to claim I and 2 wherein the core fertilizer in the granular form is any one of the salts containing phosphorous.

11. The granular coated fertilizer according to claim 1, 2 and 10 wherein the core fertilizer in the granular form is any one of the salts containing calcium superphosphate, humic acid phosporous fertilizer, magnesium superphosphate, ammonium polyphosphate, potassium meta phosphate, calcium meta phosphate and magnesium phosphate.
12. The granular coated fertilizer according to claim 1 and 2 wherein the core fertilizer in the granular form is any one of the salts containing sulphur.
13. The granular coated fertilizer according to claim 1, 2 and 12 wherein the core fertilizer in the granular form is any one of the salts containing sulfate.

14. The granular coated fertilizer according to claim 1,2, 12 and 13 wherein the core fertilizer in the granular form is any one of the salts containing potassium sulfate, magnesiimi sulphate or manganese sulfate.
15. The granular coated fertilizer according to claim 1 and 2 wherein the core fertilizer in the granular form is any one of the salts containing chloride.
16.The granular coated fertilizer according to claim 1, 2 and 15 wherein the
core fertilizer in the granular form is any one of the salts containing
potassium chloride and magnesium chloride. 17.The granular coated fertilizer according to claim 1 and 2 wherein the core
fertilizer in the granular form is any one of the salts containing borates or
boric acid.

18.The granular coated fertilizer according to claim 1, wherein the amount of the extract from the sea weed gracilaria edulis is from 2.0 to 2.5 parts by weight based on 100 parts by weight of the fertilizer central core.
19. The granular coated fertilizer according to claim 1 and 2 wherein the
dehydrating compound is any one from the group of metal sulphates and
mixtures thereof
20. The granular coated fertilizer according to claim 3, the dehydrating agent is gypsum.
21. The granular coated fertilizer according to claim 1 and claim 3 wherein the ratio of gypsum to urea inner core is 0.1:100.
22.The granular coated fertilizer according to claim 1 wherein the polymer
added is one that provides a coat which prevents interaction with
moisture by the core fertilizer. 23.According to claim 1 and 5, wherein the coated polymer is aniline black. 24.The granular coated fertilizer according to claims 1, 5 and 6 wherein the
ratio of the polymer to urea is 0.1:100. 25.A method for producing a granular coated fertilizer comprising of the
following steps:
a. Preparing a mixture of aqueous extract of the sea-weed, Gracilaria
edulis (200 Parts) and aniline black (Range: 5.0-15.0 parts).
b. The amount of aniline black according to step a of claim 10 is 10
parts per 200 parts of the G. edulis extract.
c. Adding gypsum (Range: 4.0 - 14.0 parts) to the mixture (210 parts)
mentioned in steps a and b to get a paste.
d. The amount of gypsum according to step c of claim 10 is 10 parts
per 210 parts of the mixture.
e. Coating the granular urea (1,00,000 parts) with tiie paste prepared
in step c and d (220 parts).

f. Heating the coated granular fertilizer (Temperature range is 30° -
40°C) and drying it.
g. The method according to step f of claim 10 wherein the
temperature is 35*^C.
h. Alternatively, combining steps a-b-c-d-e, mixing the granular urea with all ingredients such as aniline black, extract of G.edulis and gypsum collectively (Ratio of urea is extract : gypsum : aniUne black = 100 : 2 : 0.1 : 0.1) and heating the resultant pasted granules.



Documents:

1042-CHE-2007 AMENDED CLAIMS 19-07-2010.pdf

1042-CHE-2007 AMENDED PAGES OF SPECIFICATION 19-07-2010.pdf

1042-CHE-2007 EXAMINATION REPORT REPLY RECEIVED 19-07-2010.pdf

1042-che-2007 abstract.pdf

1042-che-2007 claims.pdf

1042-che-2007 correspondence-po.pdf

1042-che-2007 description (complete).pdf

1042-che-2007 drawings.pdf

1042-che-2007 form-18.pdf

1042-che-2007 form-9.pdf

1042-che-2007-correspondnece-others.pdf

1042-che-2007-description(provisional).pdf

1042-che-2007-form 1.pdf


Patent Number 243311
Indian Patent Application Number 1042/CHE/2007
PG Journal Number 41/2010
Publication Date 08-Oct-2010
Grant Date 05-Oct-2010
Date of Filing 17-May-2007
Name of Patentee V.ANANTHAPPAN
Applicant Address 19-51 SUNDAR NAGAR, 2ND STREET , THIRUNAGAR , MADURAI -625006
Inventors:
# Inventor's Name Inventor's Address
1 V.ANANTHAPPAN 19-51 SUNDAR NAGAR, 2ND STREET , THIRUNAGAR , MADURAI -625006
2 A.TAMARAICHELVAN 19-51 SUNDAR NAGAR, 2ND STREET , THIRUNAGAR , MADURAI -625006
PCT International Classification Number C05G01/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA