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A Process For Conversion Of Potassium Humate From Granules Into Water Soluble Gel

Abstract: A batch process, comprised of two steps, is described for converting potassium humate granules into water-soluble gel of potassium humate. The process employs seaweed extract, specially made - in a separate reaction vessel - from green algae and black brown algae and micronutrients mixture and yields gel form of potassium humate, which is easy to handle and is suitable for all types of end applications.

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Patent Information

Application #
Filing Date
01 December 2010
Publication Number
11/2011
Publication Type
INA
Invention Field
AGROCHEMICALS
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2017-12-18
Renewal Date

Applicants

1. SAMEER RAJAN PATHARE
112, ASHARAJ, GULMOHAR VIHAR COLONY, PIPELINE ROAD, NASHIK - 422 007 MAHARASHTRA, INDIA,

Inventors

1. SAMEER RAJAN PATHARE
112, ASHARAJ, GULMOHAR VIHAR COLONY, PIPELINE ROAD, NASHIK - 422 007 MAHARASHTRA, INDIA,

Claims

1. a process for converting granular potassium humate (10) in presence of seaweed extract (20) and micro nutrients (40) into its water-soluble gel form (50), said process comprising: (i) weighing 100 kg seaweed extract (20) and transferring to reactor (100) from sea weed extraction tank (110); (ii) maintaining sea weed extract (20) temperature between 45-50 degree C; (iii) weighing 30 kg potassium salt of humic acid (10) granules and transferring the weighed contents to said reactor (100); (iv) starting stirrer (120) of said reactor (100) and adjusting pH of the reaction mass to 7.5 to 9.0 to facilitate the reaction under shearing force resulting from said agitation involving chemical linkage of functional group of amino acid and protein hydrolysate with humic acid at said alkaline pH between 7.5 to 9. (v) adding 100 kg water (45) to said reaction mass; (vi). mixing for 3-4 hours and transferring resultant viscous solution (46) to another tank (130), by opening a bottom valve (105) on said reactor (100); (vii) after 24 hours from start of said batch, adding 10 litres of micronutrients mixture. and allowing gel formation to complete in 18-24 hours time in said holding tank (130) under ambient conditions and no stirring; (viii) yielding 160 kg of natural form of humic acid gel (50).

2. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its water-soluble gel form (50) as claimed in claim 1. wherein said seaweed extract (20) is prepared by a process comprising: (a) feeding 100 litres of water to a jacketed vessel (200). heated by hot oil circulating through jacket (210); (b). weighing 5 kg each of green algae (21) and black brown algae (22) and adding said weighed quantities to said jacketed vessel (200); (c) ensuring said both algae being properly wetted by starting agitator (205) of said jacketed vessel (200); (d) noting reaction mass temperature at 50 C and continuing heating till said reaction mass temperature reaches 90 degree C; (e) maintaining said reaction mass temperature, between 70 C to 90 C and continuing heating for 2-3 hours from time said temperature reached 90 degree C; (f) switching off circulation of heating oil and cooling resultant said reaction mass for 12 hours by circulating cooling water through limpet coil (220) of said jacketed vessel (200): (g) adding fermenting media dissolved in acetone to said cooled mass; (h). keeping said reaction mass for 12 hours under agitation from time adding said fermented media; (i) stopping said stirrer (205). filtering solution and collecting filtrate (20). measuring about 90 litres in yield.

3. A process for converting granular potassium humate (10)in presence of seaweed extract (20) and micronutrients mixture (40) into its water-soluble gel form (50) as claimed in claims 1 and 2: wherein said sea-weed extract (20) is completely soluble in water and has pH between 6.0 and 6.5.

4. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its water -soluble gel form as claimed in claims 1 and 2, wherein said sea-weed extract (20) has crude proteins between 3% and 6% by weight and amino acids of 17 to 20 types between 7% and 8% by weight.

5. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its watre -soluble gel form as substantially described herein above and illustrated in the accompanying drawings # 1 and # 2.

Specification

FORM 2
THE PATENT ACT 1970 (39 of 1970)
&
The Patents Rules, 2003 COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. TITLE OF THE INVENTION : "A PROCESS FOR CONVERSION OF POTASSIUM HUMATE FROM GRANULES INTO WATER-SOLUBLE GEL'
2. APPLICANT
(a) NAME : Sameer Rajan Pathare
(b) NATIONALITY : Indian
(c) ADDRESS : 112, ASHARAJ. GULMOHAR VIHAR
COLONY.PIPEUNE ROAD, NASH1K - 422 007 MAHARASHTRA, INDIA
3. PREAMBLE TO THE DESCRIPTION

COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it is to be performed

Title of the Invention:
A process for conversion of potassium humate from granules into water-soluble gel
Field of the Invention:
This invention relates to the field of use of potassium humate for soil conditioning applications and more particularly to the field of improving its handling and cost-to-benefit ratio for user-friendly end applications.
Background of the Invention:
There are a few prior works of art in the field, which are summarized to highlight their shortcomings and/or dissimilarities.
US Patent 5,248.327 - This prior work pertains to a process for manufacture of oxi-potassium humate. derived from oxidized coal, It is a two step process, involving first oxidation of coal in presence of oxygen gas steam, passed through a slurry of powdered coal and subsequently refluxing the oxidized coal in aqueous solution of potassium hydroxide. The present invention is vastly different from the cited work, for the former entails no oxidation, no coal and no refluxing of oxidized coal. No similarities are found in the cited work.
US Patent 3,306,714 - This prior work relates to removal of solubilized form of both humates and silica for recovery of metals. The prior work is different from the present

invention, for the former does not relate to conversion of potassium humate into gel form from granular form.
Commercial potassium humate is available in either liquid form of varying strengths or granular form. Liquid formulations of differing strengths cause confusion to farmers, who end up under-utilizing or over-utilizing the contents in the objective of improving yields per acre. Liquid formulations are available in 6/12/20/30% contents of humic acid, while powder form contains 80/85/90% by weight humic acid.
Objects of the Invention:
A primary object of the present invention is to produce in commercial quantities potassium humate in gel form that is easily soluble in water.
Another object of the present invention is to reduce the scope of adulteration which is easily possible in use of potassium humate granules or powder as well as in liquid formulation . Farmer is confused due to different rates of adulterated material being sold in market. . To come out of this situation, gel form is very useful as adulteration is not possible and farmer is assured of proper percentage of humic acid / potassium humate .
Another object of the present invention is to combine sea weed extract and other micro-nutrients with potassium humate during conversion from granular form to gel form so that farmers are not required to handle multiple soil conditioners.

Another object of the present invention is to impart adaptability of potassium humate in gel form for use as foliar spray or in drip irrigation or in drenching roots.
Summary of the Invention:
The invention describes a process, capable of converting granular potassium humate into water-soluble gel form, while employing seaweed extract and micro-nutrients mixture as two ingredients and is comprised of following steps: (i) weighing 100 kg seaweed extract (20) and transferring to reactor (100) from sea
weed extraction tank (110); (ii) maintaining sea weed extract (20) temperature between 45-50 degree C: (iii) weighing 30 kg potassium salt of humic acid (10) granules and transferring the
weighed contents to said reactor (100); (iv) starting stirrer (120) of said reactor (1000) and adjusting pH of the reaction mass to
7.5 to 9.0 to facilitate the reaction, shearing force resulting from said agitation being
adequate for promoting reaction, involving chemical linkage of functional group of
amino acid and protein hydrolysate with humic acid at said alkaline pH between 7.5
to 9. Then Add 100 Kg of water. (v). mixing for 3-4 hours and transferring the viscous solution to another tank (130), by
opening a bottom valve (105) on said reactor (100); (vi) adding on second day of batch 10 litres of micronutrients mixture, and allow gel
formation to complete in 18-24 hours time in the holding tank (130) under ambient
conditions and no stirring. (vii) yield: 160 kg of natural form of humic acid gel (50).

Description of Drawings:
Figure # 1 illustrates process flow diagram for conversion of granular potassium humate
into gel form Figure # 2 illustrates process flow diagram for preparing sea weed extract.
Detailed Description of the Invention:
This is the first of its kind preparation of potassium humate complex with sea-weed. extract &. micronutrients mixture, which is made available in water-soluble gel form (50) for the first time. Humic acid is synthetic form of HUMUS - the most fertile organic compound which is useful for growth of roots as well as overall growth and development of plants.
Normally, potassium humate-based formulations are available in liquid and powder form. Liquid formulations are available in strengths of 6/ 12/ 20/ 30% content of humic acid while powder formulations contain 60/ 65/ 70 % humic acid. The constituents of the gel form (50) are potassium salt of humic acid (10) and sea weed extracts (20).
Gel form (50) of potassium salt of humic acid offer several advantages to farmers, which
are as follows:
1. Numerous liquid formulations with varying strengths often confuse farmers with
regard to quantity to be used for end application. The formulations are costly, and .
dosage required is on high side, rendering them un-economical to farmers.

2. Potassium humate powder/ granule formulations are available but no value
addition is possible due to their inherent limitations.. Moreover, it is difficult to
dissolve powder in water, hence need for extraneous chemical solvents along with
powder not only adds to cost but hampers end application process due to delayed/
limited availability of solvents, forcing often farmers to stock excess quantities.
Humigel (50) - the gel form of potassium salt of humic acid - does not require any
extraneous chemical solvent, for it is easily soluble in water.
3. Humigel (50) balances the advantages of both liquid-based and powder-based
formulations It is easily dissolved in water and due to high purity potassion
humate used in the formulation . and it is cost-effective to farmers due to low
dosages required to obtain required yields.
4. Value addition due to sea weed extracts (20) is possible due to gel formulation process, which involves unique treatment potassium humate granules (10) with sea weed extract (20) under controlled process conditions,
5. Humigel (50) can be used for all types of applications - foliar spray, drip irrigation and root drenching.
6. There is no physical separation of humic substances as in case of liquid formulations.
Sea weed extract (20) is used to densify reaction mass and to convert dense mass into gel

form (50). Hence the product is totally organic in nature. Sea weed extract (20) contains proteins, amino acids , organic matter , natural enzymes and also micro nutrients. Hence it also provides natural nitrogen source. For gel formation, if chemicals such as ammonium nitrate or ammonium sulphate are used for nitrogen source, it has adverse effect on soil structure. The ammonium compounds are broken to release nitrous oxide. which contributes to polluting soil apart from disturbing eco-system.
In the case of humigel formulation . humic acid salt of potassium humate (10) in granular form is reacted with chains of amino acid and proteins present in sea weed extract (20). Humic acid salt (10) molecules are held together in supra molecular conformations by weak hydrophobic bonds at natural and alkaline pH. Humic acid salt (10) is heterocyclic aromatic polymer which has hydroxyl and carboxylic acid groups. Therefore it possesses both aromatic and aliphatic characteristics. The dominant functional groups which contribute to surface change and reactivity of humic substances are phenolic and carboxylic groups.
In presence of natural seaweed extract (20). humic acid granules (10) form chemical linkage with the amino acids and protein hydrolysate present in sea weed extract (20) as natural enzymes promote this reaction. Thus, there is molecular rearrangement and aggregation takes to form the gel (50).
To stabilize the gel formation, various process conditions such as pH, concentration of humic acid granules (10) and temperature of sea weed extract (20) are maintained and

monitored .
Process for gel formation is comprised of following steps:
1. Weigh 100 kg seaweed extract (20) and transfer to reactor (100) from sea weed extraction tank (110);
2. maintain sea weed extract (20) temperature between 45-50 degree C by circulating
hot heating oil through jacket of the reactor (100);
3. weigh 30 kg potassium salt of humic acid (10) granules and transfer the weighed
contents to the reactor (100);
4. start the stirrer (120) and adjust pH of the reaction mass to 7.5 to 9.0 to facilitate the reaction .It creates shearing force in the reactor (100) and promotes the reaction. The functional group of amino acid and protein hydrolysate form the chemical linkage with humic acid at alkaline pH between 7.5 to 9. Then add 100 Kg of water (45) in the tank.
5. after mixing for 3-4 hours, transfer the viscous solution (46) to another tank (130). by opening a bottom valve (105) on the reactor (100)., to a holding tank (130);
6. 24 hours later, counted from start of the batch, add 10 litres of micronutrients mixture (40) and allow gel formation to complete in 18-24 hours time in the holding tank (130):
7 natural form of humic acid gel (50) is formed.
Seaweed Extract (20) - Prepared by Green Algae & Black brown sea weed.
Green algae contains :- Proteins- 16 to 24gms.
(100 gm dry weight) :-Vitamins-1 to 2mg.

growth promoting amino acids.
natural enzymes
gibbrellins. cytokinins auxins and nutrients like
potassium phosphorous, magnesium,
calcium, ferrous, copper, zinc, boron etc.
Black Brown Seaweed :- Proteins 10 to 16gms.
(100 gm dry weight) :-Vitamins o.6 to 0.8mg.
growth promoting amino acids.
natural enzymes
gibbrellins, cytokinins auxins and nutrients like
potassium, phosphorous, magnesium.
calcium, ferrous, copper, zinc, boron etc.
Preparation of sea-weed extract (20)
The accompanying drawing # 2 illustrates the working of the process.
1. Feed 100 litres of water to a jacketed vessel (200), heated by hot oil circulating through its jacket (210);
2. weigh 5 kg each of green algae (21) and black brown algae (22) and add weighed quantities to the jacketed vessel (200);
3. ensure that both the algae are properly wetted;
4. note reaction mass temperature at 50 C and continue heating till it reaches 90 C;

5. maintain the reaction mass temperature, between 70 C to 90 C and continue heating
for 2-3 hours from time recorded in step no. 4:
6. keep it for cooling for 12 hours by circulating cooling water through limpet coil (220) of said jacketed vessel (200)
7. after 12 hours, add fermenting media to above mass dissolved in acetone.
8. again keep the mass for 12 hours, after adding fermented media (44);
9. filter the solution and collect the filtrate (20), measuring about 90 litres in yield.
Specifications of Seaweed Extract (20):-
Input :- seaweed extract (10)
colour :- blackish brown
odour :- Marine protein like
solubility :- Completely soluble in water
pH :- about 6.0-6.5
composition :-
crude protein :- 3 -6 %
amino acid :- 7- 8 % , 17-20 types of amino acids are present
organic matter :-10-15%
natural enzymes :- PPM level
essential elements are:
nitrogen ;- 1-2%
phosphorous .- 1-3%
potassium :- 2 to 5%

calcium :- 0.2 to 0.3%
sulphur :-0.6 to 0.8%
magnesium :- 0.6%
copper :-2 to 5ppm
iron :- 10 to 20ppm
Contents of Gel (50)
potassium humate :- 30kg vv/w
seaweed extract :- 100kg w/w
water :- 100kg vv/w
Total 230 kg Quantity Yield :- 150 -160kg.
Specifications Of micronutrients mixture (40):-
10 litres of micronutrients mixture is added to 230 Kg Batch.
Contents of micronutrients mixture (40) is:
Zn 4.0 %
Fe 3.0%
Mn 1.5 %
Boron 0.5 %
Cu 1.5%
Mo 0.1 %
EDTA 1.0 %

Claims:
I claim
1. a process for converting granular potassium humate (10) in presence of seaweed
extract (20) and micro nutrients (40) into its water-soluble gel form (50), said
process comprising:
(i) weighing 100 kg seaweed extract (20) and transferring to reactor (100) from sea
weed extraction tank (110);
(ii) maintaining sea weed extract (20) temperature between 45-50 degree C;
(iii) weighing 30 kg potassium salt of humic acid (10) granules and transferring the
weighed contents to said reactor (100);
(iv) starting stirrer (120) of said reactor (100) and adjusting pH of the reaction mass to
7.5 to 9.0 to facilitate the reaction under shearing force resulting from said agitation
involving chemical linkage of functional group of amino acid and protein
hydrolysate with humic acid at said alkaline pH between 7.5 to 9.
(v) adding 100 kg water (45) to said reaction mass;
(vi). mixing for 3-4 hours and transferring resultant viscous solution (46) to another tank
(130), by opening a bottom valve (105) on said reactor (100);
(vii) after 24 hours from start of said batch, adding 10 litres of micronutrients mixture.
and allowing gel formation to complete in 18-24 hours time in said holding tank
(130) under ambient conditions and no stirring;
(viii) yielding 160 kg of natural form of humic acid gel (50).

2. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its water-soluble gel form (50) as claimed in claim 1. wherein said seaweed extract (20) is prepared by a process comprising:
(a) feeding 100 litres of water to a jacketed vessel (200). heated by hot oil circulating through jacket (210);
(b). weighing 5 kg each of green algae (21) and black brown algae (22) and adding said weighed quantities to said jacketed vessel (200);
(c) ensuring said both algae being properly wetted by starting agitator (205) of said jacketed vessel (200);
(d) noting reaction mass temperature at 50 C and continuing heating till said reaction mass temperature reaches 90 degree C;
(e) maintaining said reaction mass temperature, between 70 C to 90 C and continuing heating for 2-3 hours from time said temperature reached 90 degree C;
(f) switching off circulation of heating oil and cooling resultant said reaction mass for 12 hours by circulating cooling water through limpet coil (220) of said jacketed vessel (200):
(g) adding fermenting media dissolved in acetone to said cooled mass;
(h). keeping said reaction mass for 12 hours under agitation from time adding said
fermented media; (i) stopping said stirrer (205). filtering solution and collecting filtrate (20). measuring about 90 litres in yield.

3. A process for converting granular potassium humate (10)in presence of seaweed extract (20) and micronutrients mixture (40) into its water-soluble gel form (50) as claimed in claims 1 and 2: wherein said sea-weed extract (20) is completely soluble in water and has pH between 6.0 and 6.5.
4. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its water -soluble gel form as claimed in claims 1 and 2, wherein said sea-weed extract (20) has crude proteins between 3% and 6% by weight and amino acids of 17 to 20 types between 7% and 8% by weight.
5. A process for converting granular potassium humate (10) in presence of seaweed extract (20) and micronutrients mixture (40) into its watre -soluble gel form as substantially described herein above and illustrated in the accompanying drawings # 1 and # 2.

Documents

Application Documents

# Name Date
1 3278-MUM-2010-FORM 26(25-06-2014).pdf 2014-06-25
2 3278-MUM-2010-CORRESPONDENCE(25-06-2014).pdf 2014-06-25
3 3278-MUM-2010-CORRESPONDENCE(IPO)-(HEARING NOTICE)-(14-12-2016).pdf 2016-12-14
4 Other Patent Document [05-01-2017(online)].pdf 2017-01-05
5 3278-mum-2010-NBA Approval Submission(Mandatory) [09-10-2017(online)].pdf 2017-10-09
6 3278-MUM-2010-ORIGINAL UNDER RULE 6 (1A)-AGREEMENT-11-10-2017.pdf 2017-10-11
7 3278-MUM-2010-PatentCertificate18-12-2017.pdf 2017-12-18
8 3278-MUM-2010-IntimationOfGrant18-12-2017.pdf 2017-12-18
9 3278-MUM-2010-RELEVANT DOCUMENTS [09-01-2018(online)].pdf 2018-01-09
10 abstract1.jpg 2018-08-10
11 3278-MUM-2010_EXAMREPORT.pdf 2018-08-10
12 3278-MUM-2010-REPLY TO EXAMINATION REPORT(1-10-2013).pdf 2018-08-10
13 3278-MUM-2010-original under rule 6 (1A)Correspondence-271216.pdf 2018-08-10
14 3278-MUM-2010-original under rule 6 (1A) Power of Attorney-271216.pdf 2018-08-10
15 3278-MUM-2010-FORM 9.pdf 2018-08-10
16 3278-mum-2010-form 5.pdf 2018-08-10
17 3278-mum-2010-form 3.pdf 2018-08-10
18 3278-mum-2010-form 26.pdf 2018-08-10
19 3278-mum-2010-form 2.pdf 2018-08-10
21 3278-mum-2010-form 2(title page).pdf 2018-08-10
22 3278-MUM-2010-FORM 18.pdf 2018-08-10
23 3278-mum-2010-form 1.pdf 2018-08-10
24 3278-mum-2010-drawing.pdf 2018-08-10
25 3278-mum-2010-description(complete).pdf 2018-08-10
26 3278-mum-2010-claims.pdf 2018-08-10
28 3278-MUM-2010-CLAIMS(MARKED COPY)-(1-10-2013).pdf 2018-08-10
29 3278-MUM-2010-CLAIMS(AMENDED)-(1-10-2013).pdf 2018-08-10
30 3278-mum-2010-abstract.pdf 2018-08-10
32 3278-MUM-2010-POST GRANT EVIDENCE OPPOSITION [18-12-2018(online)].pdf 2018-12-18
33 Notice of PGO 3278-MUM-2010 (290723).pdf 2019-07-29
34 3278-MUM-2010-NOTICE OF POST GRANT OPPOSITION-30-09-2019.pdf 2019-09-30
35 3278-MUM-2010-POST GRANT OPPOSITION NOTICE-07-01-2020.pdf 2020-01-07
36 3278-MUM-2010-Response to office action (Mandatory) [14-01-2020(online)].pdf 2020-01-14
37 3278-MUM-2010-Correspondence-150120.pdf 2020-01-16
38 3278-MUM-2010-Written Statement and Evidence [21-05-2020(online)].pdf 2020-05-21
39 3278-MUM-2010-CERTIFIED COPIES-CERTIFICATE U-S 72 147 & UR 133-2 [28-10-2020(online)].pdf 2020-10-28
40 3278-MUM-2010-CORRESPONDENCE(IPO)-(CERTIFIED COPY)-(21-12-2020).pdf 2020-12-21
41 3278-MUM-2010-RELEVANT DOCUMENTS [09-05-2023(online)].pdf 2023-05-09
42 3278-MUM-2010-PostGrantOppositionDocumentsDossier.pdf 2024-01-13

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