Title of Invention

AN IMPROVED METHOD FOR THE PREPARATION OF PLANT GROWTH NUTRIENT OF ENHANCED ACTIVITIES

Abstract There is provided a method for preparing an improved plant growth nutrient composition from sugar cane mud which comprises (A) first preparing high purity triacontanol of at least 96% purity according to the process describerd and claimed in our no 188438 of 07 03 1996 (413/CAL/1996) namely i. Subjecting sugarcane press mud to a step of organic solvent extraction, ii. Recovering the sugarcane wax there from, iii. Subjecting an alcoholic suspension of the sugarcane wax to a step of trans-esterification with an alkaline alkoxide, iv. Concentrating the esterified product, v. Subjecting same to organic solvent extraction in the presence of inorganic acid vi. Followed by the filtration of the extract to obtain crude triacontanol, where after vii. The crude product is subjected to crystallization using organic solvent to obtain technical grade traicontanol viii. Converting same to high purity grade by purification through column chromatography on silicagel using solvents of varying polarity and ix. collecting pure n-triacontanol from petroleum ether fraction which is filtered and dried to obtain pure n-trianontanol crystals and there after 13 (B) converting the said pure triacontanol into applicable formulations like emulsions / solutions / or other useful forms with or without conventional micro nutrients in a conventional manner using conventional ingredients.
Full Text Introduction to the Field of the Invention:
This invention relates to an improved method for the preparation of plant growth nutrient of enhanced activities
Prior Art and Drawbacks:
It is well known that higher fatty alcohol can be denved from plant sources and that triacontanol, C-30 alcohol is a prominent plant growth promoter Higher fatty alcohol such as C-28 to C32
alcohol have been extracted by many methods in the past and vanous formulations based on the same are currently used as plant growth promoters
For example, plant waxes such as nee bran wax, carnauba wax, sugarcane wax have been a source which are subjected to a first step of saponification and the unsaponified matter is then subjected is solvent extraction for obtaining higher fatty alcohol
In another method, the unsaponifiable are subjected to reduction
In yet another method, rice bran oil distillation residue is subjected to saponification, then treatment with alkaline earth metal halides and then extraction and salting out
Plant growth promoting compositions prepared by these methods have been of course effective and have given useful results
However, our research has established that the full potential of the important constituent triacontanol has not been realized due to the punty level of same not exceeding 95% or 96% at the most
It is possible to enhance the growth promotion effect and extent of areas of uses if the punty of C-30 alcohol is over 96% and of the order of 98% or even more
Objects of the Invention:
It is therefore an object of this invention to propose an improved method for the extraction of triacontanol of higher punty than possible so far from plant sources and convert the same into an effective plant growth nutrient composition
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It is another object of this invention to propose a plant growth promoter composition having higher synergistic activity than known growth promoting compositions
In the pursuit of achieving our objects, we have investigated various other sources of triacontanol and have carried out extensive experiments, prepared formulations based on the triacontanol of the new and hitherto untried source We have also applied these formulation on various plants, vegetables, fruits bearing plants, leaf bearing plants and many others and in all cases we have obtained unexpected excellent results We have also found that small quantities of micro nutrients with the new triacontanol gave excellent results BRIEF STATEMENT OF THE INVENTION
According to this invention, there us provide a method for preparing an improved plant growth
nutrient composition from sugar cane mud which comprises
( A) first preparing high purity triacontanol of at least 96% purity according to the process describerd and claimed in our no 188438 of 07 03 1996 (413/CAL/1996) namely
i. Subjecting sugarcane press mud to a step of organic solvent extraction,
II. Recovering the sugarcane wax there from,
iii. Subjecting an alcoholic suspension of the sugarcane wax to a step of trans-esterification
with an alkaline alkoxide,
iv. Concentrating the esterified product,
v Subjecting same to organic solvent extraction in the presence of inorganic acid
vi. Followed by the filtration of the extract to obtain crude triacontanol, where after
vii. The crude product is subjected to crystallization using organic solvent to obtain technical
grade traicontanol VIII. Converting same to high purity grade by purification through column chromatography on
silicagel using solvents of varying polarity and
ix. collecting pure n-triacontanol from petroleum ether fraction which is filtered and dried to
obtain pure n-triacontanol crystals and there after
(B) converting the said pure triacontanol into applicable formulations like emulsions / solutions / or other useful forms with or without conventional micro nutrients in a conventional manner using conventional ingredients
The formulations are thus prepared with or without micro nutrients suited for Application to agricultural crops cereals, floriculture, vegetables products such as potatoes and tomatoes, plantation crops such as bananas, tea and for fruit plants For further details of the extraction process, attention is invited to the parent Application
(3)
The invention will now be more fully described with reference to the following examples, which are only illustrative and not limitative in applications and preparations
Examples of Preparation of Formulations:
Example 1: A n-triacontanol formulation with micro nutrients suitable for agricultural crops:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the emulsification process, five acquous solution of different micro nutrients viz boron as bone acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and manganese and magnesium as EDTA chelates Magnesium and manganese EDTA salts are prepared by mixing equi molar acquous solution of their chloride salts and EDTA
Example 2: A n-triacontanol formulation with micro nutrients suitable for cereals:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the em unification process, five acquous solution of different micro nutrients viz boron as boric acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and Manganese as EDTA chelates Manganese-EDTA salts are prepared by mixing equi-molar acquous solution of magnesium chloride and EDTA
Example 3: (Formulated for floriculture)
A n-triacontanol formulation with micro nutrients and growth regulation suitable for floriculture:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This
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heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion During the emulsification process, five acquous solution of different micro nutrients viz boron as bone acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and manganese and magnesium as EDTA chelates Magnesium and manganese EDTA salts are prepared by mixing equi molar acquous solution of their chloride salts and EDTA The desired solution of growth substance (s) (prepared by dissolving it in a minimum quantity of 99% ethyl, alcohol) is added
Example 4: A n-triacontanol formulation with micro nutrients suitable for tomato/potato:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the emulsification process, five acquous solution of different micro nutrients viz boron as bone acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and manganese and magnesium as EDTA chelates Magnesium and manganese EDTA salts are prepared by mixing equi molar acquous solution of their chloride salts and EDTA
Example 5: A n-triacontanol formulation with micro nutrients suitable for tea and other plantation crops:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution Is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the em unification process, five acquous solution of different micro nutrients viz boron as bone acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and manganese and magnesium as EDTA chelates Magnesium and manganese EDTA salts are prepared by mixing equi molar acquous solution of their chloride slats and EDTA
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Example 6: (For tea gardens other than Darjeeling)
A n-triacontanol! formulation with growth regulator suitable for tea and other economic crops:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion During the emulsification process, the desired solution of growth substance (s) (prepared by dissolving it in a minimum quantity of 99% ethanol) is added
Example 7: (For tea gardens of Darjeeling)
A n-triacontanol formulation with growth regulator suitable for tea and other plantation crops:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the emulsification process, the desired solution of growth substance (s) (prepared by dissolving it in a minimum quantity of 99% ethyl alcohol) is added
Example 8- A n-triacontanol formulation with micro nutrients and growth regulator suitable for tea plantation:
Methods of formulation:
A dilute n-triacontanol solution is prepared by dissolving the required amount in a suitable solvent The dilute solution is added to the desired quantity of water and surfactant This heterogeneous solution is stirred by a mechanical stirrer until the solution becomes a homogeneous emulsion Dunng the emulsification process, five acquous solution of different micro nutrients viz boron as bone acid, molybdenum as ammonium molybdate, zinc as zinc sulphate and manganese and magnesium EDTA salts are prepared by mixing equi molar acquous solution of their chloride salts and EDTA The desired solution of growth substances (prepared by dissolving it in a minimum quantity of 99% ethyl alcohol is also added Vanous formulations were prepared and the efficiencies were evaluated for different applications for these
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applications the test formulation prepared as per examples stated earlier were diluted with water in the ratio of 1 5000 vol/vol
Some of the evaluation test results are reproduced below
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Name of the garden Composition of Date of Yield of tea % Increase (+)
example No Plucking leaves (kg) % Increase M
Treated Control

1 RaipurTE Example 5 05 07 1993 140 194 (-) 27 83
16 07 1993 486 338 (+) 43 78
29 07 1993 577 465 (+) 24 09
12.08.1993 593 408 (+) 45 34
Average increase of yield (+) 27.82%

2 Naxalbari T E Example 5 23.08 1993 143 168 (-) 19.66
02 09 1993 241 220 (+) 954
10 09 1993 230 180 (+) 27 70
Average increase of yield (+) 3.09%

3 AshapurTE Example 8 03 09 1993 512 412 (+) 24 27
10 09 1993 285 170 (+) 67 64
19 091993 297 231 (+) 28 57
28 09 1993 282 244 (+)15 57
Average increase of yield (+) 30.00%

4 Singhiajhora T.E Example 6 28 08.1993 321 288 (+) 11 45
07 09 1993 325 272 (+) 19 48
18 09 1993 300 248 (+) 20 96
29 09.1993 344 300 (+) 14 66
Average increase of yield (+116.25%

5 Gangamati TE Example 5 01 09 1993 86 0 86 6
08 09 1993 95 0 95 5
15 09 1993 75 8 70 2 24 09 1993 97 0 76 6 (+) 26 6
Average increase of yield (+) 7.6%

6 Gulma TE Example 7 19 08 1993 260 185 (+) 40 5
27 08 1993 208 187 (+)112
06 09 1993 146 143 (+)21
16 09 1993 245 230 (+)66
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Average increase of yield (+) 15.3%
Results of trial studies of foilar Application of phytonol on different crops: I. Effects on vegetables as per Example 4: Yield (kg) per 2000(SM)

Cabbage Potato Chili Tomato Brinjal
Foilar spray in 5190 5980 2018 5004 20927
recommended dose
No spray control
II. Effects on cereal pulses as per Example 2: Yield of grains (kg) per 2000 SM.

Paddy Pulse
Foilar spray in Recommended dose 728 550
No spray control 465 430
III. Effects on medicinal dioscorea as per Example 5:

Dry tuber (kg) per hectre % diosgenin
Foilar spray in Recommended dose 10280 3 45
No spray control 3350 2 90
IV. Effects on aromatic grass as per Example 3:

Herbage yield (kg/hectre) % oil
(-) Phytonol (+) Phytonol(-) (-) Phytonol (+) Phytonol
Lemon grass 5500 7500 0 32 0 48
Jalmarosa 7500 10600 0 36 0 51
Citronella 4620 6650 0 90 1 05
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V. Effects on ornamental plant as per Example 3
%increase/plant with Phytonol
Foliages Flowers

Tuberose 12 5 20 6
Antiihinum 182 25 5
Gladiolus 19 5 186
Dahlia 20 2 155
Zinnia 25 0 26 8
Crysanthenim 16 0 18 5
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We Claim:
1 A method for preparing an improved plant growth nutrient composition from sugar cane mud which comprises
(A) first preparing high purity triacontanol of at least 96% purity according to the process described and claimed in our no 188438 of 07 03 1996 (413/CAL/1996) namely
i. Subjecting sugarcane press mud to a step of organic solvent extraction,
II. Recovering the sugarcane wax there from,
iii. Subjecting an alcoholic suspension of the sugarcane wax to a step of
transesterification with an alkaline alkoxide,
iv. Concentrating the esterified product,
v Subjecting same to organic solvent extraction in the presence of inorganic
acid
vi. Followed by the nitration of the extract to obtain crude triacontanol, where
after
vii. The crude product is subjected to crystallization using organic solvent to obtain technical grade triacontanol
viii. Converting same to high purity grade by purification through column Chromatography on silicagel using solvents of varying polarity and
f x Collecting pure n-triacontanol from petroleum ether fraction which is filtered
and dried to obtain pure n-triacontanol crystals and there after
(B) Converting the said pure triacontanol into applicable formulations like emulsions
solutions / or other useful forms with or without conventional micro nutrients in a conventional manner using conventional ingredients
n 2 A method as claimed in claim 1 wherein, the formulations are thus prepared with or
without micro nutrients suited for Application to agricultural crops, cereals, floriculture,
vegetable products such as potatoes and tomatoes, plantation crops such as bananas,
tea and for fruit plants
3 A method as claimed in claims 1 and 2, wherein, micro nutrients are preferably selected
from for example , from, boron as boric acid, molybdenum as ammonium molybdate,
zinc as zinc sulphate and manganese and magnesium as EDTS chelates and
magnesium and manganese EDTA salts prepared by mixing equi molar aqueous solution
of their chloride salts and EDTA
4 A method for preparing an improved plant growth nutrient composition substantially as
herein described wit reference to the examples

Documents:

00224-cal-2002-abstract.pdf

00224-cal-2002-claims.pdf

00224-cal-2002-correspondence.pdf

00224-cal-2002-description(complete).pdf

00224-cal-2002-form-1.pdf

00224-cal-2002-form-2.pdf

00224-cal-2002-form-3.pdf

00224-cal-2002-gpa.pdf

00224-cal-2002-letters patent.pdf

224-cal-2002-granted-abstract.pdf

224-cal-2002-granted-acceptance publication.pdf

224-cal-2002-granted-claims.pdf

224-cal-2002-granted-correspondence.pdf

224-cal-2002-granted-description (complete).pdf

224-cal-2002-granted-form 1.pdf

224-cal-2002-granted-form 2.pdf

224-cal-2002-granted-form 3.pdf

224-cal-2002-granted-gpa.pdf

224-cal-2002-granted-letter patent.pdf

224-cal-2002-granted-reply to examination report.pdf

224-cal-2002-granted-specification.pdf


Patent Number 193527
Indian Patent Application Number 224/CAL/2002
PG Journal Number 30/2009
Publication Date 24-Jul-2009
Grant Date 07-Mar-1996
Date of Filing 07-Mar-1996
Name of Patentee WEST BENGAL PHARMACEUTICALS & PHYTOCHEMICAL DEVELOPMENT CORPORATION LIMITED
Applicant Address ILACO HOUSE (2ND FLOOR), 1 & 3, BIPLABI TRAILAKYA MAHARAJ SARANI, CALCUTTA
Inventors:
# Inventor's Name Inventor's Address
1 SALIL KUMAR CHATTERJEE C/O. WEST BENGAL PHARACEUTICAL & PHYTOCHEMICAL DEVELOPMENT CORPORATION LIMITED, OF ILLACO HOUSE, 2ND FLOOR, 1&3, BIPLABI TRAILAKYA MAHARAJ SARANI, CALCUTTA - 700 001
2 PRANAY KANTI GHOSH C/O. WEST BENGAL PHARACEUTICAL & PHYTOCHEMICAL DEVELOPMENT CORPORATION LIMITED, OF ILLACO HOUSE, 2ND FLOOR, 1&3, BIPLABI TRAILAKYA MAHARAJ SARANI, CALCUTTA - 700 001
PCT International Classification Number A01N 65/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA