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Herbicidal / Weedicidal Composition

Abstract: A herbicidal and weedicidal composition comprising quizalofop-ethyl in an amount of 5-15% by weight, Imazethpyr in an amount of 10-40% by weight, and one or more excipients in an amount of 45-85% by weight.

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Patent Information

Application #
Filing Date
06 February 2015
Publication Number
36/2016
Publication Type
INA
Invention Field
AGROCHEMICALS
Status
Email
archana@anandandanand.com
Parent Application

Applicants

Insecticides (India) Ltd.
401-402 Lusa Tower, Azadpur Commercial Complex, Delhi - 110033, India

Inventors

1. Rajesh Aggarwal
401-402 Lusa Tower, Azadpur Commercial Complex, Delhi - 110033, India
2. L.C. Rohela
401-402 Lusa Tower, Azadpur Commercial Complex, Delhi - 110033, India

Specification

TITLE
Herbicidal / Weedicidal Composition
FIELD OF INVENTION
The present invention relates to a synergistic herbicidal and weedicidal composition containing
an Aryloxyphenoxy herbicide and an Imidazolinone herbicide and a process for preparing the
said synergistic herbicidal composition.
BACKGROUND AND OBJECT OF THE INVENTION
The protection of crops from weeds and other vegetation which inhibit crop growth is a
constantly recurring problem in agriculture. To help combat this problem researchers in the field
of synthetic chemistry have produced an extensive variety of chemicals and chemical
compositions effective in the control of such unwanted growth. Chemical herbicides of many
types have been disclosed in the literature and a large number are in commercial use.
The currently available herbicide is limited for controlling a particular type of weeds as the
weedicides are selective. Thus there is a need for developing a herbicidal combination
formulation which controls a broad spectrum of weeds.
The present invention is the result of continuation efforts of the inventors to develop a herbicidal
composition for controlling grassy as well as broad leaf weeds in soybean, peas and other pulse
crops.
The present invention resides in the novel combination formulation of Aryloxyphenoxy herbicide
such as diclofop methyl,fenoxyprop-p ethyl,fluzifop-p butyl,Quizalofop ethyl/p ethyl, etc. and
Imidazolinone herbicide such as imazapyr, Imazaquin, imazamox, Imazapic, imazethapyr, etc.
The said compounds are already known for their herbicidal potency. However, it has now been
found by the inventors of the present invention that the combination of said
herbicidal/weedicidal compounds displays a synergism when applied in a specific manner.
The compounds which have been combined to form the synergistic herbicidal/weedicidal
compositions of the present invention are already known in the art as herbicides. One such
compound is 2-(2-chloro-4-methanesulfonylbenzoy)-1,3-cyclohexanedione. This compound is
disclosed in European Patent Publication No. 1,37,963, published on 04-04-1985. It is also
disclosed and claimed in U.S. application Ser. No. 6,34,408. Yet another compound used in the
synergistic compositions of this invention is 2-chloro-4-N-isopropylacetanilide, commonly known
3
as Propachor. Chinese patent 99114323 claims a “Caodashuai" weedicide which possesses
spectrum-broadening and synergistic action at a reduced dosage.
It has been observed by the inventors of the present invention that the combination of an
Aryloxyphenoxy herbicide such as quizalofop-ethyl (5-15%) and an Imidazolinone herbicide such
as Imazethapyr (10–40%) when formulated in the form of an emulsifiable concentrate, suspoemulsion
and wettable dispersible granules and applied in combination with a non-ionic
surfactant exhibited synergism and activity widened to control both grassy and broad leaf weeds.
Owing to the physico-chemical properties of Quizalofop-ethyl and Imazethapyr the wettable
granule formulation could be formulated to provide easy to use and stable formulation.
SUMMARY OF THE INVENTION
The present invention discloses a formulation/composition which employs synergism in the
control of undesirable vegetation comprising a mixture of the following components:
(a) a herbicidally effective amount of Quizalofop ethyl selected from the group of
Aryloxyphenoxy propionate ; and
(b) a herbicidally effective amount of Imazethapyr selected from the group of Imidazolinone.
It has been further identified that the novel combination formulation/composition comprises:
- 5-15% by weight Quizalofop ethyl;
- 10-40% by weight Imazethapyr; and
- optionally comprising one or more excipients selected from the group consisting of
organic solvents, wetting agent, dispersing agent, binder, disintegrating agent,
emulsifiers, stabilizers, anticoagulating agent, anti-freeze agent, anti-foaming agent, pH
buffer, penetrating agent, inerts, etc.
The composition is prepared in the form of emulsifiable concentrate, suspo-emulsion and
wettable granule.
Said compounds are already known for their herbicidal potency. However, it has now been
identified by the inventors of the present invention that the combination of said herbicidal
compounds displays a synergism when applied in a specific manner.
The present invention also provides a unique process for manufacturing the homogeneous
formulation by combining the said compounds in a liquid and granular composition.
4
These and other aspects of the present invention will become apparent form the following
detailed description of the invention.
DESCRIPTION OF THE INVENTION
The instant application discloses an invention which employs synergism in the control of
undesirable vegetation exhibited by a composition comprising a mixture of the following
components:
(a) a herbicidally effective amount of Quizalofop-ethyl ; and
(b) a herbicidally effective amount of Imazethapyr.
It has been further identified that the present formulation comprises the herbicidal actives
quizalofop-ethyl (5-15% by weight) and Imazethpyr (10-40% by weight) along with excipients
(45-85% by weight).
The composition comprises one or more excipients selected from polar organic solvent in an
amount of 20-30% by weight and non polar organic solvent 50-65%by weight, wetting agent in
an amount of 4-10% by weight, dispersing agent in an amount of 5-10% by weight, binder in an
amount of 0.5-3% by weight, disintegrating agent in an amount of 3-15% by weight, inerts in an
amount of 20-50% by weight, anti-foaming agent in an amount of 0.3-1% by weight, emulsifiers
in an amount of 5-20% by weight, stabilizers in an amount of 0.5-3% by weight, anticoagulating
agents in an amount of 5-8% by weight, anti-freeze agents in an amount of 5-8%
by weight, pH buffer in an amount of 5-10% by weight, either alone or in combination thereof.
The composition is prepared in the form of emulsifiable concentrate, suspo-emulsion and
wettable granule and the excipients are selected in accordance with the form of composition.
The solvent used in the composition are selected from the group of polar and non-polar aromatic
solvents. Preferably the polar solvents are selected from N-methylpyrrolidone and Dimethyl
sulfoxide and non polar solvents from aromatic hydrocarbons.
The wetting agents are selected from anionic or non ionic surfactants or a combination of both.
The anionic surfactants is selected from the group consisting of salts of alkylbenzene
sulphonates, alpha olefin sulphonates, alkyl phenol ethoxylates, sodium salts of alkyl sulphates,
alkyl sulphosuccinates. Preferably sodium alkyl sulphate is employed in the composition.
5
Preferred anionic surfactant is calcium salt of dodecyl benzene sulphonate and sodium lauryl
sulphate.
Non-ionic surfactant is selected from the group consisting of nonyl phenol ethoxylate, octyl
phenol ethoxylate, styrenated phenol ethoxylate, and vegetable oil ethoxylates. Preferred nonionic
surfactant is blend of nonyl phenol ethoxylate and striated phenol ethoxylate.
The dispersing agents are selected from group comprising poly carboxylates, alkyl naphthalene
sulphonates, phenol sulphonic acid condensates, sodium salt of ligno sulphonates or N-methyl-Noleyl
taurate, Acrylic polymer and Tristyrenated phenol ethoxylated phosphate ester and its
potassium salt.
The binding agent is selected from the group consisting of polyvinyl pyrolidone, polysaccharides,
partially hydrolysed polyvinyl acetate or dissacharides. The preferred binding agent is polyvinyl
pyrollidone.
The disintegrating agents are selected from ionic compounds such as inorganic salts and
nitrogen containing compounds such as ammonium sulphate, urea, mono-di and triammonium
phosphate or combination of water soluble organic acid and alkali carbonates such as sodium
carbonate.
The inert carriers are selected from the group consisting of demineralised water (DM Water),
solvent CIX (C9 Aromatic Hydrocarbon Solvents), starch, calcite, kaolin, montmorillonite or
attapulugite clay, china clay and diatomaceous earth. The preferred inert for emulsifiable
concentrate formulation is Solvent CIX, suspo-emulsion is DM Water and wettable granule
formulation is starch and china clay.
The emulsifiers are selected from the group consisting of anionic and non-ionic emulsifiers. The
anionic emulsifier is selected from Calcium alkyl benzene sulfonate, preferably calcium dodecyl
benzene sulphonate. Non-ionic emulsifier is selected from the group comprising of nonyl phenol
ethoxylate, Octylphenol ethoxylate, Castor oil ethoxylate, Tris styrenated phenol ethoxylate,
tweens either alone or in combination.
The stabilizer employed is selected from epoxidised vegetable oil preferably epoxidised soyabean
oil. The preferred viscoelastic products are such as xanthan gum, polyvinyl alcohol, and natural
gums.
6
The defoaming or anti-foaming agent is selected from silicone defoamers.
The anti-coagulating agent is diatomaceous earth.
The anti-freeze agent is Propylene glycol
The pH buffer is selected from sodium carbonate and citric acid, either alone in combination
thereof.
The penetrating agent is Tri siloxane ethoxylate.
The terms "synergism" and "synergistic" are used herein to convey the result observed when a
combination of herbicides demonstrates potency in excess of that which the combination would
be expected to produce on the basis of the potencies of each herbicide applied individually.
The term "herbicide" is used herein to denote a compound which controls or modifies the growth
of plants. The term "herbicidally effective amount" is used to indicate the quantity of such a
compound or combination of such compounds which is capable of producing a controlling or
modifying effect. Controlling or modifying effects include all deviations from natural
development, for example: killing, retardation, leaf burn, dwarfing and the like. The term
"plants" is used to include all post-emergent vegetation, ranging from seedlings to established
vegetation.
The combination of the herbicides Quizalofop ethyl and Imazethapyr is unique since the end
product is the result of two systemic herbicides chosen from the groups of herbicides having
different modes of action. Quizalofop ethyl is selected from a group of herbicides
Aryloxyphenoxy propionate which are selective, systemic, grass herbicides characterized by
absorption by leaves and which rapidly trans-locate to the growing points of leaves and stems.
This group of herbicides inhibits acetyl CoA carboxylase in grassy weed plants leading to death
of unwanted plant.
The other herbicide Imazethapyr is selected from a group of herbicides Imidazolinone which too
are selective, in action but have a different mode of action. It reduces the level of amino acids,
isoleucine, leucine and valine, through the inhibition of aceto-hydroxyacid synthase, an enzyme
common to the biosynthetic pathway for these amino acids. This inhibition causes a disruption in
protein synthesis which, in turn, leads to interference in DNA synthesis and cell growth, finally
7
leading to death of target weeds. Interestingly, this Imazethapyr acted on both types of weed
grassy as well as broad leaved weeds.
The present invention, which is the combination of Quizalofop ethyl and Imazethapyr, is a
composition in the form of an emulsifiable concentrate, a suspo emulsion and a granular
composition. The synergistic effect of the invention and consequently its enhanced efficacy
compared to the efficacy of its individual constituents Quizalofop ethyl and Imazethapyr, is
primarily attributable to the process of achieving a uniform homogeneous mixture of Quizalofop
ethyl and Imazethapyr.
Accordingly, one of the embodiment of the invention provides a unique process of manufacturing
a granule homogeneous composition. The pulverized mass was transferred to a dough mixer and
a solution of non ionic surfactant in isopropanol-water was sprayed to form dough suitable for
extrusion. The dough was extruded from a basket extruder and dried at suitable temp. (60-
90°C).
Another embodiment of the invention is the product of this unique process which exhibits
enhanced efficacy over and above the efficacy of the individual herbicides which constitute the
invention.
Accordingly, the primary embodiment of the invention is a unique process of manufacturing a
liquid homogeneous composition comprising Quizalofop ethyl and Imazethapyr.
Another embodiment of the invention is a unique process of manufacturing a liquid
homogeneous composition comprising Quizalofop ethyl and Imazethapyr. The process also
involves the use of surfactant which enables direct adhesion of the composition on the surface of
weeds.
The emulsifiable concentrate formulation is prepared by using the toxicants in the aforesaid
concentration ranges and is dissolved in combination of polar and non polar aromatic solvents.
Emulsifiers containing anionic (calcium or amine salts of linear and branched alkyl benzene
sulphontes) and non ionic (ethoxylates of nonyl-phenol, castor oil, octyl-phenol, tristyrenated
phenol, tweens) are added so that the formulation exhibits good emulsion stability. Stabilizers
such as epoxidised vegetable oil or dibutyl or octyl-phthalates or epichlohydrin are added to
provide long term stability to the formulation.
8
The suspo-emulsion was prepared by adding Imazethapyr (10-40%) to an aqueous solution of
wetting agents (NaLABSA, sodium lauryl sulphate, non ionic ethoxylates, etc), dispersing agents
(tristyrenated phenol ethoxylates potassium or amine salt, nonyl phenol phosphate esters), anti
coagulating agents (silica, diatomeceous earth), anti-freeze agents (glycols), anti-foaming agents
(silicone based), penetrating agent (trisilicone ethoxylate) and pH buffer and micronising in a
horizontal pressurized bead mill to a partical size D90 less than 7 micron analysed on Malvern
master sizer. To this were added the emulsiifiable concentrate of quizalofop ethyl (5-15%) to
form a stable homogeneous suspension. To make it stable over a long time the visco elastic
products such as xantham gum, polyvinyl alcohol, natural gums were added.
The wettable granules were prepared by making dough of Imazethapyr (10-40%), quizalofop
ethyl (5-15%), inerts (lactose, china clay, di-atomeceous earth, ammonium sulphate), wetting
agent (NaLABSA, sodium lauryl sulphate, non ionic ethoxylates, etc), dispersing agent
(lignosulphonates, alphaolefine sulphonates, etc.), disintegrating agent an organic acid and
inorganic base and required quantity of water to form a dough suitable for granulation. The
dough formed was extruded in a basket extruder having sieve aperture 0.8 - 1.0 mm. The
extruded granules were dried on fluid bed drier.
The known formulation of Imazethapyr 10% SL is used by the farmer at dose 300ml/acre to
control leaf weeds. The quizalofop ethyl 5%EC formulation is used by the farmer at dose 300ml/
acre to control narrow leaf weeds. It was observed by the inventors that the present composition
has better efficacy to control both weeds narrow and broad leaf at dose 100ml-250ml/acre.
The best results of the herbicidal composition were observed when it was tank mixed with a non
ionic surfactant selected from a group of fatty alcohol ethoxylated having HLB 10 -14. The use of
surfactant at tank mix stage resulted in the uniform spreading, penetration and coverage of the
herbicide and yielded effective control of the broad leaf and narrow leaf weeds.
The present invention will now be explained with the help of the following examples and
experiment, however; the scope of the invention should not be limited to said examples and
experiments. It is to be understood that the above described embodiments are merely illustrative
principles of the present invention and that many variations may be devised by those skilled in
the art without departing from the scope of the present invention. It is, therefore, intended that
such variations be included with the scope of the claims.
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Formulation Examples 1: Preparation of emulsifiable concentrate of Quizalofop ethyl
5% + Imazethapyr 10%
The emulsifiable concentrate formulation of quizalofop ethyl and imazethapyr was prepared
having the following composition.
Table – 1
Component Amount
Quizalofop ethyl tech. 5.2 parts by weight
Imazethapyr tech. 10.2 parts
N-methyl pyrollidone 5.0 parts
Dimethyl sulfoxide 15.0 parts
Solvent CIX (Aromatic hydrocarbon containing
9 carbon atoms. CAS No. : 64742-95-6)
55.6 parts
Blend of anionic (calcium alkyl benzene
sulfonate) and non-ionic emulsifier
(nonylphenol ethoxylate and styrenated
phenol ethoxylated)
8 parts
Epoxidised soya bean oil 1.0 part
N-Methyl pyrollidene 5 parts by weight, Dimethyl sulfoxide 15.0 parts by weight and solvent CIX
55.6 parts by weight are charged to a mixing vessel and mixed till homogenized. To the mixed
mass is added Imazethpyr tech. 10.2 part by weight and mixed till solubilized. Quizalofop ethyl
tech 5.2 parts by weight is added and mixed till a homogenized blend is obtained. To the said
blend are added anionic emulsifier (calcium alkyl benzene sulfonate), non-ionic emulsifier
(nonylphenol ethoxylate and styrenated phenol ethoxylated) all mixed to form 8.0 parts by
weight. Finally epoxydised soybean oil, 1.0 parts by weight is added and mixed till complete
homogenization. The entire process is carried out at ambient temperature and pressure.
Formulation Examples 2: Preparation of Wettable granules of Quizalofop ethyl 10%
+ Imazethapyr 20%
The Wettable granule formulation of quizalofop ethyl and imazethapyr was prepared having the
following composition.
Table – 2.
Component Amount
Quizalofop ethyl tech. 10.5 parts by weight
10
Imazethapyr tech. 20.8 parts
Sodium Alkyl sulphate 8.0 parts
Sodium lignosulphonate 4.0 parts
Alkyl naphthalene sulphonate 3.0 parts
Polyvinylpyrollidone 1.0 parts
Sodium carbonate 5.5 parts
Citric acid 1.0 parts
Ammonium sulphate 9.0 parts
Di atomeceous earth 3.0 parts
Starch 13.0 parts
Lavigated china clay 21.2 parts
Pre mixing:
In a premixer suitable for mixing powders was taken lavigated china clay, 21.2 parts by weight,
starch, 13.0 parts by weight, ammonium sulphate, 9.0 parts by weight, sodium carbonate, 5.0
parts by weight, citric acid, 1.0 parts by weight, Poly Vinyl pyrollidone, 1.0 parts by weight, Alky
naphthalene sulfonate, 3.0 parts by weight, Sodium lignosulfonate, 4.0 parts by weight and
sodium alkyl sulphate, 8.0 parts by weight. The material was mixed till homogenized. Quizalofop
ethyl, 10.5 parts was sprayed over the above mixed mass and mixed till the material is
homogenized.
Pulverization:
The homogenized pre mixed mass was pulverized in air jet mill to achieve particle size D90 less
than 20 micron.
Dough formation:
The pulverized mass was charged to dough mixer and sufficient quality of water was sprayed to
form dough suitable for extrusion.
Extrusion:
The dough prepared was charged to a basket extruder and the material extruded through sieve
of aperture 0.8-1.2 mm.
Drying:
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The extruded granules were dried in a fluid bed drier, keeping inlet air temperature 60°-90° C to
form wettable granule of quizalofop ethyl 10%+Imazethapyr 20%.
Formulation Examples 3: Process for preparation of Suspo-emulsion of Quizalofop
ethyl 10% + Imazethapyr 20%
The suspo-emulsion formulation of quizalofop ethyl and imazethapyr was prepared having the
following composition.
Table – 2.
Component Amount
Quizalofop ethyl tech 10.6parts by weight
Imazethpyr tech 20.5 parts by weight
Soyabean oil 3.0 parts by weight
Tristyrenated phenol ethoxylated phosphate
ester, Potassium
2.5 parts by weight
Nonyl phenol ethoxylate 4.0 parts by weight
Acrylic graft polymer 2.5 parts by weight
Propylene glycol 5.0 parts by weight
Trisiloxane ethoxylate HS grade 429 0.5
Silicone defoamer 0.6 parts by weight
Xanthum Gum 2% aqueous solution 10.0 parts by weight
DM water 40.8 parts by weight
Formation of oil-in- water emulsion of Quizalofop ethyl:
In a vessel fitted with high shear mixer is added 16.6 parts by weight of dimineralized (DM)
water, 0.3 parts by weight silicone defoamer, 2.5 parts potassium salt of Tristyrenated phenol
etoxylate phosphate ester, 2.0 parts nonyl phenol ethoxylate, 3.0 parts soybean oil. The material
is mixed at 900-1200 RPM at temperature 10-60° C, preferably 40°C and under these conditions
10.6 parts of quizalofop ethyl tech is added slowly over a period of 2 hrs to form oil- in- water
emulsion.
Formations of suspension concentrate of Imazethpyr:
In a vessel fitted with high shear mixer is added 24.2 parts by weight of DM water, 0.3 parts
silicone defoamer, 2.5 parts acrylic graft copolymer, 2.0 parts nonyl phenol ethoxylate, 5.0 parts
propylene glycol. Under high shear mixing 20.5 part by weight Imazethapyr technical is added
slowly and material pulverized in a horizontal pressurized bead mill.
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Formation of suspoemulsion of Quizalofop ethyl 10% + Imazethapyr 20%:
In a post mixing vessel is transferred the above prepared suspension concentrate of Imazethapyr
54.7 parts by weight. Under continuous mixing is then changed 35 parts by weight of above
prepared oil-in-water emulsion of Quizalofop ethyl technical. The material is mixed and 0.3 parts
by weight of trisiloxane ethoxylate (HS grade 429 of M/s Momentive) is added.
Finally 10 parts by weight, 2% aqueous solution of xanthen gum is added and material mixed till
homogenized to form viscous flowable suspo emulsion of Quizalofop ethyl 10% and Imazethapyr
20%.
The invention will now be explained with the help of the experiments conducted in the fields.
Experiment 1: Bio-efficacy & Phytotoxicity of Quizaofop ethyl 10% + Imazethapyr
20% WG against Mixed Weed flora of Soybean
The Bio-efficacy & Phytotoxicity were conducted in Hasanapur, Tal- Tivasa, Dist- Amaravati of
Maharashtra.
Crop Stage at the time of experimentation: 17 Days
Stage of Weed flora (Leaf Stage & Height): Narrow Leaf weeds: 2-4 leaf, 1-4 cm
Broad Leaf Weeds: - 1-2 leaf, 1-4 cm
Date of Sowing: 4/07/2015
Date of Treatment: 21/07/2015
Name of Weed Flora:
Narrow Leaf weeds: Cynadon dactylon, Echinochola spp., and Digiteria spp.
Broad Leaf Weeds: Parthenium sp., Euphorbia geniculata, Cynnotis sp., Ageratum conyzoidas,
Xanthium strumarium, Commelina benghalensis, and Digera arvensis
Sedges: Cyperus rotundus
The following treatments were conducted are as follows:
S.
No. Treatments
Treatment
No.
1 Quizalofop ethyl 10% + Imazethapyr 20% WG @125g/acre +Surfactant@225 ml/acre T-1
2 Quizalofop ethyl 10% + Imazethapyr 20% WG @150 g/acre+Surfactant@225 ml/acre T-2
3
Quizalofop ethyl 10% + Imazethapyr 20% WG @125 g/acre + Ammonium Sulphate
@300 g/acre+Surfactant@225 ml/acre
T-3
4
Quizaofop ethyl 10% + Imazethapyr 20% WG @150 g/acre + Ammonium
Sulphate@300 g/acre+Surfactant@225 ml/acre
T-4
5 Imazethapyr 70% WDG @ 50 g /acre T-5
6 Quizalofop Ethyl 5%EC@ 300 ml/acre T-6
7 Control T-7
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The table below provides the results of the various treatments mentioned above. The data was
collected as Number of weeds/sq.m (Mean of three places/treatment)
Narrow Leaf Broad Leaf Sedges
Treatments Pre 7 DAT* 15 DAT Pre 7 DAT 15 DAT Pre 7 DAT 15 DAT
T-1 65.33 0 0 53.66 5.66 0.00 5.33 5.33 5.33
T-2 29.66 0 0 76.66 11.66 0.00 2.66 2.66 2.66
T-3 17.33 0 0 56.33 3.66 0.00 3.33 3.33 3.33
T-4 27.33 0 0 69.33 16.33 0.00 1.66 1.66 1.66
T-5 33.33 0 0 92.33 11.66 0.00 2.33 2.33 2.33
T-6 41.33 0 0 103.66 103.66 103.66 3.66 3.66 3.66
T-7 29.33 32.33 32.33 106.66 113.33 113.33 6.33 6.33 6.33
*DAT: Days After Treatment
The results above provide that the T4 i.e. the composition of Quizalofop ethyl 10% +
Imazethapyr @ 20% WG @ 150 g/acre + Ammonium sulphate @ 300 g/acre + Surfactant @
225 ml/acre gave the best control over other treatments because-
 Provided the faster killing of weeds over other treatments
 Less Growth suppression (Yellowing) over other treatments
 Less number of new weeds germination over other treatment
T1 and T2 shown the crop yellowing and stunted growth up to 15 days while T3 and T5 provides
less yellowing and stunted growth of crop.
New germination of weeds flora are seen at 15 DAT in all treatments
Experiment 2: Efficacy & Phyto-toxicity of Quizaofop ethyl 10% + Imazethapyr 20%
WG against Mixed Weed flora of Soybean
The Bio-efficacy & Phyto-toxicity were conducted in Village Berkheda (Doraha) Thesil Shyampur
Crop Stage at the time of experimentation: 22 day old crop
Stage of Weed flora (Leaf Stage & Height): Narrow Leaf weeds: 2-4 leaf stage, 1-4inch
Broad Leaf Weeds: 2-5 leaf stage, 1-5 inch
Date of Sowing: 24 June 015
Date of Treatment: 16 July 2015
Name of Weed Flora:
Narrow leaf weeds: Echinochloa colonum, Echinochloa crusgalli,Dinebra sp. Elusine Indica,
Hemarthria sp.
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Broad leaf weeds: Commelina benghalensis, Cynnotis sp.
Spray Solution: 120 liter / acre
Methodology: Taken the recommended quantity as per treatment and sprayed with the help of
flood jet nozzle thru knap sack pump
Observations: Marked 1 sq.m area at 3 places/ treatment and counted the weeds as per
observation table and written the mean value of weeds in below table
Treatments details:
The observation were taken on 7 day after sowing. It was observed that in all the treatments
given, sever yellowing in T1 to T5 to the main crop as compared with Control plot and T6.
Further the growth of all narrow leaf weeds was checked which showed yellowing and slight
violet in color, which clearly separates the Soybean from weeds in all the treatments. Some
yellowing and suppression in growth observed in Cyprus rotundus in T1 to T5. Broad leaf weeds
shown significant effects includes yellowing and stunting of growth in T1 to T5.
Table: Number of weeds/sq.m (Mean of three places/treatment)
Tr.
Number of weeds/Sq.mt ( Mean of 3 places /treatment) and % mortality
NARROW LEAF WEEDS BROAD LEAF WEEDS SEDGES WEEDS
Pre Spray
7 DAS
% Mortality
**15 DAS
% mortality
Pre Spray
7 DAS
% Mortality
15 DAS
% Mortality
Pre Spray
7 DAS
% Mortality
15 DAS
% Mortality
T-1 133 104 22 84 37 27 11 60 8 70 4 4 0 4 0
S.
No. Treatments
Treatment
No.
1
Quizalofop ethyl 10% + Imazethapyr 20% WG @125 g/acre+Surfactant@225
ml/acre
T-1
2
Quizalofop ethyl 10% + Imazethapyr 20% WG @150 g/acre+Surfactant@225
ml/acre
T-2
3
Quizalofop ethyl 10% + Imazethapyr 20% WG @125 g/acre +Ammonium
Sulphate @300 g/acre+ Surfactant @225 ml/acre
T-3
4
Quizaofop ethyl 10% + Imazethapyr 20% WG @150 g/acre +Ammonium
Sulphate@300 g/acre+Surfactant@225 ml/acre
T-4
5 Imazethapyr 70% WDG @ 50 g /acre T-5
6 Quizalofop Ethyl 5%EC@ 300 ml/acre T-6
7 Control T-7
15
T-2 123 39 68 27 78 152 56 63 40 74 44 44 0 44 0
T-3
137 92 33 84 39 196 48 76 48 76 20 20 0 20 0
T-4
248 80 68 44 82 336 88 74 68 80 0 0 0 0 0
T-5
220 140 36 92 58 288 56 81 56 81 4 4 0 0 0
T-6 223 67 70 38 83 118 118 0 118 0 4 4 0 4 0
T-7
Con
trol
268 268 0 268 0 128 128 0 128 0 172 172 0 172 0
NOTE: ** The left over weeds were Hemarthria sp, which is a perennial grassy weed
The best results were observed in T4 i.e. Quizaofop ethyl 10% + Imazethapyr 20% WG @150
g/acre +Ammonium Sulphate@300 g/acre+Surfactant@225 ml/acre in regards of narrow, broad
and sedges which also confirms with the data table above.
ADVANTAGES OF THE PRESENT INVENTION
Owing to the unique process of manufacture, the liquid composition increases the amount of
crop yield significantly which is attributable to its homogeneity. Further, the presence of the
special surfactant ensure direct adhesion of the composition on the weed which quickens the
rate of weed death and saves loss of valuable nutrients from the soil.

We claim:
1. A herbicidal and weedicidal composition comprising:
(a) Quizalofop-ethyl in an amount of 5-15% by weight,
(b) Imazethpyr in an amount of 10-40% by weight,
(c) One or more excipients in an amount of 45-85% by weight.
2. The composition as claimed in claim 1, wherein the composition is prepared in the form
of emulsifiable concentrate, suspo-emulsion and wettable granule.
3. The composition as claimed in claim 1and 2, wherein the excipients are selected from the
group of
- polar organic solvent in an amount of 20-30% by weight,
- non polar organic solvent 50-65%by weight,
- wetting agent in an amount of 4-10% by weight,
- dispersing agent in an amount of 5-10% by weight,
- binder in an amount of 0.5-3% by weight,
- emulsifiers in an amount of 5-20% by weight,
- disintegrating agent in an amount of 3-15% by weight,
- stabilizers in an amount of 0.5-3% by weight,
- anti-coagulating agents and anti-freeze agents in an amount of 5-8% by
weight,
- anti-foaming agents in an amount of 0.3-1% by weight,
- pH buffer in an amount of 5-10% by weight, and
- inerts in an amount of 20-50% by weight,
either alone or in combination thereof.
4. The composition as claimed in claims 1 and 2, wherein emulsifiable concentrate
formulation comprises solvent selected from N-methyl pyrrolidone, Dimethyl sulfoxide
and aromatic hydrocarbon or combination thereof.
5. The composition as claimed in claim 3, wherein the emulsifiers are selected from the
group consisting of anionic and non-ionic emulsifiers in emulsifiable concentrate
formulation.
17
6. The composition as claimed in claim 5, wherein the anionic emulsifier is selected from
the group consisting of Calcium alkyl benzene sulfonate, preferably calcium dodecyl
benzene sulphonate.
7. The composition as claimed in claim 5, wherein the non-ionic emulsifier is selected from
the group consisting of nonyl phenol ethoxylate, Octyl phenol ethoxylate, Castor oil
ethoxylate, Tristyrenated phenol ethoxylate, tweens either alone or in combination.
8. The composition as claimed in claim 3, wherein the stabilizer is selected from epoxydised
vegetable oils such as epoxidised soyabean oil in emulsifiable concentrate formulation.
9. The composition as claimed in claim 3, wherein the wetting agent is selected from
anionic surfactants in wetteble granule formulation.
10. The composition as claimed in claim 9, wherein the anionic surfactants is selected from
the group consisting of salts of alkyl benzene sulphonates, alpha olefin sulphonates, alkyl
phenol ethoxylates, sodium salts of alkyl sulphates and alkyl sulphosuccinates or
combination thereof preferable sodium lauryl sulphate.
11. The composition as claimed in claims 1 and 2, wherein wetteble granule formulation
comprises dispersing agents selected from the group consisting of polycarboxylates, alkyl
naphthalene sulphonates, phenol sulphonic acid condensates, sodium salt of ligno
sulphonates, N-methyl-N-oleyl taurate, Acrylic polymer more preferably acrylic polymer.
12. The composition as claimed in claims 1 and 2, wherein wetteble granule formulation
comprises binding agent selected from the group consisting of polyvinyl pyrollidone,
polysaccharides, partially hydrolysed polyvinyl acetate or disaccharides and preferable
polyvinyl pyrollidone.
13. The composition as claimed in claims 1 and 2, wherein wetteble granule formulation
comprises disintegrating agents selected from the group consisting of ammonium
sulphate, urea, mono-di and triammonium phosphate and sodium carbonates.
14. The composition as claimed in claims 1 and 2, wherein wetteble granule formulation
comprises inert carriers selected from the group consisting of starch, calcite, kaolin,
montmorillonite or attapulugite clay, china clay and diatomaceous earth.
18
15. The composition as claimed in claims 1 and 2, wherein the oil in water emulsion
prepared by using dispersing agent, wetting agent defoaming agent and organic solvent.
16. The composition as claim in claim 15, wherein the dispersing agent is a salt of
tristyrenated phenol etoxylate phosphate etc.
17. The composition as claimed in claim 15, wherein the wetting agent is an alkyl phenol
ethoxylate.
18. The composition as claimed in claim15, wherein the organic solvent is vegetable oil.
19. The composition as clamed in claim 15, wherein the defoaming agent is a silicone based
defoaming agent.
20. The composition as claimed in claims 1 and 2, wherein the suspo emulsion formulation
comprises suspension concentrate prepared by using a solvent, wetting agent, dispersing
agent, ant freezing agent, penetrating agent, defoaming agent and rheology modifier.
21. The composition as claimed in claim 20, wherein the dispersing agents is an acrylic graft
polymer.
22. The composition as claimed in claim 20, wherein the anti-freeze agent is a polyglycol
preferably propylene glycol and the rheology modifier is a natural gum preferably the
Xanthan gum.
23. The composition as claimed in claim 20, wherein the defoamer is a silicone based
defoaming agent and the penetrant is a trisiloxane ethoxylate HS grade
24. A method of manufacturing the emulsifiable concentrate formulation comprising:
- making a homogenous blend of the excipients ,
- mixing Imazethapyr to the homogenized blend till solubilized,
- adding Quizalofop ethyl followed by a combination of anionic and non-ionic
emulsifier and stirring the solution till complete homogenization is attained,
- adding stabilizer and mixing till homogenization is complete.
25. A method of manufacturing the suspo-emulsion comprising:
19
- adding 10-40% by weight of Imazethapyr to an aqueous solution of wetting
agents, dispersing agents, anti-coagulating agents, anti-freeze agents, antifoaming
agents, penetrating agent and pH buffer, and
- micronizing in a horizontal pressurized bead mill to a particle size D90 less than 7
micron,
- adding the emulsifiable concentrate of quizalofop ethyl (5-15%) to form a stable
homogeneous suspension, and
- adding stabilizers such as viscoelastic products such as xantham gum, polyvinyl
alcohol, natural gums.
26 A method of manufacturing the wettable granules comprising:
- making dough of Imazethapyr (10-40%), quizalofop ethyl (5-15%), inerts,
wetting agent, dispersing agent, disintegrating agent, an organic acid and
inorganic base and required quantity of water,
- extruding the dough in a basket extruder having sieve aperture 0.8-1.0 mm,
- drying extruded granules on fluid bed drier at a temperature of 50-70°C.

Documents

Orders

Section Controller Decision Date
Section 25 (1)(Refused ) Rajendra Lohiya 2023-09-04
Section 15 (Refused ) Rajendra Lohiya 2023-09-04

Application Documents

# Name Date
1 344-DEL-2015-Correspondence to notify the Controller [31-08-2023(online)].pdf 2023-08-31
1 Form 3.pdf 2015-03-12
2 13694-4_Provisional Specification.pdf 2015-03-12
2 344-DEL-2015-Correspondence to notify the Controller [30-08-2023(online)].pdf 2023-08-30
3 Description(Complete) [05-02-2016(online)].pdf 2016-02-05
3 344-DEL-2015-PreGrant-HearingNotice-(HearingDate-01-09-2023).pdf 2023-08-10
4 Form 18 [10-08-2016(online)].pdf 2016-08-10
4 344-DEL-2015-RELEVANT DOCUMENTS [08-08-2023(online)].pdf 2023-08-08
5 344-DEL-2015-FORM-26 [15-09-2021(online)].pdf 2021-09-15
5 344-DEL-2015-FER.pdf 2018-07-17
6 344-DEL-2015-OTHERS [14-01-2019(online)].pdf 2019-01-14
6 344-DEL-2015-OTHERS [02-09-2021(online)].pdf 2021-09-02
7 344-DEL-2015-PRE GRANT OPPOSITION DOCUMENT [02-09-2021(online)].pdf 2021-09-02
7 344-DEL-2015-FER_SER_REPLY [14-01-2019(online)].pdf 2019-01-14
8 344-DEL-2015-PRE GRANT OPPOSITION FORM [02-09-2021(online)].pdf 2021-09-02
8 344-DEL-2015-COMPLETE SPECIFICATION [14-01-2019(online)].pdf 2019-01-14
9 344-DEL-2015-OTHERS [31-01-2020(online)].pdf 2020-01-31
9 344-DEL-2015-Proof of Right (MANDATORY) [18-01-2019(online)].pdf 2019-01-18
10 344-DEL-2015-FORM-26 [18-01-2019(online)].pdf 2019-01-18
10 344-DEL-2015-PRE GRANT OPPOSITION DOCUMENT [31-01-2020(online)].pdf 2020-01-31
11 344-DEL-2015-Power of Attorney-250119.pdf 2019-01-30
11 344-DEL-2015-PRE GRANT OPPOSITION FORM [31-01-2020(online)].pdf 2020-01-31
12 344-DEL-2015-Correspondence-250119.pdf 2019-01-30
12 344-DEL-2015-OTHERS-250119.pdf 2019-01-30
13 344-DEL-2015-Correspondence-250119.pdf 2019-01-30
13 344-DEL-2015-OTHERS-250119.pdf 2019-01-30
14 344-DEL-2015-Power of Attorney-250119.pdf 2019-01-30
14 344-DEL-2015-PRE GRANT OPPOSITION FORM [31-01-2020(online)].pdf 2020-01-31
15 344-DEL-2015-FORM-26 [18-01-2019(online)].pdf 2019-01-18
15 344-DEL-2015-PRE GRANT OPPOSITION DOCUMENT [31-01-2020(online)].pdf 2020-01-31
16 344-DEL-2015-OTHERS [31-01-2020(online)].pdf 2020-01-31
16 344-DEL-2015-Proof of Right (MANDATORY) [18-01-2019(online)].pdf 2019-01-18
17 344-DEL-2015-PRE GRANT OPPOSITION FORM [02-09-2021(online)].pdf 2021-09-02
17 344-DEL-2015-COMPLETE SPECIFICATION [14-01-2019(online)].pdf 2019-01-14
18 344-DEL-2015-PRE GRANT OPPOSITION DOCUMENT [02-09-2021(online)].pdf 2021-09-02
18 344-DEL-2015-FER_SER_REPLY [14-01-2019(online)].pdf 2019-01-14
19 344-DEL-2015-OTHERS [14-01-2019(online)].pdf 2019-01-14
19 344-DEL-2015-OTHERS [02-09-2021(online)].pdf 2021-09-02
20 344-DEL-2015-FORM-26 [15-09-2021(online)].pdf 2021-09-15
20 344-DEL-2015-FER.pdf 2018-07-17
21 Form 18 [10-08-2016(online)].pdf 2016-08-10
21 344-DEL-2015-RELEVANT DOCUMENTS [08-08-2023(online)].pdf 2023-08-08
22 Description(Complete) [05-02-2016(online)].pdf 2016-02-05
22 344-DEL-2015-PreGrant-HearingNotice-(HearingDate-01-09-2023).pdf 2023-08-10
23 344-DEL-2015-Correspondence to notify the Controller [30-08-2023(online)].pdf 2023-08-30
23 13694-4_Provisional Specification.pdf 2015-03-12
24 Form 3.pdf 2015-03-12
24 344-DEL-2015-Correspondence to notify the Controller [31-08-2023(online)].pdf 2023-08-31

Search Strategy

1 searchstrategy344-del-2015_17-07-2018.pdf