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Field of the Invention
The present invention relates to a synergistic insecticidal combination
formulation of a phenylthio urea compound and a neonecotinyl compound in
wettable powder form and a process for preparation thereof for pest control.
Background of the Invention
Various chemicals and their formulations have been developed and are currently
in use for effective control of pest and insects. Due to non-judicious use of
hitherto known pesticides, the pest gain resistance and is hard to kill. Physically
compatible pesticide mixtures exhibit a better pest management. Processes for
insecticidal agents and compositions have been developed to control insect, pest
and in practice have been used as a single or a mixed agent. However, processes
for economically and ecologically safe insect control composition are still
being sought. The development of combination formulation is necessitated
because of resistance developed of the continued use and over and above at
higher dosage which becomes detrimental to the environment also. For the
protection of crop and the environment the activity of the pesticide be improved
and the activity should be persistent over a period of time.
A further problem associated with liquid formulation comprising solid pesticide
results from tendency of crystalline materials to form large crystal upon aging
resulting in increased setting of solid. Solid pesticidal composition such as
wettable powder and soluble powder (WPISP) and water dispersible or soluble
granules (WGISG) containing combination of agriculture actives with different
mode of action can be difficult to produce and store due to tendency to
physically degrade and agglomerate to cake when subject to range of
temperature and shear stress normally encountered during processing and
storage .In addition these compositions may suffer from poor dispersion in
water and poor delivery of the active ingredient to the locus of the pests
requiring control of elimination.
Certain mixture of active ingredients are proposed in literature for controlling of
pest. However the biological properties of these mixture of known compounds
are not entirely satisfactory in the field of pest control, that is why a demand for
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providing further mixture having synergistic pesticidal properties in particular
for controlling pests.
To develop a stable pesticide formulation which also exhibits satisfactory
pesticidal action is a challenge for the skilled person. A central parameter in
formulation technology is the control of physio chemical properties of the
pesticide, both in the formulation per se and the application form of the
formulation e.g. in tank mix, where in the respective formulation is diluted with
water.
The prior art utilized combination formulation of Acetamiprid with several agro
chemicals active substances to increase its spectrum for controlling pests.
Similarly attempts have been made to broaden spectrum of Diafenthiuron by
making its combination formulation with other agro chemical active substances.
US 20 120220463 discloses a form of crystalline complex of Acetamiprid with
4-Hydroxy Benzoic acid .The art requires a free flowing powder formulation of
Acetamiprid which does not cake on storage and inorder to accomplish the same
combination formulation with Diafenthiuron has been designed. Diafenthiuron
is a fi-ee flowing crystalline material and thus it provided a grinding aid to
Acetamiprid.
EP 0736252A2 describes synergistic combination formulation of Diafenthiuron
with various agro chemically active compounds including Acetamiprid for
controlling diverse nature of insects. This describes preparation in the form of
emulsifiable concentrate, dusting powder and suspension concentrates.
EP 2534951 describes a method of transgenic plant production potential
utilization involving utilizing of a plant with an effective quantity of
Diafenthiuron and Acetamiprid and their combination.
CN102626077 discloses an ultra low volume liquid composition containing
Flubendamide as active ingredient (I) and diafenthuron or Acetamiprid as active
ingredient( 11) in the combination formulation for controlling pest attack by
ultra low volume spraying ,low volume spraying or ultra low volume
electrostatic spraying.
WO 20 12 10 1659 describes a pesticidal composition comprising an effective
amount of Sulphur and effective amount of at least one insecticide selected fi-om
Diafenthiuron, Fipronil, Acetamprid and Abamectin.
CN 102 1 135 10 describes a composition containing Metaflumizone as active
ingredient( I) and Diafenthiuron or Acetamiprid as in ingredient (11). The
composition prepared exhibits synergy and the combination also deferred the
resistance developed by use of Chlorantraniliprole.
CN 1021 135 16 describes an invention of a combination formulation of
Chlorantraniliprole as active ingredient (A) and Diafenthiuron or Acetamiprid
as an active ingredient ( B). The Invention describes that on reducing the dosage
of active ingredient (A) the drug resistance of insect and mites on the
Chlorantraniliprole is reduced.
DE 102009028001 describes use of an active agent combination comprising at
least a 3-phenyl-1-aza-spiro (4, 5) dec-3-en-2-one as compound (1) and one or
more Insecticidal IAcaricidal agentor controlling animal pests where
insecticidal/acaricidal agent is Acetamiprid or mite growth inhibitor
Diafenthiuron.
CN 101589722 discloses a synergistic combination formulation of Emamectin
Benzoate or Abamectin as component (1) and Acetamiprid or Diafenthiuron as
component (2) for controlling agriculture, forestry and gardening insects and
pests.
EP 2090 170 describes a combination formulation of 1 - {2,4-dimethyl-5-(2,2,2-
trifluro ethane sulfinyl> phenyll-3-trifluoromethyl-lH-(1, 2, 4) Triazole as
active ingredient (1) and insecticidelacaricide Acetamiprid or Diafenthiuron as
active ingredient( 2). The composition exhibits synergistic effect.
Diafenthiuron is an insecticide and acaricide which kills larvae, nymphs and
adults by contact/stomach action and also exhibits ovicidal action. It inhibits
ATPase in mitochondria and blocks utilization of energy (ATP). It is rapidly
desulhrated abiotically by light or in vivo to the corresponding carbodimide
which is an inhibitor of mitochondria1 respiration. It is effective against mites,
aphids and jassids in cotton, various field and h i t crops, ornaments and
vegetable.
Diafenthiuron is the common name of 1-@- butyl-3-(2, 6-Di-isopropyl
phenoxyphenyl) thiourea. It is white to off white powder with the following
physic- chemical properties:
Melting point - 146.6- 147.7" C
Solubility: In water 0.06mglL (25"C), In Ethanol 43, Acetone 320, Toluene
330, n-hexane 9.6, n-octanol26(all in gll25"c)
Stability: Stable in air, water and to light.
Acetamiprid is the common name of (E)-N-[(6-chloro-3-pyridyl) methyl]-Ncyano-
N-methyl acetamidine. It is off white to pale yellow powder with the
following physico- chemical properties:
Melting point - 98.9"C,
Solubility in water - 25gdl at 25°C
V.P. < 1 .OX10 m Pa at 25"c
Stable at PH 5-8 and is stable in most organic solvent e.g. acetone, ethanol,
methanol, chloroform, dichloromethane, acetonitrile.It is stable under normal
storage conditions and unstable above 45°C. Hazardous decomposition products
are carbon monoxide and hydrogen chloride.
Diafenthiuron has very poor solubility in water and has high melting point and
is formulated as wettable powder and aqueous suspension concentrate.
Acetamiprid is soluble in water and has low melting point and is formulated as
soluble powder, emulsifiable concentrate and water dispersible granule
formulation. (Ref. CN102919223A). It has poor flow ability and low
amorphous structure resulting processing difficulties , formulation instabilities
and application unreliability due to caking and setting of fine particles.
Hence there is a long felt need to develop an alternative, simple and efficient
process for the preparation of insecticidal composition which allows reduced
effective dosage rates, increased environmental safety and lower incidence of
insect resistance. Also a need to develop a composition that addresses the
problem of resistance, controls the environmental damage, offers broad crop
protection spectrum, saves labor improves plant growth and cost effective.
There is a need to develop a synergistic formulation of Diafenthiuron and
Acetamiprid which diminishes the risk of exposure , provides greater handler
safety and exhibits increased bio- efficacy with reduced dosages.
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Advantages of the Present Invention
1. beneficial behaviour during formulating and upon application, for example
upon grinding, , mixing and storage spraying.
2. control vide variety and stages of the insects at lower dosages.
3. does not cake on storage and exihibits improved dispersion in water.
4. broadening of the spectrum of pesticidal activity to other pests.
5. synergistic effect is more pronounced when trisiloxane ethoxylate is
incorporated in the composition primarily to decrease foaming at the time of
spray.
Objective of the Invention
The main objective of the present invention is to provide a synergistic
insecticidal combination formulation of Diafenthiuron and Acetamiprid in
wettable powder form and a process for preparation thereof to control insect.
Another objective of the invention is to provide a combination formulation
which is better tolerated by plant i.e. they are less phototoxic and also control
the various stages of the insects.
Still another objective of the present invention is to provide a favorable
conditions with respect to grinding, mixing and storage for Acetamiprid and
Diafenthiuron.
Yet another objective of the present invention is to provide a synergistic
composition which exhibits increased efficacy with reduced dosage as
compared to the individual insecticide components.
Summary of the Invention
The present invention relates to a synergistic insecticidal combination
formulation of a phenylthio urea compound and a neonecotinyl compound in
wettable powder form and a process for preparation thereof to control insect
attack on agricultural crops. The combination formulation of Diafenthiuron and
Acetarnniprid in the wettable powder form relates to the composition
comprising of Diafenthiuron and Acetamniprid , wetting and dispersing agent ,
anti-caking agent, silicon based antifoaming agent and inert such as silica and
lavigated clay .
The process for preparation of a synergistic insecticidal composition comprises
of certain steps. Firstly antifoam agent, silica and lavigated clay are
homogenously mixed in parts by weight. Secondly Diafenthiuron , Acetamiprid
, wetting agent , dispersing agent, trisodium citrate and lavigated clay are
thoroughly mixed in parts by weight in a ribbon blender. The mass generated in
second step was mixed with mass generated in the first step. The homogenously
mixed mass of second step was air jet milled to particle size less than 20
microns and thoroughly homogenized in post ribbon blender.
Detailed Description of the Invention
The present invention relates to a synergistic insecticidal combination
formulation of Diafenthiuron and Acetamiprid in wettable powder form and a
process for preparation thereof to control insect attack on agricultural crops. The
invention fbrther relates to a method for combination formulation of
Diafenthiuron and Acetamiprid, wherein the chemical properties of both the
compounds are retained, but provides a synergistic effect by controlling vide
variety of insects at lower dosages.
According to a preferred embodiment of the present invention combination
formulation of Diafenthiuron and Acetamiprid in wettable powder comprises of
Diafenthiuron (25- 40%) , Acetamiprid (5-15%),wetting and dispersing agent
(8-12%) , inerts (35-58%) , anti-caking agent (2-5%) and deforming agent (0.1-
1.0%). Proper solution of wetting and dispersing agents, anti
cakinglagglomeration suppressant , stabilizer and defoaming agent is most
important in preventing caking, providing good dispersing and thereby
providing broad crop coverage area. The dispersing agent is a compound which
ensures that the particles remain suspended in water. The dispersing agent can
be ionic or non ionic or a mixture of such surface active agents or graft co0
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polymer dispersant . The wetting agent is a compound which facilitates rapid
wetting of the powder when added to the water . Solid inert carriers are used as
ground natural minerals such as calcite, talc, kaolin, and montmorillonite or
attapulugite . Highly disperse silica or highly disperse absorptive polymers may
also be used to improve physical properties.
In another embodiment , the dispersing agent are selected from group
comprising polycarboxilates, alkyl naphthalene sulfonates, phenol sulphonic
acid condensates, lignosulphonates, methyl oleyl taurates and poly vinyl
alcohols. The dispersing agent is present in the composition in a range of about
5-8% of the total weight of the composition .The wetting agent are selected
from group comprising alpha olefin sulfonates, sodium lauryl sulphate,
polyoxyalkylene alkyl ether, polyoxyalkylene alkyl ether, polyoxyalkylene
alkyl phenyl ether sulfonates, dialkyl succinate etc.The wetting agent in the
present composition in a range about 5-8%of the total weight of the
composition. The inert carrier ispresent in the composition in a range of about
40-55% of the total weight of the composition.
In yet another embodiment of the present invention, the composition further
comprises a silicone based antifoaming agent, a stabilizing agent and a
stabilizer. The antifoaming agent used are a blend of trisiloxane ethoxylates in
composition and are in the range of 0.1-1 .O% of the total weight of the
composition. The stabilizing agent is in the range of 1.0-5.0% of the total
weight of the composition such as stearic acid ,tricalcium phosphate , trisodium
citrate.
The present invention will be illustrated in more detail with reference to the
following formulation examples and product test results. These examples are
just illustrative and are not meant to be limiting.
The following examples illustrate the basic methodology and versatility of the
invention.
According to another preferred embodiment of the present invention , process
for preparation of wettable powder formulation of Diafenthiuron(40%) and
Acetamiprid(1 1 %) comprises of the following steps:
The antifoaming agent 0.3 parts by weight, silica 2.0 parts by weight and
lavigated clay 10 parts by weight were blended together and homogenized.
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40 parts by weight of Diafenthiuron , 11 parts by weight of Acetamiprid , 3
parts by weight wetting agent , 6 parts by weight of dispersing agent , 4 parts
by weight of trisodium citrate and 23.7 parts by weight of lavigated clay were
thoroughly mixed in a ribbon blender. The above blended mass was then mixed
with 12.3 parts by weight of material mixed in step 1.
Step 3
The homogenously mixed mass of step 2 was air jet milled to particle size less
than 20 microns and thoroughly homogenized in post ribbon blender.
The following tables illustrate the various combinations of diafenthiuron
technical (30-45%m/m) and acetamiprid (9-15%m/m) were prepared and
evaluated for synergistic effect . The below table also illustrate the composition
prepared to achieve the best suspension, wetting and storage stability.
Table 1
Preparation
Diafenthiuron
Acetamiprid
Wetting Agent
Dispersing
Agent
Antifoam
Trisodium
Citrate
Table 2
Silica
Lavigated
Clay
Total
1
30
15
3
6
0.3
4.0
2.0
39.7
100
Preparation
Diafenthiuron
2
35
13
3
6
0.3
4.0
2.0
36.7
100
5
40
3
40
11
3
6
0.3
4.0
4
45
9
3
6
0.3
4.0
2.0
33.7
100
6
40
2.0
30.7
100
7
40
8
40

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Diafenthiuron40%+ Acetamiprid 11 % WP combination has been tested against
white fly and other sucking pest complex of cotton and found that due to strong
synergy of both the compound which belongs to non neonicotioid (Thio-urea
compound) and neonicotioid given the good and long duration control of white
fly and other sucking pest at the dose of ranging from 437.5 -500 glha.
Difenthiuron is a pro insecticide, which has first to be converted to its active
form. The active compound then acts on a specific parts of the energy producing
enzyme in the mitochondria of white fly and other sucking pests of cotton
resultant into immediate paralysis of the pest after intake or contact and also
due to strong vapour action.
Acetamiprid also kills the sucking pest through contact and stomach poisoning
and also due to strong translaminar action provides the effective control of
hidden sucking pest on the dorsal side of the leaves.
The combination has very strong synergy and thus provides quick and long
duration control of sucking pest given 87.34% control of sucking pest while
Diafenthiuron has given control of 76.26% and Acetarniprid provides only
64.39% control and shown the yield enhancement of 14% & 18% as compared
to Diafenthiuron and Acetamiprid alone respectively.
1 No. of treatment : 5 1
Plant to plant Distance: 0.5 rn.
Row to row spacing : 0.5 m
Plot size: 5x3 m
No. of spray: 1
Bio-efficacy of Diafenthiuron 40% + Acetarniprid 11 % WP against cotton
whitefly.
S.N Treatme Dose Mean of No. of whiteflylleaf Per cent mortality of
o. nt (mug> (1 5 leaves15 whitefly
/ha plantsltreatment)
Pre 24 48 7 15 24 48h 7D 15D
treatm hrs hrs DA DA hrs rs AS AS
ent S S
1 Diafenthi 375 18.33 16. 11. 7.1 8.1 11. 34. 61.1 55.6
uron 20 93 3 3 62 91 0 4
40% +
Acetami
Results:
Diafenthiuron 40% +Acetarniprid 11% WP @ 437.5 g/ha and Diafenthiuron
40% + Acetamiprid 11 % WP @ 500 gha dose were at par as they exhibited
whitefly mortality 89.19, 91.70 per cent after 7 days and 90.03, 92.46 per cent
after 15 day of spray.
Diafenthiuron 40% +Acetarniprid 11% WP @ 437.5 g/ha and @500g/ha dose
showed synergistic effect and significantly superior to standard check of
Bifenthrin 10 % EC @ 800 mlha for control of whitefly after 7 and 15 days of
spray.
Although the present invention has been disclosed in terms of a preferred
embodiment, it will be understood that numerous additional modifications and
variations could be made thereto without departing from the scope of the
present invention.
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We Claim:
1. An insecticidal composition , comprising;
- diafenthiuron , ranging from 25 - 40% by w/v of said composition;
- acetamiprid, ranging fiom 5-15% by w/v of said composition;
- a wetting and dispersing agent (5-20%);
- an anticaking agent(2-5%);
- an anti foam agent (0.1 - 1 %);
- an inert carrier(35-58%); and
- a stabilizer 1-5%.
to obtain a synergistic composition in a wettable powder form.
2. An insecticidal composition as claimed in Claim 1, wherein said
wetting agent is 3% by mass of anionic surfactant and said dispersing
agent is 6% by mass of anionic sulphate surfactant.
3. An insecticidal composition as claimed in Claim 1, wherein said
stabilizer is 4% by mass of citric acid.
4.An insecticidal composition as claimed in Claim 1, wherein said inert
carrier are silica and lavigated clay.
5. An insecticidal composition as claimed in Claim 1 , wherein said anti
foam agent used are a blend of trisiloxane ethoxylates.
6.An insecticidal composition as claimed in Claims 1 and 2 , wherein said
wetting agent is selected fiom a group comprising polyoxyallcylene alkyl
ether, polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether
sulfonates and dialkyl succinate etc.
7. An insecticidal composition as claimed in Claims 1 and 2 ,wherein said
dispersing agent is selected from group comprising polycarboxilates,
alkyl naphthalene sulfonates, phenol sulphonic acid condensates,
lignosulphonates, methyl oleyl taurates and poly vinyl alcohols.
8. A process for preparing wettable powder insecticidal composition as
claimed in any of the above preceding claims, comprising steps of:
- mixing of antifoaming agent and an inert parts by w/v in a blender to
form a mass;
- adding said mass to a mixture of Diafenthiuron , Acetamiprid , wetting
agent , dispersing agent , trisodium citrate and lavigated clay parts by
weight in a ribbon blender to generate a mixture mass; and
- micronization of said mixture mass with the help of air jet mill.
9.A process for preparing wettable powder insecticidal composition, as
claimed in Claim 8 , wherein said dispersing agent is silica poly ether
copolymer.
10. A process for preparing wettable powder composition , as claimed in
Claim 8, wherein said mixture mass are air milled to average particle size
of less than 20 microns.
11. An insecticidal composition as claimed in any of the proceeding
claims substantially as herein described with reference to foregoing
examples.
12. A process for preparing wettable powder form insecticidal
composition as claimed in any of the proceeding claims substantially as
herein described with reference to foregoing examples.