FORM-2
THE PATENTS ACT, 1970
COMPLETE SPECIFICATION
SECTION 10
TITLE A PROCESS FOR THE GRANULAR PREPARATION OF
SYNERGISTIC INSECTICIDAL COMPOSITION.
APPLICANT(S) : UNITED PHOSPHORUS LIMITED, UNIPHOS HOUSE, C D. MARG, KHAR
(WEST), MUMBAI-400 052, MAHARASHTRA, INDIA, INDIAN COMPANY.
The following Specification particularly describes and ascertains the nature of this invention and the manner in which it is to be performed:-

Hie present invention relates to a process for the granular preparation of synergistic insecticidal
composition of two active insecticides Cypermethrin and Acephate.
The protection of crops and its produce from pest damage is essential in agriculture produce enhancement. To help combat these problems, various chemicals and its formulation- were invented in effective management of pests,

Insecticides of many types and groups are reported in the literature and a large number are in use, commercially, for effective control of pests in agriculture.
Li many cases, active insecticides have shown more effectiveness in combination than when applied individually. Since the combination demonstrates a potency and activity level exceeding that, which might be expected, from a mere addition of the individual potencies of the components, are mere by called as 'synergism'. The present invention highlights the synergistic effect of combination of two known active insecticides "Cypermethrin" and "Acephate", Both individual insecticides, forming this combination, which is the subject of this invention are known to be potent insecticides, for their activity independent of each other.
In modern agriculture scenario, where insect has attained resistance, due to indiscriminate and non-judicious use of pesticide, in view to manage insect pests for a desire of higher yields and those insects which are hard to kill by the existing commercial insecticides solely and in cyclic spray mixtures, warrants invention of a potent synergistic insecticidal composition,
Cypermethrin and Acephate in a synergistic composition can have higher potentiation, as insecticide, and is highly effective in controlling pests including even hard to kill pests. The synergic composition gives a quick knockdown kill of the pests. It is comparatively more persistent. It penetrates deep in leaves, killing many internal feeders. It is strongly active as a contact and stomach insecticide. It is especially a potent lethal weapon to kill, hard-to-kill, resistance pests, which are normally not controlled by other insecticides. The said mixture of the insecticides has the good effect for controlling Cotton bollworms and sucking pests. Its toxicity is low and safe for human and animals. Its residue is also small.
The name Cypermethrin an insecticide, belongs to synthetic pyrethroid group describes a chemical substance having a solubility in water of 0.004 m§/\ (at pH7); corresponds to a mixture of cis and trans isomers having following formula:

2

So being almost insoluble in water, it is soluble in acetone/chloroform cyclohexanone, xylene >450 (g/1); ethanoi 337 (g/i), hexane 103 (g/1) at 20°C.
Cypermethrin is presently recognised as the non-systemic insecticide with contact and
stomach action. It also exhibits antifeeding action and good residual activity on treated
plants. It is used to control a wide range of insects, especially Lepidoptera, but also
Coleoptera, Dipetera, Hemiptera and other classes in fruits ( including Cirrus), Vines,
Vegetables, Potatoes, Cucurbits, Lettuce, Capsicums, tomatoes, cereals, maize,
soyabeans., cotton, coffee.. Cocoa., rice., peacans, oilseed rape, beet, ornamentals,
forestry, etc. It is also used for control of flies and other insects in animal houses; and
mosquitoes, Cockroaches, houseflies and other insect, pests in public health. It is also
used as an animal ectoparasiticide.
. ~
Presently Cypermethrin is most preferably formulated in the form of emulsifiable concentrate (EC) which consists of Cypermethrin active ingredient dissolved in solvent(s) alongwith surfactants at a levels required to give maximum stability with the formation of homogeneous emulsion on dilution. The use of organic solvenr(s) is disadvantageous from environmental and cost view point. These organic solvents may exhibit toxicity and side-effects which may be adverse to the effect of the agricultural chemical itself or to the plant or crop as a whole or to its parts produced in treated fields. They show hazards during manufacturing, filling, packing, storage, transit, and use. During use dermal and respiratory toxic exposure to user are frequently observed. By using the organic solvents percutaneous toxicity and inflammability may also occur.

It is a systemic insecticide of moderate persistence with residual activity lasting about 10-15 days. It is effective against a wide range of aphids, leaf miners, lepidopterous larvae, sawflies and thrips. It is non-phytotoxic on many crop plants. Technical grade Acephate (purity 80-90%) is a colourless solid; melting point 82-89°C; solubility at room temperature : about 650 g/1 water ; > 100 g/1 acetone, ethanoi; < 50g/I aromatic solvents.
The formulation of Acephate presently in use is Acephate 75% Soluble Powder (SP) consists of Acephate active ingredient 75% (w/w), Surfactant 1 to 2% (w/w), inert filter
' 3 *

(Precipitated Silica) to make 100% (w/w). It poses the problems like dust, low pourability, high transportation cost, high capital manufacturing investment, not easily measurable, difficulties in packing material disposal, handling problems, high risk of caking and others.
The earlier known art discloses about a composition of both these compounds in 0.5 to 5% Cypermethrin and 10 to 40% Acephate combination in liquid formulation EC and has claimed the synergic effect (Patent No. CN 1110082).
To have it in liquid formulation (EC) the technical(s) has to be dissolved in solvents preferably organic solvent/a mixture of solvent(s) alongwith surfactants. The disadvantage is that the organic solvents) used have a bad effect on environment and also adds the cost to the product. These organic solvents) may exhibit toxicity and side effect which may be adverse to the effect of the agricultural chemicals itself or to the plant or crop as a whole or its parts produced in the treated fields: During manufacturing filling packing, storage, transit and use they show hazards. During use the dermal and respiratory toxic exposure to user are frequently observed. By using organic solvent(s) percutaneous toxicity and flammability may also occur.
The present invention minimises dermal and respiratory toxic exposure to users, also eliminates the percutaneous toxicity and flammability hazard since it does not contains any organic solvent. The product provided by this invention is relatively more advantageous and exhibit very desirable characteristics noted herein after. It is thus, an object of the present invention to provide dust free granules of insecticide Cypermethrin containing concentration in the range of 0.1 to 10.0% (active ingredient) + Acephate containing concentration in the range of 1.0 to 50.0% of active ingredient. It is a further object of the present invention to provide method for making such dry flow, low compact, dust free, granular compositions.
The granular composition prepared by the prefered method and the [refered composition of the present invention provides dust free ; good pourability; low transportation cost ; low capital investment; good stability of product ; free flowability ; free from Solvents/Less solvent; no exposure to solvent vapours during manufacturing, storage, transit and use ; less Expensive packing ; minimum contamination of packing material ; can be packed in Environment friendly packings like Water soluble Sachets/bags ; easy to measure ; best utilization of energy sources ; less wastage during processing ; better bioefficacy ; easy disposal of packing material; easy to handle ; limited risk of Caking ; safe during storage, transit and use ; good dispersibility ; good resistance to attrition ; semi skilled operator required ; less space required for production ; with good market potential ; easily reproducible during processing ; less risk of inhalation and irritation ; spillage is easy to collect and clean ; less health hazards to operators ; optimum coverage per application ; sustained action for longer effect ; no need to prepare slurry or paste simply to pour into water ; less expensive ; use of less surfactant (s).
. 4 .

Both of these compounds are capable of controlling a large spectrum of insects especially Lepidoptera, Coleoptera, Diptera, Hemiptera and other class in fruits, vegetables, ornamentals etc. Cypermethrin is distinguished for its sudden shock effect alongwith good residual activity on treated plants. Acephate is a systemic insecticide of moderate persistence with residual activity and is effective against a wide range of aphids, leafminers, lepidoptrous larvae, sawflies and thrips. It is non phytotoxic on many crop plants.
In the present invention, the two effects i.e. residual activity and antifeeding action are synergistically combined into a formulation of improved (high yielding) efficiency assuming that the dosage (mass of active ingredients per hectare) significantly lesser than that required, when these two components are utilised separately, under identical conditions, and also reduces the chances of resistance development (which will result when a single active ingredient is used for a long time and in high doses). It is also providing a ready to use, compatible plant-mix in an effective synergistic composition along with the improvement in insecticidal activity
The present invention provides a process to find out a synergistic composition of "Cypermethrin" and "Acephate" and the process for preparing the synergistic mixture with solubilizer, wetting cum dispersing agent, emetic agent, antifoaming agent, anticaking agent, dye and fillers.
The preliminary pilot trials of various strength of Cypermethrin and Acephate carried to find out the composition, of Cypermethrin + Acephate, which exhibits optimum synergistic value.
The process for the preparation of synergistic insecticidal composition in the form of dry flow, low compact, dust free granules of Cypermethrin + Acephate comprises of the following steps :
* the required quantity of Cypermethrin technical is premixed with specified quantity of solubilizer and emetic agent to prepare a spray solution (A);
* the required quantity of Acephate technical is premixed with specified quantity of wetting cum dispersing agent, emetic agent, antifoaming agent, disintegrating agent, anticaking agent, dye and required inert filler(s). Thereafter grinded to achieve intimate and efficient mixing of particles. The grinded mixture is then post mixed to have a homogeneous mixture of all these (B);
* thereafter the above prepared spray solution (A) is sprayed on the homogeneous mixture (B) and again mixed thoroughly for sufficient time to have a homogeneous bulk which (on passing quality tests) is feed through a screw feeder into the hopper of granulator for granulation. After which these granules are processed for sizing and sieving. The fines collected are recycled. The product obtained is with synergistic insecticidal composition in the form of dry flow, low compact, dust free granules of Cypermethrin + Acephate.
* the granules are tested for required quality specifications and on passing filled and packed in desired packing . This granulation technique gives 99.5% of yield conversion. The granules with incorporation of inert ingredients, by proper choice, enjoys all the formulation advantages as discussed before. All the advantages makes it beneficial from economic aspect, handling aspect and shows a very good performance during application.
: 5 :

We have found that by using (1) Cypermethrin technical (with cis-isomer 45-80%); (2) Acephate technical; (3) solubilizer ; (4) emetic agent; (5) thereafter spraying a solution of (1), (3) and (4) on a homogeneous mixture of (2) Acephate technical and Disintegrating agent, Antifoaming agent , Wetting cum dispersing agent, Anticaking agent, Dye(s) , Fillers) and mixing thoroughly to produce homogeneous bulk; (6) feeding the homogeneous bulk (5) into granulator to obtain granules; which are then processed for sizing and sieving to have a synergistic insecticidal composition in the form of dry flow, low compact, dust free granules of Cypermethrin + Acephate which overcomes the disadvantages of emulsifiable concentrates and soluble powders.
This invention comprises essentially of a synergistic insecticidal composition in the form of dry flow, low compact, dust free granules of 0.5 mm to 1. 0 mm diameter and 1.0 to 10.0 mm long granules of Cypermethrin + Acephate characterized by aging stability of minimum two years and with following specific compositions. Composition
Quantity (% w/w> Minimum 1.0 to 50.0 Max. Minimum 0.1 to 10.0 Max. Min. 0.01 to 10.0 Max. Min. 0.002 to 0.005 Max. Min. 1.0 to 10.0 Max. Min. 0.01 to 0.5 Max. Min. 0.5 to 5.0 Max.
Min. 0.1 to 5.0 Max. Min. 0.05 to 0.5 Max. q.s.
Ingredient
Acephate active ingredient
Cypermethrin active ingredient
Solubilizer
Emetic agent
Disintegrating agent
Antifoaming agent
Wetting cum dispersing agent
Anticaking agent
Dye(s)
Fillers (s)
Total 100.00 % (w/w)
• The preferred Cypermethrin technical is of purity 92.5% with 45 to 80% cis-isomer.
• The preferred Acephate Technical is of purity 97% minimum.
• The prefered solubilizer is ethoxylates of vegetable oil/ derivative or a mixture thereof.
• The preferred emetic agent is lignocaine derivative or a formulation of lignocaine derivative .
• The preferred disintegrating agent is absorbing type of clays like bentonite, Zeolite, Attapulgite and inorganic salts like Sodium and Ammonium Sulphate..
• The preferred antifoaming agent is Silicone oil derivative.
• The preferred Wetting cum dispersing agent is alkyl phenol ehtoxylate and salts of alkyl naphthyl sulphonate.
• The prefered anticaking agent is fumed silica and /or anhydrous Magnesium sulphate .
• The preferred dye is having a sunset yellow color.
: 6 :

« The preferred fillers is precipitated Silica and diatomaceous earth kaolin in the ratio of 1:10 to 10:1.
The following examples presented to illustrate but not restrict the invention. Parts and
percentage are by weight unless otherwise specified.
Example-1
Cypermethrin 1.0% + Acephate 50 % [51.0% DF] granules can be prepared as follows:
Composition Quantity(% w/w)

Acephate Tech. of 97.0% purity Cypermethrin Tech. of 92.5% purity Solubilizer 51.550 1082 0.300
Emetic agent 0.002
Disintegrating agent Antifoaming agent 2.000 0.030
Anticaking agent 0.100
Wetting cum dispersing agentDye(s)Filler(s) 1.000 0.100 43.836
Total 100.00 %w/w
For the preparation of a granular synergistic insecticidal composition in the form of dry flow, low compact, dust free granules of Cypermethrin + Acephate, requires to prepare a spray solution by homogenously mixing the Cypermethrin technical, emetic agent and solubilizer in the right proportion (say A). Then requires the preparation of a homogenous mixture of Acephate technical, wetting cum dispersing agent, disintegrating agent antifoaming agent, anticaking agent, dye(s) and the filler(s) which is later grinded and thereafter the spray solution (A) is sprayed on the grinded mixture and thoroughly mixed to have a homogenous mass. This mass is feed through a screw feeder into hopper of granulator thereafter the granules are dried and then processed for sizing and sieving to remove fines which can be recycled to obtain maximum yield of granular synergistic insecticidal composition of Cypermethrin + Acephate .
7

Example .-2
Cypermethrin 5% + Acephate 25 % [ 30 % DF] Granules can be prepared as follows ;-.
Composition Quantity (% w/w).

A cephate tech. of 97% purity 25.780
Cypermethrin tech. of 92.5% purity 5.410
Solubilizer L000
Emetic agent 0.003
Disintegrating agent 4.000
Antifoaming agent 0.040
Wetting cum dispersing agent 2,000
Anticaking agent 0.150
Dye(s) 0.100
Filler(g) 61.517
Total 100.00 0
Cypermethrin 5% + Acephate 25% [30 %DF] Granules with above composition can be prepared by the process described in example-1.
Example - 3
Cypermethrin 10% + Acephate 10% [20%DF] Granules can be prepared as follows :-
Composition Quantity (% w/w)
Acephate tech. of 97% purity 10.310
Cypermethrin tech. of 92.5% purity 10.820
Solubilizer 3.000
Emetic agent 0.004
Disintegrating agent 5.000
Antifoaming agent 0.050
Wetting cum dispersing agent 3.000
Anticaking agent 0,200
Dye(s) " 0.100
Filler(s) 67.516
Total 100.000
Cypermethrin 10% + Acephate 10% [20 %DF] granules with above composition can be prepared by following the process as described in example-!.
: 9 :

Example - 4
Cypermethrin 10% + Acephate 35% [45 %DF] Granules can be prepared as follows :-
Composition Quantity (% w/w)
Acephate tech. of 97% purity 36.090
Cypermethrin tech. of 92,5% purity 10.82$
Solubilizer . 3.000 ;•
Emetic agent 0,003>***"
Disintegrating agent 3.000
Antifoaming agent 0.060
Wetting cum dispersing agent 3.000
Anticaking agent 0,200
Dye(s) ' 0.200
Filler(s) 43.627
Total 100.00
Cypermethrin 10% + Acephate 35% [45 %DF] granules with above composition can be prepared by following the process as described in example-1.
Example -5
Cypermethrin 2% + Acephate 48% [50 %DF] Granules can be prepared as follows :-
Composition Quantity (% w/w)
Acephate tech, of 97% purity 49.490
Cypermethrin tech. of 92.5% purity 2.163
Solubilizer 4.000
Emetic agent 0.004
Disintegrating agent 4,000
Antifoaming agent 0.070
Wetting cum dispersing agent 5.000
Anticaking agent 0.500
Dye(s) 0.200
Filler(s) 34.573
Total 100.000.
Cypermethrin 2%.+ Acephate 48% [50 % DF] granules with above composition can be prepared by following the process as described in example-!.
: 10 :

Example -6
Cypermethrin 2.5% + Acephate 37.5% [ 40 % DF] Granules can be prepared as follows
Acephate tech. of 97% purity 38.660
Cypermethrin tech. of 92.5% purity 2,703
Solubilizer 1.000
Emetic agent 0.005
Disintegrating agent 5.000
Antifoaming agent 0.100
Wetting cum dispersing agent \ 3.000
Anti caking agent 1.000
Dye(s) '■ " 0.150
Filler(s) 48.382
Total ' 100.000
Cypermethrin 2.5% + Acephate 37.5% {40 %DF] granules with above composition can be prepared by following the process as described in example - 1.
Example-?
Cypermethrin 5 % + Acephate 45 % [ 50 % DF] Granules can be prepared as follows :■
Composition Quantity (% w/w)
Acephate tech. of 97% purity 46.392
Cypermethrin tech. of 92.5% purity 5.410
Solubilizer 1.500
Emetic agent 0.005
Disintegrating agent 5.000
Antifoaming agent 0.100
Wetting cum dispersing agent 4.000
Anticaking agent 2.000
Dye(s) 0.100
Filler(s) 35.493
Total 100.000
Cypermethrin 5 % + Acephate 45 % [50 %DF] granules with above composition can be prepared by following the process as described in example -1.
: 11 ;

Example -8
Cypermethrin 5% + Acephate 40% [ 45 % DF] Granules can be prepared as"folfo#s :-
Composition Quantity (% w/w)
Acephate tech. of 97% purity 41.237
Cypermethrin tech. of 92.5% purity 5.410
Solubilizer 1.500
Emetic agent 0.005
Disintegrating agent 5.000
Antifoaming agent 0.100
Wetting cum dispersing agent 4.000
Anti caking agent 2.000
Dye(s) 0.100
Filler(s) 40.648
Total 100.000
Cypermethrin 5% + Acephate 40% {45 %DF] granules with above composition can be prepared by following the process as described in example - 1.
Example -9
Cypermethrin 2.5% + Acephate 40% [ 42,5 % DF] Granules can be prepared as folios
Composition Quantity (% w/w)
Acephate tech. of 9?% purity 41.23?
Cypermethrin tech. of 92,5% purity 2.703
Solubilizer 1.000
Emetic agent 0.003
Disintegrating agent 4.500
Antifoaming agent. 0.500
Wetting cum dispersing agent 2.000
Anti caking agent 4.000
Dye(s) 0.200
Filler(s) 43.857
Total 100.000
Cypermethrin 2.5% + Acephate 40% {42.5 %DF} .granules with above composition can be prepared by following the process as described in example - 1.
: 12 :

Example -10
Cypermethrin 0.5% + Acephate 40% [ 40.5 % DF] Granules can be prepared as follows
Composition Quantity (% w/w)
A cephate tech. of 97% purity 41.237
Cypermethrin tech. of 92.5% purity 0.541
Solubilizer 0.250
Emetic agent 0.003
Disintegrating agent 4.000
Antifoaming agent 0.100
Wetting cum dispersing agent 5.000
Anticaking agent 5.000
Dye(s) 0.300
Filler(s) 43.569
Total 100.000
Cypermethrin 0.5% + Acephate 40% [40.5 %DF] granules with above composition can be prepared by following the process as described in example -1.
Example-ll
In the table set forth below, the results of a series of tests are indicated shows synergistic activity between the two classes of compounds which make up the composition of the present invention.
The effects observed by comparing the extent of bollworm incidence, for sucking pests population per leaf in the test fields treated with insecticidal combination of the invention against that occurring in untreated and individually treated fields. The crop considered was cotton and insects were Cotton bollworm and sucking pests

D etails of Experiment
a) Design
b) Replications
c) Treatment
d) Plot size (net plot)
e) Variety
f) Crop

Randomised block design (RBD)
Three
Nineteen (19)
4.5 x 4.2 sq.m
NHH-44 - hybrid Cotton
Cotton

: 13 :

g) Application time : Seven spray

1. 2. 3. 4. 5. 6. 7.

60 days after sowing 9 days after first spray 9 days after second spray 5 days after third spray
9 days after fourth spray
10 days after fifth spray
17 days after sixth spray

h) Application rate : Two litres per plot
i) Untreated control plots were sprayed with the same quantity of water (i.e. 2 litres
per plot) without insecticides,
j) Spray mixture used 1000 litres/ha with knapsack sprayer
k) Common sprays for early
sucking pests Two sprays
Methodology
a) Sucking Pests:
Five plants per replications were selected and tagged. The number of leaf hoppers, whitefly and aphids were counted on the three leaves from each plant (3,5 and 7th leaf on the main stem from top). Population count was made on one day before spraying and four days after spraying. The mean population per leaf per plant for all the sprays was estimated.
b) Bollworms
Five plants per replication were selected and tagged. The number of fruiting bodies damaged and healthy were recorded. Observation were made on one day before spraying and four days after spraying. The percentage of fruiting bodies damaged is computed. Similarly, at picking, the number of good opened bolls (GOB) and bad opened bolls (BOB) on five tagged plants were recorded at each picking and then the mean values per plant was computed in percent
: 14 :

Table -1 Bioefflcacy of Cypermethrin + Acephate on Cotton sucking Insect pests.

3.N0. Treatment Dossage of &i, gm/Ltr Mean Pest Population leaf
Leaf hopper Whitefly Aphids
1 CPN(3)+Acephate(40) 43%DF 0.5 0.35 4.80 12.99
2 CPN(3}+Acephate(43) 46%DF 0,5 0.32 4.76 12.95
3 CPN(3)+Acephate(45) 48% DF 0.5 0.30 4.73 12.90
4 CPN(3)+Acepnate(47) 50% DF 0.5 0.28 4.50 12.68
5 CPN(5)+Acephate(40) 45%DF 0.5 0.25 4.34 12.45
6 CPN(5)+Acephate(43) 48%DF 0.5 0.21 4.25 12.25
7 CPN(5)+Acephate(45) 50%DF 0.5 0.20 4.21 12.02
8 CPN(5)+Acephate(47) 52% DF 0.5 0.19 4.16 11.94
9 CPN(5)+Acephate(40) 45%DF 0.5 0.18 4.11 11.88
10 CPN(7)4-Acephate(43) 50% DF 0.5 0.17 4.05 11.79
11 CPN(?)+Acephate(45) 52%DF 0.5 0.17 4.01 11.73
12 CFN(7)+Acephate (47)54%DF 0.5 0.15 3.93 11.65
13 CPN(10)+Acephate(40) 50%DF 0.5 0.15 3.80 11.03
14 CPN(10>+Acephate (43) 53% DF 0.5 0.13 3.76 10.98
15 CPN(10>+Acephate(45)55%DF 0.5 0.12 3.73 10.92
16 CPN(10)+Acephate(47)57%DF 0.5 0.10 3.70 10.88
1? CPN10%EC 0.5 0.70 7.22 35.30 5.70
18 Acephate 75% SP 0.5 0.58 4.05
19 Untreated control - 5.72 6.20 11.35
CPN - Cypermethrin active ingredient
Acephate - Acephate active ingredient
EC - Emulsifiable Concentrate
SP - Soluble Powder
DF - Dry flowable granules
: 15 :

Table -2 Bioefflcacy of Cypermethrin and/or Acephate DF OR Cotton Bollworms

S.No. Treatment Dossage of ai, gm/Ltr %bollwor m incidence GOBperPlant BOB per Plant
1 CPN(3)+Acephate(40) 43%DF 0.5 18.39 26.1 10
2 CPN(3)+Acephate(43) 46%DF 0.5 18.26 26.3 9.9
3 CPN(3)+Acephate(45) 48% DF 0.5 18.11 26.4 9.5
4 CPN(3)+Acephate(47) 50% DF 0.5 18.00 26.9 9.2
5 CPN(5)+Acephate(40) 45%DF 0.5 17,92 27,5 8.7
6 CPN(5)+Acephate (43) 48%DF 0.5 17.79 28.19 8.1
7 CPN(5) +Acephate(45) 50%DF 0.5 17.73 29.1 7.9
8 CPN(5)+Acephate(47) 52% DF 0.5 17.62 29.3 7.9
9 CPN(7)+Acephate(40) 45%DF 0.5 16.98 29.40 7.7
10 CPN(7)+Acephate(43) 50% DF 0.5 16.65 29.6 7.6
11 CPN(7)+Acephate(45) 52%DF 0.5 16.23 29.8 7.5
12 CPN(7)+Acephate (47) 54%DF 0.5 15.71 29.9 7.4
13 CPN(10)+Acephate(40) 50%DF 0.5 15.20 30.1 7.4
14 CPN(10)+Acephate(43) 53% DF 0.5 14.72 30.2 7.3
15 CPN(10)+Acephate(45)55%DF 0.5 14.19 30.3 7.3
16 CPN(10)+Acephate(47)57%DF 0.5 13.88 30.7 7.0
17 CPN10%EC 0.5 28.05 24.8 10.2
18 Acephate 75% SP 0.5 28.05 25.5 10.2
19 Untreated control - 41.77 11.8 14.6
CPN - Cypermethrin active ingredient
Acephate - Acephate active ingredient
EC - Emutsifiable Concentrate
SP - Soluble Powder.
DF - Dry flow able granules
; 16 ;

The test results of all the formulated product samples reveals that the samples could be classified into four groups according to their efficiency.
Group A (Grad»-1)
50% DF(w/w) 50%DF(w/w) 54% DF(w/w) 52% DF (w/w) 52% DF(w/w) 50% DF(w/w) 47% DF (w/w)
1. Cypermethrin (5) + A cephate (4 5)
2. Cypermethrin (3) + Acephate (47)
3. Cypermethrin (7) + Acephate (47)
4. Cypermethrin (5) + Acephate (47)
5. Cypermethrin (7) + Acephate (45)
6. Cypermethrin (7) + Acephate (43)
7. Cypermethrin (7) + Acephate (40)

Gronp-B (Grade II)
1. Cypermethrin (5) + Acephate (43) 2= Cypermethrin (5) + Acephate (45) 3. Cypermethrin (3) + Acephate (45)

48% DF(w/w) 50%DF(w/w) 48% DF(w/w)

Group-C (Grade III)
1. Cypermethrin (3) + Acephate (43)
2. Cypermethrin (3) +Acephate (40)

46% DF(w/w) 43% BF(w/w)

Group d-P (Grade-IV)
Untreated
Result
Out of Grade-I results in group A, the concentration of Cypermethrin (5) + Acephate (45) 50% DF (w/w) earns the preference on the others due to low residual value, lower loading of toxicant/ha, without compromising the preferred results.
: 17 :

Advantages
• The selected synergistic composition of Cypermethrin (5.0) + Acephate (45) 50%
DF (w/w) has:
? low residual value ;
? lower loading of toxicant/ha to achieve same results.
? good effect in controlling cotton boll worm and sucking pests.
• The composition proposed by the present invention is very effective against Cotton
bollworms, leaf hoppers , whitefly and aphids, when used in 1: 9 ratio of
Cypermethrin : Acephate (on active ingredient basis) due to synergic activity.
• The DF(dry flow) granules when added into water disperses the active content easily.
• The suspension prepared exhibits good stability and helps in uniform distribution of active ingredient while spraying on plants.
• The granular product is safe for humans and animals.
Conclusion
The overall results and observation from table 1 and 2 shows that Cypermethrin (5) + Acephate (45) 50%DF (w/w) is showing a good synergic property in comparison to existing formulation of Cypermethrin and Acephate individually.
Test-2
Aim : Evaluation of Cypermethrin (5) + Acephate (45) 50% DF (w/w) ready mix against cotton insect pests.
Details of the experiment

a) Design
b) Replications

R.B.D Three : 18 :

c) Treatments ; Twelve
1. Cypermethrin 5% DF (at 50 g. a.i./ha)
2. Cypermethrin 5% DF (at 60 g a.i./ha)
3. Cypermethrin 5% DF (at 70g a.i./ha)
-■ 4. Cypermethrin (5)+Acephate(45) 50% DF (w/w) (at 400 g a.i./ha)
5. Cypermethrin (5)+Acephate(45) 50% DF (w/w) (at 425 ga.i./ha)
6. Cypermethrin(5)+Acephate (45) 50%DF(w/w) (at 450 g. a.i./ha)
7. Acephate 75% DF (at 550 g a.i./ha)
8. Acephate 75% DF (at 575 g. a.i./ha)
9. Acephate 75% DF (at 585 g a.i./ha)
10. Cypermethrin 25% EC (at 60 g a.i. /ha)
11. Acephate 75% SP (at 575 g a.i./ha)
12. Untreated Control
d) Plot size (net plot) 4,5 x4.2 sq, m
«) Variety NHH44 hybrid Cotton
f> No. of spraying Seven sprays
i) 60 days after sowing
2) 8 days after first spray
3) 8 days after second spray
4) 5 days after third spray
5) 8 days after fourth spray
6) 10 days after fifth spray
?) 20 days after sixth spray
8) Spray mixture used ; 1000 1/ha with Knapsack sprayer
h) Common sprays for early
Sucking pests. • Two sprays with systemic insecticides.
Methodology:
Sucking Pests
Five plants per replications were selected and tagged. The number of leaf hoppers, whiteflies and aphids were counted on 3 leaves from each plant (3, 5 and 7th leaf on the main steam from top). Population count was made on one day before spraying and four days after spraying. The mean population per leaf per plant for all sprays was estimated.
15

Boll worms
Five plants per replications were selected and tagged. The number of fruiting bodies damaged and healthy were recorded. Observations were made on one day before spraying and four days after spraying. The percentage of fruiting bodies damaged is computed.
Similarly at the picking, the number of good opened bolls and bad opened bolls on five tagged plants, were recorded at each picking.
Cotton yield per plot was recorded separately and it was computed to quintal/ha.
Results
Sucking insect population
All the various treatment dosage of Cypermethrin 5% DF , Acephate 75% DF and Cypermethrin (5) + Acephate (45) 50% DF, did reduce leafhopper population and they were at par with each other. Untreated control recorded a maximum of 5.72 leafhopper per leaf.
All the dosage levels of Acephate 75% DF and Cypermethrin + Acephate ready mix combination recorded lower population of whiteflies and they were with each other and also Acephate 75% SP treatment. Whereas all the dosage level treatments of Cypermethrin 5% DF and Cypermethrin 25% EC were comparable to untreated control in recording whiteflies population. Mini mum aphid population was recorded in all die dosage treatments of Acecphate 75% DF and Acephate 75% SP insecticide. Whereas Cypermethrin 5% DF and 25% EC treatments recorded relatively high population of aphids and in ready mix (Cypermethrin + Acephate) aphid population was significantly less than the Cypermethrin alone treatment because inclusion of Acephate, But these treatments were comparable to untreated control which recorded 11.35 aphids per leaf. (Table - 3)
Percent bollworm incidence.
AH the dosage level' treatments of Cypermethrin + Acephate reach/mix recorded lower percent bollworm incidence and they were at par with each other and significantly superior over rest of the treatments. Alone treatments of Cypermethrin 5% DF at 70g a.i./ha treatment records 27.02 % bollworm indicence which was significantly superior over its lower dosage treatments and also Cypermethrin 25% EC and Acephate 75 SP treatments. Untreated control recorded a maximum of 41.77 percent bollworm incidence. (Table-4)
: 20 :

GOB and BOB per plant.
Maximum number of GOBs and minimum number of BOBs per paint were recorded; in all the dosage level treatments of Cypermethrin + Acephate readymix treatments and these treatments significantly superior over other treatments. Alone treatments of Cypermethrin 5% DF at 70 g a.i./ha treatment recorded 25,0 GOBs and 10 BOBs per plant respectively which was superior to its lower dosage treatments but comparable to all the dosage level treatments of Acephate 75 DF and SP treatments. Untreated control recorded 11.8 and 14.6 GOB and BOB per plant respectively. (Table-4)
Yield
Ready mix treatment of Cypermethrin (5) + Acephate (45) 50% DF at all the dosage levels recorded relatively higher seed cotton yield and its treatments were significantly superior over other treatments. Cypermethrin at 60 g a.i./ha treatments recorded 10.45 q/ha seed cotton which was at par with its higher its higher dosage treatments but superior to its lower dosage treatments, Whereas Acephate 75% DF at 575 g a.i.ha treatment recorded 11.42 q/ha seed cotton yield which was at par with both its higher as well as lower dosage treatments and also comparable standard check treatments. Untreated control recorded a minimum of 6.38 q/ha seed cotton yield. (Table-4)
Conclusion
i. All the dosage level treatments of Cypermethrin (5) + Acephate (45) 50% DF
recorded lowest percent bollworm damage and higher cotton yield than alone
treatments of Cypermethrin 5% DF and Acephate 75% DF.
ii. Cypermethrin 5% DF at 70g a.i./ha treatment was comparable to all the dosage
level treatments of Acephate 75% DF.
T able=3 Bioefficacy of Cypermethrin 5% DF and Cypermethrin 5% DF + Acephate 45% DF ready
mix against cotton sacking insect pests.

: 21 :

The synergic effect which is the base of of the composition proposed by the present invention has been demonstrated by way of results. The effect is described as follows.
The mentioned numbers for cash component - Cypermethrin + Acephate corresponds to %grams/ kg in the formulation in three different concentration ( 4 + 36; 5+45, 6+54) all in % g/kg were tested using same operating condition as described in example 11,12 except variation in active ingredient in the ratio (by weight) of 1:9 (i.e. 5:95 in parts of a.i. Cypermethrin: Acephate).
: 22 :

Test: 3
Crop Cotton
Sort of Pest a. Bollworm (Cotton Crop)
b. Jassid.
Experiment-1 (Percentage of incidence after spraying)

Concentration % (w/w) % of incidence
Bollworm Jassid
Cypermethrin 4+ Acephate 36 25.03 16.24
Cypermethrin 5 + Acephate 45 18.95 11.73
Cypermethrin 6 + Acephate 54 16.71 10,89
Experiment-2

Concentration % (w/w) % of incidence
Bollworm Jassid
Cypermethrin 4+ Acephate 36 26.27 17.03
Cypermethrin 5 + Acephate 45 19.40 12.46
Cypermethrin 6 + Acephate 54 17.92 11.31
Con elusion

Concentration % (w/w) Performance Crop Residual
Bollworm Jassid
Cypermethrin 4+ Acephate 36 Noraml Normal BDL
Cypermethrin 5 + Acephate 45 Very good Very good BDL
Cypermethrin 6 + Acephate 54 Very good Very good Trace
BDL : Below detectable level
: 23 :

The above experiment on the Cotton for bollworms and Jassids established that Cypermethrin (5) + Acephate (45) 50% DF & Cypermethrin (6) + Acephate (54) 60% DF are showing the efficiency in controlling at par to each other whereas that with Cypermethrin (4) + Acephate(36) 40% DF shows normal results when used at the required active ingredient, dosage per hectare.
From the above test 3, it is conclused that Cypermethrin (5) + Acephate (45) 50% DF is very effective when compared to higher concentration combinations. As it is evident that the higher concentration combination does not exhibit any considerable improvement in effectiveness but it only adds to unnecessary, excess use of active ingredient to cause environment pollution.
The minimum dosage of Cypermethrin (5) + Acephate (45) 50% DF depend upon the type and the evaluation of the filed of cultivation. The experiments conducted make it possible to recommend the following initial doses.

Crop Pest (type of culture) Dose gm/ha Waiting period in days
a.i. DF
Cotton American bollworm Spotted bollworm Jassids 400-450 800-900 15 days
a,i. - active ingredient
DF - Dry flow able granules
Test ;-4
Phototoxicity studies on Cotton
Table - 5 shows the observations taken for ten days on necrosis, epinasty, hyponesty, leaf lip injury, leaf surface injury, vein clearing etc. for evaluation of Cypermethrin (5) + Acephate (45) 50DF readymix, Cypermethrin 5% DF and Acephate 75DF and SP for phytotoxicity on cotton.
Results:-
There were no visible phytoxicity symptoms on Cotton Plants treated with various dosage level treatment of Cypermethrin (5) + Acephate (45) 50% DF , Cypermethrin 5% DF, Acephate 75% DF & SP insecticides.
: 24 :


• The above examples, their results and observations concluded that Cypermethrin + Acephate exhibits synergistic insecticidal activity in the range of 1:1 to 1.10 (Cypermethrin: Acephate) at the required active ingredient, dosage per hectere.
• The synergistic insecticidal composition of Cypermethrin + Acephate can be prepared by followiskng method as described in example 1 to 10.
• It also revelas that optimum synergistic activity is being noticed in the ratio of 1:9 (i.e. 1:9 parts of Cypermethrin: Acephate) at the required active ingredient dosage per hectere.
• Cypermethrin (5) + Acephate (45) 50%DF is very effective among the lower and higher concentration in the same ratio of 1:9 and is very effective against Cotton bollworm, leaf hopper and sucking pest.
• The synergistic composition of Cypermethrin and Acephate reveals that the active ingredient dosage per hectare is significantly lesser then than that required when Cypermethrin and Acephate applied individually for same performance.

• The synergistic compoisition proposed reduces the chances of resistance development and act as a potent lethal weapon to kill these insects.
• The formulated product provides uniform distribution of active on treated plants.
• The formulated product of Cypermethrin + Acephate provides a compatible, plant mix ready to use synergistic composition.

26

We claim
1. A process for the granular preparation of synergistic insecticidal composition of
Cypermethrin and Acephate comprises of following steps :
a) preparation of a spray solution by homogeneously mixing the Cypermethrin active with solubilizer and emetic agent;
b) preparation of a homogeneous mixture of Acephate active with wetting cum dispersing agent, additives and filler(s);
c) spraying the spray solution prepared in (a) on to the mixture prepared in (b);
d) homogenously mixing the whole mass of step ( c );
e) feeding the mass of the step (d) into the granulator for granulation;
f) the granules of the step (e) are then processed for sizing and sieving to have the granular preparation of the synergistic insecticidal composition of mis invention.

2. A process as claimed in claim (1) wherein additives comprises of the antifoaming agent, disintegrating agent, anticaking agent, and dye(s).
3. A process as claimed in claim (2) comprises of grinding of the ingredients to a homogenous mixture.
4. A process as claimed in claim (1) (e) comprises the feeding of the mass through the feeder into the hopper of the granulator.
5. A process as claimed in claim (1) comprises of conditioning and drying of the granules obtained.

6. A process as claimed in claim (1) comprises the recycling of the fines and oversized granules to have a maximum yield.
7. A process as claimed in claim (1) wherein Cypermethrin and Acepahte has been mixed in the ratio of 1:1 to 1:10.
: 27 :

8. A process as claimed in claim (7) wherein the preferred ratio of Cypermethrin and Acephate is U9,
9. A process as claimed in claim (1) wherein Cypermethrin used is having 45-80% of cis-isomers.
10.A process as claimed in claim (1) wherein solubilizer selected is ethoxylate of vegetable oil.
11. A process as claimed in the claim (1) wherein wetting cum dispersing agent selected is Alkyl Phenol Ethoxylate and salts of alkyl naphthyl sulphonate.
12.A proces as claimed in the claim (1) (a) wherein the emetic agent selected is lignocaine derivative or a formulation of lignocaine derivative.
13.A process as calimed in the claim (2) wherein the antifoaming agent selected is silicone oil derivative.
14.A process as claimed in the claim (2) wherein the disintegrating agent is absorbing type clays like bentonite, Zeolite, Attapulgite and inorganic salts like sodium and Aluminium sulphate.
15.A process as claimed in the claim (1) wherein filler(s) selected is/are silica, kaoline and/or a mixture of these two in 1 : 10 to 10 : 1.
16.A process as claimed in claim (2) wherein the anticaking agent selected is Fumed silica and /or anhydrous Magnesium sulphate.
: 28 :

17.A process for the granular preparation of synergistic insecticidal composition o^" Cypermethrin and Acephate as herein defined and exemplified.
Dated 26 th, day of December, 2000.
: 29 :
FORM-2
THE PATENTS ACT, 1970
PROVISIONAL SPECIFICATION
SECTION 10
TITLE A PROCESS FOR THE GRANULAR PREPARATION OF
SYNERGISTIC INSECTICIDAL COMPOSITION.
APPLICANT(S) : UNITED PHOSPHORUS LIMITED, UNIPHOS HOUSE, C.D.MARG, KHAR
(WEST), MUMBAI-400 052, MAHARASHTRA, INDIA, INDIAN COMPANY.
The following Specification describes the nature of this invention.

The following specification describes the nature of this invention .
The present invention relates to a process for the, preparation of granular composition of Cypermethrin + Acephate with enhanced synergistic insecticidal activity.
The protection of crops and its produce from insect pest damage is essential in agriculture produce enhancement. To help combat these problems, various chemicals and its formulations were invented in effective management of pests.
Insecticides of many types and groups are reported in the literature and a large number are in use, commercially, for effective control of pests in agriculture.
In many cases, active insecticides have shown more effectiveness in combination than when applied individually. Since the combination demonstrates a potency and activity level exceeding that, which might be expected, from a mere addition of the individual potencies of the components, are there by called as 'synergism'. The present invention highlights the synergistic effect of combination of two known active insecticides "Cypermethrin" and "Acephate". Both individual insecticides, forming this combination, which is the subject of this invention are known to be potent insecticides, for their activity independent of each other.
In modern agriculture scenario, where insect has attained resistance, due to indiscriminate and non-judicious use of pesticide, in view to manage insect pests for a desire of higher yields and those insects which are hard to kill by the existing commercial insecticides solely and in cyclic spray mixtures, warrants invention of a potent synergistic insecticidal composition.
Cypermethrin and Acephate in a synergistic composition has a higher potentiation, as insecticide, and is highly effective in controlling insect pests including even hard to kill pests. The synergic composition gives a quick knockdown kill of the pests. It is comparatively more persistent. It penetrates deep in leaves, killing many internal feeders. It is strongly active as a contact and stomach insecticide. It is especially a potent lethal weapon to kill, hard-to-kill, resistance insect pests, which are normally not controlled by other insecticides. The said mixture insecticides has the good effect for controlling Cotton bollworms and sucking pests. Its toxicity is low and safe for human and animals. Its residue is also small.
The name 'Cypermethrin', is an insecticide, belongs to synthetic pyrethroid group describes a chemical substance having a solubility in water of 0.004 mg/1 (at pH7); corresponds to a mixture of cis and trans isomers. So being almost insoluble in water, it is soluble in acetone,
chloroform, cyclohexanone, xylene >450 (g/1); ethanol 337 (g/1), hexane 103 (g/1) at 20°C.
: 2 :

Cypermethrin is presently recognised as the non-systemic insecticide with contact and stomach action. It also exhibits antifeeding action and good residual activity on treated plants. It is used to control a wide range of insects, especially Lepidoptera, but also Coleoptera, Diptera, Hemiptera and other classes in fruits, ( including Citrus), Vines, Vegetables, Potatoes, Cucurbits, Lettuce, Capsicums, tomatoes, cereals, maize, soyabeans, cotton, coffee, Cocoa, rice, peacans, oilseed rape, beet, ornamentals, forestry, etc^ It is also used for control of flies and other insects in animal houses; arid mosquitoes, cockroaches, houseflies and other insect pests in public health. It is also used as an animal ectoparasiticide.
Presently Cypermethrin is most preferably formulated in the form of emulsifiable concentrate (EC) which consists of Cypermethrin active ingredient dissolved in solvent(s) alongwith surfactants at a levels required to give maximum stability with the formation of homogeneous emulsion on dilution. The use of organic solvent(s) is disadvantageous from environmental and cost view point. These organic solvents may exhibit toxicity and side-effects which may be adverse to the effect of the agricultural chemical itself or to the plant or crop as a whole or to its parts produced in treated fields. They shows hazards during manufacturing, filling, packing, storage, transit, and use. During use, dermal and respiratory toxic exposure to user are frequently observed. By using the organic solvents percutaneous toxicity and inflammability may also occur.
'Acephate' (0,S-dimethylacetylphosphoramidothioate) is a systemic insecticide of moderate persistence with residual activity lasting about 10-15 days. It is effective against a wide range of aphids, leaf miners, lepidopterous larvae, sawflies and thrips. It is non-phytotoxic on many crop plants. Technical grade Acephate (purity 80-90%) is a colourless solid; melting point 82 -89°C; solubility at room temperature : about 650 g/1 water; > 100 g/1 acetone, ethanol; < 50g/l aromatic solvents.
The formulation of Acephate presently in use is Acephate 75% Soluble Powder (SP) consists of Acephate active ingredient 75% (w/w), Surfactant 1% to 2% (w/w), & inert filter (Precipitated Silica) to make 100% (w/w). It poses the problems like dust, low pourability, high transportation cost, high capital manufacturing investment, not easily measurable, difficulties in packing material disposal, handling problems, high risk of caking and others.
The present invention minimises dermal and respiratory toxic exposure to users, also eliminates the percutaneous toxicity and flammability hazard since it does not contains any organic solvent. The product provided by this invention is relatively more advantageous and exhibit very desirable characteristics noted herein after. It is thus, an object of the present invention to provide dust free granules of insecticide Cypermethrin containing concentration in the range of 0.1 to 10.0% Active Ingredient + Acephate containing concentration in the range of 1.0 to 50.0% of active ingredient. It is a further object of the present invention to provide method for making such dry flow, low compact, dust free granular compositions.
: 3 :

Both of these compounds, are capable of controlling a large spectrum of insects especially Lepidoptera, Coleoptera, Diptera, Hemiptera and other class in fruits, vegetables, ornamentals etc. Cypermethrin is distinguished for its sudden shock effect alongwith good residual activity on treated plants. Acephate is a systemic insecticide of moderate persistence with residual activity and is effective against a wide range of aphids, leafminers, lepidoptrous larvae, sawflies and thrips. It is non phytotoxic on many crop plants.
The earlier known art discloses about a composition of both these compounds in 0.5 to 5% Cypermethrin and 10 to 40% Acephate combination in liquid formulation EC and has claimed the synergic effect (Patent No. CN 1110082).
In the present invention, die two effects i.e. residual activity and antifeeding action are
synergistically combined into a formulation of improved (high yielding) efficiency assuming
that the dosage (mass of active ingredients per hectare) significantly lesser than that required,
when these two components are utilised separately, under identical conditions, and also
reduces the chances of resistance development (which will result when a single active
ingredient is used for a long time and in high doses). It is also providing a ready to use,
compatible plant-mix in an effective synergistic composition along with the improvement in
insecticidal activity .,= ..;
The preliminary pilot trials of various strength of Cypermethrin and Acephate carried to find out the composition, of Cypermethrin + Acephate, which exhibits optimum synergistic value.
The granular composition prepared by the prefered method and prefered composition of the present invention provides dust free; good pourability; low transportation cost; low capital investment; good stability of product; free flowability; free from solvents/less solvent; no exposure to solvent vapours during manufacturing, storage, transit and use; less expensive packing; minimum contamination of packing material; can be packed in environment friendly packings like Water soluble Sachets/ bags; easy to measure; best utilization of energy sources; less wastage during processing; better bioefficacy; easy disposal of packing material; easy to handle; limited risk of caking; safe during storage, transit and use; good dispersibility; good resistance to attrition; semi skilled operator required; less space required for production; with good market potential; easily reproducible during processing; less risk of inhalation and irritation; spillage is easy to collect and clean; less health hazards to operators; optimum coverage per application; sustained action for longer effect; no need to prepare slurry or paste simply pour into water; less expensive; use of less surfactant(s).
The selected synergistic composition of Cypermethrin (5) + Acephate (45) 50% DF (w/w) has :
? low residual value ;
? lower loading of toxicant/ha to achieve same results.
? good effect in controlling cotton bollworm and sucking pests.
:4:

• The composition proposed by the present invention is very effective against Cotton bollworms, leaf hoppers, whitefly and aphids, when used in 1:9 ratio of Cypermethrin: Acephate (on active ingredient basis) due to synergic activity.
• The DF(dry flow) granules on addition to water disperse the active content easily.
• The suspension prepared exhibits good stability. This helps in uniform distribution of active ingredient on plants when applied.
• The granules are safe for humans and animals.
The synergic effect which is the base of of the composition proposed by the present invention has been demonstrated by way of results. The effect is described as follows:
The mentioned numbers for cash component - Cypermethrin + Acephate corresponds to % (gm/ kg) in the formulation in three different concentration ( 4 + 36; 5+45; 6+54) all in % (g/kg) were tested using same operating condition as described in example 11,12 except variation in active ingredient in the ratio (by weight) of 1:9 (i.e. 5:45 in parts of a.i. Cypermethrin : Acephate).
Test
Crop Cotton
Sort of Pest a. Bollworm (Cotton Crop)
b. Jassid.
Experiment-1 (Percentage of incidence after spraying)

Concentration % (w/w) , % of incidence
Bollworm Jassid
Cypermethrin 4 + Acephate 36 25.03 16.24
Cypermethrin 5 + Acephate 45 18.95 11.73
Cypermethrin 6 + Acephate 54 16.71 10.89
Experiment-2

Concentration % (w/w) % of incidence
Bollworm | Jassid
Cypermethrin 4+ Acephate 36 26.27 17.03
Cypermethrin 5 + Acephate 45 19.40 12.46
Cypermethrin 6 + Acephate 54 i 17.92 11.31
: 5 :

Conclusion

Concentration % (w/w) Performance Crop Residual BDL
Bollworm Jassid
Cypermethrin 4+ Acephate 36 Noraml Normal
Cypermethrin 5 + Acephate 45 Very good Very good BDL Trace
Cypermethrin 6 + Acephate 54 Very good Very good
BDL : Below detectable level '
The above experiment on the Cotton for bollworms and Jassids established that Cypermethrin (5) + Acephate (45) 50% DF & Cypermethrin (6) + Acephate (54) 60% DF are showing the efficiency in controlling at par to each other whereas that with Cypermethrin (4) + Acephate(36) 40% DF shows normal results when used at the required active ingredient, dosage per hectare.
The minimum dosage of Cypermethrin (5) + Acephate (45) 50% DF depend upon the type and the evaluation of the filed of cultivation. The experiments conducted make it possible to recommend the following initial doses.

Crop Cotton Pest (type of culture)American bollworm Spotted bollworm Jassids Dose gm/ha Waiting period in days15 days
a.i. 400-450 DF 800-900 OF -
u.i. active ingredient - i Dry flowable granules
The synergistic composition of Cypermethrin and Acephate reveals that the active ingredient dosage per hectare is significantly lesser than that required when Cypermethrin and Acephate applied individually for same performance.
The synergistic composition proposed reduces the chances of resistance development and act as a potent lethal weapon to kill these insects;
The formulated product provides uniform distribution of active ingredient or component on treated plants.
The formulated product of Cypermethrin + Acephate provides a compatible, plant mix ready to use synergistic composition.
: 6 :

For the preparation of a granular composition of Cypermethrin + Acephate with
enhanced synergistic insecticidal activity. : /'"'
* the required quantity of Cypermethrin technical (preheated) is premixed with specified quantity of solubilizer and emetic agent to prepare spray/solution (A);
* the required quantity of Acephate technical is premixed with specified quantity of wetting cum dispersing agent, antifoaming agent, disintegrating /agent, anticaking agent, dye and required inert filler(s). Thereafter this pre-mix is grinded to achieve intimate and efficient mixing of particles. The grinded mixture is then post mixed to have a homogeneous mixture of all these (B);
* thereafter the above prepared spray solution (A) is sprayed on the homogeneous mixture (B) and again mixed thoroughly for sufficient time to have a homogeneous bulk which (on passing quality tests) is feed through a screw feeder into the hopper of granulator for granulation. After which these granules are processed for sizing and sieving. The fines collected are recycled. The product obtained is dry flow, low compact, dust free granules with enhanced synergistic insecticidal activity of Cypermethrin + Acephate composition.
* the granules are tested for required quality specifications and on passing filled and packed
in desired packing. This granulation technique gives, greater than 99.5% of yield
conversion. The granules with incorporation of inert ingredients, by proper choice, enjoys
all the formulation advantages as discussed before. All the advantages makes it beneficial
from economic aspect, handling aspect and snows a very good performance during
application.
Dated 26th day of Dec. ,2000 .

7
ABSTRACT
A process for the granular preparation of synergistic insecticidal composition of Cypermethrin and Acephate comprises of following steps :
a) preparation of a spray solution by homogeneously mixing the Cypermethrin active with solubilizer;
b) preparation of a homogeneous mixture of Acephate active with wetting cum dispersing agent and filler(s);
c) spraying the spray solution prepared in (a) on to the mixture prepared in (b);
d) homogenously mixing the whole mass of step (c);
e) feeding the mass of the step (d) into the granulator for granulation;
f) the granules of the step (e) are then processed for sizing and sieving to have the granular preparation of the synergistic insecticidal composition of this invention.

To,
The Controller of Patents,
The Patents Office,
Mumbai.
: 30: