Form - 2
THE PATENTS ACT
1970 (39 of 1970)
SPECIFICATION
(See Section 10)
A storage stable, granular insecticidal cum acaricidal composition of 2-chloro-2-diethylcarbamoyl-1-methylvinyldiemthylphosphate.

We, UNITED PHOSPHORUS LIMITED, a company incorporated under the Companies Act, 1956 and having its registered office at 3-11, GIDC, Vapi - 396 195, State of Gujarat, India and having its office at Uniphos House, CD. Marrg, Khar (West), Mumbai - 400 052, State of Maharashtra.


The following specification describes the nature of this invention :-
The present invention provides a storage stable, granular insecticidal cum acaricidal composition of 2-chIoro-2-diehtylcarbamoyl-l-methyl vinyl dimethyl phosphate (PHOSPHAMIDON), dispersing agent ,wetting agent, binding agent, disintegrating agent, antifoaming agent, stabilizers, bittering agent and filler(s).
In general, the active ingredient Phosphamidon presently available in the market is in the form of a soluble liquid/concentrates. The present formulation includes the Technical, solvent, adjuvants and dye. 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.
The present invention minimises dermal and respiratory toxic exposure to users and also eliminates the percutaneous toxicity and flammability hazard since it does not involves the use of 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 a storage stable, dry flow, low compact, dust free granular insecticidal and acaricidal composition of 2-chloro-2-diehtylcarbamoyl-l-methyl vinyl dimethylphosphate (PHOSPHAMIDON) and to provide a method for making such granular compositions.
The present invention provides compositions and the method for preparation of storage stable dry flow, low compact, dust free granular insecticidal cum acaricidal composition of Phosphamidon alongwith dispersing agent ,wetting agent, binding agent, disintegrating agent, antifoaming agent, stabilizers, bittering agent and filler(s) to give safer and effective product

Phosphamidon is a systemic insecticide and acaricide with stomach and slight contact action. It is absorbed by the leaves and roots. It is Cholinesterase inhibitor. It is used in control of sucking, chewing and boring insects and spider mites on a very wide range of crops. Specifically used in control of leaf beetles and stem borers in rice; stem borers in sugarcane; colarado beetles in potatoes; thrips in cotton; etc It is also used to control aphids, sawflies, suckers, fruit flies, leaf miners, moth and beetle larvae and many other insects in fruits, vines, olives, vegetables, ornamentals, cereals, beet, maize, alfalfa, many other crops and in forestry. It is non-phytotoxic, except some varities of cherry, plum, peach and sorghum. It is compatible with many other pesticides, but incompatible with alkaline materials.
The commercial compound (i.e. PHOSPHAMIDON) contains 70 % m/m (Z)-isomer (P-isomer) ( which has the greater insecticidal activity) and 30 %m/m (E)-isomer (a-isomer). It is a pale yellow liquid. It has a boiling point 162 °C(at 1.5mm Hg); solubility-miscible with water, acetone, dichloromethane, toluene and other common organic solvents, with the exception of aliphatic hydrocarbons e.g. solubility in hexane 32 g/1 ( 25 ° C). It rapidly hydrolysis in alkali: DT50 (calculated) (20 °C) 60 d (pH 5); 54 d (pH 7);12d(pH9).
Its acute oral LD50 for rats 17.9-30 mg/Kg. Acute percutaneous LD50 for rats 374-530, rabbits 267 mg/Kg. Slight skin irritation, moderate eye irritation in rabbits observed. During inhalation LC50 (4h) for rats is about 0.18, mice 0. 033 mg/1 air. No observable effect level (NOEL) in 2 years for rats is 1. 25, dogs 0.1 mg/Kg daily. It has Acceptable Daily Intake (ADI) of 0.0005 mg/Kg body weight The toxicity class WHO la; EPA I.
In mammals, following oral administration, 85-90 % of the dose is expected within 24 hours, almost entirely in the urine. Complete metabolism occurs during the passage, by oxidative dealkylation of the amide group and hydrolysis of the phosphorus ester bond.
In plants, an ethyl group is split off from the amide group and simultaneously or subsequently the ester bond between the side chain and phosphorus atom is hydroh/tically cleaved. De-chlorination also occurs, as does further degradation to small 1 fragments.
The present invention provides composition and the process of preparing Phosphamidon granules to provide a product with a high degree of stability and good activity against assorted insect pests. It is well known and recognised that the scope of the insecticidal activity of a substance can be widened by making the product more stable during storage. If the product is not stable during storage, its activity get decreased and the control of the insect pest is not achieved upto a desired level because as the storage time increases, the decrease in activity occurs, which in turn gives poor results when compared to that of a stable formulation product.

Moreover, the insects and acarides with a diminished sensitivity to insecticide and acaricide can also be fully and effectively controlled with such compositions prepared by following this invention. Therefore the present invention is a new and original and constitutes a substantial contribution to enrichment of state of art
The present invention provides the compositions) of the active component Phosphamidon with a very useful activity as a systemic insecticide and acaricide and with stomach and slight contact action for protecting cultivated plants.
The present invention provides a storage stable insecticidal cum acaricidal composition of Phosphamidon which can be applied in accordance with the recommendations prescribed on the label/leaflet of the product by mixing the insecticide and water in the prescribed proportions. The product should be sprayed immediately on the appearance of symptoms of pest attack. The product may be sprayed by using a High Volume Sprayer, namely Knapsack sprayer using 500 to 1000 litres of water per hectare.
Without prejudice to the generality of forgoing or implying any limitation, the target crops to be protected within the scope of the present invention are interalia for example: barley, wheat, maize, paddy, peas, sugarcane, cotton, mustard, brinjal, apple, mango, tea, banana etc.
The concentration of Phosphamidon in these granules varies and can be made in the range as per requirements. For preparing the granules of Phosphamidon , the required quantity of technical is premixed with specified stabilizers), bittering agent and then sprayed on a homogenous mixture of other necessary inert ingredients; thereafter the whole mass is again mixed throughly for sufficient time to have a homogenous bulk which ( on passing quality tests) is fed through a screw feeder into the hopper of the granulator for granulation; thereafter these granules are processed for sizing and sieving and the fines collected are recycled, and the product obtained is a storage stable, dry flow, low compact, dust free granular composition of PHOSPHAMIDON ( an insecticide cum acaricide).

According to the preferred method of making a storage stable granular insectigidal and acaricidal composition of 2-chloro-2 diethylcarbamoyl-1-methylvinyl dimethylphosphate in the form of dry flow, low compact, dust free granules is best described by referring to the drawing of flow - chart on page -13. The required quantity of dispersing agent, wetting agent, disintegrating agent antifoaming agent, stabilizers, bittering agent and filler(s) are mixed homogenously to have a uniform mixture and the spraying the 2-chloro-2 diethylcarbamoyl-1- methylvinyl dimethylphosphate active over this mixture is done and the whole mass is throughly mixed for sufficient time to obtain the homogenous bulk until the required percentage of active ingredient is obtained . Thereafter this homogenous bulk on passing the quality test is fed through a screw feeder into the hopper of granulator preferably maintaining the inlet temperature of 30 - 35 ° C and the outlet temperature of 40 - 45 ° C and the rate and quantity of material fed to the granulator to minimize clumping together of the granulated product. The granules obtained are then processed for sizing and sieving to get the required quality granules. The fines collected after sieving are recycled.
The graules according the present invention are typically cylindrically shaped, although they can take on any suitable shape in cross section depending on the shape of the granulator sieve orifice. An average diameter of thegranule in cross-section can be from 1 to about 15 mm, preferably 2 to 10 mm. The granules produced according to the present invention are chemically stable, and have a commercially satisfactory shelf life on the order of about 1 -2 years, during which time they generally remain free-flowing and avoid the raw powder's tendency to agglomerate.
Once formulated, the granules are useful in a method for the controlling insects by application of the granules onto the insect's habbitat in an amount sufficient to provide acceptable control of the insects.
To avoid clumping of the granules as they exits the orifice of the gianulator, cooled air can be blown across the outer orifice to accelerate cooling and hardening of the granules, which results in decrease in tackiness and clumping as they haden or the throughput rate of the material being granulated can be lowered, giving the granules more time to cool before coming into contact with each other.
This invention comprises essentially storage stable granules of granular insecticidal and acaricidal composition of 2-chloro-2 diethylcarbamoyl-1- methylvinyl dimethylphosphate in the form,of dry flow, low compact, dust free granules with following specific compositions.

Composition
Ingredient Quantity (% w/w)
Phosphamidon active ingredient Minimum 1.0 to 50 Max.
Stabilizer Min. 0.1 to 5 Max.
Bittering agent Min. 0.001 to 0.01 Max.
Disintegrating agent Min. 0.5 to 20 Max.
Antifoaming agent Min. 0.1 to 3.0 Max.
Wetting agent Min. 0.5 to 10 Max.
Dispersing agent Min. 0.1 to 5.0 Max.
Binding agent Min.0.01 to 5.0 Max.
Dye(s) Min. 0.01 to 5.0 Max.
Fillers q. s.
total 100.00 %(w/w)
The preferred Phosphamidon technical is of purity 92% min.
The preferred stabilizer a blend of the derivatives of epoxylated vegetable oil, Ethoxylated polyoxyethylene amine and pyroolidine and / or lactone.
The prefered bittering agent is lignocaine derivative or a mixture thereof.
The preferred disintegrating agent is swelling type clays like bentonite, Zeolite, Attapulgite and inorganic salts like Sodium and Ammonium Sulphate..
The preferred antifoaming agent is Silicone oil derivative or a mixture thereof.
The preferrred wetting agent is calcium /sodium sale of alkyl aryl sulphonate.
The prefered dispersing agent is formaldehyde condensate of alkyl phenols.
The preferred binding agent is polyvinylpyrralidone of any suitable grade.
The preferred dye(s) are selected from any suitably and easily available water solube dye(s)
The preferred filler(s) is precipitated Silica and diatomaceous earth kaolin in the ratio of 1:10 to 10:1.

Dust free granules prepared by the prefered method and prefered composition of the present invention provides following advantages.
♦ Dust free
♦ Good pourability
♦ Low transportation cost
♦ Low capital investment
♦ Good stability of product
♦ Free flowability
♦ Free from Solvents
♦ 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.
♦ 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

The granules are tested for requited 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.
The following examples presented to illustrate but not restrict the present invention. Parts and percentage are by weight unless otherwise specified.

Example- 1.
Phosphamidon 1.0 % granules can be prepared as follows :
Composition
Ingredient Phosphamidon Technical @, 92% Stabilizer Bittering agent Disintegrating agent Antifoaming agent Wetting agent Dispersing agent Binding agent Dye(s) Fillers
total

Quantity (% w/w) 1.0870 0.1000 0.0010 20.0000 2.5000 5.0000 5.0000 3.0000 1.0000 62.3120
100.00 %(w/w)

The required quantity of dispersing agent , wetting agent, disintegiating agent antifoaming agent, stabilizers, bittering agent and filler(s) are mixed homogenously to have a uniform mixture and the spraying of Phosphamidon technical (the 2-chloro-2 diethylcarbamoyl-1- methylvinyl dimethylphosphate) active over this mixture is done and the whole mass is throughly mixed for sufficient time to obtain the homogenous bulk until the required percentage of active ingredient is obtained . Thereafter this homogenous bulk on passing the quality test is fed through a screw feeder into the hopper of granulator preferably maintaining the inlet temperature of 30 - 35 ° C and the outlet temperature of 40 - 45 ° C and the rate and quantity of material fed to the granulator to minimize clumping together of the granulated product. The granules obtained are then processed for sizing and sieving to get the required quality granules. The fines collected after sieving are recycled.

Example - 2.
Phosphamidon 5.0 % granules can be prepared as follows:
Composition
Ingredient Quantity (% w/w)
Phosphamidon Technical @ 92% 5.4348
Stabilizer 0.3000
Bittering agent 0.0010
Disintegrating agent 18.0000
Antifoaming agent 2.5000
Wetting agent 6.0000
Dispersing agent 5.0000
Binding agent 3.5000
Dye(s) 1.0000
Fillers total 58.2642



100.00% (w/w)
The granules with the above composition can be prepared by the process as described in Example -1.

Example - 3
Phosphamidon 10.0% granules can be prepared as follows :
Composition
Ingredient Ouantitv (% w/w)
Phosphamidon Technical @, 92% 10.8700
Stabilizer 0.5000
Bittering agent 0.0020
Disintegrating agent 17.5000
Antifoaming agent 3.0000
Wetting agent 7.0000
Dispersing agent 5.0000
Binding agent 4.0000
Dye(s) 0.9000
Fillers total 51.2280



100.00% (w/w)
The granules with the above composition can be prepared by the process as described in Example -1.

Example -4.
Phosphamidon 15.0 % granules can be prepared as follows :
Composition
Ingredient Quantity (% w/w)
Phosphamidon Technical @ 92% 16.3044
Stabilizer 0.7500
Bittering agent 0.0030
Disintegrating agent 15.0000
Antifoaming agent 2.0000
Wetting agent 5.0000
Dispersing agent 3.0000
Binding agent 1.8500
Dye(s) 0.8000
Fillers total 55.2926


100.00% (w/w)
The granules with the above composition can be prepared by the process as described in Example -1.

Example - 5.
Phosphamidon 20.0 % granules can be prepared as follows :
Composition
Ingredient Ouantitv (% w/w)
Phosphamidon Technical @ 92% 21.7392
Stabilizer 1.0000
Bittering agent 0.0030
Disintegrating agent 14.0000
Antifoaming agent 3.0000
Wetting agent 7.5000
Dispersing agent 2.5000
Binding agent 2.0000
Dye(s) 0.6000
Fillers total 47.6578



100.00% (w/w)
The granules with the above composition can be prepared by the process as described in Example -1.

Example - 6 Phosphamidon 30.0 % granules can be prepared as follows Composition
Ingredient Phosphamidon Technical @ 92% Stabilizer Bittering agent Disintegrating agent Antifoaming agent Wetting agent Dispersing agent Binding agent Dye(s) Fillers
total

Quantity (% w/w) 32.6087
1.5000 0.0050 12.0000
2.0000
6.0000
4.0000
2.5000
0.6500 38.7363
100.00% (w/w)

The granules with the above composition can be prepared by the process as described in Example -1.

Example - 7
Phosphamidon 40.0% granules can be prepared as follows :
Composition
Ingredient Phosphamidon Technical @, 92% Stabilizer Bittering agent Disintegrating agent Antifoaming agent Wetting agent Dispersing agent Binding agent Dye(s) Fillers

Quantity (% w/w) 43.4783 3.0000 0.0020
7.5000
1.0000 10.0000
2.5000
1.0000
0.5000 31.0197

total

100.00 % (w/w)

The granules with the above composition can be prepared by the process as described in Example -1.

Example - 8
Phosphamidon 50.0% granules can be prepared as follows :
Composition
Ingredient Phosphamidon Technical @ 92% Stabilizer Bittering agent Disintegrating agent Antifoaming agent Wetting agent Dispersing agent Binding agent Dye(s) Fillers

Quantity (%w/w) 52.6316 4.5000 0.0020
2.5000
1.0000
2.5000
1.0000
0.5000
0.1500 35.2164

100.00 %(w/w) be prepared by the process as
total
The granules with the above composition can described in Example -1.
The following physical properties relating to the quality of these granules are determined before and after ageing at 45°C for 500 hrs like flowability, wetting time, pH, a.i. test, tap density, suspensibility, sedimentation and persistent foam. No noticeable difference in all the above properties observed.
The dynamic wet time (records) is detennined by adding 1 g sample of formulation into 250 ml water in a 500 ml beaker stirred at 850 rpm (MT-167 of CIPAC).
The pH of a 5% aq. Mixture is detennined by using a standard electrode as per MT-75 of
CIPAC.
The flowability is measured as per MT-172 of CIPAC.
The diy sieve test is measured as per MT-170 of CIAPC
The sedimentation is measured as per MT - ]51 of CIPAC.
The dispersibility is measured as per MT-174 of CIPAC.
The tap density is measured as per MT 58.4 and MT-33 of CTPAC.
The Phosphamidon content can be detennined by GLC or by classical method published
in AOAC.
The persistent foam is measured for 0.5% aqueous mixture as per MT-47.1 of CIPAC

Diagram of Flow-Chart for Manufacturing of granular composition of 2chtoro-2 diethvlcarbamovl-1- methvlvinyl dimethvlphosphate (Phosphamidon)


WE CLAIM
1. A storage stable, granular insecticide and acaricidal composition of 2-chloro-2-diethylcarbamoyl-1-methylvinyl dimethyl phosphate comprising of 2-chloro-2-diethylcarbamoyl-1 -methylvinyl dimethylphosphate active ingredient 1.0 to 50% along with stabilizer, bittering agent, disintegrating agent, antifoaming agent, dispersing agent, wetting agent, binding agent, dye(s) and filler(s).
2. A composition as claimed in claim 1 wherein the antifoaming agent is in 0.1% to 3.0 %; wetting agent 0.5 to 10%; dispersing agent in 0.1 to 5.0 %; binding agent in 0.01 to 0.01%; disintegrating agent 0.5 to 20% and fillers to make the composition 100% w/w.
3. A composition as claimed in claim 1 wherein the stabilizer is a blend of the derivative of epoxylated vegetable oil, ethoxylated polyoxyethylene amine and pyrollidone and/or lactone.
4. A composition as claimed in claim 1 wherein the bittering agent is a Hgnocaine derivative or a mixture thereof.
5. A composition as claimed in claim 1 wherein the disintegrating agent is swelling type class like bentonite, Zeolite, Attapulgite and inorganic salts like sodium and ammonium sulphate.
6. A composition as claimed in claim 1 wherein the antifoaming agent is silicone oil derivative or a mixture thereof.

7. A composition as claimed in claim 1 wherein the wetting agent is calcium / sodium salt of alkyl aryl sulphonate.
8. A composition as claimed claim 1 wherein the dispersing agent is formaldehyde condensate of alkyl phenols.
9. A composition as claimed in claim 1 wherein the binding agent is polyvinylpyrollidone of any suitable grade.
10. A composition as claimed in claim 1 wherein the dye is sunset yellow colour.
11. A composition as claimed in claim 1 wherein the filler is precipitated silica and diatomaceous earth kaolin in the ratio of 1:10.
12. A composition for storage stable granular insecticidal and acaricidal composition as claimed in any of the above claims and substantially as herein described and exemplified.
Dated this 26th day of December 2000

M.B . TRIVEDI (COMPANY SECRETARY)
FOR UNITED PHOSPHORUS LIMITED