WO2021255664A1 - Insecticidal wdg formulations and process for preparing and use thereof - Google Patents

Insecticidal wdg formulations and process for preparing and use thereof Download PDF

Info

Publication number
WO2021255664A1
WO2021255664A1 PCT/IB2021/055309 IB2021055309W WO2021255664A1 WO 2021255664 A1 WO2021255664 A1 WO 2021255664A1 IB 2021055309 W IB2021055309 W IB 2021055309W WO 2021255664 A1 WO2021255664 A1 WO 2021255664A1
Authority
WO
WIPO (PCT)
Prior art keywords
composition
water dispersible
dispersible granule
sodium
hexythiazox
Prior art date
Application number
PCT/IB2021/055309
Other languages
French (fr)
Inventor
Kiran Pawar
Ramesh Kumar DURGA
Balaram BHAVANI
Aminul Islam
Original Assignee
Coromandel International Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Coromandel International Limited filed Critical Coromandel International Limited
Publication of WO2021255664A1 publication Critical patent/WO2021255664A1/en

Links

Classifications

    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P7/00Arthropodicides
    • A01P7/04Insecticides
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/30Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl

Definitions

  • the present invention relates to insecticidal water dispersible granule (WDG) composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
  • WDG water dispersible granule
  • the present invention also relates to insecticidal water dispersible granule composition
  • insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, a wetting agent and dispersing agent.
  • the present invention specifically relates to insecticidal water dispersible granule composition
  • insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention specifically relates to insecticidal water dispersible granule composition
  • insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 50 : l to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention preferably relates to insecticidal water dispersible granule composition
  • insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention also relates to a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
  • Diafenthiuron is a pro-insecticide, which has to be first converted to its active form. The active compound then acts on a specific part of the energy-producing enzymes in the mitochondria. These results in immediate paralysis of the pest after intake or contact with the product. Diafenthiuron is chemically known as (4RS, 5RS)-5-(4-chlorophenyl)-N- cyclohexyl-4-methyl-2-oxo-l,3-thiazolidine-3-carboxamide and has the following structure.
  • Diafenthiuron was first reported in 1988 and first marketed in 1990. This product is not registered in EU under EC regulation 1107/2009.
  • Hexythiazox is used as an acaricide on a number of fruits, wines, hops and ornamental varieties such as lemons and oranges. Chemically Hexythiazox is known as trans-5-(4- Chlorophenyl)-N-cyclohexyl-4-methyl-2-oxothiazolidine-3-carboxamide and is depicted by the structure given below :
  • Hexythiazox was initially registered in April 13, 1989 in US EPA by E.I.Du Pont de Nemlours and marketed under the brand name of Savey®. The product was approved on June
  • Hexythiazox is sold in the form of an Emulsifiable concentrate (EC) in 50%,
  • CN 101305731 A discloses combination of acaricidal composition containing hexythiazox and diafenthiuron characterized in that the active ingredient is composed of Hexythiazox and diafenthiuron and the ratio of hexythiazox and diafenthiuron is between 50: 1 ⁇ 1: 50 (weight ratio).
  • the active ingredient is composed of Hexythiazox and diafenthiuron and the ratio of hexythiazox and diafenthiuron is between 50: 1 ⁇ 1: 50 (weight ratio).
  • all the examples relate to emulsifiable concentrate composition.
  • EP 0 837 633 A1 discloses a pesticidal composition which comprises a combination, which can be varied in terms of amounts, of the pesticidally active compound of diafenthiuron, in the free form or in the form of an agrochemically tolerated salt, and of the pesticidally active compound of hexythiazox in the free form or in the form of an agrochemically tolerated salt, and at least one auxiliary.
  • This application discloses compositions of wettable powders, granules. However, the compositions of the present invention are not enabled by the disclosure of this application.
  • US 20060013846 A1 discloses an agricultural or horticultural granular composition comprising as the essential components, (a) at least one of an agrochemically active ingredient, (b) at least one of a surfactant selected from a sulfonate-type surfactant, a sulfate- type surfactant and a phosphate-type surfactant, and (c) at least one of a metal salt of a fatty acid of 6 to 28 carbon atoms.
  • WDGs Water dispersible granules
  • WP wettable powder
  • WDG compositions of combinations which are environmentally safer and stable insecticidal / acaricidal compositions having two active ingredients with different physical and chemical properties, easy and effective combination formulation of two active with enhanced efficacy and stable product during storage.
  • a selective combination composition of two active ingredients comprising diafenthiuron, hexythiazox, a wetting agent and / or dispersing agent and other agrochemical auxiliaries, possesses enhanced efficacy, improved penetration and long duration control of phytopathogens as compared to its other traditional formulations with long storage stability across a wide temperature range and having no adverse impact on photosynthetic activity in plant and fruit quality.
  • the main objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
  • Another objective of the present invention is to provide an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, wetting agent and dispersing agent.
  • Another objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • Another objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox at a weight in the ratio of 50 : 1 to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • Another objective of the present invention is to provide preferably insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • Another objective of the present invention is to provide a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
  • the present invention provides an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
  • the present invention provides an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, wetting agent and dispersing agent.
  • the present invention provides an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention provides an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 50 : 1 to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention provides an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
  • the present invention provides an insecticidal water dispersible granule composition comprising;
  • the present invention provides an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising;
  • the present invention provides an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising;
  • pH adjusting agent 0.1 to 10% (w/w) of pH adjusting agent, and 5 to 50% (w/w) of inert fillers.
  • the present invention provides an insecticidal water dispersible granule composition
  • an insecticidal water dispersible granule composition comprising;
  • hydrous aluminosilicate 5 to 15% (w/w) of hydrous aluminosilicate, and 5 to 40% (w/w) of sodium sulphate.
  • the present invention provides a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
  • the present invention provides a process for the preparation of insecticidal water dispersible granule composition
  • a. blending active ingredients, wetting agent, dispersing agent along with other auxiliaries to obtain a homogenous mixture
  • b. milling the blended mixture to obtain particle size in the range of 10-15 m
  • c. mixing the milled material with water to make a dough
  • d. extruding the dough obtain in step (c) and drying the granules.
  • the present invention provides a process for the preparation of insecticidal water dispersible granule composition comprising the steps of; a. blending active ingredients, wetting agent, dispersing agent, disintegrating agents defoamer, pH stabilizer, and inert fillers to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules to obtain water- dispersible granules.
  • the present invention provides method of preparing a combination insecticidal composition comprising the steps of: a.
  • Diafenthiuron and Hexythiazox dialkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, nonionic and sodium ligno sulphonate blend, ammonium sulphate, polydimethyl siloxane, citric acid, hydrous aluminosilicate and sodium sulphate to obtain a homogenous mixture
  • the present invention provides insecticidal water-dispersible granules (WDG) composition comprising combination of diafenthiuron and hexythiazox in ratio of 50: 1 to 35 : 10, more preferably in the ratio of 42 : 3.5.
  • WDG water-dispersible granules
  • variables of the ratios of each of the active ingredients can be used and the selection of the particular amount is dependent upon many factors including, for example, type of formulations, the crop, disease sought to be controlled and environmental conditions. The selection of the proper quantity of active agent to be applied, however, is within the expertise of one skilled in the art.
  • the combination compositions of the present invention can be used on a number of fruits, wines, hops and ornamental varieties such as lemons and oranges.
  • T product is also used as a foliar application in labeled crops.
  • composition of the present invention could be applied to plants, seeds, fruits, soil as preventive and curative state.
  • insecticidal water dispersible granules composition comprising combination of diafenthiuron and hexythiazox, which comprises wetting agents, dispersing agents, disintegrating agents, defoamer, pH adjusting agents and fillers.
  • the wetting agent is a compound that facilitates rapid wetting of the powder when added to the water.
  • the wetting agent employed in the formulation composition is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.
  • the wetting agents as used in the present invention are selected from and not limited to polycondensation products of naphthalene sulfonic acid, which is alkyl Naphthalene sulphonate sodium salt, Polyalkyl Naphthalene sulphonate; Aqarius BP14332 Yellow IH, salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, salts of polyarylether sulphates such as tristyrylphenolethoxylate sulphate salts, alkoxylated alkylphenols and alcohols as well as block copolymers of ethyleneoxide and propylene oxide.
  • Preferred wetting agent used in the composition of the present invention is polycondensation product of naphthalene sulfonic acid (Supragil WP, Supragil MNS-90).
  • the wetting agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 2 to 10% of the total weight of the composition.
  • the wetting agent may also be used as a dispersing agent.
  • the dispersing agents as used in the present invention are selected from and not limited to sodium ligno sulphonates, sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers and graft copolymers ,polycarboxylates, alkyl naphthalene sulfonates (such as Morwet IP, Morwet EFW, Morwet 3028), phenol sulphonic acid condensates, alkyl sulfonates, alkenyl sylfonates, mixture of alkyl sulfonates and alkenyl sylfonates (Lissapol D), alkyl suflosuccinates (Geropon), L-Wet, methyl oleyltaurates and poly vinyl alcohols.
  • Preferred dispersing agents are polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols, Borresperse -NA is sodium lingo sulphonate, STEPSPERSE DF-600 is a blend of nonionic surfactant and sodium lignosulfonate, BREAK-THRU® DA 646 is a non ionic dispersant based on a specialty polyether, BREAK-THRU® DA 647, a modified polyether, is a non-ionic dispersant, BREAK-THRU® DA 655 is a polyether phosphate, BREAK-THRU® DA 675 is a non-ionic, aqueous based organically modified polymer, Atlox MetasperseTM 550S Modified styrene acrylic polymer.
  • 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 co-polymer dispersant.
  • Preferred dispersing agent used in the composition of the present invention is blend of nonionic surfactant (STEPSPERSE DF-600) and sodium lignosulfonate or sodium lignosulphonate (Borresperse).
  • the dispersing agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 2% to 10% of the total weight of the composition.
  • the disintegrating agents as used in the present invention are selected from and not limited to microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenyl sulphonates, sodium starch glycolate, sodium lignin sulfonate, sodium lauryl sulfate, combinations of carbonates with solid acids, agar, starch, hydroxypropylstarch, sodium alginate, carboxymethyl starch ether, gum arabic, gum tragacanth, gelatin, casein, crystalline cellulose, carboxymethylcellulose calcium, Tween, Pluronic, sodium laurate, carboxylic resins, potassium chloride, sodium chloride, urea, anionic surfactants, calcium chloride, magnesium chloride, aluminum chloride, glucose, lactose, sodium glutamate, sodium inosinate, dextrin, blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof).
  • Preferred disintegrating agent is
  • defoamers as used in the present invention are selected from and not limited to absorbed polydimethyl siloxane (Rhodosil EP-6703), stearates; silicones (SILFOAM®, SILFAR®, PUFPSIF® and WACKER® AK) and ethoxylates.
  • defoamer is polydimethyl siloxane (Rhodosil EP-6703).
  • the defoamers present in the composition of the present invention are in the range of 0.1% to 10%, more preferably 0.1% to 5% of the total weight of the composition.
  • the pH stabilizer or adjusting agents as used in the present invention are selected from and not limited to acids or bases which are conventionally used to adjust the pH of any medium. Acids that can be used to adjust pH is selected from phosphoric acid, citric acid.
  • the pH stabilizer or adjusting agent present in the composition of the present invention is in the range of 0.1% to 10%, more preferably 0.1% to 5% of the total weight of the composition.
  • the inert fillers used in the present invention are selected from and not limited to natural minerals such as calcite, talc, china clay series like hydrous aluminosilicate, and montmorillonite or attapulgite clays including various forms of Bentonite, Kaolin; lactose anhydrous, lactose monohydrate, starches, sodium sulphate, sodium bicarbonate, calcium carbonate, calcium sulphate, calcium phosphate, sodium tripoly phosphate (STPP), woodflours, activated carbon, sugars, diatomaceous earth, cereal flours, fine-grain inorganic solids, and the like.
  • natural minerals such as calcite, talc, china clay series like hydrous aluminosilicate, and montmorillonite or attapulgite clays including various forms of Bentonite, Kaolin; lactose anhydrous, lactose monohydrate, starches, sodium sulphate, sodium bicarbonate, calcium carbonate, calcium sulphate, calcium
  • Clays and inorganic solids which may be used include calcium bentonite, perlite, mica, vermiculite, silicas, quartz powder, montmorillonite and mixtures thereof.
  • Sugars which may be useful include dextrin and maltodextrin.
  • Preferred inert fillers are lactose anhydrous, hydrous aluminosilicate (China clay), sodium sulphate, sodium bicarbonate and mixtures thereof.
  • the inert fillers present in the composition of the present invention are in the range of 5 to 50%, more preferably 10 to 45% of the total weight of the composition.
  • the water dispersible granule composition according to the present invention can comprise from 0.5 to 35 wt% of adjuvants commonly used in this field and well known to those expert in the art, such as antidrift agents, adhesives, penetrants, stickers and spreaders.
  • the water dispersible granule compositions of the present invention can be diluted with water or water solutions of agronomic compounds before use to produce a sprayable composition which is used in treating plants or increasing plant growth. Dilution in water usually results in suspensions, emulsions, suspo-emulsions or solutions of the agrochemical active ingredient at a concentration of at least 0.001 g/1.
  • compositions according to the present invention possess advantageous curative, preventive and antisporulant fungicidal activity to protect plants, fruit and seeds.
  • the present composition can be used to protect plants or parts of plants, e.g. fruit, blossoms, flowers, foliage, stems, roots, cuttings, tubers of plants or culture plants infected, harmed or destroyed by micro-organisms, whereby later-growing parts of plants are protected against such micro organisms.
  • Application may be made by ground or aerial spray equipment.
  • cereals e.g. wheat, barley, rye, oats, rice, sorghum and the like
  • beets e.g. sugar beet and fodder beet
  • pome and stone fruit and berries e.g. apples, pears, plums, peaches, almonds, cherries, strawberries, raspberries and blackberries
  • leguminous plants e.g. beans, lentils, peas, soy beans
  • oleaginous plants e.g.
  • rape mustard, poppy, olive, sunflower, coconut, castor-oil plant, cocoa, ground-nuts; cucurbitaceae, e.g. pumpkins, gherkins, melons, cucumbers, squashes; fibrous plants, e.g. cotton, flax, hemp, jute; citrus fruit, e.g. orange, lemon, grapefruit, mandarin; vegetables, e.g. spinach, lettuce, asparagus, brassicaceae such as cabbages and turnips, carrots, onions, tomatoes, potatoes, hot and sweet peppers; laurel-like plants, e.g.
  • avocado, cinnamon, camphor tree or plants such as maize, tobacco, nuts, coffee, sugar-cane, tea, vines, hops, bananas, rubber plants, as well as ornamental plants, e.g. flowers, shrubs, deciduous trees and evergreen trees such as conifers. This enumeration of culture plants is given with the purpose of illustrating the invention and not to delimiting it thereto.
  • a particular mode of administering the composition of the present invention is the administration to the aboveground parts of plants, in particular to the leaves thereof (leaf- application).
  • the number of applications and the administered doses are chosen in accordance with the biological and climatic conditions of life of the causative agent.
  • the antifungal compositions though, can also be applied to the soil and get into the plants through the root system (systemic activity), in case the locus of the plants is sprayed with a liquid composition or if the components are added to the soil in a solid formulation e.g. in the form of granulate (soil application).
  • the application rate can be varied within a relatively wide range, depending on the kind of application.
  • the active-compound combination application rates are generally between 0.1 and 10 000 g/ha, preferably between 100 and 2500 g/ha.
  • the active compound combination application rates are generally between 0.001 and 50 g per kilogram of seed, preferably between 0.01 and 20 g per kilogram of seed.
  • the active-compound combination application rates are generally between 0.1 and 10000 g ha preferably between 1 and 5000 g/ha.
  • Step 1 Pre- blending
  • the pre-blended material of step -01 was air jet milled to particle size less than 10 microns at pressure of minimum 6.0kg/Cm . particle size analyzed by doing sieve test using 500 mesh sieve and the desired particle size is achieved. Collected the material from the post blender.
  • Step 3 preparation of granules
  • the post blend material was made into dough by adding distilled water and the dough was subjected to extrusion using basket extruder and the granules achieved are subjected to drying.
  • compositions of examples 2-7 were also prepared using the similar method used for the preparation of example 1 composition.
  • Example 2 Example 3:
  • Diafenthiuron 42% + Hexythiazox 3.5% WDG composition has shown excellent efficacy as well as residual control over the both Diafenthiuron 42% WP and Hexythiazox 3.5 % EC solo composition and combination of Diafenthiuron 15% + Hexythiazox 3% EC compositions.
  • Chilli, Capsicum annum L. belongs to the family Solanaceae is one of the important commercial crops grown in India. Nearly 35 species of insect pests occur on chilli which includes thrips, mites, whiteflies, aphids, fruit borers, cutworm, and other minor pests. The field efficacy trials were conducted on sucking pest complex in chilli.
  • the sucking pests viz., yellow mite, Polyphagotarsonemus latus, thrips, Scirtothrips dorsalis and whitefly Bemisia tabaci (Gennadius) causes severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield.
  • Some sucking pests are cosmopolitan, polyphagous, widely distributed in tropical, sub-tropical and temperate regions and are also vectors for several viral diseases in large number of plants.
  • Brinjal, Solanum melongena L. is known as King of Vegetables originated from India where a wide range of wild types and land races occurs. In India, the crop is damaged by 30 insect pests obtaining from nursery stage. Of which includes shoot and fruit borer, mites, whiteflies, aphids, jassids and epilachna beetle. The field efficacy trials were conducted on mites and whiteflies in Brinjal.
  • the sucking pests viz., mites, Tetranychus urticae, and whitefly Bemisia tabaci (Gennadius) causes severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield. Insecticide application is one of the management options that can substantially reduce yield losses by controlling sucking pests. Therefore, bio efficacy of newer insecticide combinations needs to be studied for formulating effective and economical management strategies of insect pests.
  • Table 2 Sucking Pests control in Brinjal against Mites, Whitefly adults and nymphs.
  • WDG- Water Dispersible Granules, WP- Wettable Powder, EC- Emulsifiable Concentrate DAA Days after Application The trial results illustrated in Table 2 shows excellent efficacy of WDG composition of the present invention against mites and whiteflies in Brinjal.
  • the solo application as well as the combination of two active ingredients tested here against mites, whitefly nymphs and adults.
  • Diafenthiuron 42% WP and Hexythiazox 3.5 % EC solo compositions did not provide satisfactory control of sucking pest complex, whereas WDG composition of the present invention has shown excellent efficacy as well as residual control.
  • Tomato (Solarium lycopersicum L) is one of the most widely cultivated and consumed food crops among the vegetables in India. Tomato production has been fluctuating due to many biotic and abiotic constraints. Among biotic constraints pests and diseases which reduces the yields and quality of marketable fruits.
  • the major insect pests include borers, leaf miners, whiteflies, mites, thrips and aphids and mealybugs.
  • the field trials were conducted to evaluate the efficacy of innovative mixtures of Diafenthiuron and Hexythiazox against sucking pests of tomato viz., Mites, Tetranychus urticae, Whitefly, Bemisia tabaci, Thrips, Thrips tabaci, F. rankliniella which cause severe damage.
  • Table 3 Sucking Pests control in Tomato against mites, thrips, and whiteflies

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
  • Dentistry (AREA)
  • Insects & Arthropods (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The present invention relates to insecticidal water dispersible granule (WDG) composition comprising combination of a) thiourea derivative, and b) thiazox acaricide. The present invention specifically relates to insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries. The present invention also relates to a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.

Description

INSECTICIDAL WDG FORMULATIONS AND PROCESS FOR PREPARING AND USE THEREOF
FIELD OF THE INVENTION
The present invention relates to insecticidal water dispersible granule (WDG) composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
The present invention also relates to insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, a wetting agent and dispersing agent.
The present invention specifically relates to insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
The present invention specifically relates to insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 50 : l to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
The present invention preferably relates to insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
The present invention also relates to a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
BACKGROUND OF THE INVENTION
Diafenthiuron is a pro-insecticide, which has to be first converted to its active form. The active compound then acts on a specific part of the energy-producing enzymes in the mitochondria. These results in immediate paralysis of the pest after intake or contact with the product. Diafenthiuron is chemically known as (4RS, 5RS)-5-(4-chlorophenyl)-N- cyclohexyl-4-methyl-2-oxo-l,3-thiazolidine-3-carboxamide and has the following structure.
Figure imgf000003_0001
Diafenthiuron was first reported in 1988 and first marketed in 1990. This product is not registered in EU under EC regulation 1107/2009.
Hexythiazox is used as an acaricide on a number of fruits, wines, hops and ornamental varieties such as lemons and oranges. Chemically Hexythiazox is known as trans-5-(4- Chlorophenyl)-N-cyclohexyl-4-methyl-2-oxothiazolidine-3-carboxamide and is depicted by the structure given below :
Figure imgf000003_0002
Hexythiazox was initially registered in April 13, 1989 in US EPA by E.I.Du Pont de Nemlours and marketed under the brand name of Savey®. The product was approved on June
I, 2011 in EU. Hexythiazox is sold in the form of an Emulsifiable concentrate (EC) in 50%,
II.8 and 24.2% strengths. The product is also approved as WDG in 50% concentration.
Though, conventionally each of the insecticidal / agaricidal Active ingredients are used individually, there is increased interest in the use of Active ingredients in combination to give synergistic results.
Few prior-art references discloses the use of combinations of diafenthiuron and hexythiazox in different ratios, however, no product is approved so far with the specific combination.
CN 101305731 A discloses combination of acaricidal composition containing hexythiazox and diafenthiuron characterized in that the active ingredient is composed of Hexythiazox and diafenthiuron and the ratio of hexythiazox and diafenthiuron is between 50: 1 ~ 1: 50 (weight ratio). However, all the examples relate to emulsifiable concentrate composition.
EP 0 837 633 A1 discloses a pesticidal composition which comprises a combination, which can be varied in terms of amounts, of the pesticidally active compound of diafenthiuron, in the free form or in the form of an agrochemically tolerated salt, and of the pesticidally active compound of hexythiazox in the free form or in the form of an agrochemically tolerated salt, and at least one auxiliary. This application discloses compositions of wettable powders, granules. However, the compositions of the present invention are not enabled by the disclosure of this application.
US 20060013846 A1 discloses an agricultural or horticultural granular composition comprising as the essential components, (a) at least one of an agrochemically active ingredient, (b) at least one of a surfactant selected from a sulfonate-type surfactant, a sulfate- type surfactant and a phosphate-type surfactant, and (c) at least one of a metal salt of a fatty acid of 6 to 28 carbon atoms.
Water dispersible granules (WDGs) are a solid, non-dusty granular formulation which disperses or dissolves quickly when added to water in the spray tank to give a fine particle suspension. They provide a system for delivering solid active ingredients to a target organism. They allow for the production of highly-concentrated formulations which are wettable and easily disintegrated on contact with water. WDGs are an attractive alternative to wettable powder (WP) formulations due to their reduction in dust production.
Accordingly, there is a need in the art to provide WDG compositions of combinations which are environmentally safer and stable insecticidal / acaricidal compositions having two active ingredients with different physical and chemical properties, easy and effective combination formulation of two active with enhanced efficacy and stable product during storage.
It was surprisingly and unexpectedly found by the present inventors that a selective combination composition of two active ingredients comprising diafenthiuron, hexythiazox, a wetting agent and / or dispersing agent and other agrochemical auxiliaries, possesses enhanced efficacy, improved penetration and long duration control of phytopathogens as compared to its other traditional formulations with long storage stability across a wide temperature range and having no adverse impact on photosynthetic activity in plant and fruit quality.
OBJECTIVE OF INVENTION
The main objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
Another objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, wetting agent and dispersing agent.
Another objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
Another objective of the present invention is to provide an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox at a weight in the ratio of 50 : 1 to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries. Another objective of the present invention is to provide preferably insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
Another objective of the present invention is to provide a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
SUMMARY OF INVENTION
Accordingly, the present invention provides an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, and b) thiazox acaricide.
In one embodiment, the present invention provides an insecticidal water dispersible granule composition comprising combination of a) thiourea derivative, b) thiazox acaricide, wetting agent and dispersing agent.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 50 : 1 to 35 : 10 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient, wetting agent, dispersing agent and other agrochemical auxiliaries. In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient,
1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent, and 0.1 to 70% (w/w) of other additives / auxiliaries.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient,
1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 10% (w/w) of dialkyl naphthalene sulphonate sodium salt,
1% to 10% (w/w) of polyalkyl naphthalene sulphonate,
1% to 10% (w/w) of nonionic and sodium ligno sulphonate blend, and 0.1 to 70% (w/w) of other additives / auxiliaries.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient,
1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent,
0.5 to 20% (w/w) of disintegrating agent,
0.1 to 10% (w/w) of defoamer,
0.1 to 10% (w/w) of pH adjusting agent, and 5 to 50% (w/w) of inert fillers.
In another embodiment, the present invention provides an insecticidal water dispersible granule composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient, 1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 10% (w/w) of dialkyl naphthalene sulphonate sodium salt,
1% to 10% (w/w) of polyalkyl naphthalene sulphonate,
1% to 10% (w/w) of nonionic and sodium ligno sulphonate blend,
0.5 to 20% (w/w) of ammonium sulphate,
0.1 to 10% (w/w) of absorbed polydimethyl siloxane,
0.1 to 10% (w/w) of citric acid,
5 to 15% (w/w) of hydrous aluminosilicate, and 5 to 40% (w/w) of sodium sulphate.
In another embodiment, the present invention provides a process for the preparation of insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wherein the granules are prepared by extrusion process.
In another embodiment, the present invention provides a process for the preparation of insecticidal water dispersible granule composition comprising the steps of: a. blending active ingredients, wetting agent, dispersing agent along with other auxiliaries to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules.
In another embodiment, the present invention provides a process for the preparation of insecticidal water dispersible granule composition comprising the steps of; a. blending active ingredients, wetting agent, dispersing agent, disintegrating agents defoamer, pH stabilizer, and inert fillers to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules to obtain water- dispersible granules. In another embodiment, the present invention provides method of preparing a combination insecticidal composition comprising the steps of: a. blending Diafenthiuron and Hexythiazox, dialkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, nonionic and sodium ligno sulphonate blend, ammonium sulphate, polydimethyl siloxane, citric acid, hydrous aluminosilicate and sodium sulphate to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules to obtain water- dispersible granules.
DETAILED DESCRIPTION OF THE INVENTION
The term "comprising", which is synonymous with "including", "containing", or "characterized by" here is defined as being inclusive or open-ended, and does not exclude additional, unrecited elements or method steps, unless the context clearly requires otherwise.
The present invention provides insecticidal water-dispersible granules (WDG) composition comprising combination of diafenthiuron and hexythiazox in ratio of 50: 1 to 35 : 10, more preferably in the ratio of 42 : 3.5. However, variables of the ratios of each of the active ingredients can be used and the selection of the particular amount is dependent upon many factors including, for example, type of formulations, the crop, disease sought to be controlled and environmental conditions. The selection of the proper quantity of active agent to be applied, however, is within the expertise of one skilled in the art.
The combination compositions of the present invention can be used on a number of fruits, wines, hops and ornamental varieties such as lemons and oranges. T product is also used as a foliar application in labeled crops.
The composition of the present invention could be applied to plants, seeds, fruits, soil as preventive and curative state. In preferred embodiment the insecticidal water dispersible granules composition comprising combination of diafenthiuron and hexythiazox, which comprises wetting agents, dispersing agents, disintegrating agents, defoamer, pH adjusting agents and fillers.
The wetting agent is a compound that facilitates rapid wetting of the powder when added to the water. The wetting agent employed in the formulation composition is selected from the group consisting of non-ionic surfactants, anionic surfactant and a mixture of anionic and non-ionic surfactant and polymeric surfactant.
The wetting agents as used in the present invention are selected from and not limited to polycondensation products of naphthalene sulfonic acid, which is alkyl Naphthalene sulphonate sodium salt, Polyalkyl Naphthalene sulphonate; Aqarius BP14332 Yellow IH, salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, salts of polyarylether sulphates such as tristyrylphenolethoxylate sulphate salts, alkoxylated alkylphenols and alcohols as well as block copolymers of ethyleneoxide and propylene oxide. Preferred wetting agent used in the composition of the present invention is polycondensation product of naphthalene sulfonic acid (Supragil WP, Supragil MNS-90).
The wetting agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 2 to 10% of the total weight of the composition.
The wetting agent may also be used as a dispersing agent.
The dispersing agents as used in the present invention are selected from and not limited to sodium ligno sulphonates, sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters; aliphatic alcohol ethoxylates; alky ethoxylates; EO-PO block copolymers and graft copolymers ,polycarboxylates, alkyl naphthalene sulfonates (such as Morwet IP, Morwet EFW, Morwet 3028), phenol sulphonic acid condensates, alkyl sulfonates, alkenyl sylfonates, mixture of alkyl sulfonates and alkenyl sylfonates (Lissapol D), alkyl suflosuccinates (Geropon), L-Wet, methyl oleyltaurates and poly vinyl alcohols. Preferred dispersing agents are polycarboxylates, alkyl naphthalene sulfonates, phenol sulphonic acid condensates, lignosulphonates, methyl oleyltaurates and poly vinyl alcohols, Borresperse -NA is sodium lingo sulphonate, STEPSPERSE DF-600 is a blend of nonionic surfactant and sodium lignosulfonate, BREAK-THRU® DA 646 is a non ionic dispersant based on a specialty polyether, BREAK-THRU® DA 647, a modified polyether, is a non-ionic dispersant, BREAK-THRU® DA 655 is a polyether phosphate, BREAK-THRU® DA 675 is a non-ionic, aqueous based organically modified polymer, Atlox Metasperse™ 550S Modified styrene acrylic polymer. Once the granule has been diluted in water, ready for spraying (with the aid of the wetting agent), a dispersant is required to maintain the particles in suspension and prevent them from agglomerating. 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 co-polymer dispersant. Preferred dispersing agent used in the composition of the present invention is blend of nonionic surfactant (STEPSPERSE DF-600) and sodium lignosulfonate or sodium lignosulphonate (Borresperse).
The dispersing agents present in the composition of the present invention are in the range of 1% to 15%, more preferably 2% to 10% of the total weight of the composition.
The disintegrating agents as used in the present invention are selected from and not limited to microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates, sodium phenyl sulphonates, sodium starch glycolate, sodium lignin sulfonate, sodium lauryl sulfate, combinations of carbonates with solid acids, agar, starch, hydroxypropylstarch, sodium alginate, carboxymethyl starch ether, gum arabic, gum tragacanth, gelatin, casein, crystalline cellulose, carboxymethylcellulose calcium, Tween, Pluronic, sodium laurate, carboxylic resins, potassium chloride, sodium chloride, urea, anionic surfactants, calcium chloride, magnesium chloride, aluminum chloride, glucose, lactose, sodium glutamate, sodium inosinate, dextrin, blend of sulphonates (Sodium, calcium, potassium, magnesium or mixture thereof). Preferred disintegrating agent is ammonium sulphate. The disintegrating agents present in the composition of the present invention are in the range of 0.5% to 20%, more preferably 2% to 15% of the total weight of the composition.
The defoamers as used in the present invention are selected from and not limited to absorbed polydimethyl siloxane (Rhodosil EP-6703), stearates; silicones (SILFOAM®, SILFAR®, PUFPSIF® and WACKER® AK) and ethoxylates. Preferably defoamer is polydimethyl siloxane (Rhodosil EP-6703).
The defoamers present in the composition of the present invention are in the range of 0.1% to 10%, more preferably 0.1% to 5% of the total weight of the composition.
The pH stabilizer or adjusting agents as used in the present invention are selected from and not limited to acids or bases which are conventionally used to adjust the pH of any medium. Acids that can be used to adjust pH is selected from phosphoric acid, citric acid.
The pH stabilizer or adjusting agent present in the composition of the present invention is in the range of 0.1% to 10%, more preferably 0.1% to 5% of the total weight of the composition.
The inert fillers used in the present invention are selected from and not limited to natural minerals such as calcite, talc, china clay series like hydrous aluminosilicate, and montmorillonite or attapulgite clays including various forms of Bentonite, Kaolin; lactose anhydrous, lactose monohydrate, starches, sodium sulphate, sodium bicarbonate, calcium carbonate, calcium sulphate, calcium phosphate, sodium tripoly phosphate (STPP), woodflours, activated carbon, sugars, diatomaceous earth, cereal flours, fine-grain inorganic solids, and the like. Clays and inorganic solids which may be used include calcium bentonite, perlite, mica, vermiculite, silicas, quartz powder, montmorillonite and mixtures thereof. Sugars which may be useful include dextrin and maltodextrin. Preferred inert fillers are lactose anhydrous, hydrous aluminosilicate (China clay), sodium sulphate, sodium bicarbonate and mixtures thereof.
The inert fillers present in the composition of the present invention are in the range of 5 to 50%, more preferably 10 to 45% of the total weight of the composition.
The water dispersible granule composition according to the present invention can comprise from 0.5 to 35 wt% of adjuvants commonly used in this field and well known to those expert in the art, such as antidrift agents, adhesives, penetrants, stickers and spreaders.
The water dispersible granule compositions of the present invention can be diluted with water or water solutions of agronomic compounds before use to produce a sprayable composition which is used in treating plants or increasing plant growth. Dilution in water usually results in suspensions, emulsions, suspo-emulsions or solutions of the agrochemical active ingredient at a concentration of at least 0.001 g/1.
The compositions according to the present invention possess advantageous curative, preventive and antisporulant fungicidal activity to protect plants, fruit and seeds. The present composition can be used to protect plants or parts of plants, e.g. fruit, blossoms, flowers, foliage, stems, roots, cuttings, tubers of plants or culture plants infected, harmed or destroyed by micro-organisms, whereby later-growing parts of plants are protected against such micro organisms. Application may be made by ground or aerial spray equipment.
As examples of the wide variety of culture plants in which the combinations of present invention can be used, there may be named for example cereals, e.g. wheat, barley, rye, oats, rice, sorghum and the like; beets, e.g. sugar beet and fodder beet; pome and stone fruit and berries, e.g. apples, pears, plums, peaches, almonds, cherries, strawberries, raspberries and blackberries; leguminous plants, e.g. beans, lentils, peas, soy beans; oleaginous plants, e.g. rape, mustard, poppy, olive, sunflower, coconut, castor-oil plant, cocoa, ground-nuts; cucurbitaceae, e.g. pumpkins, gherkins, melons, cucumbers, squashes; fibrous plants, e.g. cotton, flax, hemp, jute; citrus fruit, e.g. orange, lemon, grapefruit, mandarin; vegetables, e.g. spinach, lettuce, asparagus, brassicaceae such as cabbages and turnips, carrots, onions, tomatoes, potatoes, hot and sweet peppers; laurel-like plants, e.g. avocado, cinnamon, camphor tree; or plants such as maize, tobacco, nuts, coffee, sugar-cane, tea, vines, hops, bananas, rubber plants, as well as ornamental plants, e.g. flowers, shrubs, deciduous trees and evergreen trees such as conifers. This enumeration of culture plants is given with the purpose of illustrating the invention and not to delimiting it thereto.
A particular mode of administering the composition of the present invention is the administration to the aboveground parts of plants, in particular to the leaves thereof (leaf- application). The number of applications and the administered doses are chosen in accordance with the biological and climatic conditions of life of the causative agent. The antifungal compositions though, can also be applied to the soil and get into the plants through the root system (systemic activity), in case the locus of the plants is sprayed with a liquid composition or if the components are added to the soil in a solid formulation e.g. in the form of granulate (soil application).
When using the active compound combinations according to the invention, the application rate can be varied within a relatively wide range, depending on the kind of application. For the treatment of parts of plants, the active-compound combination application rates are generally between 0.1 and 10 000 g/ha, preferably between 100 and 2500 g/ha. For seed dressing, the active compound combination application rates are generally between 0.001 and 50 g per kilogram of seed, preferably between 0.01 and 20 g per kilogram of seed. For the treatment of the soil, the active-compound combination application rates are generally between 0.1 and 10000 g ha preferably between 1 and 5000 g/ha.
Although the invention has been described above with reference to the disclosed embodiments, those skilled in the art will readily appreciate that the specific embodiments detailed are only illustrative of the invention. It should be understood that various modifications can be made without departing from the spirit of the invention. Accordingly, the invention is limited only by the claims.
The following examples describes the nature of the invention which are given only for the purpose of illustrating the present invention in more detail and are not limitative and relate to solutions, which have been particularly effective on bench scale.
EXAMPLES Example 1:
Figure imgf000015_0001
Manufacturing process: Step 1: Pre- blending
43.4 parts by weight of diafenthiuron technical, 3.8 parts by weight of hexythiazox technical, 3.0 parts by weight of dialkyl naphthalene sulphonate sodium salt, 3.0 parts by weight of polyalkyl naphthalene sulphonate, 3.0 parts by weight of nonionic and sodium ligno sulphonate blend and remaining excipients ammonium sulphate, absorbed polydimethyl siloxane, citric acid, hydrous aluminosilicate and sodium sulphate were preloaded in pre blender and mixed the contents to form homogenous mixture. Step 2: Air-Jet milling of WP
The pre-blended material of step -01 was air jet milled to particle size less than 10 microns at pressure of minimum 6.0kg/Cm . particle size analyzed by doing sieve test using 500 mesh sieve and the desired particle size is achieved. Collected the material from the post blender.
Step 3: preparation of granules
The post blend material was made into dough by adding distilled water and the dough was subjected to extrusion using basket extruder and the granules achieved are subjected to drying.
Compositions of examples 2-7 were also prepared using the similar method used for the preparation of example 1 composition.
Example 2:
Figure imgf000016_0001
Example 3:
Figure imgf000017_0001
Example 4:
Figure imgf000017_0002
Figure imgf000018_0001
Example 5:
Figure imgf000018_0002
Example 6:
Figure imgf000018_0003
Figure imgf000019_0001
Example 7:
Figure imgf000019_0002
Field Trials Data: The water dispersible granule combination composition of Diafenthiuron and Hexythiazox of the present invention were prepared and field efficacy trials were done in the fields of Chilli, Brinjal and Tomato. The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control with the WDG composition of the present invention is greater than the solo compositions and synergistic effect is observed (Ratio of O/E > 1, means synergism observed).
The field efficacy and Sucking Pests control against various insects i.e., Mites, Thrips, Whitefly adults and Whitefly Nymphs were observed and compared with solo composition. The combination of Diafenthiuron 42% + Hexythiazox 3.5% WDG composition has shown excellent efficacy as well as residual control over the both Diafenthiuron 42% WP and Hexythiazox 3.5 % EC solo composition and combination of Diafenthiuron 15% + Hexythiazox 3% EC compositions.
Trial 1: Pests of Chilli
Chilli, Capsicum annum L. belongs to the family Solanaceae is one of the important commercial crops grown in India. Nearly 35 species of insect pests occur on chilli which includes thrips, mites, whiteflies, aphids, fruit borers, cutworm, and other minor pests. The field efficacy trials were conducted on sucking pest complex in chilli. The sucking pests viz., yellow mite, Polyphagotarsonemus latus, thrips, Scirtothrips dorsalis and whitefly Bemisia tabaci (Gennadius) causes severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield. Some sucking pests are cosmopolitan, polyphagous, widely distributed in tropical, sub-tropical and temperate regions and are also vectors for several viral diseases in large number of plants.
Field trials were conducted and the efficacy of WDG composition of the present invention was evaluated against sucking pests in Chilli. The chilli crop was raised with all standard agronomic practices. The experiments were laid out in a Randomized Block Design (RBD) and replicated thrice with an individual plot size of 5 m X 6 m. Spraying was done with manual operated knapsack sprayer with 500 liter of water spray volume per hectare at 20-50 days after transplanting. The observations were recorded by counting the number of sucking insects (Mites, thrips and whitefly adults and nymphs) per leaf, six leaves per plant and five plants per plot. The observations were recorded before spraying, 10 DAA (Days After Application). The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control for the combination is greater than the expected percentage, there is a synergistic effect. (Ratio of O/E > 1 , means synergism observed). Table 1: Sucking Pests control in Chilli against Mites, Thrips, Whitefly adults and Whitefly nymphs
Figure imgf000021_0001
WDG- Water Dispersible Granules, WP- Wettable Powder, EC-Emulsifiable Concentrate DAA Days after Application.
The trial results given in Table 1 shows that WDG compositions of the present invention show excellent efficacy against sucking pest control in Chilli. The solo application Diafenthiuron 42% WP and Hexythiazox 3.5 % EC and combination of Diafenthiuron 15% + Hexythiazox 3% EC did not provide satisfactory control of sucking pest complex, whereas the WDG composition of the present invention has shown excellent efficacy as well as residual control.
Trial 2: Pests of Brinjal
Brinjal, Solanum melongena L. is known as King of Vegetables originated from India where a wide range of wild types and land races occurs. In India, the crop is damaged by 30 insect pests obtaining from nursery stage. Of which includes shoot and fruit borer, mites, whiteflies, aphids, jassids and epilachna beetle. The field efficacy trials were conducted on mites and whiteflies in Brinjal. The sucking pests viz., mites, Tetranychus urticae, and whitefly Bemisia tabaci (Gennadius) causes severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield. Insecticide application is one of the management options that can substantially reduce yield losses by controlling sucking pests. Therefore, bio efficacy of newer insecticide combinations needs to be studied for formulating effective and economical management strategies of insect pests.
Field trials were conducted and evaluated the efficacy of WDG composition of the present invention against mites and whiteflies in Brinjal. The brinjal crop was raised with all standard agronomic practices. The experiments were laid out in a Randomized Block Design (RBD) and replicated thrice with an individual plot size of 5 m X 6 m. Spraying was done with manual operated knapsack sprayer with 500 liter of water spray volume per hectare at 30-50 days after transplanting. The observations were recorded by counting the number of sucking insects (Mites and whitefly adults and nymphs) per leaf, six leaves per plant and five plants per plot. The observations were recorded before spraying, 10 DAA (Days After Application). The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control for the combination is greater than the expected percentage, there is a synergistic effect.
Table 2: Sucking Pests control in Brinjal against Mites, Whitefly adults and nymphs.
Figure imgf000022_0001
Figure imgf000023_0001
WDG- Water Dispersible Granules, WP- Wettable Powder, EC- Emulsifiable Concentrate DAA Days after Application The trial results illustrated in Table 2 shows excellent efficacy of WDG composition of the present invention against mites and whiteflies in Brinjal. The solo application as well as the combination of two active ingredients tested here against mites, whitefly nymphs and adults. Diafenthiuron 42% WP and Hexythiazox 3.5 % EC solo compositions did not provide satisfactory control of sucking pest complex, whereas WDG composition of the present invention has shown excellent efficacy as well as residual control.
Trial 3: Pests of Tomato:
Tomato (Solarium lycopersicum L) is one of the most widely cultivated and consumed food crops among the vegetables in India. Tomato production has been fluctuating due to many biotic and abiotic constraints. Among biotic constraints pests and diseases which reduces the yields and quality of marketable fruits. The major insect pests include borers, leaf miners, whiteflies, mites, thrips and aphids and mealybugs. The field trials were conducted to evaluate the efficacy of innovative mixtures of Diafenthiuron and Hexythiazox against sucking pests of tomato viz., Mites, Tetranychus urticae, Whitefly, Bemisia tabaci, Thrips, Thrips tabaci, F. rankliniella which cause severe damage.
Field trials were conducted and evaluated the efficacy of WDG composition of the present invention against mites, thrips, and whiteflies in tomato. The tomato crop was raised with all standard agronomic practices. The experiments were laid out in a Randomized Block Design (RBD) and replicated thrice with an individual plot size of 5 m X 6 m. Spraying was done with manual operated knapsack sprayer with 500 liter of water spray volume per hectare at 50 days after transplanting. The observations were recorded by counting the number of sucking insects (Mites, thrips and whitefly adults and nymphs) per leaf, six leaves per plant and five plants per plot. The observations were recorded before spraying, 10 DAA (Days After Application). The percent insect control and % disease control, the synergism was calculated and it was observed that the percentage of pesticidal control for the combination is greater than the expected percentage, there is a synergistic effect.
Table 3: Sucking Pests control in Tomato against mites, thrips, and whiteflies
Figure imgf000024_0001
WDG- Water Dispersible Granules, WP- Wettable Powder, EC-Emulsifiable Concentrate DAA Days after Application
The trial results of Table 3 show excellent efficacy of WDG composition of the present invention against sucking pest complex in tomato. The solo application as well as the combination of two active ingredients were tested against mites, thrips, whitefly nymphs and adults. Diafenthiuron 42% WP and Hexythiazox 3.5 % EC solo compositions did not provide satisfactory control of sucking pest complex, where as WDG composition of the present invention has shown excellent efficacy as well as residual control.

Claims

WE CLAIM:
1. An insecticidal water dispersible granule composition comprising combination of diafenthiuron and hexythiazox, wetting agent, dispersing agent and other agrochemical auxiliaries.
2. The insecticidal water dispersible granule composition as claimed in claim 1, wherein said composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 50 : 1 to 35 : 10 of first active ingredient to the second active ingredient.
3. The insecticidal water dispersible granule composition as claimed in claim 2, wherein said composition comprising combination of diafenthiuron and hexythiazox in the weight ratio of 42 : 3.5 of first active ingredient to the second active ingredient.
4. The insecticidal water dispersible granule composition as claimed in claim 1, wherein said composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient,
1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent, and 0.1 to 70% (w/w) of other additives / auxiliaries.
5. The insecticidal water dispersible granule composition as claimed in claim 4, wherein said composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient,
1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 15% (w/w) of wetting agent,
1% to 15% (w/w) of dispersing agent,
0.5 to 20% (w/w) of disintegrating agent,
0.1 to 10% (w/w) of defoamer,
0.1 to 10% (w/w) of pH adjusting agent, and 5 to 50% (w/w) of inert fillers.
6. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said wetting agent is selected from polycondensation products of naphthalene sulfonic acid, which is dialkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, salts of alkylphenol condensates, salts of sulphonated lignins, salts of poly acid resin copolymers, salts of polyphenol formaldehyde resins, salts of polyarylether sulphates such as tristyrylphenolethoxylate sulphate salts, alkoxylated alkylphenols and alcohols as well as block copolymers of ethyleneoxide and propylene oxide and mixtures thereof.
7. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said dispersing agent is s selected from sodium ligno sulphonates, sodium naphthalene sulphonate formaldehyde condensates; tristyrylphenol ethoxylate phosphate esters, alkyl sulfonates, alkenyl sylfonates, mixture of alkyl sulfonates and alkenyl sylfonates, methyl oleyltaurates and poly vinyl alcohols or mixtures thereof.
8. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said disintegrating agent is selected from microcrystalline cellulose, crosslinked PVP, ammonium sulphate, sodium sulphate, sodium citrate, polycarboxylates or mixtures thereof.
9. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said defoamer is selected absorbed polydimethyl siloxane, stearates; silicones and ethoxylates or combinations thereof.
10. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said pH stabilizer or adjusting agent is selected from acids or bases which are phosphoric acid, citric acid, sodium hydroxide or mixtures thereof.
11. The insecticidal water dispersible granule composition as claimed in claim 5, wherein said inert filler is selected from natural minerals such as calcite, talc, china clay series like hydrous aluminosilicate, lactose anhydrous, lactose monohydrate, starches, sodium sulphate, sodium bicarbonate, calcium carbonate, calcium sulphate, calcium phosphate or and mixtures thereof.
12. A process for the preparation of insecticidal water dispersible granule composition comprising the steps of: a. blending active ingredients, wetting agent, dispersing agent along with other auxiliaries to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules.
13. The insecticidal water dispersible granule composition as claimed in claim 5, wherein composition comprising;
35 to 50 % (w/w) of diafenthiuron as first active ingredient, 1% to 10% (w/w) of hexythiazox as second active ingredient,
1% to 10% (w/w) of dialkyl naphthalene sulphonate sodium salt,
1% to 10% (w/w) of polyalkyl naphthalene sulphonate,
1% to 10% (w/w) of nonionic and sodium ligno sulphonate blend, 0.5 to 20% (w/w) of ammonium sulphate,
0.1 to 10% (w/w) of absorbed polydimethyl siloxane,
0.1 to 10% (w/w) of citric acid,
5 to 15% (w/w) of hydrous aluminosilicate, and 5 to 40% (w/w) of sodium sulphate.
14. The process for the preparation of insecticidal water dispersible granule composition as claimed in claim 12, wherein said process comprising the steps of: a. blending Diafenthiuron and Hexythiazox, dialkyl naphthalene sulphonate sodium salt, polyalkyl naphthalene sulphonate, nonionic and sodium ligno sulphonate blend, ammonium sulphate, polydimethyl siloxane, citric acid, hydrous aluminosilicate and sodium sulphate to obtain a homogenous mixture, b. milling the blended mixture to obtain particle size in the range of 10-15 m, c. mixing the milled material with water to make a dough, and d. extruding the dough obtain in step (c) and drying the granules to obtain water-dispersible granules.
PCT/IB2021/055309 2020-06-19 2021-06-16 Insecticidal wdg formulations and process for preparing and use thereof WO2021255664A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN202041025888 2020-06-19
IN202041025888 2020-06-19

Publications (1)

Publication Number Publication Date
WO2021255664A1 true WO2021255664A1 (en) 2021-12-23

Family

ID=79268544

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2021/055309 WO2021255664A1 (en) 2020-06-19 2021-06-16 Insecticidal wdg formulations and process for preparing and use thereof

Country Status (1)

Country Link
WO (1) WO2021255664A1 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997002748A1 (en) * 1995-07-10 1997-01-30 Novartis Ag Synergistic pesticidal composition of diafenthiuron and hexythiazox
CN101185435A (en) * 2007-11-21 2008-05-28 张少武 Miticide composition containing diafenthiuron active ingredient and uses thereof
CN101305731A (en) * 2008-06-18 2008-11-19 张少武 Acaricidal combination containing hexythiazox and diafenthiuron

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997002748A1 (en) * 1995-07-10 1997-01-30 Novartis Ag Synergistic pesticidal composition of diafenthiuron and hexythiazox
CN101185435A (en) * 2007-11-21 2008-05-28 张少武 Miticide composition containing diafenthiuron active ingredient and uses thereof
CN101305731A (en) * 2008-06-18 2008-11-19 张少武 Acaricidal combination containing hexythiazox and diafenthiuron

Similar Documents

Publication Publication Date Title
KR101747922B1 (en) A method for increasing the vigor and/or crop yield of agricultural plants under essentially non-existent pathogen pressure
AU2019265885B2 (en) Novel crop nutrition and fortification composition
EP2477485B1 (en) Method for reducing nitrous oxide emission from soils
CN102771510B (en) Insecticidal composition containing fosthiazate
CN105638701B (en) Nematicidal composition and application thereof
WO2019239358A1 (en) Agricultural composition
AU2023207319A1 (en) Fungicidal mixtures comprising combination containing phthalimide fungicides
CN110352967B (en) Composition, preparation, application and preparation method thereof
EP3087836B1 (en) Herbicidal composition and method for controlling plant growth
US20190104737A1 (en) Use of heterocyclic fluoroalkenyl sulfone compounds for repelling molluscs
WO2010015578A1 (en) Method for controlling fungal diseases in legumes
WO2022023912A1 (en) Synergistic herbicidal formulations, process for preparing thereof
WO2021255664A1 (en) Insecticidal wdg formulations and process for preparing and use thereof
CN117062530A (en) Synergistic insecticidal composition and method for preventing or controlling harmful organisms
WO2022029706A1 (en) Synergistic fungicidal composition
WO2013067894A1 (en) Agrochemical formulation and use thereof
US20210051954A1 (en) Method for increasing the resistance of a cereal plant
CN111820233B (en) Jiangchuan mycin and ningnanmycin compounded pesticide composition and preparation method and application thereof
US20240276981A1 (en) Novaluron solid composition
CN102657177A (en) Insecticidal composition and preparation and application thereof
CN107318879B (en) Insecticidal composition
EP4215047A1 (en) A method of controlling pest
WO2023079309A1 (en) A method of controlling insects
CA3225280A1 (en) Fungicidal use
Imoloame et al. Effect of method of weed control and insecticide (Lambdacyhalothrin) rates on the productivity of cowpea (Vigna unguiculata (L) Walp) in a Southern Guinea Savanna of Nigeria.

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21825034

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 21825034

Country of ref document: EP

Kind code of ref document: A1