High-load solid composition of asulam

Abstract

The present invention relates to a solid composition comprising at least about 300 g / kg of asulam or its salts thereof, with respect to the total composition; and processes for preparing the same.

Description

[0001] HIGH-LOAD SOLID COMPOSITION OF ASULAM

[0002] FIELD OF THE INVENTION:

[0003] The present invention relates to a solid composition of asulam or its salts thereof; and processes for preparing the same.

[0004] BACKGROUND OF THE INVENTION:

[0005] Asulam, also known as methyl 7V-(4-aminophenyl)sulfonylcarbamate), is a broadspectrum carbamate herbicide. Asulam is a plant growth inhibitor which inhibits folate synthesis by suppression of dihydropteroate synthase (DHPS) in plants. The structure of asulam is represented as:

[0006] Asulam is especially useful for post-emergence control of perennial grasses in crops such as sugarcane, soybean, cotton, etc. It provides effective control for a wide variety of herbicide-resistant and herbicide-tolerant weeds while reducing phytotoxicity in crops.

[0007] Asulam or its salts such as alkali metal salt (like sodium and potassium), ammonium salt, amine salt (like diethanolamine, triethanolamine, octylamine, morpholine and dioctylmethylamine) and alkaline earth metal salts (like calcium and magnesium) are known to possess herbicidal properties. Asulam, active against monocotyledonous and dicotyledonous weeds, is of substantial commercial importance, particularly because of its low toxicity to mammals, birds, fish and wildlife in general, and has a short soil persistence. Generally, asulam is available as soluble liquid (SL) formulation. The highest concentration in soluble liquid formulation usually is about 400 grams / litre of Asulam equivalent, beyond which the liquid formulation attains saturation and active ingredient may crystallize out. Another problem with soluble liquid formulation is that when prepared in combination with other active ingredient sometimes leads to incompatibility and degradation of one of the active ingredients thereby resulting in poor efficacy.

[0008] Solid formulations of any active ingredient are easier to handle and minimise the risk of exposure of active ingredients to the end-user. Furthermore, the use and development of solid formulation which contains active ingredient in higher concentration is always desired, as the high-load formulations reduce the overall cost of pest control through lower packaging costs, increased transportation efficiency and reduction in container disposal costs. However, such increase in concentration of active ingredient may lead to other challenges such as delayed disintegration / dispersion of active ingredient in field dilutions, incompatibility with other active ingredient when used in combination with other active ingredient and the likes. This challenge can be overcome by usage of suitable surfactants and stabilizing agents, which will successfully retain the integrity of the active(s) in the formulation and provide enhanced stability.

[0009] Therefore, there still exists a need to develop a commercially viable, efficient, high- load, solid composition of asulam or salts thereof which is user-friendly, stable and economic.

[0010] OBJECTIVES OF THE INVENTION:

[0011] It is an objective of the present invention to provide a high-load, solid composition of asulam or its salts thereof.

[0012] It is an objective of the present invention to provide a high-load, solid composition of asulam or its salts thereof, which is stable and economic. It is another objective of the present invention to provide a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof, with respect to the total composition.

[0013] It is another objective of the present invention to provide a stable, high-load, solid composition comprising asulam or its salts thereof and an additional pesticide.

[0014] It is yet another objective of the present invention to provide a process for preparation of a high-load, solid composition of asulam or its salts thereof.

[0015] It is yet another object of the present invention to provide a method for controlling undesired vegetation / weeds by applying a high-load, solid composition of asulam or its salts thereof.

[0016] SUMMARY OF THE INVENTION:

[0017] In an aspect of the present invention, there is provided a high-load, solid composition of asulam or its salts thereof.

[0018] In another aspect of the present invention, there is provided a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof, with respect to the total composition.

[0019] In another aspect of the present invention, there is provided a high-load, solid composition comprising:

[0020] (a) at least about 300 g / kg of asulam or its salts thereof;

[0021] (b) at least one surfactant; and

[0022] (c) a stabilizing agent. In another aspect, the present invention provides a process for preparation of a high- load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof.

[0023] In another aspect, the present invention provides use of a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof; for controlling growth of undesired vegetation / weeds.

[0024] In another aspect, the present invention provides a method for controlling growth of undesired vegetation / weeds, said method comprising applying a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof to a locus where vegetation / weeds control is desired.

[0025] DETAILED DESCRIPTION OF THE INVENTION:

[0026] The following description is provided to assist in a comprehensive understanding of exemplary embodiments of the invention. It includes various specific details to assist in that understanding but these are to be regarded as merely exemplary. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope of the invention. In addition, descriptions of well-known functions and constructions are omitted for clarity and conciseness. The terms used in the following description and claims are not limited to the bibliographical meanings but are merely used by the inventor to enable a clear and consistent understanding of the invention. Accordingly, it should be apparent to those skilled in the art that the following description of exemplary embodiments of the present invention are provided for illustration purpose only and not for limiting the scope of the invention as defined by the appended claims and their equivalents.

[0027] For the purposes of the present invention, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of materials / ingredients used in the specification are to be understood as being modified in all instances by the term “about”. Thus, before describing the present invention in detail, it is to be understood that this invention is not limited to particularly exemplified systems or process parameters that may of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments of the invention only and is not intended to limit the scope of the invention in any manner. The use of examples anywhere in this specification including examples of any terms discussed herein is illustrative only, and in no way limits the scope and meaning of the invention or of any exemplified term. Prior to setting forth the present subject matter in detail, it may be helpful to provide definitions of certain terms used herein.

[0028] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the invention, suitable methods and materials are described herein.

[0029] As used herein, the terms “comprising”, “including”, “having”, “containing”, “involving” and the like are to be understood to be open-ended, i.e., to mean including but not limited to. The terms “preferred” and “preferably” refer to embodiments of the invention that may afford certain benefits, under certain circumstances. The aspects and embodiments described herein shall also be interpreted to replace the clause “comprising” with either “consisting of’ or with “consisting essentially of’ or with “consisting substantially of’.

[0030] “About” or “approximately” as used herein is inclusive of the stated value and means within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art, considering the measurement in question and the error associated with measurement of the particular quantity (i.e., the limitations of the measurement system). For example, “about” can mean within one or more standard deviations, or within ±10% or ±5% of the stated value.

[0031] The use of the terms “a”, “an” and “the” and similar referents (especially in the context of the following claims) are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. The terms first, second etc., as used herein are not meant to denote any particular ordering, but simply for convenience to denote a plurality of, for example, layers.

[0032] All methods described herein can be performed in a suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”), is intended merely to better illustrate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention as used herein.

[0033] While the invention has been described with reference to an exemplary embodiment, it will be understood by those skilled in the art that various changes may be made, and equivalents may be substituted for elements thereof without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention is not limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.

[0034] The expression of various quantities in terms of “%” or “% w / v” or “% w / w” means the percentage by weight of the total solution or composition unless otherwise specified. The terms (grams per kilogram) (g / kg) and % weight by weight (%w / w) both express the concentration of active ingredient in composition in different units. Both can be converted into one another, for example, a 30% w / w active ingredient is equivalent to 300g / kg. The quantity of asulam or its salt is expressed either in g / kg or %w / w, throughout the specification.

[0035] As used herein the term “plant” or “crop” refers to whole plants, plant organs (e.g., leaves, stems, twigs, roots, trunks, limbs, shoots, fruits etc.), plant cells, or plant seeds. This term also encompasses plant crops such as fruits. The term “plant” may further include the propagation material thereof, which may include all the generative parts of the plant such as seeds and vegetative plant material such as cuttings and tubers, which can be used for the multiplication of the plant. This includes seeds, tubers, spores, corms, bulbs, rhizomes, sprouts basal shoots, stolons, and buds and other parts of plants, including seedlings and young plants, which are to be transplanted after germination or after emergence from soil.

[0036] The term “locus” as used herein denotes the vicinity or area designated for growth of a desired crop, and in which control of the growth and / or spread of undesirable vegetation is desired. The locus includes the vicinity of desired crop plants wherein undesirable vegetation growth has either occurred, is most likely to occur, or is yet to occur.

[0037] The term “plant propagation material” is understood to denote generative parts of a plant, such as seeds, vegetative material such as cuttings or tubers, roots, fruits, tubers, bulbs, rhizomes and parts of plants, germinated plants and young plants which are to be transplanted after germination or after emergence from the soil. These young plants may be protected before transplantation by a total or partial treatment by immersion.

[0038] Subsequently, the term “herbicide” encompasses both herbicides as well as plant growth regulators, as far as this does not otherwise emerge from the context. The term herbicide as used herein denotes a compound which controls or modifies the growth of undesired weeds / plants.

[0039] The term “herbicidally effective amount” indicates the quantity of such a compound or combination of such compounds which is capable of controlling or modifying effect on the growth of harmful plants / undesired vegetation / weeds. Controlling effects include all deviation from natural development, for example: killing, retardation, leaf bum, albinism, dwarfism, etc.

[0040] The terms “excipient” or “additive” mean inactive substance that forms a part of the composition. The terms “excipient” or “additive” mean essentially the same thing and can be used interchangeably.

[0041] As used herein, the term “improving plant growth” results in an increase in either the yield, as described above, or the vigour of the plant, as described above, or both the yield and the vigour of the plant. Improvement in plant vigour means that certain traits are improved qualitatively or quantitatively when compared with the same trait in a control plant which has been grown under the same conditions in the absence of the method of the invention. Such traits include, but are not limited to, early and / or improved germination, improved emergence, the ability to use less seeds, increased root growth, a more developed root system, increased root nodulation, increased shoot growth, increased tillering, stronger tillers, more productive tillers, increased or improved plant stand, less plant verse (lodging), an increase and / or improvement in plant height, an increase in plant weight (fresh or dry), bigger leaf blades, greener leaf colour, increased pigment content, increased photosynthetic activity, earlier flowering, longer panicles, early grain maturity, increased seed, fruit or pod size, increased pod or ear number, increased seed number per pod or ear, increased seed mass, enhanced seed filling, less dead basal leaves, delay of senescence, improved vitality of the plant, increased levels of amino acids in storage tissues and / or less inputs needed (e.g. less fertiliser, water and / or labour needed). A plant with improved vigour may have an increase in any of the aforementioned traits or any combination or two or more of the aforementioned traits. Improvement in plant growth means that certain traits are improved qualitatively or quantitatively when compared with the same trait in a control plant which has been grown under the same conditions in the absence of the method of the invention. Such traits include, but are not limited to, improved visual appearance of the plant, reduced ethylene (reduced production and / or inhibition of reception), improved quality of harvested material, e.g., seeds, fruits, leaves, vegetables (such improved quality may manifest as improved visual appearance of the harvested material) and the like.

[0042] As used herein, the “compositions” are interchangeably referred to as “formulations”.

[0043] As described herein, the term “SG” refers to soluble granules. A preparation consisting of granules to be applied as a true solution of active substance after dissolution in water but may contain insoluble inert ingredients. Water-soluble granules are formulated by various process as granules by extrusion, agglomeration, spray dying / prilling of active ingredient along with surfactants and other formulation ingredients.

[0044] As described herein, the term “GR” refers to extruded granules or spheronised granules or agglomerated granules. A free-flowing solid preparation of a defined granule size range ready for use.

[0045] Unless otherwise specified, the structures shown include all stereoisomers, enantiomers, diastereomers, geometric isomers, and the like, as understood by one skilled in the art. The compounds and compositions also include, for example, salts, solvates, polymorphs, and the like. As used throughout the invention, asulam or other active ingredients, include their salts, esters, ethers, polymorphs including solvates and hydrates. A salt includes salts that retain the biological effectiveness and properties of the active ingredient, and which are not biologically or otherwise undesirable, and include derivatives of the disclosed compounds in which the parent compound is modified by making inorganic and organic, non-toxic, acid or base addition salts thereof. The salts can be synthesized from the parent compound by conventional chemical methods.

[0046] High load solid agrochemical formulations are highly desirable due to their numerous benefits, such as reduced transportation and storage costs, lower application rates, and potentially longer-lasting efficacy. However, electrolytic active ingredients like asulam sodium tend to precipitate when used with hard water. This occurs because hard water contains high concentrations of calcium and magnesium ions, which react with the active ingredient, forming an insoluble solid that precipitates out of solution. This precipitation reduces the availability of the active ingredient for its intended purpose, negatively impacting the efficacy of the composition. The inventor of the present invention has successfully addressed this issue with their innovative solution.

[0047] In an embodiment of the present invention, there is provided a high-load, solid composition of asulam or its salts thereof.

[0048] In an embodiment, the formulation of the high-load, solid composition of asulam or its salts is solid formulations including but not limited to dusts, granules, soluble granules, pellets, wettable powders, dry flowables, soluble powders and likes.

[0049] In an embodiment, the high-load, solid composition of asulam or its salts thereof is present in a form of soluble granular (SG) formulation.

[0050] In another embodiment of the present invention, there is provided a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof, with respect to the total composition. In another embodiment of the present invention, there is provided a high-load, solid composition comprising at least about 30% w / w of asulam or its salts thereof, with respect to the total composition.

[0051] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0052] (a) at least about 300 g / kg of asulam or its salts thereof;

[0053] (b) at least one surfactant; and

[0054] (c) a stabilizing agent.

[0055] In another embodiment of the present invention, there is provided a soluble granular (SG) composition comprising:

[0056] (a) at least about 300 g / kg of asulam or its salts thereof;

[0057] (b) at least one surfactant; and

[0058] (c) a stabilizing agent.

[0059] In an embodiment, said high-load, solid composition comprises at least about 300 g / kg of asulam or its salts thereof, preferably at least about 400 g / kg of asulam or its salts thereof, preferably at least about 500 g / kg of asulam or its salts thereof, preferably at least about 600 g / kg of asulam or its salts thereof, preferably at least about 700 g / kg of asulam or its salts thereof, preferably at least about 800 g / kg of asulam or its salts thereof, and more preferably at least about 900 g / kg of asulam or its salts thereof, with respect to the total composition.

[0060] In an embodiment, said high-load, solid composition comprises about 300 g / kg to about 990g / kg of asulam or its salts thereof, with respect to the total composition.

[0061] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0062] (a) at least about 30% w / w of asulam or its salts thereof;

[0063] (b) at least one surfactant; and (c) a stabilizing agent.

[0064] In an embodiment, the amount solid asulam in the composition ranges from about 30% w / w to about 99% w / w with respect to the total composition.

[0065] In an embodiment, the purity of solid asulam is in a range from about 50% to about 99%, preferably from about 70% to about 95%, and more preferably from about 75% to about 99%.

[0066] In an embodiment, at least one surfactant is selected from the group comprising of non-ionic surfactants, anionic surfactants, or combinations thereof.

[0067] In an embodiment, the surfactant is a non-ionic surfactant. In an embodiment, the non-ionic surfactant is selected from the group comprising of polyalkylene oxide block co-polymers, linear or branched polyethoxylated Cio-Cis fatty alcohols, wherein the ethoxyl number (EO) ranges from 5 to 10; poly ethoxylated castor oil, wherein the ethoxyl number ranges from 15 to 40; alkoxylated phosphate esters; alkoxylated sulphate esters; polyethoxylated di styrylphenols having an ethoxylation number between 12 to 25; polyethoxylated tri styrylphenols having an ethoxylation number between 15 to 40; C12-C18 mono-, di and tri-esters of poly ethoxylated sorbitan wherein the ethoxylation number ranges from 4 to 20; C10- C 16 mixtures of alkyl polyglycosides optionally polyethoxylated or polypropoxylated wherein said alkylpolyglycosides have a different ethoxylation or propoxylation number, comprised between 10 to 25; polyethoxylated- polypropoxylated Cs-Cu aliphatic alcohols; polyaryl phenolethoxylate wherein the ethoxyl / propoxyl number is between 15 to 40, alkyl amine oxides, alkypolysaccharide, alkoxylated alkylether polyamine or combinations thereof.

[0068] In an embodiment, the non-ionic surfactant is selected from polyalkylene oxide block co-polymers comprising ethylene oxi de-propylene oxide copolymer. In an embodiment, the non-ionic surfactant is selected from polyalkylene oxide block co-polymers, polyethoxylated castor oil, alkoxylated phosphate esters, alkoxylated sulphate esters, alkyl amine oxides, alkypolysaccharide, alkoxylated alkylether polyamine or combinations thereof.

[0069] In an embodiment, the surfactant is anionic surfactant. In an embodiment, the anionic surfactant is selected from the group comprising alkali or alkaline salt of alkoxylated phostphate esters; alkali or alkaline salt of alkoxylated sulphate esters; alkali or alkaline salt of carboxylates, alkali or alkaline-earth salts of alkyl benzene sulfonates, alkylbenzene phosphonates, alkyl ether sulfates, salts or derivatives of lignosulfonates, alkali or alkaline earth salts of sulfosuccinate esters, alkali or alkaline earth salts of alkyl sulfates or polyacid polymers such as potassium polycarboxylate, sodium polyacrylate, sodium polymethacrylate or mixed combinations (copolymers) of styrene, acrylic, methacrylic acid monomer residues and polymaleic acid (e.g., from maleic acid or maleic anhydride), or combinations thereof.

[0070] In an embodiment, the anionic surfactant is selected from the group comprising of calcium salt of alkyl benzene sulfonate such as calcium dodecyl sulfonate; polyoxyethylene sorbitan monolaurate; alkali salt of lauryl sulfate such as sodium lauryl sulfate; alkyl naphthalene sulfonate or its alkali salt such as sodium alkyl naphthalene sulfonate, sodium naphthalene sulfonate, sodium alkyl naphthalene sulfonate sulfosuccinate, derivatives of lignosulfonates such as sodium lignosulfonate, alkali salt of naphthalene sulfonate condensate such as sodium salt of naphthalene sulfonate condensate, tri styrylphenol sulphate, tri styrylphenol phosphate esters, linear benzene sulphonates and alkyl ether sulphates, alkali salt resin of styrene methacrylic copolymer such as sodium salt resin of styrene methacrylic copolymer, modified styrene acrylic polymer, alkali salt of polycarboxylate such as potassium polycarboxylate, or combinations thereof. In an embodiment, the anionic surfactant is selected from the group comprising of alkyl naphthalene sulfonate, modified styrene acrylic polymer or mixture thereof.

[0071] In an embodiment, the composition may further comprise cationic surfactants or zwitterionic surfactants. The cationic surfactants or zwitterionic surfactants are selected from the group comprising alkylene oxide adducts of fatty amines, quaternary ammonium compounds having 8 to 22 carbon atoms (C8-C22), surfaceactive zwitterionic compounds such as taurides, betaines and sulfobetaines, or combinations thereof.

[0072] In an embodiment, the amount of the surfactant in the composition ranges from about 0.01% w / w to about 20% w / w.

[0073] In an embodiment, the amount of the surfactant in the composition ranges from about 0.01% w / w to about 10% w / w, preferably from about 0.05% w / w to about 8% w / w, and more preferably from about 0.1% w / w to about 5% w / w, with respect to the total composition.

[0074] In an embodiment, the composition comprises a stabilizing agent selected from the group comprising of ethylenediamine derivatives (such as EDTA and DTPA), sodium citrate, tannic acid, DL-tartaric acid, or combinations thereof.

[0075] In a preferred embodiment, the stabilizing agent is ethylenediaminetetraacetic acid (EDTA).

[0076] In another preferred embodiment, the stabilizing agent is trisodium citrate.

[0077] In an embodiment, the stabilizing agents have the ability to form coordination complexes with free metal ions in water which prevents unwanted reactions and sedimentation / turbidity. In general, presence of a stabilizing agent in the composition of the present invention exhibits prolonged shelf stability. In an embodiment, the amount of stabilizing agent in the high-load, solid composition ranges from about 0.1% w / w to about 10% w / w, preferably from about 0.5% w / w to about 8% w / w, and more preferably from about 1% w / w to about 5% w / w.

[0078] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0079] (a) about 300 g / kg to about 990g / kg of asulam or its salts thereof;

[0080] (b) about 0.01% w / w to about 10% w / w of surfactant; and

[0081] (c) about 0.1% w / w to about 10% w / w of stabilizing agent.

[0082] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0083] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0084] (b) about 0.01% w / w to about 20% w / w of surfactant; and

[0085] (c) about 0.1% w / w to about 10% w / w of stabilizing agent.

[0086] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0087] (a) about 300 g / kg to about 990g / kg of asulam or its salts thereof;

[0088] (b) about 0.05% w / w to about 8% w / w of surfactant; and

[0089] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0090] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0091] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0092] (b) about 0.05% w / w to about 8% w / w of polyalkylene oxide block co-polymers; and

[0093] (c) about 0.5% w / w to about 8% w / w of stabilizing agent. In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0094] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0095] (b) about 0.05% w / w to about 8% w / w of polyethoxylated castor oil; and

[0096] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0097] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0098] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0099] (b) about 0.05% w / w to about 8% w / w of alkylamine oxide; and

[0100] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0101] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0102] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0103] (b) about 0.05% w / w to about 8% w / w of modified styrene acrylic polymer; and

[0104] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0105] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0106] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0107] (b) about 0.05% w / w to about 8% w / w of alkyl naphthalene sulfonate; and

[0108] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0109] In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0110] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0111] (b) about 0.05% w / w to about 8% w / w of alkypolysaccharide,; and

[0112] (c) about 0.5% w / w to about 8% w / w of stabilizing agent. In another embodiment of the present invention, there is provided a high-load, solid composition comprising:

[0113] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0114] (b) about 0.05% w / w to about 8% w / w of alkoxylated alkylether polyamine,; and

[0115] (c) about 0.5% w / w to about 8% w / w of stabilizing agent.

[0116] In another embodiment of the present invention, there is provided a high-load, soluble granular composition comprising:

[0117] (a) about 300 g / kg to about 990g / kg of asulam or its salts thereof;

[0118] (b) about 0.1% w / w to about 5% w / w of surfactant; and

[0119] (c) about 1% w / w to about 5% w / w of stabilizing agent.

[0120] In an embodiment, the high-load solid composition further comprises a carrier. The carrier selected is soluble, insoluble or partially insoluble in water. The carrier is selected from the group comprising mineral carriers, plant carriers, synthetic carriers, water-soluble carriers, or combinations thereof. However, those skilled in the art will appreciate that it is possible to utilize different carriers without departing from the scope of the present invention. The carriers are commercially manufactured and available through various companies.

[0121] In another embodiment, the carrier is selected from the group comprising of minerals like clay such as china clay, acid clay, kaolin such as kaolinite, dickite, nacrite, and halloysite, serpentines such as chrysotile, lizardite, antigorite, and amesite, synthetic and diatomaceous silicas, precipitated silica, colloidal silica, attapulgite, bentonite, magnesium aluminum silicate, white carbon black, dolomite, montmorillonite minerals such as sodium montmorillonite, smectites, such as saponite, hectorite, Sauconite, and hyderite, micas, such as pyrophyllite, talc, agalmatolite, muscovite, phengite, sericite, and illite, silicas such as cristobalite and quartz, such as attapulgite and sepiolite; vermiculite, laponite, pumice, bauxite, hydrated aluminas, perlite, sodium bicarbonate, volclay, vermiculites, limestone, natural and synthetic silicates, charcoal, silicas, wet process silicas, dry process silicas, calcined products of wet process silicas, surface-modified silicas, mica, zeolite, diatomaceous earth, derivatives thereof; chalks, fuller's earth, loess, mirabilite, white carbon, slaked lime, synthetic silicic acid, starch, modified starch, cellulose, plant carriers such as cellulose, chaff, wheat flour, wood flour, starch, rice bran, wheat bran, and soyabean flour, casein sodium, sucrose, salt cake, inorganic and organic salt like sulphates, phosphates, nitrates , chlorides , citrates, acetates, ex. potassium pyrophosphate, sodium tripolyphosphate, their derivatives, other sodium based inert carrier such as sodium sulphate, trisodium citrate, sodium phosphate, sodium chloride, sodium nitrate, sodium acetate or combinations thereof. Commercially available silicates can also be used.

[0122] In an embodiment, the carrier used is selected from the group comprising sodium based inert carrier such as sodium sulphate, trisodium citrate, sodium phosphate, sodium chloride, sodium nitrate, sodium acetate, or combinations thereof.

[0123] In a preferred embodiment sodium sulphate is used as a carrier.

[0124] In an embodiment, the composition comprises from about 0.1% w / w to about 99% w / w, preferably from about 0.1% w / w to about 80% w / w, preferably from about 0.1% w / w to about 50% w / w, and more preferably from about 0.1% w / w to about 30% w / w, carrier of total weight of the composition.

[0125] In an embodiment, the high-load, soluble granular composition comprises:

[0126] (a) at least about 300 g / kg of asulam or its salts thereof;

[0127] (b) at least one surfactant;

[0128] (c) a stabilizing agent; and

[0129] (d) optionally a carrier.

[0130] In an embodiment, the high-load, soluble granular composition comprises:

[0131] (a) at least about 300 g / kg of asulam or its salts thereof;

[0132] (b) at least one surfactant; (c) a stabilizing agent; and

[0133] (d) a carrier.

[0134] In another embodiment, the high-load, soluble granular composition comprises:

[0135] (a) about 300 g / kg to about 990g / kg of asulam or its salts thereof;

[0136] (b) about 0.01% w / w to about 20% w / w of at least one surfactant;

[0137] (c) about 0.1% w / w to about 10% w / w of a stabilizing agent; and

[0138] (d) about 0.1% w / w to about 99% w / w of a carrier.

[0139] In another embodiment, the high-load, soluble granular composition comprises:

[0140] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0141] (b) about 0.01% w / w to about 20% w / w of at least one surfactant;

[0142] (c) about 0.1% w / w to about 10% w / w of a stabilizing agent; and

[0143] (d) about 0% w / w to about 99% w / w of a carrier.

[0144] In another embodiment, the high-load, soluble granular composition comprises:

[0145] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0146] (b) about 0.01% w / w to about 10% w / w of at least one surfactant;

[0147] (c) about 0.1% w / w to about 10% w / w of a stabilizing agent; and

[0148] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0149] In another embodiment, a high-load, soluble granular composition comprising:

[0150] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0151] (b) about 0.01% w / w to about 10% of polyalkylene oxide block co-polymers;

[0152] (c) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0153] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0154] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0155] (a) about 30% w / w to about 99% w / w asulam or its salts thereof;

[0156] (b) about 0.1% w / w to about 1% w / w of polyalkylene oxide block co-polymers; (c) about 0.1% w / w to about 6% w / w of modified styrene acrylic polymer;

[0157] (d) about 0.1% w / w to about 3% w / w of alkyl naphthalene sulfonate;

[0158] (e) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0159] (f) about 0.1% w / w to about 10% w / w of a carrier.

[0160] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0161] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0162] (b) about 0.01% w / w to about 10% of polyethoxylated castor oil;

[0163] (c) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0164] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0165] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0166] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0167] (b) about 0.01% w / w to about 10% of modified styrene acrylic polymer;

[0168] (c) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0169] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0170] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0171] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0172] (b) about 0.01% w / w to about 10% of alkyl amine oxides;

[0173] (c) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0174] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0175] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0176] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof; (b) about 0.01% w / w to about 10% of blend of alkypolysaccharide and alkoxylated alkylether polyamine;

[0177] (c) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0178] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0179] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0180] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0181] (b) about 0.01% w / w to about 2% of polyalkylene oxide block co-polymers

[0182] (c) about 0.05% w / w to about 6% w / w of modified styrene acrylic polymer;

[0183] (d) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0184] (e) about 0.1% w / w to about 10% w / w of a carrier.

[0185] In another embodiment of the present invention, there is provided a high-load, soluble granular composition comprising:

[0186] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0187] (b) about 0.01% w / w to about 3% w / w of polyalkylene oxide block co-polymers

[0188] (c) about 0.01% w / w to about 3% w / w of alkyl naphthalene Sulfonate

[0189] (d) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0190] (e) about 0.1% w / w to about 10% w / w of a carrier.

[0191] In another embodiment of the present invention, there is provided a high-load, soluble granular composition comprising:

[0192] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0193] (b) about 0.01% w / w to about 2% w / w of polyalkylene oxide block co-polymer ;

[0194] (c) about 0.01% w / w to about 2% w / w of alkyl naphthalene sulfonate;

[0195] (d) about 0.01% w / w to about 6% w / w of modified styrene acrylic polymer; and

[0196] (e) about 0.1% w / w to about 10% w / w of stabilizing agent; and

[0197] (f) about 0.1% w / w to about 10% w / w of a carrier. In an embodiment, the high-load solid composition may further comprise one or more agrochemically acceptable excipient.

[0198] In an embodiment, said agrochemically acceptable excipient is selected from the group comprising aqueous or organic solvent(s), buffering agent(s), neutralizing agent(s), pH modifying agent(s), surfactant(s), wetting agent(s), spreading agent(s), tackifier(s), sticker(s), filler(s), thickener(s), emulsifier(s), dispersant(s), sequestering agent(s), anti-settling agent(s), coalescing agent(s), rheology modifier(s), defoaming agent(s), photo-protector(s), anti-freeze agent(s), biocide(s), penetrant(s), mineral or vegetable oil(s), pigment(s), drift control agent(s), or combinations thereof.

[0199] In an embodiment, the high-load, solid composition comprises a pH modifying agent selected from organic and inorganic water-soluble acid comprising phosphoric acid, citric acid, acetic acid, sulfuric acid, hydrochloric acid, nitric acid, or combinations thereof.

[0200] In an embodiment, the high-load, solid composition comprises a defoaming / antifoaming agent. The defoaming / antifoaming agents are employed to prevent any unwanted foam generated while manufacturing the compositions. Exemplary defoaming / antifoaming agents include silicone-based compounds, alcohols, glycol ethers, mineral spirits, acetylene diols, polysiloxanes, organosiloxanes, siloxane glycols, reaction products of silicon dioxide and organosiloxane polymer, polydimethylsiloxanes, polydimethylsiloxane emulsion, or polyalkylene glycols alone or in combination. Exemplary defoaming / antifoaming agent comprises silicone antifoam emulsions.

[0201] In an embodiment, the high-load, solid composition according to the present invention may further comprise one or more additional pesticide / s. In an embodiment, the additional pesticide is a herbicide. In an embodiment, the high-load, solid composition comprises one or more additional pesticide is a herbicide selected from the group comprising 4-CPA, 4- CPB, 4-CPP, 3,4-DA, 3,4-DB, 2,4-DEB, 2,4-DEP, 3,4-DP, 2,3,6-TBA, 2,4,5-T, 2,4,5-TB, 2,4-D sodium, acetochlor, acifluorfen, aclonifen, alachlor, allidochlor, alloxydim, alorac, ametridione, ametryn, amibuzin, amicarbazone, amidosulfuron, aminocyclopyrachlor, aminopyralid, amiprofos-methyl, amitrole, ammonium sulfamate, anilofos, anisuron, atraton, atrazine, azafenidin, azimsulfuron, aziprotryne, barban, BCPC, beflubutamid, benazolin, bencarbazone, benfluralin, benfuresate, bensulfuron-methyl, bensulide, benthiocarb, bentazone sodium, benzadox, benzfendizone, benzipram, benzobicyclon, benzofenap, benzofluor, benzoylprop, benzthiazuron, bialaphos, bicyclopyrone, bifenox, bilanafos, bispyribac-sodium, borax, bromacil, bromobonil, bromobutide, bromofenoxim, bromoxynil, brompyrazon, butachlor, butafenacil, butamifos, butenachlor, buthidazole, buthiuron, butralin, butroxydim, buturon, butylate, cacodylic acid, cafenstrole, calcium chlorate, calcium cyanamide, cambendichlor, carbasulam, carbetamide, carboxazole, chlorprocarb, carfentrazone-ethyl, CDEA, CEPC, chlomethoxyfen, chloramben, chloranocryl, chlorazifop, chlorazine, chlorbromuron, chlorbufam, chloreturon, chlorfenac, chlorfenprop, chlorflurazole, chlorflurenol, chloridazon, chlorimuron, chlornitrofen, chloropon, chlorotoluron, chloroxuron, chloroxynil, chlorpropham, chlorsulfuron, chlorthal, chlorthiamid, cinidon-ethyl, cinmethylin, cinosulfuron, cisanilide, clethodim, cliodinate, clodinafop-propargyl, clofop, clomazone, clomeprop, cloprop, cloproxydim, cloransulam- methyl, CMA, copper sulfate, CPMF, CPPC, credazine, cresol, cumyluron, cyanatryn, cyanazine, cycloate, cyclopyrimorate, cyclosulfamuron, cycloxydim, cycluron, cyhalofop- butyl, cyperquat, cyprazine, cyprazole, cypromid, dalapon, dazomet, delachlor, desmedipham, desmetryn, di-allate, dichlobenil, dichloralurea, dichlormate, dichlorprop, dichlorprop-P, diclofop- methyl, diclosulam, diethamquat, diethatyl, difenopenten, difenoxuron, difenzoquat, diflufenican, diflufenzopyr, dimefuron, dimethachlor, dimethametryn, dimethenamid, dimethenamid-P, dimexano, dimidazon, dinitramine, dinofenate, dinoprop, dinosam, dinoseb, dinoterb, diphenamid, dipropetryn, diquat, disul, dithiopyr, diuron, DMPA, DNOC, DSMA, EBEP, eglinazine, endothal, epronaz, EPTC, erbon, esprocarb, ethalfluralin, ethametsulfuron, ethidimuron, ethiolate, ethofumesate, ethoxyfen, ethoxysulfuron, etinofen, etnipromid, etobenzanid, EXD, fenasulam, fenoprop, fenoxaprop, fenoxaprop-P-ethyl, fenoxaprop-P-ethyl + isoxadifen-ethyl, fenoxasulfone, fenteracol, fenthiaprop, fentrazamide, fenuron, flamprop, flamprop-M, flazasulfuron, florasulam, fluazifop, fluazifop-P -butyl, fluazolate, flucarbazone, flucetosulfuron, fluchloralin, flufenacet, flufenican, flufenpyr-ethyl, flumetsulam, flumezin, flumiclorac- pentyl, flumioxazin, flumipropyn, fluometuron, fluorodifen, fluoroglycofen, fluoromidine, fluoronitrofen, fluothiuron, flupoxam, flupropacil, flupropanate, flupyrsulfuron, fluridone, flurochloridone, flurtamone, fluthiacet, fomesafen, foramsulfuron, fosamine, fumiclorac, furyloxyfen, glufosinate salts and esters, glufosinate- ammonium, glufosinate-P-ammonium, glyphosate salts and esters, halosafen, halosulfuron-methyl, haloxydine, haloxyfop or derivatives thereof, hexachloroacetone, hexaflurate, hexazinone, imazamethabenz, imazamox, imazapic, imazapyr, imazaquin, imazethapyr, imazosulfuron, indanofan, indaziflam, iodobonil, iodomethane, iodosulfuron, iodosulfuron-ethyl-sodium, iofensulfuron, ioxynil, ipazine, ipfencarbazone, iprymidam, isocarbamid, isocil, isomethiozin, isonoruron, isopolinate, isopropalin, isoproturon, isouron, isoxaben, isoxachlortole, isoxaflutole, isoxapyrifop, karbutilate, ketospiradox, lactofen, lenacil, linuron, MAA, MAMA, mecoprop, mecoprop-P, medinoterb, mefenacet, mefluidide, mesoprazine, mesosulfuron, mesotrione, metam, metamifop, metamitron, metazachlor, metazosulfuron, metflurazon, methabenzthiazuron, methalpropalin, methazole, methiobencarb, methiozolin, methiuron, methometon, methoprotryne, methyl isothiocyanate, methyldymron, metobenzuron, metobromuron, metolachlor, metosulam, metoxuron, metribuzin, metsulfuron, metsulfuron- methyl, molinate, monalide, monisouron, monochloroacetic acid, monolinuron, monuron, morfamquat, MSMA, naproanilide, napropamide, napropamide-M, naptalam, neburon, nicosulfuron, nipyraclofen, nitralin, nitrofen, nitrofluorfen, norflurazon, noruron, orbencarb, orthosulfamuron, oryzalin, oxadiargyl, oxadiazon, oxapyrazon, oxasulfuron, oxaziclomefone, oxyfluorfen, paraflufen-ethyl, parafluron, paraquat, pebulate, pelargonic acid, pendimethalin, penoxsulam, pentachlorophenol, pentanochlor, pentoxazone, perfluidone, pethoxamid, phenisopham, phenmedipham, phenmedipham-ethyl, phenob enzuron, phenylmercury acetate, picloram, picolinafen, pinoxaden, piperophos, potassium arsenite, potassium azide, potassium cyanate, pretilachlor, primisulfuron-methyl, procyazine, prodiamine, profluazol, profluralin, profoxydim, proglinazine, prohexadione-calcium, prometon, prometryn, pronamide, propachlor, propanil, propaquizafop, propazine, propham, propisochlor, propoxycarbazone, propyrisulfuron, propyzamide, prosulfalin, prosulfocarb, prosulfuron, proxan, prynachlor, pydanon, pyraclonil, pyraflufen-ethyl, pyrasulfotole, pyrazogyl, pyrazolynate, pyrazosulfuron-ethyl, pyrazoxyfen, pyribenzoxim, pyributicarb, pyriclor, pyridafol, pyridate, pyriftalid, pyriminobac, pyrimisulfan, pyrithiobac- sodium, pyroxasulfone, pyroxsulam, quinclorac, quinmerac, quinoclamine, quinonamid, quizalofop, quizalofop-P-ethyl, rhodethanil, rimsulfuron, saflufenacil, S-metolachlor, sebuthylazine, secbumeton, sethoxydim, siduron, simazine, simeton, simetryn, SMA, sodium arsenite, sodium azide, sodium chlorate, sulcotrione, sulfallate, sulfentrazone, sulfometuron, sulfosate, sulfosulfuron, sulfuric acid, sulglycapin, swep, SYN-523, TCA, tebutam, tebuthiuron, tefuryltrione, tembotrione, tepraloxydim, terbacil, terbucarb, terbuchlor, terbumeton, terbuthylazine, terbutryn, tetrafluron, thenylchlor, thiazafluron, thiazopyr, thidiazimin, thidiazuron, thiencarbazone-methyl, thifensulfuron, thifensulfuron-methyl, thiobencarb, tiocarbazil, tioclorim, topramezone, tralkoxydim, triafamone, tri-allate, triasulfuron, triaziflam, tribenuron, tribenuron- methyl, tricamba, tridiphane, trietazine, trifloxysulfuron, trifluralin, triflusulfuron, trifop, trifopsime, trihydroxytriazine, trimeturon, tripropindan, tritac, tritosulfuron, vernolate, xylachlor and salts, esters, optically active isomers and mixtures thereof.

[0202] In a preferred embodiment, the additional herbicide is selected from trifloxysulfuron; glyphosate; bentazone; metribuzin; 2,4- D; their salts; derivatives or mixtures thereof. In an embodiment, the additional herbicide is a moisture sensitive active ingredient, i.e., the additional herbicide is susceptible to degradation on exposure to moisture.

[0203] In an embodiment, the composition comprises from about 0.001% w / w to about 80% w / w additional herbicide of total weight of the composition.

[0204] In an embodiment, the high-load, solid composition can be formulated with the additional herbicide(s), tank-mixed with additional herbicide(s) or applied sequentially with the additional herbicide(s).

[0205] In another embodiment, a high-load, soluble granular composition comprising:

[0206] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0207] (b) about 0.01% w / w to about 10% of polyalkylene oxide block co-polymers;

[0208] (c) about 0.1% w / w to about 10% w / w of ethylenediamine derivatives;

[0209] (d) about 0.01% w / w to about 5% w / w of trifloxysulfuron or its salt; and

[0210] (e) about 0.1% w / w to about 10% w / w of a carrier.

[0211] In another embodiment, a high-load, soluble granular composition comprising:

[0212] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0213] (b) about 0.01% w / w to about 10% of polyalkylene oxide block co-polymers;

[0214] (c) about 0.1% w / w to about 10% w / w of ethylenediamine derivatives;

[0215] (d) about 1% w / w to about 40% w / w of glyphosate or its salt; and

[0216] (e) about 0.1% w / w to about 10% w / w of a carrier.

[0217] In another embodiment, a high-load, soluble granular composition comprising:

[0218] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0219] (b) about 0.01% w / w to about 10% of polyalkylene oxide block co-polymers;

[0220] (c) about 0.1% w / w to about 10% w / w of ethylenediamine derivatives;

[0221] (d) about 1% w / w to about 40% w / w of bentazone or its salt; and

[0222] (e) about 0.1% w / w to about 10% w / w of a carrier. In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0223] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0224] (b) about 0.1% w / w to about 1% w / w of polyalkylene oxide block co-polymers;

[0225] (c) about 0.1% w / w to about 6% w / w of modified styrene acrylic polymer;

[0226] (d) about 0.1% w / w to about 3% w / w of alkyl naphthalene sulfonate;

[0227] (e) about 0.1% w / w to about 10% w / w of ethylenediamine derivatives;

[0228] (f) about 1% w / w to about 20% w / w of metribuzin or its salt; and

[0229] (g) about 0.1% w / w to about 10% w / w of a carrier.

[0230] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0231] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0232] (b) about 0.1% w / w to about 1% w / w of polyalkylene oxide block co-polymers;

[0233] (c) about 0.1% w / w to about 6% w / w of modified styrene acrylic polymer;

[0234] (d) about 0.1% w / w to about 3% w / w of alkyl naphthalene sulfonate;

[0235] (e) about 0.1% w / w to about 10% w / w of ethylenediamine derivatives;

[0236] (f) about 1% w / w to about 50% w / w of 2,4 D or its salt; and

[0237] (g) about 0.1% w / w to about 10% w / w of a carrier.

[0238] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0239] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0240] (b) about 0.01% w / w to about 10% of polyethoxylated castor oil;

[0241] (c) about 0.1% w / w to about 10% w / w of trisodium citrate; and

[0242] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0243] In another embodiment of the present invention, there is provided a high-load, soluble granular composition comprising:

[0244] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0245] (b) about 0.01% w / w to about 5% w / w of alkyl naphthalene sulfonate; (c) about 0.01% w / w to about 3% w / w of modified styrene acrylic polymer; and

[0246] (d) about 0.1% w / w to about 10% w / w of trisodium citrate; and

[0247] (e) about 0.1% w / w to about 10% w / w of a carrier.

[0248] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0249] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0250] (b) about 0.01% w / w to about 10% of alkyl amine oxides;

[0251] (c) about 0.1% w / w to about 10% w / w of trisodium citrate; and

[0252] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0253] In another embodiment, there is provided a high-load, soluble granular composition comprising:

[0254] (a) about 30% w / w to about 99% w / w of asulam or its salts thereof;

[0255] (b) about 0.01% w / w to about 10% of blend of alkypolysaccharide and alkoxylated alkylether polyamine;

[0256] (c) about 0.1% w / w to about 10% w / w of trisodium citrate; and

[0257] (d) about 0.1% w / w to about 10% w / w of a carrier.

[0258] In another aspect, the present invention provides a process for preparation of a high- load, soluble granular composition of asulam or its salts thereof; the process comprising:

[0259] (a) obtaining solid asulam or its salts thereof;

[0260] (b) mixing the solid asulam obtained in step (a) with at least one surfactant, a stabilizing agent and optionally a carrier to obtain a mixture;

[0261] (c) adding water to the mixture and extruding the mixture to form granules; and

[0262] (d) drying the granules to obtain a high-load, soluble granular composition of asulam.

[0263] In an embodiment, in step (a) the solid asulam is obtained by removing solvent from a solution comprising asulam or its salt. In an embodiment, in step (a) the solid asulam is obtained by removing solvent from a solution comprising asulam sodium.

[0264] In an embodiment, in step (a) the solvent removed is water.

[0265] In an embodiment, in step (a) the solid asulam is obtained by removing water from an aqueous solution comprising asulam or its salt.

[0266] In an embodiment, the aqueous solution comprising asulam sodium is having purity in a range from about 10% to about 70% w / w, and preferably in a range from about 30% to about 60% w / w.

[0267] In an embodiment, the solid asulam is obtained by removing solvent from a solution comprising asulam or it salt by one of the process such as spray-drying, fluidized spray drying, agitated thin-film drying, drum drying or freeze-drying, and converting into a powder form.

[0268] In an embodiment, the solid asulam is obtained by removing solvent from a solution comprising asulam or its salt by agitated thin-film drying. In an embodiment, the agitated thin-film drying is carried out at temperature ranging from about 30°C to about 250°C, preferably from about 50°C to about 200°C, preferably from about 100°C to about 200°C, and more preferably from about 120°C to about 160°C.

[0269] In an embodiment, the agitated thin-film drying is carried out at atmospheric pressure. In an embodiment, the agitated thin-film drying is carried out at reduced atmospheric pressure.

[0270] In an embodiment, the solution comprising salt of asulam may be added dropwise or continuously. In an embodiment, the feed rate of the solution comprising asulam sodium in the agitated thin-film drying process is in a range from about 1 kg / hr to about 10 kg / hr, preferably from about 2 kg / hr to about 8 kg / hr, and more preferably from about 4 kg / hr to about 6 kg / hr.

[0271] In an embodiment, the solid asulam is obtained by removing solvent from a solution comprising salt of asulam by drum drying. In drum drying, the heated surface is the envelope of a rotating horizontal metal cylinder wherein the cylinder is heated by steam condensing inside.

[0272] In an embodiment, the solid asulam is obtained by drum drying wherein the steam pressure is in a range from about 1 kg / cm2to about 10 kg / cm2, preferably from about 2 kg / cm2to about 8 kg / cm2, and more from about 4 kg / cm2to about 6 kg / cm2.

[0273] In another embodiment, the drum rotation speed is below 2 revolutions per minute.

[0274] In an embodiment, the solvent removed from a solution comprising asulam sodium is water.

[0275] In an embodiment, the solid asulam is obtained by removing solvent from a solution comprising salt of asulam by spray drying. In spray drying, the outlet temperature is ranging from 60°C to 150°C.

[0276] In an embodiment, the purity of solid asulam obtained in step (a) is in a range from about 50% to about 99%. In another embodiment, the purity of solid asulam obtained in step a) is in a range from about 60% to about 99%, preferably from about 70% to about 95%, and more preferably from about 75% to about 90%.

[0277] In an embodiment, the step (b) of the process may further comprise adding one or more of agrochemically acceptable excipient / s or additional pesticide / s to the mixture.

[0278] In an embodiment, the step (b) of the process may further comprise adding one or more agrochemically acceptable excipients to the mixture. In an embodiment, the agrochemically acceptable excipient is a neutralizing agent. In an embodiment, the agrochemically acceptable excipient is a defoaming agent.

[0279] In an embodiment, the step (b) of the process may further comprise adding one or more additional pesticide to the mixture. In an embodiment, the additional pesticide is a herbicide.

[0280] In an embodiment, the present invention provides a process for preparation of a high-load, solid composition of asulam or its salts thereof; the process comprising:

[0281] (a) obtaining solid asulam or its salts thereof having purity of at least about 50%;

[0282] (b) mixing asulam obtained in step (a) with at least one surfactant(s), a stabilizing agent, one or more agrochemically acceptable excipient and optionally a carrier to obtain a mixture;

[0283] (c) adding water to the mixture and extruding the mixture to form granules; and

[0284] (d) drying the granules to obtain the high-load solid composition of asulam or its salts thereof.

[0285] In an embodiment, the present invention provides a process for preparation of a high-load, solid composition of asulam or its salts thereof; the process comprising:

[0286] (a) obtaining solid asulam or its salts thereof having purity of at least about 50%;

[0287] (b) mixing asulam obtained in step (a) with at least one surfactant(s), a stabilizing agent, one or more agrochemically acceptable excipient, one or more additional herbicide(s) and optionally a carrier to obtain a mixture;

[0288] (c) adding water to the mixture and extruding the mixture to form granules; and

[0289] (d) drying the granules to obtain the high-load solid composition of asulam or its salts thereof.

[0290] In an embodiment, the present invention provides a process for preparation of a high-load, solid composition of asulam or its salts thereof; the process comprising: (a) mixing a solution comprising asulam with at least one surfactant(s), a stabilizing agent, one or more agrochemically acceptable excipient, one or more additional herbicide(s) and optionally a carrier to obtain a semi-solid mixture; and

[0291] (b) drying and / or granulating the semi-solid mixture to obtain the high-load solid composition of asulam or its salts thereof.

[0292] In an embodiment, the solution comprises asulam sodium. In an embodiment, the solution comprising asulam is an aqueous solution. In an embodiment, the aqueous solution comprising asulam has purity / concentration in a range from about 1% to about 50%.

[0293] In an embodiment, the drying in step (b) comprises drying by one of the processes such as, but not limited to, spray-drying, fluidized spray drying, agitated thin-film drying, drum drying or freeze-drying. In an embodiment, the step (b) of the process comprises steps of drying and granulation to obtain the desired product.

[0294] In an embodiment, the drying in step (b) is carried out by spray-drying.

[0295] In another embodiment, the present invention provides use of a high-load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof; for controlling growth of undesired vegetation / weeds.

[0296] In another embodiment, the present invention provides use of a high-load, solid composition comprising about 30% w / w to about 99% w / w of asulam or its salts thereof; for controlling growth of undesired vegetation / weeds.

[0297] In another embodiment, the compositions according to the invention have an outstanding herbicidal activity however, the crop plants of economically important crops such as soybeans, cotton, oilseed rape, sugarbeet, or graminaceous crops such as wheat, barley, rye, oats, sorghum and millet, sugarcane, coffee, tea, cacao, coconut, bananas or maize, only suffer a minor extent of damage, or none at all. This is why the solid compositions according to the invention are highly suitable for selectively controlling undesired vegetation / weeds in plantations of agricultural useful crops or in ornamental plantations. Owing to their herbicidal properties, the high-load, solid compositions according to the invention can also be employed for controlling harmful plants in crops of genetically modified plants which are known or yet to be developed.

[0298] In another embodiment, the present invention provides a method for controlling growth of undesired vegetation / weeds, said method comprising applying a high- load, solid composition comprising at least about 300 g / kg of asulam or its salts thereof to a locus where vegetation / weeds control is desired.

[0299] In another embodiment, the present invention provides a method for controlling growth of undesired vegetation / weeds, said method comprising applying a high- load, solid composition comprising about 30% w / w to about 99% w / w of of asulam or its salts thereof; and an additional pesticide.

[0300] The additional pesticide is in accordance with embodiments provided above.

[0301] In another embodiment, the present invention furthermore also relates to a method for controlling growth of undesired vegetation / weeds, preferably in crops of plants such as cereals (for example wheat, barley, rye, oats, rice, maize, sorghum and millet), sugar beet, sugarcane, oilseed rape, cotton and soybeans, especially preferably in monocotyledonous crops such as cereals, for example wheat, barley, rye, oats, their hybridization products such as triticale, rice, maize, sorghum and millet. The high-load solid composition of asulam according to the invention being applied to the harmful plants, plant parts, plant seeds or the area on which the plants grow, for example the area under cultivation.

[0302] In another embodiment, the plant crops can also have been genetically modified or have been obtained by mutation selection and are preferably tolerant to acetolactate synthase (ALS) inhibitors. In view of the above, it will be seen that the several advantages of the disclosure are achieved, and other advantageous results attained. Although the present disclosure has been disclosed in full, it will be understood that numerous additional modifications and variations could be made thereto without departing from the scope of the disclosure.

[0303] The disclosure may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore, to be considered in all respects as illustrative and not restrictive.

[0304] EXAMPLES:

[0305] Example 1: Preparation of solid asulam sodium (by agitated thin-film drying)

[0306] 35 kgs of aqueous solution of asulam sodium salt with asulam sodium content of about 44%)was subjected to agitated thin-film drying at a temperature in a range from about 130°C to about 145°C with a feed rate from about 4 kg / hr to about 6kg / hr to yield about 15.82 kg of dry solid asulam sodium having purity of about 88.6% w / w.

[0307] Example 2: Preparation of solid asulam sodium (by drum drying)

[0308] 10 kgs of aqueous solution of asulam sodium salt (with asulam sodium content of about 44%) was subjected to drum drying with steam pressure from about 4 kg / cm2to about 6 kg / cm2and drum rotation speed below about 2 revolutions per minute to yield about 4.614 kg of dry solid asulam sodium having purity of about 88.7% w / w.

[0309] Example 3: Preparation of high-load soluble granules composition asulam sodium

[0310] Asulam sodium solid material (about 86% to 89% purity) obtained according to processes provided in Examples 1 or 2, were mixed together with a surfactant, carrier and a stabilizing agent to obtain a homogenous mixture. To this mixture was optionally added a pH modifying agent and / or a grinded additional herbicide. In sample 1, 2 and 8 to 12 wherein no additional herbicide was added, the homogenous mixture obtained was used as it is for dough preparation. Whereas, in sample 3, 4 & 5 an additional herbicide was ground and added directly or as solution in water to the homogeneous mixture; and in samples 6 & 7, a premix was prepared by 5 combining herbicides (such as glyphosate, benzoate sodium, metribuzin, and 2,4-D sodium) with one or more additive s / surfactants (such as polydimethylsiloxane emulsion, modified styrene acrylic polymer, and alkyl naphthalene sulfonate) before being added to the homogeneous mixture. To the mixture was then added required quantity of water to obtain an extrudable dough. The dough was then 10 extruded to granules of desired size. The extruded granules were subj ected to drying to obtain high-load soluble granular composition of asulam.

[0311] Following 12 samples were prepared according to the present invention.

[0312] Table 1 represents composition of these 12 samples prepared according to the 15 present invention.

[0313] Table 1

[0314] Comparative example 1 (82.7% w / w asulam SG composition without stabilizer)

[0315] Asulam sodium solid material (about 88% purity) obtained according to processes 5 provided in Examples 1, was mixed together with a surfactant and carrier to obtain a mixture. To the mixture was then added required quantity of water to obtain an extrudable dough. The dough was then extruded to granules of desired size. The extruded granules were subjected to drying to obtain high-load soluble granular composition of asulam having strength of 82.7% w / w.

[0316] Comparative example 2 (Asulam sodium 33.33% w / w + Trifloxysulfuron sodium 0.35% w / w soluble liquid composition)

[0317] Asulam sodium solid material (about 88% purity) obtained according to processes provided in Examples 1, was mixed together with water, non-ionic surfactant and Trifloxysulfuron Sodium (about 89% purity) to obtain soluble liquid composition.

[0318] Evaluation of physiochemical parameters

[0319] I. Stability of composition

[0320] The composition of above samples was evaluated for various physicochemical parameters. Soluble granules prepared according to present invention appeared as free flowing granules, free from extraneous matter and remained as such in accelerated heat storage. (AHS) study conducted at 54°C for 14 days & 16 months real time study. The active content of asulam remained quite stable in composition according to sample 1 to 3. The samples were analysed for degree of dissolution residue and persistent foam and were quite acceptable for the composition of the present invention. The detailed evaluation can be provided as in Table 2 below

[0321] Table 2

[0322] * Degree of Dissolution Residue of product retained on a 75 pm test sieve after dissolution of 10g in 100 ml CIPAC water D at 20 ± 2°C

[0323] The inventors of the present invention successfully developed high load solid compositions in the form of soluble granules of asulam comprising at least about 30% w / w of asulam or its salts thereof. The active ingredients were found to remain quite stable after preparation and even during storage and accelerated heat stability studies. The comparative example 1, wherein stabilizer is not added shows turbidity when sample is dissolved in water which is not acceptable.

[0324] II. For composition according to present invention with additional pesticide The solid composition of according to sample 3, having two active ingredient i.e. asulam & trifloxysulfuron sodium was evaluated for stability / degradation of active ingredients as compared to soluble liquid formulation provided in comparative example 2 at accelerated heat storage (AHS) study conducted at 54°C for 14 days & 16 months real time. It was observed that the active content of asulam remained quite stable in composition according present invention as compared to soluble liquid composition of comparative example 2. The detailed evaluation is provided as in Table 3 below

[0325] Table 3 Above table confirms that high load solid composition according to present invention, having additional pesticide was found to be stable as compared to soluble liquid compositions known in prior art. Both the active ingredients were found to remain quite stable at ambient conditions and during storage. The comparative example 2, wherein soluble liquid composition is prepared shows upto 100% degradation of trifloxysulfuron sodium.

[0326] Example 4: Preparation of 75% w / w soluble granules composition asulam sodium (By spray drying)

[0327] A homogeneous mixture was prepared by combining an aqueous solution of asulam sodium salt (with asulam sodium content of 36.53%) with surfactants, stabilizing agents, defoamers, and a carrier. This mixture was then subjected to spray drying at an outlet temperature ranging from 70°C to 95°C. The resulting spray-dried material was further dried in a fluid bed dryer at 75°C to reduce the moisture content to below 2.5%. Finally, the granules obtained were sieved through a 30 mesh by 100 mesh sieve to separate the fine and oversized material, yielding the final product.

Claims

We claim1. A high-load solid composition comprising i) at least about 30% w / w of asulam or salts thereof; ii) at least one surfactant; and iii) a stabilizing agent.

2. The composition as claimed in claim 1, wherein the amount of asulam or its salts thereof, ranges from about 30% w / w to about 99% w / w of asulam with respect to the total composition.

3. The composition as claimed in claim 1, wherein the surfactant is selected from the group comprising of non-ionic surfactants, anionic surfactants, or combinations thereof.

4. The composition as claimed in claim 3, wherein the non-ionic surfactants is selected from the group comprising polyalkylene oxide block co-polymers, linear or branched poly ethoxylated Cio-Cis fatty alcohols, wherein the ethoxyl number (EO) ranges from 5 to 10; poly ethoxylated castor oil, wherein the ethoxyl number ranges from 15 to 40; alkoxylated phosphate esters; alkoxylated sulphate esters; polyethoxylated di styrylphenols having an ethoxylation number between 12 to 25; polyethoxylated tri styrylphenols having an ethoxylation number between 15 to 40; C12-C18 mono-, di and triesters of polyethoxylated sorbitan wherein the ethoxylation number ranges from 4 to 20; C10-C16 mixtures of alkyl polyglycosides optionally polyethoxylated or polypropoxylated wherein said alkylpolyglycosides have a different ethoxylation or propoxylation number, comprised between 10 to 25; polyethoxylated-polypropoxylated Cs-Cu aliphatic alcohols; polyaryl phenol ethoxyl ate wherein the ethoxyl / propoxyl number is between 15 to 40, alkyl amine oxides, alkypolysaccharide, alkoxylated alkylether poly amine or combinations thereof.

5. The composition as claimed in claim 3, wherein the anionic surfactant is selected from the group comprising calcium salt of alkyl benzene sulfonate such as calcium dodecyl sulfonate; polyoxyethylene sorbitan monolaurate; alkali salt of lauryl sulfate such as sodium lauryl sulfate; alkyl naphthalene sulfonate or its alkali salt such as sodium alkyl naphthalene sulfonate, sodium naphthalene sulfonate, sodium alkyl naphthalene sulfonate sulfosuccinate, derivatives of lignosulfonates such as sodium lignosulfonate, alkali salt of naphthalene sulfonate condensate such as sodium salt of naphthalene sulfonate condensate, tri styrylphenol sulphate, tri styrylphenol phosphate esters, linear benzene sulphonates and alkyl ether sulphates, alkali salt resin of styrene methacrylic copolymer such as sodium salt resin of styrene methacrylic copolymer, modified styrene acrylic polymer, alkali salt of polycarboxylate such as potassium polycarboxylate, or combinations thereof.

6. The composition as claimed in claim 1 , wherein the amount of the surfactant ranges from about 0.01% w / w to about 20% w / w.

7. The composition according to claim 1, wherein the stabilizing agent is selected from the group comprising of ethylenediamine derivatives, trisodium citrate, tannic acid, DL-tartaric acid, or combinations thereof.

8. The composition as claimed in claim 1, wherein the amount of stabilizing agent ranges from about 0.1% w / w to about 10% w / w.

9. The composition as claimed in claim 1, further comprises one or more additional pesticide.

10. The composition as claimed in claim 9, wherein the additional pesticide is a herbicide selected from trifloxysulfuron; glyphosate; bentazone; metribuzin; 2,4- D; their salts; derivatives or mixtures thereof.

11. A method for controlling growth of undesired vegetation / weeds comprising applying the composition as claimed in claim 1, to a locus where vegetation / weeds control is desired.

12. A high-load, soluble granular composition comprising:(a) about 30% w / w to about 99% w / w of asulam or its salts thereof;(b) about 0.01% w / w to about 20% w / w of at least one surfactant;(c) about 0.1% w / w to about 10% w / w of a stabilizing agent; and(d) about 0% w / w to about 99% w / w of a carrier.

13. A process for preparation of a high -load, soluble granular composition of asulam or its salts thereof; the process comprising:(a) obtaining solid asulam or its salts thereof;(b) mixing the solid asulam obtained in step (a) with at least one surfactant, a stabilizing agent and optionally a carrier to obtain a mixture;(c) adding water to the mixture and extruding the mixture to form granules; and(d) drying the granules to obtain a high-load, soluble granular composition of asulam.

14. The process as claimed in claim 13, wherein in the step (a) the solid asulam is obtained by removing water from an aqueous solution comprising asulam or its salt.

15. The process as claimed in claim 14, wherein, the solid asulam is obtained by removing solvent from a solution comprising asulam or it salt by one of the process such as spray-drying, fluidized spray drying, agitated thin-film drying, drum drying or freeze-drying, and converting into a powder form.

16. The process as claimed in claim 13, wherein the step (b) of the process may further comprise adding one or more agrochemically acceptable excipient / s or additional pesticide / s to the mixture.

17. A process for preparation of a high-load, solid composition of asulam or its salts thereof; the process comprising:(a) mixing a solution comprising asulam with at least one surfactant(s), a stabilizing agent, one or more agrochemically acceptable excipient, one or more additional herbicide(s) and optionally a carrier to obtain a semi- solid mixture; and(b) drying and / or granulating the semi-solid mixture to obtain the high-load solid composition of asulam or its salts thereof.

18. The process as claimed in claim 17, wherein step (b) comprises drying by one of the processes such as spray-drying, fluidized spray drying, agitated thin-film drying, drum drying or freeze-drying.

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