Gas blanketing for an agrochemical composition

Abstract

The invention relates to a container (100), comprising a liquid phase of a composition of dimpropyridaz (103); and a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / vol. It also relates to the use of the gas phase (102) for protecting the composition of dimpropyridaz from agglomeration; and to a process for manufacturing the container (100).

Description

[0001] 241124

[0002] 1

[0003] Gas blanketing for an agrochemical composition

[0004] The invention relates to a container (100), comprising a liquid phase of a composition of dimpropyridaz (103) and a gas phase (102). The invention also relates to the use of said gas phase for protecting the composition of dimpropyridaz and to a process for manufacturing the container.

[0005] Agrochemical compositions are susceptible to various storage-related issues. One such problem is agglomeration, which occurs when small particles within the composition adhere to one another, forming larger solid masses. This issue is particularly prevalent in environments with temperature fluctuations and affects the physical properties of the composition, impacting its usability and rendering it ineffective or even dangerous in certain applications.

[0006] The objective of the present invention was thus to overcome these problems by stabilizing the composition of dimpropyridaz during storage.

[0007] The objective has been achieved by a container (100), comprising

[0008] a) a liquid phase of a composition of dimpropyridaz (103); and

[0009] b) a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / voL

[0010] The invention further pertains to the use of the gas phase (102) for protecting the composition of dimpropyridaz (103); and to a process for manufacturing the container (100) comprising the steps

[0011] a) utilizing the container to be filled with a liquid phase of a composition of dimpropyridaz (103); and

[0012] b) introducing the gas phase (102) into the container as defined herein.

[0013] Combinations of embodiments and preferred features described herein are within the scope of the invention.

[0014] It was surprisingly found that the high concentration of gases selected from noble gases, nitrogen or carbon dioxide within the container is crucial to achieve a stable dimpropyridaz composition within the container.

[0015] Figure 1 shows the schematic representation of the container (100) of the invention, which comprises a closing element (101), a liquid phase of a composition of dimpropyridaz (103) and a gas phase (102).

[0016] The container (100) is filled with the liquid phase of a composition of dimpropyridaz (103), which is covered by the gas phase (102) or the gas phase (102) is first introduced into the container (100) and then the liquid phase of a composition (103) is filled into the container (100). The closing element (101) is used to close the container (100). If the container (100) is standing upright with the closing element (101) on top of the bottle, the gas phase (102) is typically filling the space between the liquid phase of the composition of dimpropyridaz (103)241124

[0017] 2

[0018] and the closing element (101). The space between the liquid phase of the composition (103) and the closing element (101) is hereafter referred to as the head space of the container.

[0019] The container (100) may be a vessel to hold, store, or transport agrochemical compositions. The container may have various shapes or forms, such as cans, drums, bags, or bottles. The container may be made from a variety of materials, including metals, plastics, glass, and paper. The choice of material may be determined by factors such as the nature of the contents, required durability, environmental considerations, and intended use. The container (100) may be selected based on the nature of the content. The container (100) may protect its contents from contamination, spoilage, and damage during handling and transportation.

[0020] The container (100) comprises a liquid phase of a composition of dimpropyridaz (103). The liquid phase (103) is typically liquid at 20°C. The liquid phase (103) may be liquid at a range from -5°C up to 120°C, preferably from 0°C to 100°C, more preferably from 0°C to 80°C. The liquid phase (103) may be liquid from at least 0°C and preferably from at least 5°C.

[0021] The liquid phase contains a composition of dimpropyridaz. Dimpropyridaz (IUPAC: 1-[(1RS)-1 ,2-dimethylpropyl]-N-ethyl-5-methyl-N-pyridazin-4-yl-1 H-pyrazole-4-carboxamide) is a compound of formula I:

[0022]

[0023] Dimpropyridaz has one centre of chirality; it is present as mixture of enantiomers. The invention provides both the use of the pure enantiomers of dimpropyridaz or its mixtures. In case dimpropyridaz is present in solid form, e.g. as particles, it may be present as an amorphous or a crystalline solid. In one embodiment, dimpropyridaz is present as a polymorph of crystalline form B described in W02020 / 144308.

[0024] Compositions of dimpropyridaz may include suspensions, powders, granules, pastes and dispersions. The compositions of dimpropyridaz are prepared in a known manner, such as described by Mollet and Grubemann, Formulation technology, Wiley VCH, Weinheim, 2001; or Knowles, New developments in crop protection product formulation, Agrow Reports DS243, T&F Informa, London, 2005. The compositions of dimpropyridaz usually comprise at least one auxiliary.

[0025] Suitable auxiliaries are solvents, liquid carriers, solid carriers or fillers, surfactants, dispersants, emulsifiers, wetters, adjuvants, solubilizers, penetration enhancers, protective colloids, adhesion agents, thickeners, humectants, repellents, attractants, feeding stimulants, compatibilizers, bactericides, anti-freezing agents, anti-foaming agents, colorants, tackifiers and binders.

[0026] Suitable solvents and liquid carriers are water and organic solvents, such as mineral oil fractions of medium to high boiling point, e.g. kerosene, diesel oil; oils of vegetable or animal241124

[0027] 3

[0028] origin; aliphatic, cyclic and aromatic hydrocarbons, e. g. toluene, paraffin, tetrahydronaphthalene, alkylated naphthalenes; alcohols, e.g. ethanol, propanol, butanol, benzylalcohol, cyclohexanol; glycols; DMSO; ketones, e.g. cyclohexanone; esters, e.g. lactates, carbonates, fatty acid esters, gamma-butyrolactone; fatty acids; phosphonates; amines; amides, e.g. N-methylpyrrolidone, fatty acid dimethylamides; and mixtures thereof.

[0029] Suitable solid carriers or fillers are mineral earths, e.g. silicates, silica gels, talc, kaolins, limestone, lime, chalk, clays, dolomite, diatomaceous earth, bentonite, calcium sulfate, magnesium sulfate, magnesium oxide; polysaccharides, e.g. cellulose, starch; fertilizers, e.g. ammonium sulfate, ammonium phosphate, ammonium nitrate, ureas; products of vegetable origin, e.g. cereal meal, tree bark meal, wood meal, nutshell meal, and mixtures thereof.

[0030] Suitable surfactants are surface-active compounds, such as anionic, cationic, nonionic and amphoteric surfactants, block polymers, polyelectrolytes, and mixtures thereof. Such surfactants can be used as emulsifier, dispersant, solubilizer, wetter, penetration enhancer, protective colloid, or adjuvant. Examples of surfactants are listed in McCutcheon’s, Vol.1: Emulsifiers & Detergents, McCutcheon’s Directories, Glen Rock, USA, 2008 (International Ed. or North American Ed.).

[0031] Suitable anionic surfactants are alkali, alkaline earth or ammonium salts of sulfonates, sulfates, phosphates, carboxylates, and mixtures thereof. Examples of sulfonates are alkylarylsulfonates, diphenylsulfonates, alpha-olefin sulfonates, lignine sulfonates, sulfonates of fatty acids and oils, sulfonates of ethoxylated alkylphenols, sulfonates of alkoxylated arylphenols, sulfonates of condensed naphthalenes, sulfonates of dodecyl- and tridecylbenzenes, sulfonates of naphthalenes and alkylnaphthalenes, sulfosuccinates or sulfosuccinamates. Examples of sulfates are sulfates of fatty acids and oils, of ethoxylated alkylphenols, of alcohols, of ethoxylated alcohols, or of fatty acid esters. Examples of phosphates are phosphate esters. Examples of carboxylates are alkyl carboxylates, and carboxylated alcohol or alkylphenol ethoxylates.

[0032] Suitable nonionic surfactants are alkoxylates, N-substituted fatty acid amides, amine oxides, esters, sugar-based surfactants, polymeric surfactants, and mixtures thereof. Examples of alkoxylates are compounds such as alcohols, alkylphenols, amines, amides, arylphenols, fatty acids or fatty acid esters which have been alkoxylated with 1 to 50 equivalents. Ethylene oxide and / or propylene oxide may be employed for the alkoxylation, preferably ethylene oxide.

[0033] Examples of N-substituted fatty acid amides are fatty acid glucamides or fatty acid alkanolamides. Examples of esters are fatty acid esters, glycerol esters or monoglycerides. Examples of sugar-based surfactants are sorbitans, ethoxylated sorbitans, sucrose and glucose esters or alkylpolyglucosides. Examples of polymeric surfactants are home- or copolymers of vinylpyrrolidone, vinylalcohols, or vinylacetate.

[0034] Suitable cationic surfactants are quaternary surfactants, for example quaternary ammonium compounds with one or two hydrophobic groups, or salts of long-chain primary amines. Suitable amphoteric surfactants are alkylbetains and imidazolines. Suitable block polymers are block polymers of the A-B or A-B-Atype comprising blocks of polyethylene oxide and polypropylene241124

[0035] 4

[0036] oxide, or of the A-B-C type comprising alkanol, polyethylene oxide and polypropylene oxide. Suitable polyelectrolytes are polyacids or polybases. Examples of polyacids are alkali salts of polyacrylic acid or polyacid comb polymers. Examples of polybases are polyvinylamines or polyethyleneamines.

[0037] Suitable adjuvants are compounds, which have a neglectable or even no pesticidal activity themselves, and which improve the biological performance of the compound I on the target. Examples are surfactants, mineral or vegetable oils, and other auxiliaries. Further examples are listed by Knowles, Adjuvants and additives, Agrow Reports DS256, T&F Informa UK, 2006, chapter 5.

[0038] Suitable thickeners are polysaccharides (e.g. xanthan gum, carboxymethylcellulose), anorganic clays (organically modified or unmodified), polycarboxylates, and silicates.

[0039] Suitable bactericides are bronopol and isothiazolinone derivatives such as alkylisothiazolinones and benzisothiazolinones.

[0040] Suitable anti-freezing agents are ethylene glycol, propylene glycol, urea and glycerin.

[0041] Suitable anti-foaming agents are silicones, long chain alcohols, and salts of fatty acids.

[0042] Suitable colorants (e.g. in red, blue, or green) are pigments of low water solubility and water-soluble dyes. Examples are inorganic colorants (e.g. iron oxide, titan oxide, iron hexacyanoferrate) and organic colorants (e.g. alizarin-, azo- and phthalocyanine colorants).

[0043] Suitable tackifiers or binders are polyvinylpyrrolidons, polyvinylacetates, polyvinyl alcohols, polyacrylates, biological or synthetic waxes, and cellulose ethers.

[0044] The container (100) typically comprises a liquid phase of a composition of dimpropyridaz (103), preferably wherein dimpropyridaz is present in form of suspended particles. The particles may be characterized by their size distribution, which can be determined by dynamic light scattering techniques. Suitable dynamic light scattering measurement units are inter alia produced under the trade name Malvern Mastersizer 3000. The particles may be characterized by their median diameter, which is usually abbreviated as D50 value. The D50 value refers to a particular particle diameter, wherein half of the particle population by volume is smaller than this diameter. The D50 value is typically determined according to ISO 13320:2009.

[0045] The dimpropyridaz particles typically have an D50 value from 0.05 pm to 30 pm, preferably from 0.1 pm to 20 pm, more preferably from 0.5 to 20 pm, even more preferably from 0.5 pm to 15 pm, especially preferably from 0.5 pm to 10 pm. The particles typically have an D50 value of at least 0.75 pm and preferably at least 1 pm. The suspended particles may be present in the form of crystalline or amorphous particles which are solid at 20°C.

[0046] Usually, the composition of dimpropyridaz comprises from 0.1 to 40 wt%, preferably from 5 to 35 wt%, and in particular from 15 to 25 wt% of dimpropyridaz, based on the total weight of the241124

[0047] 5

[0048] composition. Typically, the composition of dimpropyridaz comprises at least 7 wt%, preferably at least 10 wt%, more preferably at least 15 wt% and in particular at least 18 %wt based on the total weight of the composition. The composition of dimpropyridaz may comprise up to 50 wt%, preferably up to 40 wt%, more preferably up to 30 wt% and in particular up to 25 wt% of dimpropyridaz based on the total weight of the composition.

[0049] The composition of dimpropyridaz is typically a suspension. The suspension of dimpropyridaz typically comprise a dispersant, a wetting agent, a stabilizer, an antifoam, one or more biocides, a thickener, a pH adjuster and a diluent. Suspensions of dimpropyridaz are described in detail in WO2020 / 224942, WO2020 / 224944 and WO2020 / 224943.

[0050] The suspension of dimpropyridaz typically comprise a dispersant in a concentration from 0.01 to 10 wt%, preferably from 0.2 to 8 wt%, and in particular from 0.5 to 3.5 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.2 wt%, more preferably at least 0.5 wt% and in particular at least 1 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 8 wt%, more preferably up to 5 wt% and in particular up to 3 wt%, based on the total weight of the suspension.

[0051] The suspension of dimpropyridaz typically comprise a wetting agent in a concentration from 1 to 20 wt%, preferably from 2 to 15 wt%, and in particular from 3 to 10 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 1 wt%, preferably at least 2 wt%, more preferably at least 3 wt% and in particular at least 5 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 20 wt%, preferably up to 15 wt%, more preferably up to 12 wt% and in particular up to 10 wt%, based on the total weight of the suspension.

[0052] The suspension of dimpropyridaz typically comprise a stabilizer in a concentration from 0.01 to 10 wt%, preferably from 0.1 to 5 wt%, and in particular from 0.5 to 3 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.1 wt%, more preferably at least 0.3 wt% and in particular at least 0.5 %wt, based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 5 wt%, more preferably up to 3 wt% and in particular up to 2 wt%, based on the total weight of the suspension.

[0053] The suspension of dimpropyridaz typically comprise an antifoam in a concentration from 0.01 to 10 wt%, preferably from 0.1 to 5 wt%, and in particular from 0.2 to 3 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.1 wt%, more preferably at least 0.2 wt% and in particular at least 0.3 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 5 wt%, more preferably up to 3 wt% and in particular up to 2 wt%, based on the total weight of the suspension.

[0054] The suspension of dimpropyridaz typically comprise a biocide in a concentration from 0.01 to 10 wt%, preferably from 0.05 to 5 wt%, and in particular from 0.1 to 3 wt%, based on the total241124

[0055] 6

[0056] weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.05 wt%, more preferably at least 0.1 wt% and in particular at least 0.2 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 5 wt%, more preferably up to 3 wt% and in particular up to 1 wt%, based on the total weight of the suspension.

[0057] The suspension of dimpropyridaz typically comprise a thickener in a concentration from 0.01 to 10 wt%, preferably from 0.05 to 5 wt%, and in particular from 0.1 to 3 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.05 wt% and in particular at least 0.1 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 5 wt%, more preferably up to 3 wt% and in particular up to 1 wt%, based on the total weight of the suspension.

[0058] The suspension of dimpropyridaz typically comprise a pH adjuster in a concentration from 0.01 to 10 wt%, preferably from 0.05 to 5 wt%, and in particular from 0.08 to 3 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 0.01 wt%, preferably at least 0.05 wt%, more preferably at least 0.08 wt% and in particular at least 0.1 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 10 wt%, preferably up to 5 wt%, more preferably up to 3 wt% and in particular up to 1 wt%, based on the total weight of the suspension.

[0059] The suspension of dimpropyridaz may comprise a diluent in a concentration from 20 to 90 wt%, preferably from 25 to 85 wt%, and in particular from 30 to 80 wt%, based on the total weight of the suspension. Typically, the suspension of dimpropyridaz comprises at least 20 wt%, preferably at least 25 wt%, more preferably at least 30 wt% and in particular at least 50 %wt based on the total weight of the suspension. The suspension of dimpropyridaz may comprise up to 90 wt%, preferably up to 85 wt%, more preferably up to 80 wt% and in particular up to 75 wt%, based on the total weight of the suspension. The diluent of the suspension of dimpropyridaz is typically water.

[0060] The suspension of dimpropyridaz typically comprise dimpropyridaz in an amount up to 30 wt%, a dispersant up to 5 wt%, a wetting agent up to 15 wt%, a stabilizer up to 5 wt%, an antifoam up to 3 wt%, one or more biocides up to 5 wt%, a thickener up to 3 wt%, a pH adjuster up to 1 wt% and water up 90 wt%, based on the total weight of the suspension.

[0061] The liquid phase of the composition of dimpropyridaz (103) may be an aqueous or nonaqueous phase. The term “non-aqueous phase” means that the non-aqueous phase may contain not more than 10 wt% of water, preferably not more than 5 wt%, more preferably not more than 3 wt%, even more preferably not more than 1 wt% each time based on the total weight of the liquid phase. The term “aqueous phase” means that the aqueous phase may contain at least 10 wt% of water, preferably at least 20 wt%, more preferably at least 30 wt%, even more preferably at least 40 wt% of water each time based on the total weight of the liquid phase. Preferably, the liquid phase is an aqueous phase.241124

[0062] 7

[0063] The liquid phase of the composition of dimpropyridaz (103) may comprise at least one additional agrochemical active ingredient in addition to dimpropyridaz. Agrochemical active ingredients may be selected from the group of fungicides, insecticides, nematicides, herbicides, safeners, nitrification inhibitors, urease inhibitors, plant growth regulators, micronutrients, biopesticides and / or growth regulators.

[0064] The skilled worker is familiar with such pesticides, which can be found, for example, in the Pesticide Manual, 16th Ed. (2013), The British Crop Protection Council, London. Suitable insecticides are insecticides from the class of the carbamates, organophosphates, organochlorine insecticides, phenylpyrazoles, neonicotinoids, spinosins, avermectins, milbemycins, juvenile hormone analogs, alkyl halides, organotin compounds nereistoxin analogs, benzoylureas, diacylhydrazines, METI acarizides, and insecticides such as chloropicrin, pymetrozin, flonicamid, clofentezin, hexythiazox, etoxazole, diafenthiuron, propargite, pyrethroids, tetradifon, chlorofenapyr, DNOC, buprofezine, cyromazine, amitraz, hydramethylnon, acequinocyl, fluacrypyrim, rotenone, or their derivatives. Suitable fungicides are fungicides from the classes of dinitroanilines, allylamines, anilinopyrimidines, antibiotics, aromatic hydrocarbons, benzanilides, benzenesulfonamides, benzimidazoles, benzisothiazoles, benzophenones, benzothiadiazoles, benzotriazines, benzyl carbamates, carbamates, carboxamides, carboxylic acid diamides, chloronitriles cyanoacetamide oximes, cyanoimidazoles, cyclopropanecarboxamides, dicarboximides, dihydrodioxazines, dinitrophenyl crotonates, dithiocarbamates, dithiolanes, ethylphosphonates, ethylaminothiazolecarboxamides, guanidines, hydroxy-(2-amino)pyrimidines, hydroxyanilides, imidazoles, imidazolinones, inorganic substances, isobenzofuranones, methoxyacrylates, methoxycarbamates, morpholines, N-phenylcarbamates, oxazolidinediones, oximinoacetates, oximinoacetamides, peptidylpyrimidine nucleosides, phenylacetamides, phenylamides, phenylpyrroles, phenylureas, phosphonates, phosphorothiolates, phthalamic acids, phthalimides, piperazines, piperidines, propionamides, pyridazinones, pyridines, pyridinylmethylbenzamides, pyrimidinamines, pyrimidines, pyrimidinonehydrazones, pyrroloquinolinones, quinazolinones, quinolines, quinones, sulfamides, sulfamoyltriazoles, thiazolecarboxamides, thiocarbamates, thiophanates, thiophenecarboxamides, toluamides, triphenyltin compounds, triazines, triazoles. Suitable herbicides are herbicides from the classes of the acetamides, amides, aryloxyphenoxypropionates, benzamides, benzofuran, benzoic acids, benzothiadiazinones, bipyridinium, carbamates, chloroacetamides, chlorocarboxylic acids, cyclohexanediones, dinitroanilines, dinitrophenol, diphenyl ether, glycines, imidazolinones, isoxazoles, isoxazolidinones, nitriles, N-phenylphthalimides, oxadiazoles, oxazolidinediones, oxyacetamides, phenoxycarboxylic acids, phenylcarbamates, phenylpyrazoles, phenylpyrazolines, phenylpyridazines, phosphinic acids, phosphoroamidates, phosphorodithioates, phthalamates, pyrazoles, pyridazinones, pyridines, pyridinecarboxylic acids, pyridinecarboxamides, pyrimidinediones, pyrimidinyl(thio)benzoates, quinolinecarboxylic acids, semicarbazones, sulfonylaminocarbonyltriazolinones, sulfonylureas, tetrazolinones, thiadiazoles, thiocarbamates, triazines, triazinones, triazoles, triazolinones, triazolocarboxamides, triazolopyrimidines, triketones, uracils, ureas.241124

[0065] 8

[0066] The container (100) comprises a gas phase (102). The gas phase (102) refers to the layer of the gas within the container. The gas phase (102) comprises a noble gas, nitrogen, or carbon dioxide. Suitable noble gases include argon, helium, krypton and xenon.

[0067] The gas phase (102) may comprise a noble gas in a concentration of at least 80% vol. / vol., preferably at least 85% vol. / vol., more preferably at least 90% vol. / vol., and in particular at least 95% vol. / vol.. The gas phase (102) may comprise a noble gas in a concentration range from 80 to 99.9% vol. / vol., preferably from 85 to 99.9% vol. / vol., more preferably from 90 to 99.9% vol. / vol., and in particular from 95 to 99% vol. / vol..

[0068] The gas phase (102) may comprise nitrogen in a concentration of at least 80% vol. / vol., preferably at least 85% vol. / vol., more preferably at least 90% vol. / vol., and in particular at least 95% vol. / vol.. The gas phase (102) may comprise nitrogen in a concentration range from 80 to 99.9% vol. / vol., preferably from 85 to 99.9% vol. / vol., more preferably from 90 to 99.9% vol. / vol., and in particular from 95 to 99% vol. / vol..

[0069] The gas phase (102) may comprise carbon dioxide in a concentration of at least 80% vol. / vol., preferably at least 85% vol. / vol., more preferably at least 90% vol. / vol., and in particular at least 95% vol. / vol.. The gas phase (102) may comprise carbon dioxide in a concentration range from 80 to 99.9% vol. / vol., preferably from 85 to 99.9% vol. / vol., more preferably from 90 to 99.9% vol. / vol., and in particular from 95 to 99% vol. / vol..

[0070] The gas phase (102) may comprise oxygen in a concentration of up to 15% vol. / vol., preferably up to 13% vol. / vol., more preferably up to 10% vol. / vol., and in particular up to 5% vol. / vol.. The gas phase (102) may comprise oxygen in a concentration range from 0.01 to 20% vol. / vol., preferably from 0.01 to 15% vol. / vol., more preferably from 0.01 to 10% vol. / vol., and in particular from 0.01 to 5% vol. / vol..

[0071] The ratio of the liquid phase and gas phase may range from 20:1 to 1:1, preferably from 20:1 to 5: 1 , more preferably from 20: 1 to 10:1, most preferably from up to 20: 1 to 15:1, and in particular from 20:1 to 18:1. The ratio of the liquid phase and gas phase typically is 2:1, preferably 3:1, more preferably 4:1 and in particular 5:1.

[0072] The invention also relates to the use of a gas phase (102) as defined herein for protecting a composition of dimpropyridaz as defined herein from agglomeration.

[0073] The term “protecting from agglomeration” typically refers to the process of preventing or mitigating the clustering or sticking together of small particles within a composition, which can lead to the formation of larger, undesirable solid masses.

[0074] The invention may also relate to the method for protecting a composition of dimpropyridaz from agglomeration comprising the step of contacting the composition of dimpropyridaz with a gas phase containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / vol..241124

[0075] 9

[0076] The term "contacting" refers typically to a process of bringing two or more substances into direct contact with one another. It may involve introducing the gas phase, which contains a noble gas, nitrogen, or carbon dioxide, into the container in which the composition of dimpropyridaz was previously filled. This contact may occur through various means, such as dispersing the gas phase over the composition. Another term for “contacting” in within this meaning is “gas blanketing” which typically refers to a process to introduce a gas phase into a container to maintain the stability of the liquid phase.

[0077] The invention also relates to a process for manufacturing a container (100) comprising the steps of a) providing a container to be filled with a liquid phase of a composition of dimpropyridaz (103) as defined herein; and

[0078] b) introducing a gas phase (102) as defined herein into the container.

[0079] The skilled person understands that steps a) and b) can be carried out in any order, i.e. b) after a) and a) after b). Both options will result in a container (100) according to the invention.

[0080] The term “introducing a gas phase” refers typically to the act of adding or inserting a gas phase into the container. Typically, the composition of dimpropyridaz is filled into the container first, followed by the introduction of the gas phase. This step may involve carefully delivering the gas phase into the container in a controlled manner to ensure adequate contact between the gas and the liquid phase to prevent improper gas introduction that may cause excessive pressure buildup within the container, potentially leading to leaks or ruptures that would risk the integrity of the stored composition. Proper introduction techniques are crucial to maintaining the desired concentration of gases and achieving the intended stability of the composition.

[0081] The following embodiments represent preferred aspects of the invention:

[0082] In one embodiment, the container (100) comprises

[0083] a) a liquid phase of a suspension of dimpropyridaz (103); and

[0084] b) a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / voL

[0085] In one embodiment, the container (100) comprises

[0086] a) a liquid phase of an aqueous suspension of dimpropyridaz (103); and

[0087] b) a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 10% vol. / voL

[0088] In one embodiment, the container (100) comprises

[0089] a) a liquid phase of an aqueous suspension of dimpropyridaz (103); and

[0090] b) a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / vol.,

[0091] wherein the gas phase contains a concentration of nitrogen of at least 80% vol. / vol..In one embodiment, the container (100) comprises

[0092] a) a liquid phase of an aqueous suspension of dimpropyridaz; and

[0093] b) a gas phase, containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / vol.,

[0094] wherein the gas phase contains a concentration of nitrogen of at least 85% vol. / vol..

[0095] In one embodiment, the container (100) comprises

[0096] a) a liquid phase of an aqueous suspension of dimpropyridaz; and

[0097] b) a gas phase, containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 10% vol. / vol.,

[0098] wherein the gas phase contains a concentration of nitrogen of at least 90% vol. / vol..

[0099] In one embodiment, the container of the invention comprises

[0100] a) a liquid phase of an aqueous suspension of dimpropyridaz; and

[0101] b) a gas phase, containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 5% vol. / vol.,

[0102] wherein the gas phase contains a concentration of nitrogen of at least 95% vol. / vol..

[0103] In one embodiment, the container of the invention comprises

[0104] a) a liquid phase of an aqueous suspension of dimpropyridaz; and

[0105] b) a gas phase, containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 5% vol. / vol.

[0106] In one embodiment, the container of the invention comprises

[0107] a) a liquid phase of an aqueous suspension of dimpropyridaz; and

[0108] b) a gas phase, containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 5% vol. / vol.,

[0109] wherein the gas phase contains a concentration of nitrogen of at least 95% vol. / vol., and the ratio of the liquid phase and gas phase is from 20:1 to 1:1.

[0110] Advantages of the present invention are, inter alia, that compositions stored in the containers of the invention have a high storage stability, even at elevated temperatures or under alternating temperatures. Especially, suspensions stored in the containers of the invention have a high storage stability, even at elevated temperatures or under alternating temperatures.

[0111] Further advantages are

[0112] - the particle size growth of dispersed agrochemical active substances is slowed down or suppressed

[0113] - crystal growth of dispersed agrochemical particles is slowed down or suppressed

[0114] - the agglomeration of dispersed agrochemical particles is slowed down or suppressed - the settling of dispersed agrochemical active substances is slowed down or suppressed - disk formation of the suspension is slowed down or suppressed

[0115] - compositions of the invention are easy and economical to make

[0116] - compositions of the invention have high biological activity

[0117] - compositions of the invention are environmentally friendly- compositions of the invention suppress pesticidal resistance

[0118] - compositions of the invention are sustainable

[0119] - compositions of the invention are easy to use

[0120] - compositions of the invention are compatible with a plurality of further pesticides or other additives like fertilizers.

[0121] Examples

[0122] The following ingredients were used for preparing the agrochemical compositions of the examples.

[0123] Insecticide: 1-[(1RS)-1,2-dimethylpropyl]- / V-ethyl-5-methyl- / V-pyridazin-4-yl-1 / - / -pyrazole-4- carboxamide (dimpropyridaz, CAS registry number 1403615-77-9)

[0124] Dispersant: lignin sulfonate, organic sulfur content approximately 9 wt%

[0125] Wetting Agent: ethoxylated castor oil, 40 polymerized ethylene oxide units per molecule on average

[0126] Stabilizer: hydrophobic fumed silica particles, surface modified with dimethylsilyl groups, water solubility

[0127] below 0.1 g / l, BET surface 90-130 m2 I g, carbon content 0.6 to 1.2 wt%

[0128] Antifoam: emulsion of dimethylsiloxan on silica particles, defoamer content 20 wt%

[0129] Biocide A: glycol based solution of benzisothiazolinone

[0130] Biocide B: aqueous composition of benzisothiazolinones and 5-chloro-2-methylisothiazolin-3- one

[0131] Thickener: Xanthan gum

[0132] pH-Adjustor: Acetic acid

[0133] Diluent: Water

[0134] The example which follows illustrate the invention without imposing any limitation.

[0135] Example 1

[0136] Suspension concentrate SC-1 was prepared containing the ingredients according to Table A.

[0137]

[0138] Table A: Ingredients of suspension concentrate SC-1A premix of 3% thickener was made by adding the thickener to 0.02% of the total Biocide A and 4.19% of the total Diluent. The premix was mixed with a cowles blade until the thickener was fully hydrated and homogenous.

[0139] The suspension concentrate was prepared by adding the Insecticide, Wetting Agent, Dispersant, Antifoam, Biocide A, Biocide B, pH-Adjuster and the Stabilizer to the Diluent. The mixture was homogenized until uniform and then milled in a bead mill until a mean particle size of 2-3 pm was achieved.

[0140] Table B and Figure A show the results of atmospheric gas blanketing and nitrogen gas blanketing. The bottles were first filled with the suspension and then the top of the bottles were blanketed with nitrogen gas or with atmospheric gas. The bottles were placed into the 20°C to 40°C cycling chamber. After two weeks in storage the samples were evaluated for hard disk formation / agglomeration within the liquid phase. The results are summarized below.

[0141]

[0142] Table B: Results of atmospheric gas blanketing and nitrogen gas blanketing

Claims

13Claims1. A container (100), comprisinga) a liquid phase of a composition of dimpropyridaz (103); andb) a gas phase (102), containing a noble gas, nitrogen, or carbon dioxide, wherein the oxygen concentration in the gas phase is up to 15% vol. / vol..

2. A container according to claim 1 , wherein the gas phase contains at least 85% vol. / vol. of nitrogen.

3. A container according to any of claims 1 to 2, wherein the oxygen concentration in the gas phase (102) is up to 10% vol. / vol..4 A container according to any of claims 1 to 3, wherein the oxygen concentration in the gas phase (102) is up to 5% vol. / vol..

5. A container according to any of claims 1 to 4, wherein the ratio between the liquid phase of a composition of dimpropyridaz (103) and the gas phase (102) is from 20: 1 to 1:1.

6. A container according to any of claims 1 to 5, wherein the container is selected from the group comprising of a can, drum, bag or bottle.

7. A container according to any of claims 1 to 6, wherein the composition of dimpropyridaz is a suspension.

8. A container according to any of claims 1 to 7, wherein the composition of dimpropyridaz is an aqueous suspension.

9. Use of a gas phase (102) as defined in any of claims 1 to 8 for protecting a composition of dimpropyridaz as defined in any of claims 1 , 5, 7, or 8 from agglomeration.

10. Process for manufacturing a container (100) as defined in any of claims 1 to 8 comprising the stepsa) providing a container to be filled with a liquid phase of a composition of dimpropyridaz (103) as defined in any of the claims 1, 5, 7, or 8; andb) introducing a gas phase (102) into the container as defined in any of claims 1 to 8.

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