UA126500C2 - A stable agrochemical composition and process thereof - Google Patents

Abstract

An agrochemical composition comprising at least one low melting active ingredient; at least one moisture sensitive active ingredient; and an additive, characterised in that said additive has a softening point or melting point lower than the melting point of said low melting active ingredient; a process for the preparation thereof, a method of use thereof and a kit comprising the same is disclosed.

Description

FIELD OF TECHNOLOGY TO WHICH THE INVENTION BELONGS

This invention relates to a stable agrochemical composition. This invention, in particular, relates to a stable agrochemical composition comprising a low-melting active ingredient and a moisture-sensitive active ingredient.

PREREQUISITES AND PRIOR ART

Physically compatible agrochemical mixtures improve pest control. Compared to the use of such mixtures separately, they demonstrate various advantages. But when combining two or more agrochemicals, the main task is to achieve physical compatibility. The problem of physical compatibility is further exacerbated when a low-melting active ingredient must be mixed with another active ingredient.

Some of the soluble active ingredients, such as pyrethroids (synthetic pyrethrins), are known to control agricultural insect pests in crops. Pyrethroids interfere with the ion conduction of nerve members, prolonging the sodium current. This stimulates the nerves to discharge, which causes hypersensitivity in poisoned animals.

Active ingredients having the ability to control pests, selected from fungicides such as strobilurins and insecticides such as organophosphates, are preferred to be incorporated into the composition together with low-melting actives for better pest control. Some of these active ingredients are sensitive to moisture and thus degrade rapidly during processing into a suitable preparation or composition.

A moisture-sensitive active ingredient such as acephate (organophosphate) is a systemic and contact insecticide of moderate persistence with residual activity lasting approximately 10-15 days. Acephate, which is weakly resistant to moisture and not very stable in conventional pesticide preparations, as a result of which, in traditional preparations, depending on the storage conditions, active decomposition of acephate occurs, and as a result, the insecticidal activity of acephate sometimes cannot be fully used.

Although the incorporation of moisture-sensitive active ingredients into the formulation along with low-melting active ingredients for better pest control is desirable, the development of a stable yet effective formulation is a challenge.

There are a large number of preparations with low-melting active ingredients, which

They are used to combat pest attacks on plants. Available preparations include emulsion concentrates (EC), aqueous emulsion (E5). But such preparations cannot be prepared if the other active ingredient is sensitive to moisture and weakly resistant to water.

Dry granular preparations, such as water-dispersible granules of soluble active ingredients such as pyrethroids, are known and in fact used. Traditional methods of preparing granules include methods such as extrusion granulation, which differ in that the thick mass, which is then subjected to granulation, is prepared using water. Another way to prepare granules is to make a suspension in water and then subject it to spray drying.

When fusible ingredients such as pyrethroids must be premixed with moisture-sensitive ingredients such as organophosphates, doing so becomes difficult because the moisture-sensitive ingredient cannot be granulated using water.

Moreover, the increase in temperature during extrusion granulation can melt the low-melting active substances. After the granules are extruded and stored under ambient conditions, the low-melting actives become solid again. This "green-liquid-solid" phase transition results in a change in morphology, resulting in a change in crystalline form, or layering of the ingredient on the surface of the granules, or the granules may become solid. Field application of such a granular formulation by dilution/tank mixing results in to unsatisfactory uneven dissolution (dispersion) of the composition, the lack of homogeneity of the resulting mixture and prevents the distribution of a constant concentration of the desired active substance in the fields. The lack of necessary dispersion will reduce the availability of the active ingredient for the intended use as a pesticide, thereby rendering the product ineffective.

Another method used to premix such ingredients is to dissolve the low-melting ingredient in a suitable solvent and then mix it with the moisture-sensitive ingredient followed by granulation. This method requires the use of a large amount of organic solvents, which are not only expensive, but also not environmentally safe.

In order to remove traces of solvent from the final product, the granules may need to be subjected to a longer drying period.

UMO2015142609 AT discloses microparticles containing water-soluble organothiophosphate (for example, acephate) and pyrethroids (for example, bifenthrin). The invention proposes an effective solution for preventing the appearance of odor by adding odor-absorbing and odor-masking components. 0520090208423 discloses a synergistic insecticidal composition comprising imidacloprid, lambda-cyhalothrin and a conventional, agriculturally acceptable carrier or adjuvant formulated as an aqueous formulation or a dry formulation. The application also discloses the process of mixing active substances and excipients to obtain a homogeneous mixture of all ingredients, which is finely ground and granulated to obtain a granulated preparation. Although this process is acceptable, the fine grinding of inert fillers in which the liquid active has been absorbed can cause several problems because the liquid has a natural tendency to escape during fine grinding. Such obtained compositions, as a rule, do not demonstrate good dispersibility and shelf life, especially since low-melting active substances during storage at ambient temperatures (from -5 "C to 50 "C) undergo a phase transition, which leads to sticking and growth crystals

In the Indian patent application MO 1709/MOM/2010, a synergistic insecticidal composition of acephate and bifenthrin is disclosed, which differs in that, to obtain granules, technical bifenthrin, dissolved in a solubilizer, was sprayed onto a mixture of technical acephate and auxiliary substances of the drug. The problem with this method is the large amount of solubilizer required for bifenthrin, which gives softness to the finished granules. In this case, due to the undesirable softness of the granules, a high content of active ingredients is impossible.

МО2002076213 JSC discloses a pesticide composition containing the specified pyrethroids and organophosphates in a weight ratio of 50:1 to 1:5, which differ in that the pyrethroid is selected from deltamethrin, fenvalerate, esfenvalerate, cyfluthrin, beta-cdcyfluthrin and bifenthrin, and organophosphate insecticides selected from triazophos, profenofos, chlorpyrifos-methyl, monocrotophos, acephate, methamidophos and diethyl-1-phenyl-1,H-1,2,4-triazol-3-yl phosphate.

Although various efforts have been made in the past to develop a stable pesticidal composition containing low-melting active ingredients and moisture-sensitive active ingredients, there is still a long-standing need to develop an alternative, simple and effective product and

From the method of obtaining stable pesticidal compositions of such active substances. In addition, there is a need for the development of such preparations, which differ in that the preparation overcomes the shortcomings of the prior art and exhibits increased stability with respect to the destruction of moisture-sensitive active substances and the dispersibility/suspensionability of the low-melting active ingredient upon combination. The physical stability of the drug during storage/use is a key issue in this field of technology and should be addressed.

GOAL

The purpose of the invention is to create an agrochemical composition containing a low-melting active ingredient and a moisture-sensitive active ingredient.

Another object of the invention is to create a stable agrochemical composition containing a low-melting active ingredient and a moisture-sensitive active ingredient.

Another goal of the present invention is to create methods of pest control using the compositions of the present invention.

Another object of the present invention is to provide a non-dusty, free-flowing, storable dry composition containing at least one low-melting active ingredient and a moisture-sensitive active ingredient.

ESSENCE OF THE INVENTION

In accordance with the above objectives, this invention proposes a stable agrochemical composition containing: a) at least one low-melting active ingredient;

Jur) at least one moisture-sensitive active ingredient; and c) supplement; which is characterized in that said additive has a softening point or melting point lower than the melting point of said low-melting active ingredient.

In accordance with the above objectives, the present invention provides a method for the preparation of a stable agrochemical composition containing at least one low-melting active ingredient, at least one moisture-sensitive active ingredient and an additive characterized in that the softening temperature or melting point of the additive is lower than the melting point of the indicated low-melting active ingredient.

In accordance with the above objectives, this invention proposes the use of stable compositions according to this invention as an agrochemical composition.

In accordance with the above objectives, the present invention additionally provides a method of controlling unwanted pests, and said method includes applying an agrochemically effective amount of stable compositions according to the present invention to the pests or to the site of their location.

Additional features and advantages of the present invention will become apparent from the following detailed description, which exemplifies the most desirable features of the present invention, which should not be construed as limiting the scope of the invention described herein.

DETAILED DESCRIPTION OF THE INVENTION

The authors of the present invention unexpectedly discovered that a stable agrochemical composition in the form of a granulated composition of a low-melting active ingredient and a moisture-sensitive active ingredient can be obtained by mixing a low-melting active ingredient with a moisture-sensitive active ingredient in the presence of an additive, followed by granulation of the prepared mixture by the compaction method.

It was unexpectedly found that the additive used by the inventors prevents the crystalline modification of the low-melting active ingredient or the formation of a crust on the granules.

It was really unexpectedly discovered that the additive according to this invention allows you to store the product under any conditions and still maintain the quality of the product without impairing its dispersibility, suspension and availability of active substances.

An accepted method of testing a drug for long-term stability and functionality is a method called accelerated thermal stability testing (ASTT), in which the drug is kept at a temperature of 54 degrees for 14 days, and then tests for dispersibility, suspension and wet sieving are carried out. A decrease in the indicators of suspension and dispersibility indicate low functionality of the drug in the field after long-term storage, and an increase in the indicators during the wet sieving test indicates the formation of large particles that will clog the nozzle in the field.

The authors of the invention observed that the drug according to this invention passes all tests after AN5, thus proving its effectiveness in this field even after long-term storage. An additive used during the process is believed to provide the ability

The drug remains stable during storage for a longer period of time.

The term "composition" as used herein is used interchangeably with the term "preparation" and refers to a stable solid bulk substance designed to prevent insect and pest damage to crops and their products.

The compounds herein are referred to as "low-melting active ingredient", which is a term recognized in the relevant art, particularly in the field of agrochemical compositions.

In particular, according to the present invention, the low-melting active ingredient is a compound that has a melting point of less than about 100 "C, less than about 90 "C, less than about 85 "C, less than about 80 "C, less than about 75 " C or less than about 70 "C, or has the ability to solidify at room temperature. In certain 40 embodiments, a low-melting compound of the present invention is a compound with a melting point in the range of from about 20 "C to about 100 "C. In specific embodiments embodiment is a low-melting compound that has a melting point in the range of from about 25 "C to about 100 "C, from about 30 "C to about 100 "C, from about

C to about 90 "C, from about 30 "C to about 80 "C, from about 30 "C to about 70 "C, from about 40 "C to about 90 "C, from about 40 "C to about 80 "C, from about 50 "C to about 90 "C, from about 50 "C to about 80 "C, or from about 50 "C to about 70 "C.

The term "moisture-sensitive active ingredient" refers to a compound that has the ability to absorb moisture and undergoes destruction or other changes in physicochemical parameters.

The term "granulation by compaction" as used herein refers to a granulation process characterized by the fact that the compositions containing the active ingredients are individually, sequentially or simultaneously subjected to compaction by applying pressure, as well as granulation by means of a suitable mechanism, such as extrusion.

The term "deterioration" as used herein means the loss of active ingredient due to exposure to moisture or during storage.

The term "softening temperature" means the temperature at which the additive reaches a certain degree of softness. "softening temperature" is close to, but lower than, the melting point of the additive.

The term "site" as used herein refers to the location at which the combination of the present invention is applied. It includes application to an individual plant, a group of plants,

such as the plant and/or its environment, and the region in which the plants may be planted, as well as application directly to the insect or insects and/or the environment in which they are found.

The term "agrochemical" in the context of the present invention refers to any agent used to kill insects, arachnids, fungi, unwanted vegetation, rodents and other pests.

The term "insects" includes all organisms belonging to the class "Insects" (Ipsesia). The term "Insecticide" refers to the property of a substance to increase mortality or inhibit the growth rate of insects.

The term "plant" refers to all physical parts of a plant, including seeds, seedlings, seedlings, roots, tubers, stems, stems, leaves and fruits.

The term "agrochemically acceptable amount of active substance" refers to an amount of active substance that results in the cure or inhibition of a plant disease requiring treatment in an amount that is not too toxic to the plant being treated. "Control" or "control" of insects means the suppression by toxic effects of the ability of insect pests to survive, grow, feed and/or reproduce, or the limitation of insect-related damage to crop plants. "Controlling" insects may or may not mean killing insects, although it mostly means killing insects.

The authors of the present invention found that adding to the composition an additional moisture-sensitive active ingredient, preferably an organophosphorus insecticide, and an active ingredient with a low melting point resulted in stable compositions. Obtaining a stable composition is achieved by adding an additive that facilitates the formation of granules in the absence of water. Thus, the present invention provides compositions that avoid the use of water.

Without wishing to be bound by theory, the inventors of the present invention have surprisingly discovered that adding a low emollient or low melting additive to a combination of a low melting point active ingredient such as a pyrethroid and a moisture sensitive active ingredient such as an organophosphorus insecticide , leads to obtaining stable granular compositions.

Dry bulk substances or granules according to this invention are easily prepared and stored, have

Good dispersibility and suspension under storage conditions. The use of an additive to obtain the specified stable insecticidal composition without water avoids the ingress of moisture, which is responsible for the degradation of moisture-sensitive active ingredients such as acephate, and compaction below the melting point of low-melting pyrethroids (ie, at temperatures of 30-58 degrees Celsius) avoids the problem of cementation , which occurs due to melting and gradual cooling during temperature changes in the process and during storage.

Thus, in one aspect, the present invention may provide a stable agrochemical composition that contains: a) at least one low-melting active ingredient;

Jur) at least one moisture-sensitive active ingredient; and c) supplement; characterized in that said additive has a softening point or melting point lower than the melting point of the active ingredient with a low melting point.

In another aspect, the present invention may provide a stable insecticidal composition comprising: a) at least one pyrethroid with a low melting point;

Y) at least one moisture-sensitive insecticide; and c) supplement; characterized in that said additive has a softening point or melting point lower than that of a low melting pyrethroid.

In one embodiment, the active ingredient of the present invention may be selected from insecticides, attractants, sterilizers, bactericides, acaricides, nematicides, fungicides, growth regulators, herbicides, fertilizers and mixtures.

In a preferred embodiment, the low melting active ingredient of the present invention is selected from insecticides, attractants, sterilizers, bactericides, acaricides, nematicides, fungicides and growth regulators.

In one embodiment, the active ingredient with a low melting point according to this invention is selected from nitrothalisopropyl, myclobutanil, piproctanyl bromide, iodfenphos,

imazalil, lambda-citalthrin, triflumizole, vamidothion, xylylcarb, tolclofos-methyl, protoate, pyriproxyfen, propamocarb hydrochloride, tefluthrin, resmethrin, chlorpropham, cloetocarb, demeton-5, cyfluthrin, cypermethrin, azinphos-ethyl, azinphos-methyl, benalaxil, benazolin -ethyl, butocarboxyme, benzoximate, bioresmethrin, bromopropylate, borax, biphenyl, fluoroglycophen-ethyl, fenbucarb, phenthiocarb, phensulfothion, fosmethylan, furalaxil, dikegulak, trinexapak-ethyl, ethiophencarb, etridiazole, fenamiphos, phenazaquin, ERM, dodemorph, mecarfon, etaconazole ) cyflumetofen.

In one embodiment, the low melting point active ingredient of the present invention is selected from strobilurins or pyrethroids.

The low melting point pyrethroid may be selected from, among others, cypermethrin, fenvalerate, permethrin, alphacypermethrin, betacypermethrin, cetacypermethrin, deltamethrin, cyfluthrin, bifenthrin, lambda-cyhalothrin, and/or bioresmethrin, or mixtures thereof.

In another preferred embodiment of the present invention, the low melting pyrethroid 3 is selected from bifenthrin, cypermethrin, alphacypermethrin, betacypermethrin and cetacypermethrin.

Thus, in another preferred embodiment, the low melting point pyrethroid may be bifenthrin.

In one embodiment, the low melting strobilurin may be selected from trifloxystrobin or picoxystrobin.

In one embodiment, this invention can provide a stable agrochemical composition containing from about 0.1 95 to about 30 95 wt./wt. and preferably from about 0.2 95 to about 20 95 wt./wt. a pyrethroid with a low melting point based on the total mass of a stable agrochemical composition.

In another embodiment, this invention can provide a stable insecticidal composition containing from about 0.1 95 to about 30 95 wt./wt. and preferably from about 0.2 95 to about 20 95 wt./wt. a pyrethroid with a low melting point based on the total mass of a stable insecticidal composition.

In a preferred embodiment of the present invention, the stable insecticidal composition contains from about 1 95 to about 10 95 wt./wt. a pyrethroid with a low melting point based on the total mass of a stable insecticidal composition.

In one embodiment, the moisture-sensitive active ingredient included in the compositions can be selected from organophosphorus insecticides.

In one embodiment, the moisture-sensitive organophosphorus insecticide may be selected from the group consisting of, but not limited to, acephate, azinphos-methyl, carbofuran, chlorpyrifos, coumaphos, crufomate, dimethoate, ethoprop, famfur, fenamiphos, isofenphos, methamidophos, methidathion, methyl parathion, mevinphos, monocrotophos, metham sodium, phosalone, phosmet, phosphamidon, profenofos, TERR, terbufos, tetrachlorvinphos, trichlorfon and their combinations.

A preferred organophosphorus insecticide may be selected from acephate, profenofos, phosphamidon, or mixtures thereof.

Accordingly, in another embodiment, this invention can provide a stable insecticidal composition containing from about 0.595 to about 95 95 mabs./wt. and preferably from about 10 95 to about 85 95 wt./wt. organophosphorus insecticide calculated from the total weight of the stable insecticidal composition.

In a preferred embodiment of the present invention, the stable insecticidal composition contains from about 40 95 to about 85 95 wt./wt. organophosphorus insecticide calculated from the total weight of the stable insecticidal composition.

In one embodiment, this invention differs in that said additive has a softening point or melting point lower than the melting point of the active ingredient with a low melting point.

In another embodiment, this invention differs in that said additive has a softening point or melting point lower than the melting point of the active ingredient with a low melting point.

In one embodiment, the melting point of the additive is lower than the melting point 60 of the low melting point active ingredient.

In a preferred embodiment, the present invention includes an additive that is water soluble.

In one embodiment, the additive according to the present invention can be selected from, among others, polyethylene glycol (PEG) 6000, PEN 4000, PEG 8000, nonylphenol 30 BO or high molecular weight fatty acid ethoxylate or propoxylate, fatty acid alcohol, vegetable oils, polyvinyl alcohols, polyacrylates , starch, carboxymethyl cellulose, alginic acid, agar, gum arabic and xanthan gum.

In another embodiment, the additive according to this invention can be preferably selected from polyethylene glycol (PEG) 6000, PEG 4000, PEG 8000, vegetable oils and cellulose ethers.

In a preferred embodiment, the additive according to the present invention can be selected from polyethylene glycols.

In one embodiment, in the compositions of this invention, the additive is present in an amount of from about 1 95 to about 30 95 by weight of the composition. Preferably, the additive is present in an amount of from about C 95 to about 20 95 by weight of the composition.

Stable insecticidal compositions according to the present invention may additionally contain one (one) or more dispersing agents, wetting agents, fillers, surfactants, anti-caking agents, pH-adjusting agents, preservatives, biocides, anti-foaming agents, dyes and other means for preparing the composition.

Dispersants can be selected from ionic and nonionic dispersants that readily disintegrate the granules in water, such as polystyrene sulfonic acid salts, polyvinyl sulfonic acid salts, naphthalene sulfonic acid salts/formaldehyde condensates, naphthalene sulfonic acid condensate salts, phenol and formaldehyde, and lignosulfonic acid salts , block copolymers of polyethylene oxide/polypropylene oxide, polyethylene glycol ethers of linear alcohols, reaction products of fatty acids with ethylene oxide and/or propylene oxide, as well as polyvinyl alcohol, polyvinylpyrrolidone, copolymers of polyvinyl alcohol and polyvinylpyrrolidone, and copolymers of (meth)acrylic acid and (meth)acrylic ethers , in addition, alkyl ethoxylates and alkyl aryl ethoxylates, ethoxylated alkyl aryl phosphate and sulfated ethers. Preferred dispersing agents include derivatives of vegetable oil ethoxylates or mixtures of one or more of them; or styrene acrylic polymers or mixtures thereof.

Wetting agents may be selected from soaps; salts of aliphatic monoethers of sulfur

From acids, including, but not limited to, sodium lauryl sulfate; sulfoacylamides and their salts, including, among others, sodium M-methyl-M-oleoyltaurate; acylarylsulfonates, including, among others, acylbenzenesulfonates; acyl naphthalene sulfonates and their salts and salts of ligninsulfonic acid.

In one embodiment, the fillers can be selected from insoluble fillers and soluble fillers.

In one embodiment, the fillers may be selected primarily from precipitated silica and diatomaceous earth.

In one embodiment, the insecticidal composition according to the invention is preferably prepared in the form of a dry bulk substance.

In one embodiment, suitable antifoam agents may preferably be silicones, long-chain alcohols, and fatty acid salts.

Suitable dyes (eg, red, blue and green) are preferably pigments that are sparingly soluble in water and water-soluble dyes. Examples are inorganic dyes (eg, iron oxide, titanium oxide, and iron hexacyanoferrate) and organic dyes (eg, alizarin, azo-, and phthalocyanine dyes).

According to a preferred embodiment, the present invention can provide stable insecticidal compositions comprising acephate, bifenthrin and an additive having a softening or melting point lower than the melting point of the active ingredient with a low melting point.

According to specific embodiments, the stable insecticidal composition of the present invention may contain from about 0.595 to about 9595 mabs./wt. of acephate, from about 0.1 95 to about 30 95 wt./wt. of bifenthrin, from about 1.0 95 to about

ZO 95 wt./wt. additives whose softening or melting point is lower than the melting point of the active ingredient with a low melting point.

According to another specific embodiment, the stable insecticidal composition of the present invention may contain from about 5.095 to about 80 95 mabs./wt. of acephate, from about 1.0 95 to about 20 95 wt./wt. of bifenthrin, from about 5.0 95 to about 20 95 wt./wt. PEG 6000 as an additive.

According to one embodiment, the present invention may provide an agrochemically stable composition comprising acephate, trifloxystrobin and an additive having a softening or melting point lower than the melting point of the low-melting active ingredient.

According to specific embodiments, the agrochemically stable composition of the present invention may contain from about 0.5 95 to about 95 95 wt./wt. of acephate, from about 0.195 to about 30 95 wt./wt. of trifloxystrobin, from about 1.095 to about 30 95 wt./wt. additives whose softening or melting point is lower than the melting point of the active ingredient with a low melting point.

In another embodiment, the present invention provides a method of obtaining a stable composition from an agrochemical point of view. The process includes: 1) premixing at least one low-melting active ingredient, at least one moisture-sensitive active ingredient, and an additive having a softening or melting point lower than the melting point of the low-melting active ingredient; and 2) granulation of the premix by compaction.

In one embodiment, the present invention includes additional conventional steps that may be necessary, but not critical, to achieve the benefits of the present invention.

According to another embodiment of the present invention, in the process of preparing an agrochemically stable composition, granulation by compaction can occur in such a way that the composition can be separately, sequentially or simultaneously subjected to compaction, as well as granulation.

In one embodiment, the present invention provides a method of obtaining a composition that is stable from an agrochemical point of view. The process includes: 1) premixing at least one low-melting active ingredient, at least one moisture-sensitive active ingredient, and an additive having a softening or melting point lower than the melting point of the low-melting active ingredient; and 2) the premix is individually, sequentially or simultaneously compacted and granulated.

In the preferred embodiment, the method of obtaining a stable insecticidal composition includes the following steps:

From 1) mixing an active ingredient selected from at least one pyrethroid with a low melting point with the required amount of precipitated silica to obtain a premix; 2) grinding the premix with or without other additives in an air-jet mill to obtain powdery pyrethroid particles with a low melting point of the desired size; 3) adding to the powdered pyrethroid with a low melting point an organophosphorus active ingredient and an additive whose softening or melting point is lower than the melting point of the active ingredient with a low melting point, and any other necessary additives and mixing them to obtain a premix; 4) granulation of the premix by compacting to obtain granules.

The granules obtained in this way are preferably checked for compliance with the necessary technical characteristics. Once the pellets are tested to meet quality specifications, they are preferably filled and packaged in the preferred dry bulk form.

Premixes of low melting point active ingredient, moisture sensitive active ingredient and additives can also be processed by pre-compaction followed by extrusion. Such premixing of the moisture-sensitive active ingredient and the low-melting-point active ingredient with the additive prevents deterioration of the moisture-sensitive active ingredient; and precompaction prevents melting of low melting point active ingredients during the extrusion process.

The composition of the present invention has all the advantages described above, which makes it useful from the economic point of view and from the point of view of ease of handling, and shows very good performance during application. As will be demonstrated in the examples, the composition of the present invention has good suspendability, stability, dispersibility and free flow and passes the wet sieving test.

According to one embodiment, the present invention provides an agrochemically stable composition comprising at least one low melting point active ingredient, at least one moisture sensitive active ingredient, and an additive having a lower softening or melting point, than the melting point of the active ingredient with a low melting point, as an agrochemically active composition.

In one embodiment, stable compositions according to the present invention are used as insecticides.

Accordingly, the stable insecticidal compositions of this invention provide rapid destruction of pests. It is a particularly powerful agent for the destruction of insects that are difficult to be affected by insecticides, especially the classes Ieridoriega, SoiIeoriga, Oirieega, Neptiriega, which is mainly effective against insect pests of agricultural crops, such as Lepidoptera, shield bug and blind bug.

In one embodiment, crops that can be grown using the compositions of the present invention can be selected from the group consisting of, but not limited to, grains such as wheat, oats, barley, spelt, triticale, rye, corn, millet, rice , agricultural crops such as sugar cane, soybeans, sunflower, canola, canola, tobacco, sugar beets, fodder beets; tuberous crops such as potatoes, sweet potatoes, etc., crops such as asparagus, hops, etc.; fruit plants such as apples, pears, stone fruit plants such as, for example, peaches, nectarines, cherries, plums, apricots, citrus fruits such as oranges, grapefruits, limes, lemons, kumquats, tangerines, satsumas; nuts such as pistachios, almonds, walnuts, pecans, tropical fruits such as mango, papaya, pineapple, dates, bananas, etc., spinach, chicory, cauliflower, broccoli, Chinese cabbage, cabbage (winter cabbage or kale ), kohlrabi, Brussels sprouts, red cabbage, white cabbage and savoy, fruit vegetables such as eggplant, cucumbers, peppers, zucchini, tomatoes, zucchini, sweet corn, root vegetables such as celery, turnips, carrots, rutabagas, radishes, horseradish , radishes, beets, licorice, celery, legumes such as peas, beans, etc., bulb vegetables such as leeks, onions, etc., oil crops such as mustard, poppy, olives, sunflower, coconut, plants from which get castor oil, cocoa beans, ground nuts; fiber spinning crops such as cotton, jute, flax, hemp, crops such as tea, coffee, rubber, ornamental crops including shrubs and flowering plants, vines, pastures.

In one embodiment, the compositions of the present invention may optionally be mixed with other insecticides, attractants, sterilizers, bactericides, acaricides,

With nematicides, fungicides, growth regulators, herbicides, fertilizers and their mixtures.

In one embodiment, the present invention provides a method of controlling unwanted pests, wherein said method includes applying the stable compositions of the present invention to the pests or their locations.

Thus, in one embodiment of the present invention, methods of combating insect pests on the site may be proposed, and the specified method includes the use of an insecticidally effective amount of compositions containing: a) at least one pyrethroid with a low melting point;

Jur) at least one organophosphorus insecticide sensitive to moisture; and c) supplement; characterized in that said additive has a softening point or melting point lower than that of a low melting pyrethroid.

In one embodiment, the present invention may provide methods of combating insect pests, such as those belonging to the insecticide classes I eridoriegap, SoiIveorigap, Oiriegap, Netiriegap.

In another aspect, the present invention may provide a kit. The kit includes a plurality of components, each of which may contain at least one or more ingredients of the compositions of the present invention.

In one embodiment, the components of the kit can be added to the mixture immediately before use in any of the methods of their use described in this invention.

In one embodiment, the kit includes instructions for use that instructs the user to add the components of the kit to the mixture in predetermined amounts or proportions prior to use.

In one embodiment, the instructions for use instruct the user of the kit to apply the composition against predetermined insects on certain predetermined crops.

Accordingly, in one embodiment, the present invention may provide a kit that contains: (a) at least one active ingredient with a low melting point; 60 (B) at least one moisture-sensitive active ingredient; and

(c) an additive that differs in that it has a softening point or melting point lower than the melting point of the active ingredient with a low melting point.

In another embodiment, this invention includes a kit that contains: (a) at least one pyrethroid component with a low melting point; (B) at least one moisture-sensitive insecticidal component; and (c) an additive component characterized in that said additive has a softening point or melting point lower than the melting point of a low-melting pyrethroid.

In one embodiment, the low melting point active ingredient component of the present invention includes strobilurins or pyrethroids.

The low melting point pyrethroid may be selected from, among others, cypermethrin, fenvalerate, permethrin, alphacypermethrin, betacypermethrin, cetacypermethrin, deltamethrin, cyfluthrin, bifenthrin, lambda-cyhalothrin, and/or bioresmethrin, or mixtures thereof.

In another preferred embodiment of the present invention, the low melting pyrethroid 3 is selected from bifenthrin, cypermethrin, alphacypermethrin, betacypermethrin and cetacypermethrin.

Thus, in another preferred embodiment, the low melting point pyrethroid may be bifenthrin.

In one embodiment, the low melting strobilurin may be selected from trifloxystrobin or picoxystrobin.

In one embodiment, the kit includes instructions for use that instruct the user to use from about 0.195 wt. to approximately 3095 wt. pyrethroid component with a low melting point.

In one embodiment, the kit includes a moisture-sensitive active ingredient component selected from organophosphorus insecticides.

In one embodiment, the kit includes instructions for use, according to which the user should use from about 0.5 95 wt. to approximately 95 95 wt. organophosphorus

From an insecticide.

In one embodiment, the kit includes an additive component, which is distinguished by the fact that the additive is selected from polyethylene glycol (PEG) 6000, PEG 4000, PEG 8000, nonylphenol 30 EO or high molecular weight fatty acid ethoxylate or propoxylate, fatty acid alcohol, vegetable oils, polyvinyl alcohols , polyacrylates, starch, carboxymethyl cellulose, 35 alginic acid, agar, gum arabic and xanthan gum.

In one embodiment, the kit includes instructions for use instructing the user to mix from about 1 95 to about 30 95 of the additive component.

According to a preferred embodiment, the present invention may provide a kit that includes an acephate component, a bifenthrin component, and an additive component having a softening or melting point lower than the melting point of bifenthrin.

According to another preferred embodiment, the present invention includes a kit that includes instructions for use, according to which the user should mix from about 0.5 95 wt. to approximately 95 95 wt. acephate component, from about 0.1 95 wt. to approximately 30 95 wt. birfenthrin component and from approximately 1.095 wt. to approximately 3095 wt. additives, 45 the softening or melting point of which is lower than the melting point of bifenthrin.

According to another specific embodiment, the present invention includes a kit that includes an acephate component, which is indicated to be used in an amount from about 5.0 95 wt. to about 80 95 wt., the bifenthrin component, which is indicated to be used in an amount from about 1.095 wt. to about 2095 wt., and the component PEG 6000, which is indicated 50 to be used in an amount from about 5.0 95 wt. to approximately 20 95 wt.

In one embodiment, the kit includes an acephate component, a trifloxystrobin component, and an additive component having a softening or melting point lower than the melting point of trifloxystrobin.

In one embodiment, the kit includes instructions for mixing from about 0.5 95 55 wt. to approximately 95 95 wt. acephate component, from about 0.1 95 wt. to about 95 wt. trifloxystrobin component and from approximately 1.0 95 wt. to approximately 30 95 wt. an additive component in which the softening or melting point is lower than the melting point of trifloxystrobin.

In one embodiment, the kit includes instructions for using such components or compositions as an insecticide or fungicide.

In one embodiment, the kit includes instructions for use of the components against class I Eridoriega, SoIeoriga, Oiriega, Netiriega, preferably against Lepidoptera, shield bugs, and thrips bugs.

In one embodiment, the kit includes instructions for applying the components to crops selected from cereals such as wheat, oats, barley, spelt, triticale, rye, corn, millet, rice, crops such as sugarcane, soybeans, sunflower, canola , canola, tobacco, sugar beets, fodder beets; tuberous crops such as potatoes, sweet potatoes, etc., crops such as asparagus, hops, etc.; fruit plants such as apples, pears, stone fruit plants such as, for example, peaches, nectarines, cherries, plums, apricots, citrus fruits such as oranges, grapefruits, limes, lemons, kumquats, tangerines, satsumas; nuts such as pistachios, almonds, walnuts, pecans, tropical fruits such as mango, papaya, pineapple, dates, bananas, etc., spinach, chicory, cauliflower, broccoli, Chinese cabbage, cabbage (winter cabbage or kale ), kohlrabi, Brussels sprouts, red cabbage, white cabbage and savoy, fruit vegetables such as eggplant, cucumbers, peppers, zucchini, tomatoes, zucchini, sweet corn, root vegetables such as celery, turnips, carrots, rutabagas, radishes, horseradish , radishes, beets, licorice, celery, legumes such as peas, beans, etc., bulb vegetables such as leeks, onions, etc., oil crops such as mustard, poppy, olives, sunflower, coconut, plants from which get castor oil, cocoa beans, ground nuts; fiber spinning crops such as cotton, jute, flax, hemp, crops such as tea, coffee, rubber, ornamental crops including shrubs and flowering plants, vines, pastures.

The present inventors have succeeded in obtaining a stable composition by carefully combining at least one active ingredient sensitive to moisture, at least one active ingredient with a low melting point, and an additive characterized in that the softening or melting point of the additive is lower than the melting point of the active ingredient with low melting point, and the method of obtaining it. The optimal concentration of active substances, as well as the ingredients of the drug, which ensured the stability of the drug in the form of a dry bulk substance, was achieved by conducting experiments, which are given below.

These examples are illustrative only and should in no way be construed as limiting the scope and basic principles of the present invention. Thus, upon reading the following examples and the foregoing description, various modifications of the present invention will become apparent to those skilled in the art in addition to the embodiments already described herein.

Although the above-mentioned written description of the present invention allows the average person skilled in the art to implement and use what is considered to be the best way to implement it today, it will be obvious to those skilled in the art that there are variations, combinations, and equivalents of the specific embodiments, methods, and examples given in this document. Thus, this invention is not limited to the above-described variant of embodiment, method and examples, but includes all variants and methods that are included in the scope and correspond to the idea of the present invention.

EXPERIMENTAL EXAMPLES

The following examples illustrate the basic methodology and versatility of the present invention.

Example 1. 74 95 wt. of acephate and 6 95 wt. bifenthrin in the form of a dry bulk substance was obtained as follows: silica) "

Procedure. Technical bifenthrin was mixed with precipitated silica to obtain bifenthrin premix. The bifenthrin premix was milled in an air jet mill to obtain particles of the desired size. Acephate, castor oil ethoxylate, PEG-6000, and precipitated silica were added to the bifenthrin premix to produce a bifenthrin-acephate premix. Then the bifenthrin-acephate premix was subjected to granulation by compaction, passing the specified premix through a roller extruder, with obtaining granules by repeated passing at temperatures below the melting point of bifenthrin.

Example 2. 74 95 wt. of acephate and 6 95 wt. bifenthrin in the form of a dry bulk substance was obtained as follows: dialkylnaphthalene sulfonate "PEG-BOYU 77777777711711111119000

Procedure. Bifenthrin was mixed with silica to obtain a bifenthrin premix.

The specified premix was ground in an air jet mill to obtain particles of the desired size. Acephate, Meiazregze 5505, castor oil ethoxylate, sodium dialkyl naphthalene sulfonate, PEG 6000, and precipitated silica were added to the bifenthrin premix to obtain the bifenthrin-acephate premix. Then the bifenthrin-acephate premix was subjected to granulation by compaction, passing the specified premix through a roller extruder, with obtaining granules by repeated passing at temperatures below the melting point of bifenthrin.

Example 3. 74 95 wt. of acephate and 6 95 wt. bifenthrin in the form of a dry bulk substance was obtained as follows: dialkylnaphthalene sulfonate "

Procedure. Bifenthrin was mixed with silica to obtain a bifenthrin premix.

The bifenthrin premix was milled in an air jet mill to obtain particles of the desired size. Acephate, Meiazreghe 5505, sodium dialkyl naphthalene sulfonate, PEG 8000, and precipitated silica were added to the bifenthrin premix to obtain bifenthrin-acephate premix. Then the bifenthrin-acephate premix was subjected to granulation by compaction, passing the specified premix through a roller extruder, with obtaining granules by repeated passing at temperatures below the melting point of bifenthrin.

Example 4. 74 95 wt. of acephate and 6 95 wt. beta-cdcypermethrin in the form of a dry bulk substance was obtained as follows: dialkyl naphthalene sulfonate

Zo

Procedure. Beta-cypermethrin was mixed with silica to obtain beta-cypermethrin premix. Beta-cypermethrin premix was ground in an air-jet mill to obtain particles of the desired size. Acephate, Meiazregze 5505, sodium dialkyl naphthalene sulfonate, PPT silica, ammonium sulfate, and PEG 4000 were added to beta-cypermethrin premix to obtain beta-cypermethrin-acephate premix. The beta-cypermethrin-acephate premix was then subjected to granulation by compaction by passing said premix through a roller extruder, obtaining granules by multiple passes at temperatures below the melting point of bifenthrin.

Example 5. 74 95 wt. acephate and 6.595 wt. trifloxystrobin in the form of a dry bulk substance was obtained as follows: dialkylnaphthalene sulfonate " pESbOYU 77777771 1119.00

Procedure. Trifloxystrobin was mixed with silica to obtain a trifloxystrobin premix. The trifloxystrobin premix was ground in an air-jet mill to obtain particles of the desired size. Acephate, Meiazregbe 5505, sodium dialkyl naphthalene sulfonate, PPT silica, ammonium sulfate, and PEG 6000 were added to the trifloxystrobin premix to obtain a trifloxystrobin-acephate premix. Then the trifloxystrobin-acephate premix was subjected to granulation by compaction, passing the specified premix through a roller extruder, to obtain granules.

STABILITY DATA

Dispersity test

Compositions (Examples 6-10) according to this invention were tested for stability.

The samples were obtained using different amounts of active ingredients and other ingredients, which are listed in the table below (Table 1). The samples were prepared according to the method given in example 1. The samples were tested for dispersion by determining the number of inversions required to achieve complete dispersion.

Table 1

Supplement" | 11.50 | 13m2o | 750 | 1000 | 300 | 900

Ethoxylate of zastorovotoli | 2010125

Borghorpog40384 |. 771717 - 111300 | 200 | - | -

Sodium salt of sulfonate

Meiavregwe5505 | - | 300 | - | - | Зз00 | from 00

Sulbatamonium | -. |. Y117140 | 7 - | 2" | Evil "additive is chosen from PEG 6000, PEG 4000 and PEG 8000

The number of inversions required to achieve complete dispersion of the granules was determined as follows

With the procedure: 2 g of the sample was added to a graduated cylinder with a volume of 250 ml. Allow to infuse for 2 minutes. Then the graduated cylinder was closed with a cork, tilted at an angle of 18027C and after 2 seconds returned to the initial position.

It was found that the compositions of this invention achieved the proper dispersion after about 12-15 inversions and are quite suitable for storage.

Testing for suspendability and stability of the active substance

Preparations in the form of a dry bulk substance, obtained according to this invention, were studied for their suspensionability, degradation of the active substance and its effect on the stability of the composition.

Samples (examples 7 and 11) were obtained according to example 1.

The samples were kept at a temperature of 54°C for up to 14 days and stability parameters were determined, such as suspensionability, wet sieving analysis was performed, and degradation of active ingredients was determined. The results are summarized in Table 2.

Table 2 of sexual characteristics of 0 individual ate odv dv

Wet sieving analysis (residue on 75 μm 0.02 0.1 0.002 0.003 test sieve)

As can be seen from Table 2, the degradation of active acephate and active bifenthrin in the composition in the form of a dry bulk substance was not observed when stored at a temperature of 54 7"С322"7С for 14 days. No significant change in the suspendability of the drug was observed, which indicates that the drugs according to this invention are stable according to their physicochemical parameters. This means that the thus obtained dry bulk or granular composition of acephate and bifenthrin not only has excellent stability of the active ingredients, but also preserves the dispersibility and, therefore, the availability of the active ingredients for their intended use.

Further, according to the results of wet sieving analysis, it was found that crystalline modification of bifenthrin was prevented. The combination of active substances and auxiliary substances obtained according to the method disclosed in this invention ensures the stability of the composition in the form of a dry bulk substance, which does not undergo any chemical and physical changes during storage, in addition, it is well processed for further use.

A comparative sample (Example 12) was obtained without the addition of this invention for comparison purposes. The specified sample was tested for dispersion, determining the number of inversions required to achieve full dispersion. God bless /11111111111111111111111Г1111111111111111111000s1

Ethoxylat castorovotholii ///77777711111111Ї1111111111111111110001сС1С oVorhorpog40384. 77711111 test sieve) substance

Coo)

It was found that a sample (Example 12) obtained without the use of an additive, the softening or melting point of which is lower than the melting point of the active ingredient with a low melting point, failed to provide adequate dispersion. Therefore, the drug could not provide the required dispersion, which led to the instability of the drug.

Bifenthrin availability test for insecticidal activity

Preparations in the form of a dry bulk substance obtained according to this invention were further investigated to determine the amount of bifenthrin that remains available for action as an insecticide. The suspension of the drug can be directly extrapolated to the active ingredient remaining available for its intended use. Preparations obtained according to this invention were tested for suspensionability in comparison with preparations obtained without the use of additives. Samples were obtained according to example 1, kept at a temperature of 54 "Сж2 "C for 14 days and measured suspension.

From Table C below, it can be seen that for Examples 15-17 obtained according to this invention, the measured suspendability was unexpectedly high, which obviously indicates that this preparation can be effectively used for the target insecticidal activity.

The achieved bioavailability index of bifenthrin (96) is the same as the initial concentration of bifenthrin in the preparation. For examples 13-14, which were prepared without the addition, the measured suspensions were very low, indicating that the available bifenthrin is only about 50 95 of the amount expected in these preparations.

Table C

Availability of bifenthrin in bifenthrin preparations bifenthrin (g)

Example!i3 | 760 | 66 | 00 | 58 | 383

Applied 4 | 760 | 66 | 00 | 52 2 | for (

Example 5 760 | 66 | 75 | 95 | | 627

For example | 760 | 65 | 120 | 96 B I | 624 "additive is chosen from PEG 6000, PEG 4000 and PEG 8000

Thus, the authors of the present invention successfully obtained a preparation of an active ingredient with a low melting point, which is prone to morphological changes, together with an agrochemical product that is sensitive to moisture. The compositions of this invention have been found to be stable as well as effective for their intended use.

Claims (16)

FORMULA OF THE INVENTION 1. Agrochemical composition containing: Zo a) at least one low-melting active ingredient selected from pyrethroid insecticides and strobilurin fungicides; p) at least one moisture-sensitive active ingredient selected from the group consisting of acephate, azinphos-methyl, carbofuran, chlorpyrifos, coumaphos, crofomate, dimethoate, ethoprop, famfur, fenamiphos, isofenphos, methamidophos, methidathion, methylparathion, mevinphos, monocrotophos , metham-sodium, phosalone, phosmet, phosphamidon, profenofos, TERR, terbufos, tetrachlorvinphos, trichlorfon and their combinations; and c) an additive selected from the group consisting of polyethylene glycol (PEG)-6000, PEG-4000, and PEG-8000, wherein said additive has a softening point or melting point lower than the melting point of the active ingredient with a low melting point . 2. Agrochemical composition according to claim 1, which is characterized by the fact that the indicated active ingredient with a low melting point is selected from the group consisting of bifenthrin, cypermethrin, fenvalerate, permethrin, alpha-cypermethrin, beta-cypermethrin, zeta-cypermethrin, delta-methrin , cyfluthrin, lambda-cyhalothrin and bioresmethrin and their mixtures. 3. Agrochemical composition according to claim 1, which is characterized by the fact that the specified active ingredient with a low melting point is bifenthrin. 4. Agrochemical composition according to claim 1, which is characterized by the fact that the specified active ingredient with a low melting point is trifloxystrobin. 5. Agrochemical composition according to claim 1, which differs in that the specified composition contains from approximately 0.1 95 wt. to approximately 30 95 wt. of the active ingredient with a low melting point from the total weight of the agrochemical composition. 6. Agrochemical composition according to claim 1, which differs in that the specified moisture-sensitive active ingredient is acephate. 7. Agrochemical composition according to claim 6, which differs in that the specified composition contains from approximately 0.5 to 95 wt. to approximately 95 95 wt. of the moisture-sensitive active ingredient from the total weight of the agrochemical composition. 8. Agrochemical composition according to claim 1, which differs in that the specified composition contains from approximately 1 95 wt. to approximately 30 95 wt. additives from the total weight of the agrochemical composition. 9. Agrochemical composition according to claim 1, which differs in that the specified composition is produced in the form of a dry bulk substance. 10. A method of obtaining a stable agrochemical composition, which is characterized by the fact that it includes: (a) mixing at least one active ingredient with a low melting point, at least one active ingredient sensitive to moisture, and an additive, and the softening or melting temperature of the additive is lower, than the melting point of the active ingredient with a low melting point, to obtain a premix; (B) optional addition to the premix of one or more performance-enhancing substances; and (c) performing granulation of the premix by compaction, wherein the low-melting active ingredient is selected from pyrethroid insecticides and strobilurin fungicides, wherein the moisture-sensitive active ingredient is selected from the group consisting of acephate, azinphos-methyl, carbofuran, chlorpyrifos, coumaphos, crufomat ) from the group consisting of polyethylene glycol (PEG)-6000, PEG-4000 and PEG-8000. 11. The method according to claim 10, which is characterized by the fact that the indicated performance of premix granulation by compaction includes separate, sequential or simultaneous performance of compaction, as well as premix granulation. 12. The method according to claim 10, which includes: (a) mixing an active ingredient selected from at least one pyrethroid with a low melting point with the required amount of precipitated silica to obtain a premix; (5) grinding the premix with or without other additives in an air-jet mill to obtain low-melting pyrethroid powder particles of the desired size; (c) adding to the powdered pyrethroid with a low melting point the organophosphorus active ingredient and an additive having a softening or melting point lower than the melting point of the low melting active ingredient and any other necessary additives and mixing them to obtain a premix; (4) granulation of the premix by compaction to obtain granules. 13. A method of pest control, which includes the use of an agrochemical composition against insect pests on the site, and the specified agrochemical composition contains: a) at least one low-melting active ingredient; Jur) at least one moisture-sensitive active ingredient; and c) an additive having a softening point or melting point lower than the melting point of the low-melting active ingredient, wherein the low-melting active ingredient is selected from pyrethroid insecticides and strobilurin fungicides, wherein the moisture-sensitive active ingredient is selected from the group , consisting of acephate, azinphos-methyl, carbofuran, chlorpyrifos, coumaphos, crufomate, dimethoate, ethoprop, famfur, fenamiphos, isofenphos, methamidophos, methidathion, methylparathion, mevinphos, monocrotophos, metham-sodium, phosalone, phosmet, phosphamidon, profenofos, TERR, 60 terbufos, tetrachlorvinphos, trichlorfon and their combinations, and the additive is selected from the group consisting of polyethylene glycol (PEG)-6000, PEG-4000 and PEG-8000. 14. The method according to claim 13, which is characterized by the fact that the indicated agrochemical composition is used to control insect pests on the site, and the indicated insect pests are insect pests belonging to the classes of insecticides / erioryegap, Soieorigap, Ririegap and Netiriegap. 15. A kit containing: (a) at least one active ingredient with a low melting point; (B) at least one moisture-sensitive active ingredient; and (c) an additive having a softening point or melting point lower than the melting point of the low-melting active ingredient, wherein the low-melting active ingredient is selected from pyrethroid insecticides and strobilurin fungicides, wherein the moisture-sensitive active ingredient is selected from group consisting of acephate, azinphos-methyl, carbofuran, chlorpyrifos, coumaphos, crufomate, dimethoate, ethoprop, famfur, fenamiphos, isofenphos, methamidophos, methidathion, methylparathion, mevinphos, monocrotophos, metham-sodium, phosalone, phosmet, phosphamidon, profenofos . 16. A kit that includes an acephate component, which is indicated to be used in an amount from about 5.0 95 wt. to about 80 95 wt., the bifenthrin component, which is indicated to be used in an amount from about 1.0 95 wt. up to about 20 95 wt., and the PEG-6000 component, which is indicated to be used in an amount from about 5.0 95 wt. to approximately 20,905 wt.