MXPA96004716A - New pesticide formulations and preparation method - Google Patents

Abstract

The present invention relates to: Pesticide formulations in the form of pastes, containing 1-80% of active substances, 0-50% of effervescent agents and 0.30-2% of agents that produce micropores. The compositions of the invention are for use in agriculture, in the treatment of animals, and in public and domestic hygiene.

Description

NEW PESTICIDE FORMULATIONS AND PREPARATION METHOD DESCRIPTION OF THE INVENTION The present invention relates to new pesticidal formulations, and to their method of preparation. The subject of the invention is the pesti-cide formulations which are presented in the form of pastes, which contain: - between 1% and 80% of active substance or substance, and preferably between 1 and 20% of active substance, pure or in solution in a solvent, - between 0 and 50% of effervescent agents, - between 0.30 and 2% of micropore generating agents. The formulations of the invention which are presented in the form of a thick paste have the property of being effervescent, and of having a microporous structure, which confers them a very good dispersion in water. This paste can be presented inside a water soluble plastic bag or sachet, in erased granules, or in plates. The last two presentations need a drying operation. This paste is a composition that has a very small coefficient of viscoelasticity, it is not a colloidal solution like a gel, but it results from an absorption by a solid of a liquid until saturation, and the particle size of the solid particles is between 5 and 40 Jj. The active substance or substance is in solution in a low volatile solvent, and the emulsifiers contained in REF: 23140 this solvent allow the preparation to release the active principle in the form of an emulsion after its dilution in water. The formulations of the invention have a microporous structure that facilitates their dispersion in water at the time of use. This structure is obtained by causing a gaseous release within the paste at the time of its preparation. The gas is released by the reaction of the micropore generator and the effervescent agent. One of the advantages of the invention is to present formulations such as concentrated suspensions, or emulsifiable concentrates usually liquid, in the form of a solid or a paste. Another advantage is to avoid in this way any risk of accidental spillage in the course of storage, transport or handling of the product. Another advantage is to avoid product losses on the walls of the containers at the time of use. Another advantage is, in the case where the paste is contained in a sachet or sachet soluble in water, that of supplying a product whose remaining container after use does not contain any trace of active principle, and whose loss, in case of a Opening or accidental tearing is nu-la, opposite to a liquid or gel.

The material or active substance is a liquid or solid pesticide, soluble or insoluble in water. It can be an insecticide, an acaricide, a fungicide, or a growth regulator. As the effervescent agent, a mixture of citric acid and an alkali or alkaline earth carbonate or hydrogen carbonate, for example a sodium or potassium carbonate, or a calcium carbonate, or a sodium hydrogencarbonate; other acids other than citric acid can be used, for example ascorbic acid or adipic acid. As the micropores generating agent, a glycol can be used which reacts slowly with the effervescent agent and causes a release of carbon gas into the paste, and is preferably monopropylene glycol. The invention relates more particularly to pesticidal formulations containing 0 to 20% effervescent agents, or even more particularly, to formulations containing 30 to 50% effervescent agents. The subject of the invention is particularly the formulations which contain in addition to 3 to 10% wetting agents, or even more particularly, the formulations which contain in addition to 20 to 40% wetting agents. The wetting agent can be a sodium salt of an aliphatic acid or a lignosulfonate. The invention particularly relates to formulations containing between 5 and 40% of mineral filler or organic filler, which can optionally be replaced with humectant. Mineral fillers must have sufficient absorbing power to retain the liquid constituents of the formulation without desorption; it is preferably silicas, for example silica of the aerosil or zeosil type, or of clays such as argirec, vercoryl, or even the silicates aluminosos, potassium or sodium anhydrous, or sodium borate. The organic fillers can be selected, for example, from among the celluloses, the starch or corn derivatives, the urea, the lactose and the sugars, and the polyvinylpyrrolidone. The invention relates more particularly to pesticidal formulations which also contain between: - 0.1 and 0.5% anti-foaming product, - 0. 01 and 70% organic solvent, - 0.4 and 2% surfactant, ~ 0.01 and 0.05% of stabilizer. The solvent used is very important * for the success of the invention, it must be a good solvent for the active substance or substance, and it can be, for example, an aromatic solvent, such as Solvesso 200 MR, or a solvent solvent. isoparaffin, such as Isopar V It can also be ketone solvents, such as isophorone, acetophenone or cyclohexanone, associated with different co-solvents, such as n-nutyl acetate, arcosolv PMA (methoxy propanol acetate) , butyl benzoate or diethyl phthalate. The anti-foaming agent can be, for example, Rho-dorsyl MR. The surfactants and the stabilizers can be for example those used in the experimental part, or those known to be equivalent to them. The invention particularly relates to formulations characterized in that the effervescent agent is a mixture of citric acid and sodium carbonate, and the formulations characterized in that the micro-pore generating agent is a glycol. Among the preferred formulations of the invention, mention may be made especially of the formulations characterized in that the active substance is a pesticide fungicide, herbicide, insecticide, and more particularly, for insecticides, a pyrethrinoid selected from the group of the following products: deltamethrin, cypermethrin, alpha-metrin, tralometrine, cyhalothrin, fenvalerate, cyfluthrin, flucitrenate, fluvalinate, fenpropathrin, tefluthrin, bifenthrin, acrinatrin, betaci-flutrine, taufluvalinate, Lambdacyltrin and esfen-valerate.

The invention relates in particular to formulations in which the pyrethrinid is deltamethrin, for example those containing from 1 to 15% of deltamethrin. Another subject of the invention is a preparation method, characterized in that an emulsifiable concentrate containing the active ingredient is prepared, poured on the solid filler mixture and mixed to obtain a homogeneous paste. In a preferred embodiment of the method of the invention, the active material is preformulated in the form of an emulsifiable concentrate, or in the form of a suspension concentrated in the oil. The formulations according to the invention are introduced into water-soluble sachets or sachets, which are then stuffed and packaged in an additional container, which ensures the protection of the sachets. The invention thus also relates to formulations such as those defined above, packaged in a soluble sachet. This sachet can be constituted mainly of a water-soluble PVA film, of multiple layers or of a layer, or of a laminated film of double layer. For example, the NEDI, EF 300 or EP 300 films can be cited. In order to avoid eventual swelling during the storage of the sachets, between 2 and 10% of the agent can be added to the composition of the paste. dehydrating agent, such as sodium sulfate, calcium chloride, maleic anhydride or any of the water-capturing solvents, such as cyclohexanone or acetophenone, for example. The formulations obtained in this way have a good stability, and a good biological activity. The pastes of the invention, diluted in water, produce an emulsion, and are preferably used in agriculture, in the treatment of crops, or in the treatment of animals, or in public and domestic hygiene. The areas of use are those of the raw materials used. The following examples illustrate the invention: The formulations of the invention are prepared as follows: A - Preparation of the emulsifiable base concentrate The different ingredients, surfactants, solvents, active substances, stabilizers and others are mixed under stirring until a solution is obtained. B - Preparation of solid charges Solid charges must have a granulometry of less than 15 u. If this is not the case, they must be submitted to my-cronization. They are then mixed in a Lodige-type apparatus.

C - Preparation of the paste The emulsifiable concentrate is poured on the mixture of the solid charges, and everything is then mixed in an apparatus until obtaining a homogeneous paste. D - Preferential conditioning The paste obtained is placed in a water-soluble sachet, and then it is closed. Preparation of the emulsifiable base concentrate An emulsifiable concentrate was prepared, which contains: Deltamethrin 100% 14.50% B.H.T. 0.10% Ca Phenylsulphonate 5.03% Emulsogen EL 360 1.67% Solvesso 200 78.70% EXAMPLE 1: A paste was prepared containing 5% deltamethrin: Anhydrous sodium carbonate 22.5% Anhydrous citric acid 22.5% IS powdered humectant 20.0% Monopropylene glycol 0.4% Anti-foaming 425 0.1% Concentrated emulsifiable deltamethrin 34.5% EXAMPLE 2: A paste was prepared that corresponded to the formulation: Sodium carbonate anhydrous 12.0% Anhydrous citric acid 12.0% Minex 10 32.5% Morwet D425 2.5% IS Moisturizer powder 6.0% Anti-foaming agent 425 0.1% Monopropylene glycol 0.4% Emu latable concentrate of deltamethrin 34.5% The pastes of examples 1 and 2 can be conditioned in water soluble PVA sachets. An outer container made of aluminum coated with PVC can ensure the protection of these sachets. EXAMPLE 3: Granules with 5% deltamethrin were prepared, which contained: Anhydrous sodium carbonate 10.0% Citric acid anhydrous 10.0% Lactose 1H .-. 0 19.0% IS Moisturizer powder 26.0% Antifoam 425 0.1% Monopropylene glycol 0.4% Emu latable concentrate of deltamethrin 34.5% EXAMPLE 4: granules of formula were prepared: Anhydrous sodium carbonate 12.0% Anhydrous citric acid 12.0% Minex 10 32.5% Morwet D425 2.5% IS Moisturizer powder 6.0% Defoamer 454 0.1% Monopropylene glycol 0.4% Emu latable concentrate of deltamethrin 34.5% EXAMPLE 5: Plates or tablets with 5% deltamethrin were prepared, of the formula: Anhydrous sodium carbonate 12.0% Anhydrous citric acid 12.0% Minex 10 32.5% Morwet D425 2.5% IS moisturizer powder 4.5% Monopropylene glycol 1.9% Antifoam 425 0.1% Emu latable concentrate of deltamethrin 34.5% Operating as indicated above, were prepared the following formulations: The preparations of examples 6 to 11 were conditioned in PVA sachets, Nedi EF.210 film.

INGREDIENT Ex. 6 Ex. 7 Ex. 8 Ex. 9 Ex. 10 Ex. eleven DELTAMETRINA 5,040 5,040 5,040 5,040 5,040 5,040 BHT 0.035 0.035 -0.035 0.035 0.035 0.035 FENILSULFONATE OF CALCIUM 0.745 0.745 0.745 0.745 0.745 0.851 EMULSOGEN THE 1,738 1,738 1,738 1,738 1,738 1,631 ISOFORONA 21,278 21,278 21,278 21,278 21,278 SOLVESSO 200 6.631 ARCOSOLV PMA 6.631 ANISOL 27.909 BUTYL BENZOATE 6.631 N-BUTYL ACETATE 6.631 DITHYL FTHALATE 6.631 SODIUM CARBONATE 22,340 22,340 22,340 22,340 22,340 22,340 CITRIC ACID 22,340 22,340 22,340 22,340 22,340 22,340 WASTE IS 19.853 19.853 19.853 19.853 19.853 19.853 The preparations of examples 12 to 17 were conditioned in the PVA sachets, Nedi EF A film.

INGREDIENT Ex. 12 Ex. 13 Ex. 14 Ex. 15 Ex. 16 Ex. 1" DELTAMETRINA 5,040 5,040 5,040 5,040 5,040 5,040 BHT 0.035 0.035 Ó.035 0.035 0.035 0.035 FENILSULFONATE OF CALCIUM 0.745 0.745 0.745 0.745 0.745 0.851 EMULSOGEN THE 1,738 1,738 1,738 1,738 1,738 1,631 ISOFORONA 21,278 21,278 21,278 21,278 21,278 SOLVESSO 200 6.631 ARCOSOLV PMA 6. 631 NJ I ANISOL 27. 909 BUTYL BENZOATE 6. 631 N-BUTYL ACETATE 6. 631 DIETARY FTHALATE 6.631 SODIUM CARBONATE 22. 340 22,340 22,340 22,340 22,340 22,340 CITRIC ACID 22,340 22,340 22,340 22,340 22,340 22,340 WASTE IS 19.853 19.853 19.853 19.853 19.853 19.853 The preparation of Example 18 was conditioned in PVA sachets, Nedi EF.210 film. The preparation of Example 19 was conditioned in the PVA sachets, Nedi EF AK film. INGREDIENTS Ex. 18 Comp. % Ex. 19 Comp. % DELTAMETRINA 98.5% BHT 5.04 5.04 0.10 0.10 0.70 0.70 DIETHYL PHTHALATE ACETOPHENONE 13.90 13.90 1.90 1.90 Emulsogen THE SOLVESSO 200 13.76 13.76 15.40 15.40 Na2C03 29.30 Anhydrous Citric Acid 29.30 19.90 19.90 IS WETTING Preparation of the emulsifiable base concentrate: An emulsifiable concentrate was prepared, which contained INGREDIENT Ex. 20 Ex. 21 Ex. 22 Ex. 23 Ex. 24 DELTAMETRINA 98.5% 14.2 ^ 14.2 14.2 14.2 14.2 BHT 0.1 0.1 0.1 0.1 0.1 phenylsulfonate CALCIUM 3.5 3.5 3.5 3.5 3.5 Emulsogen EL 3.5 3.5 3.5 3.5 3.5 SOLVESSO 200 48.7 0 0 0 0 CYCLOHEXANONE 30.0 30.0 30.0 30.0 30.0 ARCOSOLV PMA 1 48.7 0 0 0 r- ' ANISOL 0 0 0 1 BENZOATE OF BUTYL 48.7 0 0 ACETATE OF N-BUTYL 48.7 0 FTHALATE OF DIETILO 48.7 Stability Study The storage behavior of the formulations of the invention was studied. Biological Study 5 The insecticidal activity of the formulations of the invention was studied on Rhopalosiphum padi (female apterous in the first and second larval stages), the host plant was tea (stage 2, Florence-Aurore variety). The formulations of the invention are as effective as the commercial formulation Décis MR EC 25 g / l. The formulations therefore have an excellent activity.

It is noted that in relation to this date, the best method known by the applicant to carry out the aforementioned invention, is that which is clear from the present description of the invention.

Having described the invention as above, property is claimed as contained in the following:

Claims (17)

1. CLAIMS 1. Pesticide formulations characterized because they are presented in the form of pastes containing: - between 1% and 80% pure active matter or in solution, - between 0 and 50% effervescent agents, - between 0.30 and 2% agents generators of micropores.
2. 2. The pesticidal formulations according to claim 1, characterized in that they contain from 0 to 20% effervescent agents.
3. 3. The pesticidal formulations according to claim 1, characterized in that they contain from 30 to 50% of effervescent agents.
4. 4. The pesticidal formulations according to claim 1, characterized in that they also contain from 3 to 10% of wetting agents.
5. 5. The pesticidal formulations according to claim 1, characterized in that they also contain 20 to 40% wetting agents.
6. 6. The formulations according to any of claims 1 or 5, characterized in that they contain between 5 and 40% mineral charge.
7. 7. The pesticidal formulations according to any of claims 1 to 6, characterized in that they also contain between: - 0.1 and 0.5% of anti-foaming product, - 0.01 and 70% of organic solvent, - 0.4 and 2% of surfactant, - 0.01 and 0.05% stabilizer.
8. 8. The formulations according to any of claims 1 to 7, characterized in that the effervescent agent is a mixture of citric acid and sodium carbonate.
9. 9. The formulations according to any of claims 1 to 8, characterized in that the micropore generating agent is a glycol.
10. 10. The formulations according to any of claims 1 to 9, characterized in that the active material is a pyrethrinoid selected from the group of the following products: deltamethrin, cypermethrin, alpha-metrin, tralometrine, cyhalothrin, fenvalerate , cyfluthrin, flucitrenate, fluvalinate, fenpropathrin, tefluthrin, bifenthrin, acrinatrine, betaciflutri-na, taufluvalinate, lambda-cyhalothrin and esfenvalerate.
11. 11. The formulations according to claim 10, characterized in that the pyrethrinide is deltamethrin.
12. 12. The formulations according to claim 11, characterized in that they contain from 1 to 15% deltamethrin.
13. 13. A method for preparing the formulations according to any of claims 1 to 12, characterized in that an emulsifiable concentrate containing the active ingredient is prepared, poured on the mixture of the solid fillers, and mixed together to obtain a homogeneous pasta. The formulations according to any of claims 1 to 12, characterized in that the active material is preformulated in the form of an emulsifiable concentrate. 15. The formulations according to any of claims 1 to 12, characterized in that the active material is preformulated in the form of a suspension concentrated in oil. 16. The formulations according to any of claims 1 to 15, characterized in that they are packaged in a soluble sachet. 17. The formulations according to any of claims 1 to 16, characterized in that they also contain from 2 to 10% dehydrating agent.