WO2014091095A1 - Quick-dissolving treatment for plants in protected solid form - Google Patents

Quick-dissolving treatment for plants in protected solid form Download PDF

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Publication number
WO2014091095A1
WO2014091095A1 PCT/FR2013/000336 FR2013000336W WO2014091095A1 WO 2014091095 A1 WO2014091095 A1 WO 2014091095A1 FR 2013000336 W FR2013000336 W FR 2013000336W WO 2014091095 A1 WO2014091095 A1 WO 2014091095A1
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WO
WIPO (PCT)
Prior art keywords
mixture
treatment
agent
soluble
water
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PCT/FR2013/000336
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French (fr)
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WO2014091095A9 (en
Inventor
Rose-Anne Raynal
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Rose-Anne Raynal
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Publication of WO2014091095A1 publication Critical patent/WO2014091095A1/en
Publication of WO2014091095A9 publication Critical patent/WO2014091095A9/en

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Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12—Powders or granules
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D7/00—Fertilisers producing carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers
    • C05D9/02—Other inorganic fertilisers containing trace elements
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/20—Liquid fertilisers
    • C05G5/27—Dispersions, e.g. suspensions or emulsions

Definitions

  • the present invention relates to a plant treatment in high solids protected solid form for the preparation of pre-dosed aqueous solutions while suppressing the contact of the user with the actives.
  • the subject of the invention is a new solid form with rapid dissolution, allowing the preparation without dosage and without contact of the user with the active agent (s) then the application of the extemporaneous aqueous form obtained for the treatment and care of plants.
  • the products used for the treatment of plants are in the form of powder as described in patent EP 1505046, granules as described in patent WO 2006/021708, briquettes or rods as described in patent EP 1063215, in a form liquid as described in patent FR2717796
  • the treatment can be done directly by application to the plant or the soil.
  • Aqueous preparations can also be obtained by solubilization of the powder or granules.
  • the use of these forms involves manipulation by the user who puts it in contact with the asset or assets of the preparation.
  • the precise dosage is very difficult and leads to additional exposure of the operator during handling.
  • the powder and the granules can leak and contaminate the environment and the manipulator.
  • the dosage In the case of liquid form, the dosage requires the use of a system for measuring a specific volume of the product and then its dilution in a given volume of water.
  • the most used systems are the burettes supplied with the product.
  • Some systems are based on the use of the cap as a metering device, the stopper having a mark that adjusts a defined quantity of the product.
  • the precise dosage is very difficult and leads to additional exposure of the operator.
  • the product leaks and contaminates the environment and the manipulator.
  • the present invention relates to a plant treatment in protected high solids solid form for the preparation of premeasured aqueous solutions while suppressing the contact of the user with the assets.
  • the subject of the invention is a new solid form with rapid dissolution, allowing the preparation without dosage and without contact of the user with the active agent (s) then the application of the extemporaneous aqueous form obtained for the treatment and care of plants.
  • the products used for the treatment of plants are in the form of powder as described in patent EP 1505046, granules as described in patent WO 2006/021708, briquettes or rods as described in patent EP 1063215, in a form liquid as described in patent FR2717796
  • the treatment can be done directly by application to the plant or the soil.
  • Aqueous preparations can also be obtained by solubilization of the powder or granules.
  • the use of these forms involves manipulation by the user who puts it in contact with the asset or assets of the preparation.
  • the precise dosage is very difficult and leads to additional exposure of the operator during handling.
  • the powder and the granules can leak and contaminate the environment and the manipulator.
  • the dosage In the case of liquid form, the dosage requires the use of a system for measuring a specific volume of the product and then its dilution in a given volume of water.
  • the most used systems are the burettes supplied with the product.
  • Some systems are based on the use of the cap as a metering device, the stopper having a mark that adjusts a defined quantity of the product.
  • the precise dosage is very difficult and leads to additional exposure of the operator.
  • ultrafast dispersion property is meant here the capacity of the solid form to disperse in one liter of water, without stirring, in less than 5 minutes and preferably in less than 1 minute and preferably in less than 30 seconds. This property makes it possible to prepare the aqueous treatment, ready to be applied, without having to proceed to a long stirring step.
  • Pre-dosed aqueous solution is here understood to mean a solution for which the addition of the solid form according to the invention makes it possible to obtain directly, without a dosing operation, a treatment volume at the required concentration.
  • the volume is 1 liter or a multiple.
  • one or more plant treatment active agents in the form of powder or microgranules which can be coated 3
  • a mixture of excipients comprising at least one agent or a mixture of fast disintegrating agents, a fast-dissolving agent or mixture of soluble agents and a slip agent, for example talc.
  • the mixture of rapid disintegrating agents and soluble agents called hydrosolubilizer according to the invention makes it possible to limit the surface passivation phenomena, to obtain rapid disintegration of the solid without having to proceed to a step of granulation of the excipients.
  • the solid form according to the invention may comprise a filler, a lubricating agent, for example glyceryl behenate, or magnesium stearate, a dye or mixtures of dyes.
  • a lubricating agent for example glyceryl behenate, or magnesium stearate
  • Other compounds well known to those skilled in the art may be added in order to modulate the mechanical properties of the form according to the invention such as hardness, elasticity, plasticity, friability.
  • Polymers of the family of polyethylene glycols as well as polyvinylpyrrolidones and crospovidone can be mentioned.
  • an anti-foaming agent such as dimethicone and its derivatives.
  • Such a solid form according to the invention is obtained by means of standard compression and / or extrusion processes well known to those skilled in the art.
  • the solid form according to the invention is obtained by compression in a pelletizer for compression forces of 3 to 50 kN, preferably 7 to 20 kN and more preferably still 9 at 18kN.
  • the pressure exerted on the powder is between 5 and 250 MPa.
  • the filler is also chosen according to its ability to modulate the elastic properties of the powder to prevent the cleavage phenomenon during the compression operation.
  • the amount of lubricating agent used in the tablet according to the invention is from 0.1 to 2% by weight of lubricating agent, based on the total weight of the tablet, preferably of the order of 0, 2 to 0.4%.
  • Hydrophilic colloidal silicas for example Aerosil® produced by Evonik, make it possible to obtain an improvement in the flowability and homogeneity properties of the powder constituting the solid according to the invention.
  • the rapid disintegrating agent or the mixture of fast disintegrating agents is the agent which makes it possible to obtain the disintegration of the solid according to the invention in water. It can be chosen from the group of synthetic or natural hydrophilic polymers called super-disintegrants. 4
  • crosslinked sodium carboxymethylcellulose and its derivatives are unsaturated by the term croscarmellose, carboxymethyl starch and its sodium salt, soluble crospovidone and mixtures thereof.
  • This compound is here introduced in order to confer a rapid disintegration tablet or solid according to the invention, while maintaining sufficient cohesion.
  • Effervescent disintegrating agents can also be used. These are based on the mixture of an acid and an alkaline carbonate.
  • the organic acids of the effervescent couple that may be used in the context of the present invention are compounds capable of reacting with alkaline carbonates to cause a release of carbon dioxide, when they are brought into contact with water.
  • Suitable acids are, for example, citric acid, fumaric acid, adipic acid, tartaric acid, malic acid, succinic acid, phosphoric acid and mixtures of these compounds.
  • the preferred acid according to the invention is citric acid.
  • An alkali carbonate that may be used in the context of the present invention is, for example, sodium bicarbonate, potassium bicarbonate, carboxylysine, calcium carbonate, sodium carbonate, potassium carbonate and magnesium carbonate. as well as mixtures of these compounds.
  • the weight ratio of the acid / carbonate pair varies from 1/3 to 3/1. All these disintegrating agents can also be used in a mixture.
  • the solid form according to the invention may also comprise one or more dehydrating agents in order to improve the physical stability over time.
  • the internal desiccant has the function of trapping traces of water likely to appear in the tablet.
  • the abovementioned antioxidant agent is chosen from alpha-tocopherol, gamma-tocopherol, delta-tocopherol, natural extracts rich in tocopherol, ascorbic acid and its salts. sodium or calcium, Ascorbic DL palmityl, propyl gallate, octyl gallate, dodecyl gallate, butyl-hydroxy anisole gallate (BHA) and butyl-hydroxy toluene gallate (BHT) .
  • the internal desiccant is magnesium citrate.
  • the disintegrating agent alone does not make it possible to obtain sufficiently rapid dissolution properties in water without continuous stirring.
  • a disintegrating agent with a soluble agent 5 makes it possible to obtain the desired effect.
  • the weight ratio between the disintegrating agent and the soluble agent can range from 1/30 to 25/1.
  • the soluble agent also called a water-solubilising agent, is a compound with a molecular weight of less than 1000 daltons, having a solubility in water of greater than 50 grams per liter of water at 25 ° C., comprising at least one chemical function among the hydroxyls , carboxylic acids, aldehydes, amines and their derivatives.
  • a soluble agent is selected from the family of carbohydrates.
  • This agent comprises at least one oligoside and preferably a diholoside or a mixture of diholosides.
  • the diholoside may be maltose, sucrose, threalose, mannose, cellobiose or lactose.
  • the soluble agent may advantageously be selected from polyols, saccharides, mono and disaccharides and oligosaccharides.
  • polyols such as glucose, galactose, mannitol, xylitol, sorbitol, maltitol, lactitol, isomaltitol, glycerol, erythritol, arabitol, ribitol and volemitol. .
  • the solubilizing agent may also be an amino acid chosen from water-soluble amino acids, for example alanine, aspartic acid, arginine, asparagine, cysteine, glutamic acid, glutamine, lysine, leucine, isoleucine, glycine, histidine, methionine, phenyalanine, proline, serine, threonine, tryptophan, tyrosine and valine. It is also possible to use aminated di or triacids chosen from the preceding ones.
  • the compressed solid comprises:
  • one or more plant treatment active agents in the form of powder or micro-granules which can be coated
  • Example No. 8 we have discovered that it is necessary to obtain an improvement in the disintegration rate, to obtain a satisfactory homogeneity of mixing between the disintegrating agent and the soluble agent, as indicated in Example No. 8 .
  • a powder mixer and have a stirring time greater than 5 minutes and preferably greater than 10 minutes.
  • the powder mixer is preferably selected from V mixers or Y well known to those skilled in the art.
  • the excipient mixture comprises one or a mixture of surfactants. 6 for stabilizing the dispersion of the hydrophobic compounds in the aqueous phase.
  • the surfactant is preferably chosen from polysorbates, sodium dodecyl sulphate and TRIS.
  • glycol esters such as ethylene glycol stearate, glycerol esters such as glycerol stearate, polyoxyethylene glycol esters of fatty acids, sorbitan esters, but especially polyoxyethylene sorbitan esters, more commonly called Tweens or polysorbates.
  • Compounds derived from naphthalenic acid and its salts can also be used as well as phospholipids.
  • the composition may also include fillers for density modulating, colorants, viscosity modifiers of the final formulation such as cellulose derivatives, carbomers, xanthans, carob derivatives, derivatized starches, gelatins, agars.
  • one or more active and / or nutritive or fertilizing substances may be added.
  • an active substance at least one of those in the group comprising phytosanitary products may be used.
  • Insecticides for the control of insects may be mentioned.
  • the group of organohalogens for example the group of organohalogens.
  • dichlorodiphenyltrichloroethane and its derivatives such as tetrachlorodiphenylethane, 2,2,2-trichloro-1,1-bis (4-chlorophenyl) ethanol perthane, 2,2-bis (paramethoxy-phenyl) 1,1,1-trichloroethane, the group of gamma-hexachlorocyclohexane (HCH) and benzene hexachloride (BHC), the group of octachloro-4,7-methanohydroindane such as heptachlor, hexachlorodimethanonaphthalene, exodimethanonaphthalene, bishomocubanes such as chlordecone, perchlordecone, and dienochlor.
  • turpentine derivatives such as endosulfan, toxaphene, polychlorocamphene
  • organophosphorus compounds There are three groups of organophosphorus pesticides. The first is organophosphorus phenyl ring. Many compounds belong to this group such as bromophos, chlorfenvinphos, fenitrothion, fenthion, fonofos, isofenphos, parathion, parathion ethyl, parathion methyl, phosalone, profenofos, protiophos.
  • the second group consists of organophosphorus heterocycles such as chlorpyrifos, diazinon, etimimos, isoxation, quinalphos, methidation, phosmet.
  • the third group consists of aliphatic organophosphorus compounds, among which mention may be made of acephate, demeton, dichlorvos, dicrotophos, dimethoate, Ethion, formothion, malathion, mevinphos, monocrotophos, naled, omethoate, phorate, phosphamidon and trichlorfon.
  • substances of the carbamate group such as naphthyl methyl carbamate, methyl and dimethyl carbamates with a heterocyclic structure, methyl carbamates with a phenyl ring structure and aliphatic chain methyl carbamates.
  • the natural and synthetic pyrethroids include the following compounds: bifenthrin, bioresmethrin, deltamethrin, depallethrin, ethofenprox, fenpropathrin, cypermethrin, fenvalerate, esfenvalerate, cyfluthrin, alphamethrin, tralomethrin, fluvalinate, permethrin, lambda-cyhalothrin, flucythrinate, tefluthrin , tralomethrin, zetacypermethrin, betacyfluthrin.
  • Sulfones and sulfonates such as 1,2,4-trichloro-5- (4-chlorophenyl) sulfonylbenzene, or propargite.
  • fungicides for removing mold and fungi parasitic plants.
  • the oldest fungicides are sulfur, copper and its organic derivatives such as the Bordeaux mixture which is a mixture of copper sulphate and calcium hydroxide.
  • Contact fungicides such as zineb, captan and the systematic fungicides triadimefon and morpholine, are distinguished.
  • the herbicide group is the third major group of active substances that can be added.
  • Mineral compounds such as calcium cyanide (Ca (CN) 2), iron sulphate (FeSO 4 ), sodium chlorate (NaClO 3).
  • Organic herbicides can also be used such as glyphosate, dinitroanilines or toluidines and their derivatives including benfluralin, butraline, fluchloraline, nitraline, on / saline, pendimethalin, trifluralin.
  • Substituted ureas such as chlortoluron, chloroxuron, cycluron, diuron, ethidimuron, fenuron, isoproturon, linuron, monolinuron, methabenzthiazuron, metobromuron, metoxuron, monuron, thiazafluron, tebuthiuron, thiazafluron, siduron, and neburon.
  • Triazines atrazine, cyanazine, methoprotrin, propazine, terbuthylazine, simazine, simetryne, secbumeton, secbumeton, terbumeton, amtreinne, desmétryne, prométryne.terbutryne.
  • Imidazolinones such as imazamethabenz, or imazapyr.
  • Sulfonylureas such as amidosulfuron, azimsulfuron, and chlorsulfuron.
  • Diphenyls-ethers such as acifluorfen-sodium, aclonifen, bifenox, bromofenoxime, chlomethoxyfene, diclofop-methyl, fluorodifen, fomesafen, lactofen, nitrofen or oxyfluorfen.
  • Synthetic phytohormones Mention may be made of indol-acetic acid or IAA and its derivatives, phenoxyalkanoic acids, such as 2,4-D or 2- (2,4-dichlorophenoxy) ethanoic acid.
  • 2,4-MCPA triclopyr, diclofop methyl, 2,4,5-T, 2,4-DP (dichlorprop), MCPP (mecoprop), 2,3,6-TBA, dicamba, picloram, clopyralid, and flurenol.
  • Carbamates including carbamic acid derivatives comprising the -NH 2 -COOH structure such as asulam, barbam, chlorbufam, chlorpropham, propham, carbetamide.
  • Quaternary ammoniums or bipyridiles such as diquat, paraquat, and difenzoquat. Pinoxaden including alloxydim-sodium and clodinafop-propargyl.
  • the solid form obtained according to the invention may also contain compounds ensuring the nutrition of plants, they are fertilizers or fertilizers.
  • plants need inputs of nitrogen, phosphorus, potassium and trace elements, to enjoy optimal growth and better resistance to aggression.
  • We can add secondary elements such as calcium, magnesium and sulfur.
  • Nitrogen can also be provided by organic compounds such as amino acids, for example alanine, aspartic acid and arginine Asparagine, cysteine, glutamic acid, glutamine, lysine, leucine, isoleucine, glycine, histidine, methionine, phenyalanine, proline, serine, threonine, tryptophan, tyrosine and valine.
  • amino acids for example alanine, aspartic acid and arginine Asparagine, cysteine, glutamic acid, glutamine, lysine, leucine, isoleucine, glycine, histidine, methionine, phenyalanine, proline, serine, threonine, tryptophan, tyrosine and valine.
  • Potassium compounds include potassium sulphate, potassium chloride, potassium oxide.
  • phosphorus oxide In the phosphorus compounds, phosphorus oxide, dicalcium phosphate, simple superphosphate, triple superphosphate, magnesium phosphate and natural phosphate are distinguished.
  • the solid according to the invention may also contain nutrients or nutrients, for example, zinc, copper, manganese, boron, calcium, iron , calcium sulphate (gypsum), magnesium, molybdenum, chlorides, selenium, sulfur or combinations thereof.
  • the copper may be copper (cupric) in the form: hydroxide, chloride, sulfate, oxide, oxysulphate, nitrate, carbonate, ammonium carbonate, cupric chloride dihydrate, proteinate, acetate, citrate, chelate, complexed, or trapped.
  • the zinc may be zinc acetate, ammonium chloride, sulfate, oxide, oxysulfate, nitrate, chloride, citrate, chelate or a trapped complex.
  • the manganese can be manganese can be in the form: nitrate, chloride, sulfate, oxide, oxysulfate, acetate, anhydrous potassium carbonate, sulfate, mangagnese tetrahydrate, nitrate hexahydrate acetate, citrate, chelate or sequestered complex.
  • the boron may be boric acid, sodium borate, potassium tetrahydrate tetraborate, calcium borate, sodium calcium borate, borax, disodium octadate tetrahydrate, orthoboric acid.
  • Calcium can be calcium: carbonate, chloride, sulfate, gypsum, calcium borate, lime, nitrate, phosphate, citrate, a chelate or sequestered complex.
  • the iron may be iron in the form of anhydrous sulphate, sulphate, chloride, tetrahydrate, hexahydrate, nitrate, nitrate hexahydrate, chloride, ammonium citrate, ammonium sulphate, chelate, sequestered, proteinate or complexes.
  • the preferred forms of the trace elements are in complexed form with EDTA.
  • Nitrogen, phosphorus and potassium compounds as well as nutrients and trace elements can be obtained in different types of agricultural and industrial waste.
  • Non-limiting examples include products and by-products of vegetable origin, such as residues of beet pulp, sunflower pulp, marc 10 grapes, oilmeal flours or meals, hulls, olive pulp, beet vinasse, coffee grounds, seaweed extract, vermicompost, feather and bone powders. They are used dry in powder form which can be added to the solid form according to the invention.
  • the compressed solid object containing one or more active substances, phytosanitary and / or nutritive or fertilizing, is wrapped in a water-soluble film. It may be contained in a hermetic unitary distribution system, making it possible to prevent any contact with the user, such as that described, for example, in patents EP 0761563 and FR 2633260, or even contained in a blister system.
  • water-soluble films are widely used in industry and are mainly made of natural materials, semisynthetic or synthetic.
  • polyvinylalcohol films and its derivatives examples include polyvinylalcohol films and its derivatives, methylcellulose films and its derivatives, carboxymethylcellulose alkyls and hydroxyalkylcellulose, modified starches, polyvinylsethers, polyethylene derivatives, polyvinylsulfonic acid, polyanhydrides, derivatives of formaldehyde resins, polyacrylates and their derivatives.
  • the film can according to the needs to include several thicknesses.
  • the water-soluble film is a polyvinyl alcohol or methylcellulose film.
  • composition of the film according to the composition of the compressed solid containing the active agent (s) according to the invention.
  • Mixture A In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
  • Example No. 1 The mixture is recovered according to Example No. 1, in the form of a fertilizer powder.
  • Example No. 2 On an alternative tabletting machine set for a 40 MPa compression we realize the manufacture of tablets of 3.9 g
  • the tablets obtained according to Example 2 are covered with a thermoplastic film of polyvinyl alcohol 60 microns thick by treatment bagpacker unit type flowpack.
  • aqueous fertilizer solution is ready for use.
  • Mixture A In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
  • Example 7 Preparation of a Tablet Covered with a Water-Resistant Film Containing a Herbicidal Composition
  • Mixture A In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
  • Example No. 3 Tablets weighing 2.36 g are obtained, dosed with 0.3 g of Dicamba, each of which makes it possible to prepare 1 liter of aqueous solution.
  • Example 4 Using a tablet according to Example 4 in which the mixture A soluble agents mannitol and sucrose with the fast disintegrating agents malic acid, citric acid and sodium hydrogencarbonate, was not realized previously.
  • the complete disintegration time according to Example 3 goes from 45 seconds to 52 seconds.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pest Control & Pesticides (AREA)
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  • Dentistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Agronomy & Crop Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

A quick-dissolving treatment for plants in protected solid form for preparing pre-dosed aqueous solutions while eliminating user contact with the active agents.

Description

Traitement végétal sous Forme solide protégée à dissolution rapide  Plant treatment in Protected solid form with rapid dissolution
La présente invention concerne un traitement pour végétaux sous forme solide protégée à dissolution ultrarapide permettant la préparation de solutions aqueuses pré- dosées tout en supprimant le contact de l'utilisateur avec les actifs. The present invention relates to a plant treatment in high solids protected solid form for the preparation of pre-dosed aqueous solutions while suppressing the contact of the user with the actives.
L'invention a pour objet une nouvelle forme solide à dissolution rapide, permettant la préparation sans dosage et sans contact de l'utilisateur avec le ou les actifs puis l'application de la forme aqueuse extemporanée obtenue pour le traitement et le soin de végétaux.  The subject of the invention is a new solid form with rapid dissolution, allowing the preparation without dosage and without contact of the user with the active agent (s) then the application of the extemporaneous aqueous form obtained for the treatment and care of plants.
De façon inattendue, il est possible d'obtenir une dissolution complète de l'objet en moins de 5 minutes et dans certains cas moins de 1 minute, dite ultrarapide, tout en présentant une faible friabilité même en présence d'un film hydrosoluble. Cette forme solide se présente enveloppée et protégée dans un film hydrosoluble.  Unexpectedly, it is possible to obtain a complete dissolution of the object in less than 5 minutes and in some cases less than 1 minute, said ultrafast, while having a low friability even in the presence of a water-soluble film. This solid form is wrapped and protected in a water-soluble film.
Etat de l'art antérieur State of the prior art
Classiquement les produits utilisés pour le traitement des végétaux se présentent sous la forme de poudre comme décrit dans le brevet EP1505046, de granules comme décrit dans le brevet WO 2006/021708, de briquettes ou bâtonnets comme décrit dans le brevet EP 1063215, sous une forme liquide comme décrit dans le brevet FR2717796 Dans le cas des poudres ou des granules, le traitement peut se faire directement par application sur le végétal ou sur le sol. Des préparations aqueuses peuvent aussi être obtenues par solubilisation de la poudre ou des granules. Cependant dans tous les cas l'emploi de ces formes implique une manipulation par l'utilisateur qui le met en contact avec le ou les actifs de la préparation. D'autre part le dosage précis est très difficile et entraine une exposition supplémentaire de l'opérateur lors de la manipulation. Enfin en cas de détérioration de l'emballage, la poudre et les granules peuvent fuir et contaminer l'environnement et le manipulateur.  Conventionally, the products used for the treatment of plants are in the form of powder as described in patent EP 1505046, granules as described in patent WO 2006/021708, briquettes or rods as described in patent EP 1063215, in a form liquid as described in patent FR2717796 In the case of powders or granules, the treatment can be done directly by application to the plant or the soil. Aqueous preparations can also be obtained by solubilization of the powder or granules. However in all cases the use of these forms involves manipulation by the user who puts it in contact with the asset or assets of the preparation. On the other hand the precise dosage is very difficult and leads to additional exposure of the operator during handling. Finally, in case of deterioration of the packaging, the powder and the granules can leak and contaminate the environment and the manipulator.
Dans le cas de forme liquide, le dosage nécessite l'utilisation d'un système permettant la mesure d'un volume précis du produit puis sa dilution dans un volume déterminé d'eau. Les systèmes les plus utilisés sont les burettes fournis avec le produit. Certains systèmes sont basés sur l'utilisation du bouchon comme doseur, le bouchon comportant un repère qui permet d'ajuster une quantité définie du produit. Là aussi le dosage précis est très difficile et entraine une exposition supplémentaire de l'opérateur. De plus il est nécessaire de nettoyer le système de dosage en fin d'opération sinon il reste contaminé jusqu'à l'opération suivante. Enfin pour toutes ces formes de produits, en cas de détérioration de l'emballage, le produit fuit et contamine l'environnement et le manipulateur.  In the case of liquid form, the dosage requires the use of a system for measuring a specific volume of the product and then its dilution in a given volume of water. The most used systems are the burettes supplied with the product. Some systems are based on the use of the cap as a metering device, the stopper having a mark that adjusts a defined quantity of the product. Here too the precise dosage is very difficult and leads to additional exposure of the operator. In addition it is necessary to clean the dosing system at the end of operation otherwise it remains contaminated until the next operation. Finally for all these forms of products, in case of deterioration of the packaging, the product leaks and contaminates the environment and the manipulator.
Certains brevets comme le brevet US 5.150.587, décrivent des formes solides en comprimés, mais ces compositions ne permettent pas d'obtenir une dissolution rapide  Certain patents, such as US Pat. No. 5,150,587, describe solid forms in tablets, but these compositions do not make it possible to obtain rapid dissolution.
FEUILLE DE REMPLACEMENT R 1 SUBSTITUTE SHEET R 1
La présente invention concerne un traitement pour végétaux sous forme solide protégée à dissolution ultrarapide permettant la préparation de solutions aqueuses prédosées tout en supprimant le contact de l'utilisateur avec les actifs. The present invention relates to a plant treatment in protected high solids solid form for the preparation of premeasured aqueous solutions while suppressing the contact of the user with the assets.
L'invention a pour objet une nouvelle forme solide à dissolution rapide, permettant la préparation sans dosage et sans contact de l'utilisateur avec le ou les actifs puis l'application de la forme aqueuse extemporanée obtenue pour le traitement et le soin de végétaux.  The subject of the invention is a new solid form with rapid dissolution, allowing the preparation without dosage and without contact of the user with the active agent (s) then the application of the extemporaneous aqueous form obtained for the treatment and care of plants.
De façon inattendue, il est possible d'obtenir une dissolution complète de l'objet en moins de 5 minutes et dans certains cas moins de 1 minute, dite ultrarapide, tout en présentant une faible friabilité même en présence d'un film hydrosoluble. Cette forme solide se présente enveloppée et protégée dans un film hydrosoluble.  Unexpectedly, it is possible to obtain a complete dissolution of the object in less than 5 minutes and in some cases less than 1 minute, said ultrafast, while having a low friability even in the presence of a water-soluble film. This solid form is wrapped and protected in a water-soluble film.
Etat de l'art antérieur State of the prior art
Classiquement les produits utilisés pour le traitement des végétaux se présentent sous la forme de poudre comme décrit dans le brevet EP1505046, de granules comme décrit dans le brevet WO 2006/021708, de briquettes ou bâtonnets comme décrit dans le brevet EP 1063215, sous une forme liquide comme décrit dans le brevet FR2717796 Dans le cas des poudres ou des granules, le traitement peut se faire directement par application sur le végétal ou sur le sol. Des préparations aqueuses peuvent aussi être obtenues par solubilisation de la poudre ou des granules. Cependant dans tous les cas l'emploi de ces formes implique une manipulation par l'utilisateur qui le met en contact avec le ou les actifs de la préparation. D'autre part le dosage précis est très difficile et entraine une exposition supplémentaire de l'opérateur lors de la manipulation. Enfin en cas de détérioration de l'emballage, la poudre et les granules peuvent fuir et contaminer l'environnement et le manipulateur.  Conventionally, the products used for the treatment of plants are in the form of powder as described in patent EP 1505046, granules as described in patent WO 2006/021708, briquettes or rods as described in patent EP 1063215, in a form liquid as described in patent FR2717796 In the case of powders or granules, the treatment can be done directly by application to the plant or the soil. Aqueous preparations can also be obtained by solubilization of the powder or granules. However in all cases the use of these forms involves manipulation by the user who puts it in contact with the asset or assets of the preparation. On the other hand the precise dosage is very difficult and leads to additional exposure of the operator during handling. Finally, in case of deterioration of the packaging, the powder and the granules can leak and contaminate the environment and the manipulator.
Dans le cas de forme liquide, le dosage nécessite l'utilisation d'un système permettant la mesure d'un volume précis du produit puis sa dilution dans un volume déterminé d'eau. Les systèmes les plus utilisés sont les burettes fournis avec le produit. Certains systèmes sont basés sur l'utilisation du bouchon comme doseur, le bouchon comportant un repère qui permet d'ajuster une quantité définie du produit. Là aussi le dosage précis est très difficile et entraine une exposition supplémentaire de l'opérateur. De plus il est nécessaire de nettoyer le système de dosage en fin d'opération sinon il reste contaminé jusqu'à l'opération suivante.  In the case of liquid form, the dosage requires the use of a system for measuring a specific volume of the product and then its dilution in a given volume of water. The most used systems are the burettes supplied with the product. Some systems are based on the use of the cap as a metering device, the stopper having a mark that adjusts a defined quantity of the product. Here too the precise dosage is very difficult and leads to additional exposure of the operator. In addition it is necessary to clean the dosing system at the end of operation otherwise it remains contaminated until the next operation.
Enfin pour toutes ces formes de produits, en cas de détérioration de l'emballage, le produit fuit et contamine l'environnement et le manipulateur.  Finally for all these forms of products, in case of deterioration of the packaging, the product leaks and contaminates the environment and the manipulator.
Certains brevets comme le brevet US 5.150.587, décrivent des formes solides en comprimés, mais ces compositions ne permettent pas d'obtenir une dissolution rapide 2 dans l'eau, nécessitent dans la pratique une agitation continue et le manipulateur est en contact direct avec le produit lors de la préparation. Certain patents, such as US Pat. No. 5,150,587, describe solid forms in tablets, but these compositions do not make it possible to obtain rapid dissolution. 2 in water, require in practice continuous agitation and the manipulator is in direct contact with the product during preparation.
Les présentations existantes des produits de traitement des végétaux comportent toutes des inconvénients qui entraînent l'exposition de l'utilisateur au principe actif, ce qui peut être nuisible pour la santé particulièrement pour l'utilisation de produits phytosanitaires ayant une toxicité comme les pesticides.  Existing presentations of plant treatment products all have drawbacks that lead to exposure of the user to the active ingredient, which can be detrimental to health especially for the use of plant protection products with a toxicity such as pesticides.
Fort de ce constat, le demandeur a relevé qu'il existait un besoin non satisfait concernant une forme de traitement pour les végétaux qui présenterait à la fois les avantages les plus souvent incompatibles suivants :  Based on this finding, the Applicant noted that there is an unmet need for a form of treatment for plants that has the following most often inconsistent benefits:
- être une forme solide  - be a solid form
- pré-dosée,  - pre-dosed,
- de ne pas nécessiter de manipulation complexe de mesure de la dose lors de la préparation de la forme aqueuse à appliquer  - Do not require complex manipulation of dose measurement during the preparation of the aqueous form to be applied
- posséder de bonnes propriétés de dissolution rapide sans agitation  have good fast dissolving properties without agitation
- ne pas être à l'origine de fuite en cas de dégradation du conditionnement.  - not be the cause of leakage in case of degradation of the packaging.
Pour obtenir une telle forme possédant l'ensemble des caractéristiques fonctionnelles énoncées ci-dessus, l'inventeur a trouvé que de façon surprenante et inattendue, il était possible de faire comporter l'ensemble de ces propriétés, dont certaines peuvent paraître incompatibles avec d'autres, à une forme solide obtenue par compression, à délitement ultrarapide capable de se désagréger au contact de l'eau en donnant une forme aqueuse aisée à appliquer. Cette forme solide est enveloppée d'un film hydrosoluble ou contenue dans un compartiment hermétique.  To obtain such a form having all of the functional characteristics set out above, the inventor has found that surprisingly and unexpectedly, it was possible to include all of these properties, some of which may appear to be incompatible with others, to a solid form obtained by compression, ultra-fast disintegration capable of disintegrating in contact with water to give an aqueous form easy to apply. This solid form is wrapped in a water-soluble film or contained in an airtight compartment.
Par propriété de dispersion ultrarapide, on entend ici la capacité de la forme solide à se disperser dans un litre d'eau, sans agitation, en moins de 5 minutes et préférentiellement en moins de 1 minute et préférentiellement en moins de 30 secondes. Cette propriété permet de préparer le traitement aqueux, prêt à être appliquée, sans avoir à procéder à une étape longue d'agitation.  By ultrafast dispersion property is meant here the capacity of the solid form to disperse in one liter of water, without stirring, in less than 5 minutes and preferably in less than 1 minute and preferably in less than 30 seconds. This property makes it possible to prepare the aqueous treatment, ready to be applied, without having to proceed to a long stirring step.
Par solution aqueuse pré-dosée, on entend ici une solution pour laquelle l'addition de la forme solide selon l'invention permet d'obtenir directement sans opération de dosage, un volume de traitement à la concentration demandée. Préférentiellement le volume est de 1 litre ou un multiple.  Pre-dosed aqueous solution is here understood to mean a solution for which the addition of the solid form according to the invention makes it possible to obtain directly, without a dosing operation, a treatment volume at the required concentration. Preferably the volume is 1 liter or a multiple.
Nous avons découvert que cette forme solide compressée selon l'invention, pour présenter une propriété de dispersion ultrarapide doit être constituée par les composés suivants :  We have discovered that this compressed solid form according to the invention, to present an ultrafast dispersion property must consist of the following compounds:
- un ou des actifs de traitement des végétaux sous forme de poudre ou de microgranules pouvant être enrobées 3 one or more plant treatment active agents in the form of powder or microgranules which can be coated 3
- un mélange d'excipients comprenant au moins un agent ou un mélange d'agents de désagrégation rapide, un agent ou un mélange d'agents solubles à dissolution rapide et un agent de glissement par exemple le talc. a mixture of excipients comprising at least one agent or a mixture of fast disintegrating agents, a fast-dissolving agent or mixture of soluble agents and a slip agent, for example talc.
Le mélange d'agents de désagrégation rapide et d'agents solubles dits hydrosolubilisant selon l'invention, permet de limiter les phénomènes de passivation de surface, d'obtenir un délitement rapide du solide sans avoir à procéder à une étape de granulation des excipients.  The mixture of rapid disintegrating agents and soluble agents called hydrosolubilizer according to the invention makes it possible to limit the surface passivation phenomena, to obtain rapid disintegration of the solid without having to proceed to a step of granulation of the excipients.
Eventuellement la forme solide selon l'invention peut comprendre un agent de charge, un agent lubrifiant par exemple le glycéryl béhénate, ou le stéarate de magnésium, un colorant ou des mélanges de colorants. D'autres composés bien connus de l'homme de l'art, peuvent être ajoutés afin de moduler les propriétés mécaniques de la forme selon l'invention comme la dureté, l'élasticité, la plasticité, la friabilité. On peut citer les polymères de la famille des polyéthylènes glycols ainsi que les polyvinylpyrrolidones et crospovidone. L'homme de l'art pourra ajouter si nécessaire, un anti-moussant comme le diméthicone et ses dérivés.  Optionally, the solid form according to the invention may comprise a filler, a lubricating agent, for example glyceryl behenate, or magnesium stearate, a dye or mixtures of dyes. Other compounds well known to those skilled in the art may be added in order to modulate the mechanical properties of the form according to the invention such as hardness, elasticity, plasticity, friability. Polymers of the family of polyethylene glycols as well as polyvinylpyrrolidones and crospovidone can be mentioned. Those skilled in the art may add if necessary, an anti-foaming agent such as dimethicone and its derivatives.
Une telle forme solide selon l'invention est obtenue au moyen de procédés standards de compression et/ou d'extrusion bien connus de l'homme de l'art.  Such a solid form according to the invention is obtained by means of standard compression and / or extrusion processes well known to those skilled in the art.
Selon un mode de réalisation avantageux du procédé conforme à l'invention, la forme solide selon l'invention est obtenue par compression dans une pastilleuse pour des forces de compression de 3 à 50kN, de préférence de 7 à 20kN et plus préférentiellement encore de 9 à 18kN. La pression exercée sur la poudre est comprise entre 5 et 250 Mpa. According to an advantageous embodiment of the process according to the invention, the solid form according to the invention is obtained by compression in a pelletizer for compression forces of 3 to 50 kN, preferably 7 to 20 kN and more preferably still 9 at 18kN. The pressure exerted on the powder is between 5 and 250 MPa.
L'agent de charge est lui aussi choisi en fonction de sa capacité à moduler les propriétés d'élasticité de la poudre pour éviter le phénomène de clivage lors de l'opération de compression.  The filler is also chosen according to its ability to modulate the elastic properties of the powder to prevent the cleavage phenomenon during the compression operation.
La quantité d'agent lubrifiant, mise en œuvre dans le comprimé conforme à l'invention, est de 0,1 à 2% exprimé en poids d'agent lubrifiant ramené au poids total du comprimé, de préférence de l'ordre de 0,2 à 0,4%.  The amount of lubricating agent used in the tablet according to the invention is from 0.1 to 2% by weight of lubricating agent, based on the total weight of the tablet, preferably of the order of 0, 2 to 0.4%.
De plus, pour conférer au mélange à sec de poudre initial des propriétés antistatiques, ceux-ci comprennent éventuellement un agent antistatique choisi préférentiellement dans le groupe comprenant la silice précipitée ou colloïdale, et le talc.  In addition, to give the initial dry powder mixture antistatic properties, these optionally include an antistatic agent preferably selected from the group comprising precipitated or colloidal silica, and talc.
Les silices colloïdales hydrophiles, par exemple l'Aerosil® produites par la société Evonik, permettent d'obtenir une amélioration des propriétés de coulabilité et d'homogénéité de la poudre constituant le solide selon l'invention.  Hydrophilic colloidal silicas, for example Aerosil® produced by Evonik, make it possible to obtain an improvement in the flowability and homogeneity properties of the powder constituting the solid according to the invention.
L'agent de désagrégation rapide ou le mélange d'agents de désagrégation rapide, est l'agent qui permet d'obtenir la désagrégation du solide selon l'invention dans l'eau. Il peut être choisi dans le groupe des polymères synthétiques ou naturels hydrophiles dénommés super-désintégrant. 4 The rapid disintegrating agent or the mixture of fast disintegrating agents is the agent which makes it possible to obtain the disintegration of the solid according to the invention in water. It can be chosen from the group of synthetic or natural hydrophilic polymers called super-disintegrants. 4
Il est choisi parmi la carboxyméthylcellulose sodique réticulée et ses dérivés désigr^ dans le métier par le terme croscarmellose, le carboxyméthylamidon et son sel de sodium, la crospovidone soluble et leurs mélanges. Ce composé est ici introduit dans le but de conférer une désagrégation rapide au comprimé ou solide selon l'invention, tout en maintenant une cohésion suffisante. Des agents de désagrégation effervescents peuvent être aussi utilisés. Ces derniers sont basés sur le mélange d'un acide et d'un carbonate alcalin. It is selected from crosslinked sodium carboxymethylcellulose and its derivatives are unsaturated by the term croscarmellose, carboxymethyl starch and its sodium salt, soluble crospovidone and mixtures thereof. This compound is here introduced in order to confer a rapid disintegration tablet or solid according to the invention, while maintaining sufficient cohesion. Effervescent disintegrating agents can also be used. These are based on the mixture of an acid and an alkaline carbonate.
Les acides organiques du couple effervescent susceptibles d'être utilisés dans le cadre de la présente invention sont des composés capables de réagir avec les carbonates alcalins pour provoquer un dégagement de dioxyde de carbone, quand ils sont mis en contact avec l'eau. Des acides convenables sont par exemple l'acide citrique, l'acide fumarique, l'acide adipique, l'acide tartrique, l'acide malique, l'acide succinique, l'acide phosphorique ainsi que des mélanges de ces composés. L'acide préféré selon l'invention est l'acide citrique.  The organic acids of the effervescent couple that may be used in the context of the present invention are compounds capable of reacting with alkaline carbonates to cause a release of carbon dioxide, when they are brought into contact with water. Suitable acids are, for example, citric acid, fumaric acid, adipic acid, tartaric acid, malic acid, succinic acid, phosphoric acid and mixtures of these compounds. The preferred acid according to the invention is citric acid.
Un carbonate alcalin susceptible d'être utilisé dans le cadre de la présente invention est par exemple le bicarbonate de sodium, le bicarbonate de potassium, la carboxylysine, le carbonate de calcium, le carbonate de sodium, le carbonate de potassium, le carbonate de magnésium, ainsi que des mélanges de ces composés. Avantageusement, on utilisera le bicarbonate de sodium. Avantageusement le rapport en poids du couple acide/carbonate varie de 1/3 à 3/1. Tous ces agents de désagrégation peuvent aussi être utilisés en mélange.  An alkali carbonate that may be used in the context of the present invention is, for example, sodium bicarbonate, potassium bicarbonate, carboxylysine, calcium carbonate, sodium carbonate, potassium carbonate and magnesium carbonate. as well as mixtures of these compounds. Advantageously, use sodium bicarbonate. Advantageously, the weight ratio of the acid / carbonate pair varies from 1/3 to 3/1. All these disintegrating agents can also be used in a mixture.
La forme solide selon l'invention peut aussi comprendre un ou des agents déshydratants afin d'améliorer la stabilité physique dans le temps. Le déshydratant interne a pour fonction de piéger les traces d'eau susceptibles d'apparaître éventuellement dans le comprimé.  The solid form according to the invention may also comprise one or more dehydrating agents in order to improve the physical stability over time. The internal desiccant has the function of trapping traces of water likely to appear in the tablet.
Pour améliorer la stabilité de certains composés, il peut être nécessaire d'ajouter à la composition des antioxydants. Selon une caractéristique particulière de l'invention, l'agent antioxydant précité est choisi parmi l'alpha-tocophérol, le gamma- tocophérol, le delta- tocophérol, les extraits d'origine naturelle riches en tocophérol, l'acide ascorbique et ses sels de sodium ou de calcium, l'acide palmityl DL ascorbique, le gallate de propyle, le gallate d'octyle, le gallate de dodécyle, le gallate de butyl-hydroxy anisole (BHA) et le gallate de butyl-hydroxy toluène (BHT). Selon une autre caractéristique particulière de l'invention, le déshydratant interne est le citrate de magnésium.  To improve the stability of certain compounds, it may be necessary to add antioxidants to the composition. According to one particular characteristic of the invention, the abovementioned antioxidant agent is chosen from alpha-tocopherol, gamma-tocopherol, delta-tocopherol, natural extracts rich in tocopherol, ascorbic acid and its salts. sodium or calcium, Ascorbic DL palmityl, propyl gallate, octyl gallate, dodecyl gallate, butyl-hydroxy anisole gallate (BHA) and butyl-hydroxy toluene gallate (BHT) . According to another particular characteristic of the invention, the internal desiccant is magnesium citrate.
Cependant, selon l'invention, l'agent désagrégeant seul, ne permet pas d'obtenir des propriétés de dissolution suffisamment rapide dans l'eau sans agitation continue. Nous avons découvert que l'association d'un agent de désagrégation à un agent soluble 5 permet d'obtenir l'effet recherché. Le rapport en poids entre l'agent désagrégeant et l'agent soluble peut aller de 1/30 à 25/1 . However, according to the invention, the disintegrating agent alone does not make it possible to obtain sufficiently rapid dissolution properties in water without continuous stirring. We have discovered that the combination of a disintegrating agent with a soluble agent 5 makes it possible to obtain the desired effect. The weight ratio between the disintegrating agent and the soluble agent can range from 1/30 to 25/1.
L'agent soluble encore appelé agent hydrosolubilisant, est un composé de poids moléculaire inférieur à 1000 daltons, ayant une solubilité dans l'eau supérieure à 50 grammes par litre d'eau à 25°C, comprenant au moins une fonction chimique parmi les hydroxyles, les acides carboxyliques, les aldéhydes, les aminés et leurs dérivés. De préférence un agent soluble est choisi dans la famille des glucides. Cet agent comprend au moins un oligoside et préférentiellement un diholoside ou un mélange de diholosides. A titre d'exemple le diholoside peut être le maltose, le sucrose, le thréalose, le mannose, le cellobiose ou le lactose.  The soluble agent, also called a water-solubilising agent, is a compound with a molecular weight of less than 1000 daltons, having a solubility in water of greater than 50 grams per liter of water at 25 ° C., comprising at least one chemical function among the hydroxyls , carboxylic acids, aldehydes, amines and their derivatives. Preferably a soluble agent is selected from the family of carbohydrates. This agent comprises at least one oligoside and preferably a diholoside or a mixture of diholosides. By way of example, the diholoside may be maltose, sucrose, threalose, mannose, cellobiose or lactose.
L'agent soluble peut de façon avantageuse être choisi parmi les polyols, les saccharides, les mono et disaccharides et les oligosaccharides. On peut citer à titre d'exemple, le glucose, le galactose, le mannitol, le xylitol, le sorbitol, le maltitol, le lactitol, l'isomaltitol, le glycérol, l'érythritol, l'arabitol, le ribitol, le volémitol. L'agent solubilisant peut aussi être un acide aminé choisi parmi les acides aminés hydrosolubles, par exemple l'alanine l'acide aspartique l'arginine l'asparagine, la cystéine, l'acide glutamique, la glutamine, la lysine, la leucine, l'isoleucine, la glycine, l'histidine, la méthionine, la phényalanine, la proline, la serine, la thréonine, le tryptophane, la tyrosine et la valine. On peut aussi utiliser des di ou triacides aminés, choisis parmi les précédents.  The soluble agent may advantageously be selected from polyols, saccharides, mono and disaccharides and oligosaccharides. By way of example, mention may be made of glucose, galactose, mannitol, xylitol, sorbitol, maltitol, lactitol, isomaltitol, glycerol, erythritol, arabitol, ribitol and volemitol. . The solubilizing agent may also be an amino acid chosen from water-soluble amino acids, for example alanine, aspartic acid, arginine, asparagine, cysteine, glutamic acid, glutamine, lysine, leucine, isoleucine, glycine, histidine, methionine, phenyalanine, proline, serine, threonine, tryptophan, tyrosine and valine. It is also possible to use aminated di or triacids chosen from the preceding ones.
De façon toute à fait inattendue nous avons découvert que l'utilisation d'un mélange de deux agents solubles, par exemple le lactose et le sucrose, permet de diminuer le temps de désagrégation et de dissolution de 20%.  Quite unexpectedly, we have discovered that the use of a mixture of two soluble agents, for example lactose and sucrose, makes it possible to reduce the disintegration and dissolution time by 20%.
Dans une forme préférentielle de l'invention, le solide compressé comprend :  In a preferred form of the invention, the compressed solid comprises:
- un ou des actifs de traitement des végétaux sous forme de poudre ou de micro-granules pouvant être enrobées  one or more plant treatment active agents in the form of powder or micro-granules which can be coated
- un agent ou un mélange d'agents de désagrégation rapide  an agent or a mixture of fast disintegrants
- deux agents solubles à dissolution rapide  - two soluble fast dissolving agents
- un agent de glissement.  - a slip agent.
De façon inattendue, nous avons découvert qu'il est nécessaire pour obtenir une amélioration de la vitesse de désagrégation, d'obtenir une homogénéité de mélange satisfaisante entre l'agent désagrégeant et l'agent soluble, comme indiqué à l'exemple n°8. Pour cela il est nécessaire d'utiliser un mélangeur à poudre et d'avoir une durée d'agitation supérieure à 5 minutes et préférentiellement supérieure à 10 minutes. Le mélangeur à poudre est préférentiellement choisi parmi les mélangeurs en V ou en Y bien connu de l'homme de l'art.  Unexpectedly, we have discovered that it is necessary to obtain an improvement in the disintegration rate, to obtain a satisfactory homogeneity of mixing between the disintegrating agent and the soluble agent, as indicated in Example No. 8 . For this it is necessary to use a powder mixer and have a stirring time greater than 5 minutes and preferably greater than 10 minutes. The powder mixer is preferably selected from V mixers or Y well known to those skilled in the art.
Selon un mode de réalisation avantageux de la forme solide conforme à l'invention, le mélange d'excipients comporte un ou un mélange d'agents tensioactifs 6 permettant de stabiliser la dispersion des composés hydrophobes dans la phase aqueuse. L'agent tensioactif est choisi préférentiellement parmi, les polysorbates, le sodium dodécylsulfate, le TRIS. On peut citer les esters de glycol comme le stéarate d'éthylène glycol, les esters de glycérol comme le stéarate de glycérol, les esters de polyoxyéthylèneglycol et d'acides gras, les esters de sorbitane, mais surtout les esters de sorbitane polyoxyéthyléniques, plus couramment appelés Tweens ou polysorbates. Les composés dérivés de l'acide naphtalénique et de ses sels peuvent aussi être utilisés ainsi que les phospholipides. La composition peut aussi comprendre des agents de charge pour moduler la densité, des colorants, des agents de modification de la viscosité de la formulation finale comme des dérivés de cellulose, des carbomères, des xanthanes, des dérivés de caroube, des amidons dérivés, des gélatines, des agars. According to an advantageous embodiment of the solid form according to the invention, the excipient mixture comprises one or a mixture of surfactants. 6 for stabilizing the dispersion of the hydrophobic compounds in the aqueous phase. The surfactant is preferably chosen from polysorbates, sodium dodecyl sulphate and TRIS. There may be mentioned glycol esters such as ethylene glycol stearate, glycerol esters such as glycerol stearate, polyoxyethylene glycol esters of fatty acids, sorbitan esters, but especially polyoxyethylene sorbitan esters, more commonly called Tweens or polysorbates. Compounds derived from naphthalenic acid and its salts can also be used as well as phospholipids. The composition may also include fillers for density modulating, colorants, viscosity modifiers of the final formulation such as cellulose derivatives, carbomers, xanthans, carob derivatives, derivatized starches, gelatins, agars.
A ces excipients constituant le solide selon l'invention, une ou plusieurs substances actives et/ou nutritives ou fertilisantes peuvent être ajoutées. Au titre de substance active, on peut utiliser au moins l'une de celles du groupe comprenant les produits phytosanitaires.  To these excipients constituting the solid according to the invention, one or more active and / or nutritive or fertilizing substances may be added. As an active substance, at least one of those in the group comprising phytosanitary products may be used.
On peut citer les insecticides destinés à lutter contre les insectes.  Insecticides for the control of insects may be mentioned.
Par exemple le groupe des organohalogénés. Parmi lesquels le dichlorodiphényltrichloroéthane et ses dérivés comme le tétrachlorodiphényléthane, le 2,2,2-trichloro-1 ,1-bis(4-chlorophényl)éthanol perthane, 2,2 bis-(paraméthoxy-phényl) 1 ,1 ,1-trichloroéthane , le groupe du gamma-hexachlorocyclohexane (HCH) et du benzène hexachloride (BHC), le groupe du octachloro-4,7-méthanohydroindane comme l'heptachlore, l'hexachlorodiméthanonaphtalène, l'exodiméthanonaphthalene, les bishomocubanes comme le chlordécone, le perchlordécone, et le diénochlore. Nous pouvons citer aussi les dérivé de l'essence de térébenthine comme l'endosulfan, le toxaphène, polychlorocamphène et les produits de chloration des terpènes, mais aussi les chlorophénols et les chlorsulfacides.  For example the group of organohalogens. Among which dichlorodiphenyltrichloroethane and its derivatives such as tetrachlorodiphenylethane, 2,2,2-trichloro-1,1-bis (4-chlorophenyl) ethanol perthane, 2,2-bis (paramethoxy-phenyl) 1,1,1-trichloroethane, the group of gamma-hexachlorocyclohexane (HCH) and benzene hexachloride (BHC), the group of octachloro-4,7-methanohydroindane such as heptachlor, hexachlorodimethanonaphthalene, exodimethanonaphthalene, bishomocubanes such as chlordecone, perchlordecone, and dienochlor. We can also mention the turpentine derivatives such as endosulfan, toxaphene, polychlorocamphene and the chlorination products of terpenes, but also chlorophenols and chlorsulfacids.
Le groupe des organophosphorés. On distingue trois groupes de pesticides organophosphorés. Le premier est constitué des organophosphorés à cycle phényl. De nombreux composés appartiennent à ce groupe comme le bromophos, le chlorfenvinphos, le fénitrothion, le fenthion, le fonofos, l'isofenphos, le parathion, le parathion éthyl, le parathion méthyl, le phosalone, le profénofos, le protiophos.  The group of organophosphorus compounds. There are three groups of organophosphorus pesticides. The first is organophosphorus phenyl ring. Many compounds belong to this group such as bromophos, chlorfenvinphos, fenitrothion, fenthion, fonofos, isofenphos, parathion, parathion ethyl, parathion methyl, phosalone, profenofos, protiophos.
Le deuxième groupe est constitué par les organophosphorés à hétérocycle comme le chlorpyrifos, te diazinon, l'étrimfos, l'isoxation, le quinalphos, le méthidation, le phosmet.  The second group consists of organophosphorus heterocycles such as chlorpyrifos, diazinon, etimimos, isoxation, quinalphos, methidation, phosmet.
Le troisième groupe est constitué par les organophosphorés aliphatiques, parmi lesquels on peut citer l'acéphate, le déméton, le dichlorvos, le dicrotophos, le diméthoate, 7 l'éthion, le formothion, le malathion, le mévinphos, le monocrotophos, le naled, l'ométhoate, le phorate, le phosphamidon et le trichlorfon. The third group consists of aliphatic organophosphorus compounds, among which mention may be made of acephate, demeton, dichlorvos, dicrotophos, dimethoate, Ethion, formothion, malathion, mevinphos, monocrotophos, naled, omethoate, phorate, phosphamidon and trichlorfon.
On peut citer comme principe actif insecticide les substances du groupe des carbamates comme le methyl carbamate de naphtyle, les méthyl et dimethyl carbamates à structure hétérocyclique, les méthyl carbamates à structure cyclique phényl et les méthyl carbamates à chaîne aiiphatique.  Mention may be made, as an insecticidal active ingredient, of substances of the carbamate group such as naphthyl methyl carbamate, methyl and dimethyl carbamates with a heterocyclic structure, methyl carbamates with a phenyl ring structure and aliphatic chain methyl carbamates.
Les pyréthrinoïdes naturels et de synthèse parmis lesquels on peut citer les composés suivants : bifenthrine, bioresméthrine, deltaméthrine, dépalléthrine, éthofenprox, fenpropathrine, cyperméthrine, fenvalérate, esfenvalérate, cyfluthrine, alphaméthrine, tralométhrine, fluvalinate, perméthrine, lambda-cyhalothrine, flucythrinate, téfluthrine, tralométhrine, zétacyperméthrine, bétacyfluthrine.  The natural and synthetic pyrethroids include the following compounds: bifenthrin, bioresmethrin, deltamethrin, depallethrin, ethofenprox, fenpropathrin, cypermethrin, fenvalerate, esfenvalerate, cyfluthrin, alphamethrin, tralomethrin, fluvalinate, permethrin, lambda-cyhalothrin, flucythrinate, tefluthrin , tralomethrin, zetacypermethrin, betacyfluthrin.
Les composés d'origine végétale comme la roténone, la nicotine, l'azadirine et les autres alcaloïdes dérivés, la quassine, la ryanodine, l'aconitine, les alcaloïdes diterpéniques estérifiés, le géraniol, et les globulines végétales.  Compounds of plant origin such as rotenone, nicotine, azadirine and other derived alkaloids, quassin, ryanodine, aconitine, esterified diterpenic alkaloids, geraniol, and plant globulins.
Les sulfones et sulfonates comme le 1 ,2,4-trichloro-5-(4- chlorophenyl)sulfonylbenzène, ou la propargite. Les formamidines sont caractérisés par la présence d'une structure -N=CH-N, on peut citer l'amitraze, le chlordimeform, et le formetanate.  Sulfones and sulfonates such as 1,2,4-trichloro-5- (4-chlorophenyl) sulfonylbenzene, or propargite. Formamidines are characterized by the presence of a structure -N = CH-N, mention may be made of amitraz, chlordimeform, and formetanate.
Comme deuxième grand groupe de substances actives, on peut aussi citer les fongicides destinés à éliminer les moisissures et les champignons parasites des plantes. Les fongicides les plus anciens sont le soufre, le cuivre et ses dérivés organiques comme la bouillie bordelaise qui est un mélange de sulfate de cuivre et d'hydroxyde de calcium. On distingue les fongicides de contact comme le zinèbe, le captane et les fongicides systématiques triadiméfon et la morpholine.  As the second major group of active substances, there may also be mentioned fungicides for removing mold and fungi parasitic plants. The oldest fungicides are sulfur, copper and its organic derivatives such as the Bordeaux mixture which is a mixture of copper sulphate and calcium hydroxide. Contact fungicides, such as zineb, captan and the systematic fungicides triadimefon and morpholine, are distinguished.
Le groupe des herbicides est le troisième grand groupe de substances actives pouvant être ajoutées. A titre d'exemple on peut citer les herbicides suivants. Les composés minéraux comme le cyanure de calcium (Ca(CN)2), sulfate de fer (FeS04), le chlorate de sodium (NaCI03). The herbicide group is the third major group of active substances that can be added. By way of example, mention may be made of the following herbicides. Mineral compounds such as calcium cyanide (Ca (CN) 2), iron sulphate (FeSO 4 ), sodium chlorate (NaClO 3).
Les herbicides organiques peuvent aussi être utilisés comme le glyphosate, les dinitroanilines ou toluidines et leurs dérivés parmi lesquels on peut citer la benfluraline, la butraline, la fluchloraline, la nitraline, l'on/saline, la pendiméthaline, trifluraline.  Organic herbicides can also be used such as glyphosate, dinitroanilines or toluidines and their derivatives including benfluralin, butraline, fluchloraline, nitraline, on / saline, pendimethalin, trifluralin.
Les urées substituées comme les chlortoluron, chloroxuron, cycluron, diuron, éthidimuron, fénuron, isoproturon, linuron, monolinuron, méthabenzthiazuron, métobromuron, métoxuron, monuron, thiazafluron, tebuthiuron, thiazafluron, siduron, et néburon. Les triazines atrazine, cyanazine, méthoprotryne, propazine, terbuthylazine, simazine, simetryne, secbumeton, secbumeton, terbuméton, amétryne, desmétryne, prométryne.terbutryne. Substituted ureas such as chlortoluron, chloroxuron, cycluron, diuron, ethidimuron, fenuron, isoproturon, linuron, monolinuron, methabenzthiazuron, metobromuron, metoxuron, monuron, thiazafluron, tebuthiuron, thiazafluron, siduron, and neburon. Triazines atrazine, cyanazine, methoprotrin, propazine, terbuthylazine, simazine, simetryne, secbumeton, secbumeton, terbumeton, amtreinne, desmétryne, prométryne.terbutryne.
Les imidazolinones comme l'imazaméthabenz, ou l'imazapyr.  Imidazolinones such as imazamethabenz, or imazapyr.
Les sulfonylurées comme l'amidosulfuron, le azimsulfuron, et le chlorsulfuron. Sulfonylureas such as amidosulfuron, azimsulfuron, and chlorsulfuron.
Les diphényls-éthers comme acifluorfène-sodium, l'aclonifen, le bifénox, le bromofénoxime, le chlométhoxyfène, le diclofop-méthyle, le fluorodifène, le fomesafen, le lactofène.le le nitrofène ou l'oxyfluorfène. Diphenyls-ethers such as acifluorfen-sodium, aclonifen, bifenox, bromofenoxime, chlomethoxyfene, diclofop-methyl, fluorodifen, fomesafen, lactofen, nitrofen or oxyfluorfen.
Les phytohormones de synthèse. On peut citer l'acide-indol-acétique ou IAA et ses dérivés, les acides phénoxyalcanoïques, comme le 2,4-D ou acide 2-(2,4 dichlorophénoxy) éthanoïque.le 2,4-MCPA, les triclopyr, diclofop-méthyl, 2,4,5-T, le 2,4- DP (dichlorprop), le MCPP (mécoprop), le 2,3,6-TBA, les dicamba, piclorame, clopyralid, et flurénol.  Synthetic phytohormones. Mention may be made of indol-acetic acid or IAA and its derivatives, phenoxyalkanoic acids, such as 2,4-D or 2- (2,4-dichlorophenoxy) ethanoic acid. 2,4-MCPA, triclopyr, diclofop methyl, 2,4,5-T, 2,4-DP (dichlorprop), MCPP (mecoprop), 2,3,6-TBA, dicamba, picloram, clopyralid, and flurenol.
Les colorants nitrés dérivés du phénol, le dinitrophénol, les dinitro-ortho-crésol, dinoterbe, pentachlorophenol.  Nitrate dyes derived from phenol, dinitrophenol, dinitro-ortho-cresol, dinoterb, pentachlorophenol.
Les carbamates parmi lesquels les dérivés de l'acide carbamique comprenant la structure -NH2-COOH comme l'asulame, le barbame, le chlorbufame, le chlorprophame, le prophame, le carbétamide. On peut citer les dérivés de l'acide thiocarbamique comme les butilate, cycloate, diallate, triallate, EPTC, molinate, prosulfocarbe, vernolate, pédulate, thiobencarbe. Les dérivés de l'acide dithiocarbamique métam-sodium, nabamequi empêchent la germination, les biscarbamates desmédiphame, phenmédiphame, karbutylate.  Carbamates including carbamic acid derivatives comprising the -NH 2 -COOH structure such as asulam, barbam, chlorbufam, chlorpropham, propham, carbetamide. Mention may be made of thiocarbamic acid derivatives such as butylate, cycloate, diallate, triallate, EPTC, molinate, prosulfocarb, vernolate, pedulate, thiobencarb. Derivatives of dithiocarbamic acid metam-sodium, nabame that prevent germination, biscarbamates desmedipham, phenmedipham, karbutylate.
Les ammoniums quaternaires oû Bipyridiles comme le diquat, le paraquat, et le difenzoquat. Le pinoxaden dont l'alloxydime-sodium et le clodinafop-propargyl.  Quaternary ammoniums or bipyridiles such as diquat, paraquat, and difenzoquat. Pinoxaden including alloxydim-sodium and clodinafop-propargyl.
A ces trois premières classes de composés actifs, les insecticides, les fongicides et les herbicides, nous pouvons bien sur ajouter les acaricides et les nematocides.  In these first three classes of active compounds, insecticides, fungicides and herbicides, we can of course add acaricides and nematocides.
La forme solide obtenue selon l'invention peut aussi contenir des composés assurant la nutrition des végétaux, ce sont les engrais ou les fertilisants. L'homme de l'art sait que les végétaux ont besoin d'apports en azote, en phosphore, en potassium et en oligoéléments, pour bénéficier d'une croissance optimale et d'une meilleure résistance aux agressions. Nous pourrons ajouter des éléments secondaires comme le calcium, le magnésium et le soufre.  The solid form obtained according to the invention may also contain compounds ensuring the nutrition of plants, they are fertilizers or fertilizers. Those skilled in the art know that plants need inputs of nitrogen, phosphorus, potassium and trace elements, to enjoy optimal growth and better resistance to aggression. We can add secondary elements such as calcium, magnesium and sulfur.
Dans les composés azotés on peut citer l'ammonitrate, le sulfate d'ammonium, l'urée, le nitrate de potassium, le nitrate de calcium, le nitrate de magnésium, le phosphate d'ammonium, le phosphate diammonium, les polyphosphate d'ammonium, l'ammonium sulfophosphate. L'azote peut aussi être apporté par des composés organiques comme les acides aminés, par exemple l'alanine, l'acide aspartique l'arginine 9 l'asparagine, la cystéine, l'acide glutamique, la glutamine, la lysine, la leucine, l'isoleucine la glycine, l'histidine, la methionine, la phényalanine, la proline, la sérine, la thréonine, le tryptophane, la tyrosine et la valine. In the nitrogen compounds, mention may be made of ammonium nitrate, ammonium sulphate, urea, potassium nitrate, calcium nitrate, magnesium nitrate, ammonium phosphate, diammonium phosphate, polyphosphates. ammonium, ammonium sulfophosphate. Nitrogen can also be provided by organic compounds such as amino acids, for example alanine, aspartic acid and arginine Asparagine, cysteine, glutamic acid, glutamine, lysine, leucine, isoleucine, glycine, histidine, methionine, phenyalanine, proline, serine, threonine, tryptophan, tyrosine and valine.
Dans les composes potassiques on peut citer le sulfate de potassium, le chlorure de potassium, l'oxyde de potasse.  Potassium compounds include potassium sulphate, potassium chloride, potassium oxide.
Dans les composés phosphorés, on distingue l'oxyde de phosphore, le phosphate bicalcique, le superphosphate simple, le superphosphate triple, le phosphate de magnésium, le phosphate naturel.  In the phosphorus compounds, phosphorus oxide, dicalcium phosphate, simple superphosphate, triple superphosphate, magnesium phosphate and natural phosphate are distinguished.
En plus des composés contenant le phosphate, l'azote, le potassium, le solide selon l'invention peut aussi contenir des nutriments ou éléments nutritifs, par exemple, le zinc, le cuivre, le manganèse, le bore, le calcium, le fer, le sulfate de calcium (gypse), le magnésium, le molybdène, les chlorures, le sélénium, le soufre ou des combinaisons de ceux-ci. A titre d'exemple illustratif mais nullement limitatif des exemples, le cuivre peut être du cuivre (cuivrique) sous forme : hydroxyde, chlorure, sulfate, oxyde, oxysulfate, nitrate, carbonate, carbonate d'ammonium, de chlorure cuivrique dihydraté, protéinate, l'acétate, le citrate, le chélate, complexé, ou piégé. Le zinc peut être de l'acétate de zinc, le chlorure d'ammonium, sulfate, oxyde, oxysulfate, nitrate, chlorure, citrate, un chélate ou un complexe piégé. Le manganèse peut être manganèse peut être sous forme : nitrate, chlorure, sulfate, oxyde, oxysulfate, acétate, carbonate anhydre de potassium, sulfate, mangagnese tétrahydraté, de l'acétate d'hexahydrate de nitrate, citrate, chélate ou un complexe séquestré. Le bore peut être l'acide borique, le borate de sodium, tétrahydraté tétraborate de potassium, le borate de calcium, le borate de sodium calcium, le borax, l'octoborate disodique tétrahydraté, l'acide orthoborique. Le calcium peut être du calcium: carbonate, chlorure, sulfate, du gypse, du borate de calcium, de la chaux, nitrate, phosphate, citrate, un chélate ou complexe séquestré. Le fer peut être le fer sous forme sulfate anhydre, sulfate, chlorure, tétrahydraté, hexahydrate, nitrate, nonahydrate de nitrate hexahydraté, chlorure, citrate d'ammonium, sulfate d'ammonium, chélaté, séquestré, protéinate ou complexes. Les formes préférées des oligoéléments sont sous forme complexée à l'EDTA.  In addition to the compounds containing the phosphate, nitrogen, potassium, the solid according to the invention may also contain nutrients or nutrients, for example, zinc, copper, manganese, boron, calcium, iron , calcium sulphate (gypsum), magnesium, molybdenum, chlorides, selenium, sulfur or combinations thereof. By way of illustrative but not limiting example of the examples, the copper may be copper (cupric) in the form: hydroxide, chloride, sulfate, oxide, oxysulphate, nitrate, carbonate, ammonium carbonate, cupric chloride dihydrate, proteinate, acetate, citrate, chelate, complexed, or trapped. The zinc may be zinc acetate, ammonium chloride, sulfate, oxide, oxysulfate, nitrate, chloride, citrate, chelate or a trapped complex. The manganese can be manganese can be in the form: nitrate, chloride, sulfate, oxide, oxysulfate, acetate, anhydrous potassium carbonate, sulfate, mangagnese tetrahydrate, nitrate hexahydrate acetate, citrate, chelate or sequestered complex. The boron may be boric acid, sodium borate, potassium tetrahydrate tetraborate, calcium borate, sodium calcium borate, borax, disodium octadate tetrahydrate, orthoboric acid. Calcium can be calcium: carbonate, chloride, sulfate, gypsum, calcium borate, lime, nitrate, phosphate, citrate, a chelate or sequestered complex. The iron may be iron in the form of anhydrous sulphate, sulphate, chloride, tetrahydrate, hexahydrate, nitrate, nitrate hexahydrate, chloride, ammonium citrate, ammonium sulphate, chelate, sequestered, proteinate or complexes. The preferred forms of the trace elements are in complexed form with EDTA.
Comme il sera apprécié par l'homme de l'art, d'autres nutriments ou des poudres nutritives peuvent être préparés de manière similaire. Comme cela sera évident pour l'homme de l'art, les différents nutriments peuvent être ajoutés à l'état de traces mais généralement de 0,1% à 90% en poids de la forme selon l'invention.  As will be appreciated by those skilled in the art, other nutrients or nutritional powders may be prepared in a similar manner. As will be apparent to those skilled in the art, the different nutrients may be added in trace amounts but generally from 0.1% to 90% by weight of the form of the invention.
Les composés azotés, phosphorés et potassiques ainsi que les nutriments et oligoéléments peuvent être obtenus dans différents types de déchets agricoles et industriels. On peut citer à titre d'exemples non limitatifs, les produits et sous produits d'origine végétale comme les résidus de pulpes de betteraves, de tournesol, de marc de 10 raisins, de farines ou tourteaux d'oléagineux, de coques, pulpe d'olive, vinasse de betterave, marc de café, extrait d'algue, de lombricompost, les poudres de plumes et d'os. Ils sont utilisés secs sous forme de poudre qui peut être ajoutée à la forme solide selon l'invention. Nitrogen, phosphorus and potassium compounds as well as nutrients and trace elements can be obtained in different types of agricultural and industrial waste. Non-limiting examples include products and by-products of vegetable origin, such as residues of beet pulp, sunflower pulp, marc 10 grapes, oilmeal flours or meals, hulls, olive pulp, beet vinasse, coffee grounds, seaweed extract, vermicompost, feather and bone powders. They are used dry in powder form which can be added to the solid form according to the invention.
L'objet solide comprimé, contenant une ou plusieurs substances actives, phytosanitaires et/ou nutritives ou fertilisantes, est enveloppée dans un film hydrosoluble. Il peut être contenu dans un système de distribution unitaire hermétique, permettant d'empêcher tout contact avec l'utilisateur comme celui décrit par exemple dans les brevets EP 0761563 et FR 2633260, ou même contenu dans un système de blister.  The compressed solid object, containing one or more active substances, phytosanitary and / or nutritive or fertilizing, is wrapped in a water-soluble film. It may be contained in a hermetic unitary distribution system, making it possible to prevent any contact with the user, such as that described, for example, in patents EP 0761563 and FR 2633260, or even contained in a blister system.
Ces films hydrosolubles, bien connus de l'homme de l'art, sont largement utilisés dans l'industrie et sont principalement constitués de matières naturelles, hémisynthétiques ou synthétiques. On peut citer à titre d'exemples les films de polyvinylalcool et ses dérivés, les films de méthylcellulose et ses dérivés, les carboxyméthylcellulose les alkyls et hydroxyalkylcellulose, les amidons modifiés, les polyvinylsethers, les dérivés polyéthyléniques, l'acide polyvinylsulfonique, les polyanhydrides, les dérivés de résines formaldéhyde, les polyacrylates et leurs dérivés. Le film pourra selon les besoins comprendre plusieurs épaisseurs. Dans une mise en forme préférentielle de l'invention, le film hydrosoluble est un film de polyvinylalcool ou de méthylcellulose.  These water-soluble films, well known to those skilled in the art, are widely used in industry and are mainly made of natural materials, semisynthetic or synthetic. Examples of polyvinylalcohol films and its derivatives, methylcellulose films and its derivatives, carboxymethylcellulose alkyls and hydroxyalkylcellulose, modified starches, polyvinylsethers, polyethylene derivatives, polyvinylsulfonic acid, polyanhydrides, derivatives of formaldehyde resins, polyacrylates and their derivatives. The film can according to the needs to include several thicknesses. In a preferred shaping of the invention, the water-soluble film is a polyvinyl alcohol or methylcellulose film.
L'homme de l'art choisira la composition du film en fonction de la composition du solide comprimé contenant le ou les actifs selon l'invention.  Those skilled in the art will choose the composition of the film according to the composition of the compressed solid containing the active agent (s) according to the invention.
Exemples  Examples
Les exemples suivants sont proposés simplement comme illustration de l'invention sans en limiter le cadre.  The following examples are provided merely as an illustration of the invention without limiting the scope thereof.
Exemple 1 : Préparation d'engrais pour rosier Example 1: Preparation of Rose Fertilizer
Mélange A : Dans un mélangeur à poudre de type en V, on mélange à 25 t/m pendant 15 minutes les composés suivants :  Mixture A: In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
Mannitol 100g  Mannitol 100g
Sucrose 150g  Sucrose 150g
Acide malique 30g  Malic acid 30g
Acide citrique 45g  Citric acid 45g
Hydrogénocarbonate de sodium 1 0g  Sodium hydrogen carbonate 1 0g
Talc 5g  Talc 5g
A ce mélange A on ajoute les produits suivant constituant le mélange B To this mixture A is added the following products constituting the mixture B
Sulfate d'ammonium 140g  Ammonium sulphate 140g
Urée 70g 11 Urea 70g 11
P205 15g P205 15g
Oxyde de potassium 42g  Potassium oxide 42g
Polyvinylpyrolidone 20g  Polyvinylpyrrolidone 20g
Stéarate de magnésium 3g  Magnesium stearate 3g
L'agitation est maintenue à 50 t/min pendant 10 minutes. On récupère ce mélange final sous forme de poudre d'engrais, prête à être utilisée pour la fabrication de tablettes de 3.9 g par compression à 40 Mpa.  Stirring is maintained at 50 rpm for 10 minutes. This final mixture is recovered in the form of a fertilizer powder, ready to be used for the manufacture of tablets of 3.9 g by compression at 40 MPa.
Exemple 2 : Préparation de tablettes pour le traitement des plantes Example 2 Preparation of Tablets for the Treatment of Plants
On récupère le mélange selon l'exemple n°1 , sous forme de poudre d'engrais. Sur une comprimeuse alternative réglée pour une compression 40 Mpa nous réalisons le fabrication de tablettes de 3.9 g The mixture is recovered according to Example No. 1, in the form of a fertilizer powder. On an alternative tabletting machine set for a 40 MPa compression we realize the manufacture of tablets of 3.9 g
Exemple 3 : Préparation de tablettes pour la fertilisation des plantes et recouvertes d'un film hvdrosoluble Example 3 Preparation of Tablets for the Fertilization of Plants and Covered with a Water-Soluble Film
Les tablettes obtenues selon l'exemple 2, sont recouvertes d'un film thermoplastique de polyvinylalcool de 60 microns d'épaisseur par traitement en ensacheuse unitaire de type flowpack.  The tablets obtained according to Example 2, are covered with a thermoplastic film of polyvinyl alcohol 60 microns thick by treatment bagpacker unit type flowpack.
Exemple 4 : Préparation d'une solution aqueuse d'engrais par utilisation de tablettes hydrodispersibles de traitement de plantes et recouvertes de film hydrosoluble EXAMPLE 4 Preparation of an aqueous fertilizer solution by using water-dispersible treatment tablets of plants and coated with water-soluble film
Dans un arrosoir de 2 litres, on ajoute 1 litre d'eau. Puis on ajoute une tablette obtenue selon l'exemple 3. Le film se désagrège et libère la tablette en moins de 10 secondes. La tablette effervescente se désagrège sous l'action de l'eau et la dispersion des constituants est complète en moins de 45 secondes. La solution aqueuse d'engrais est prête à l'emploi. In a watering can of 2 liters, 1 liter of water is added. Then added a tablet obtained according to Example 3. The film disintegrates and releases the tablet in less than 10 seconds. The effervescent tablet disintegrates under the action of water and the dispersion of the constituents is complete in less than 45 seconds. The aqueous fertilizer solution is ready for use.
Exemple 5 : Préparation de tablettes d'engrais comprenant des oligoéléments Example 5 Preparation of fertilizer tablets comprising trace elements
Composition de tablettes d'engrais selon l'exemple 3 dans laquelle nous ajoutons les oligoéléments suivants : Composition of fertilizer tablets according to Example 3 in which we add the following trace elements:
Bore 10 mg  Boron 10 mg
Cuivre EDTA 20 mg  Copper EDTA 20 mg
Fer EDTA 50 mg  Iron EDTA 50 mg
Mn EDTA 50 mg  Mn EDTA 50 mg
Mo 1 mg  Mo 1 mg
Zn EDTA 20 mg 12 Zn EDTA 20 mg 12
Exemple 6 : Préparation de tablettes recouvertes d'un film hvdrosoluble contenant une composition insecticide Example 6 Preparation of Shelves Covered with a Water-Resistant Film Containing an Insecticide Composition
Nous reprenons le protocole de décrit à l'exemple n°1  We resume the protocol of described in example n ° 1
Mélange A : Dans un mélangeur à poudre de type en V, on mélange à 25 t/m pendant 15 minutes les composés suivanst :  Mixture A: In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
Mannitol 25g  Mannitol 25g
sorbitol 10g  sorbitol 10g
Acide citrique 65g  Citric acid 65g
Hydrogénocarbonate de sodium 106 g  Sodium hydrogen carbonate 106 g
Talc 5g  Talc 5g
A ce mélange A on ajoute les produits suivant constituant le mélange B To this mixture A is added the following products constituting the mixture B
Bifenthrine 2g  Bifenthrine 2g
Polyvinylpyrolidone 20g  Polyvinylpyrrolidone 20g
Silice pyrogénée hydrophile 12g  Hydrophilic pyrogenic silica 12g
Stéarate de magnésium 2g  Magnesium stearate 2g
L'agitation est maintenue à 50 t/min pendant 10 minutes. La poudre de pesticide récupée est prête à être utilisée pour la fabrication de tablettes comprimées obtenues selon l'exemple n°3. On obtient des tablettes dosées à 0.02g de Bifenthrine permettant chacune de préparer 1 litre de solution aqueuse. Stirring is maintained at 50 rpm for 10 minutes. The recovered pesticide powder is ready to be used for the manufacture of compressed tablets obtained according to Example No. 3. Tablets dosed with 0.02 g of Bifenthrin are obtained, each making it possible to prepare 1 liter of aqueous solution.
Exemple 7 Préparation d'une Tablette recouverte d'un film hvdrosoluble contenant une composition herbicide Example 7 Preparation of a Tablet Covered with a Water-Resistant Film Containing a Herbicidal Composition
Mélange A : Dans un mélangeur à poudre de type en V, on mélange à 25 t/m pendant 15 minutes les composés suivants :  Mixture A: In a V-type powder mixer, the following compounds are mixed at 25 rpm for 15 minutes:
Mannitol 25g  Mannitol 25g
sorbitol 10g  sorbitol 10g
Acide citrique 45g  Citric acid 45g
Hydrogénocarbonate de sodium 95 g  Sodium hydrogen carbonate 95 g
Talc 5g  Talc 5g
A ce mélange A on ajoute les produits suivants constituant le mélange B  To this mixture A is added the following products constituting the mixture B
Dicamba sel de sodium et potassium 30g  Dicamba sodium salt and potassium 30g
Polyvinylpyrolidone 20g  Polyvinylpyrrolidone 20g
Silice pyrogénée hydrophile 12g  Hydrophilic pyrogenic silica 12g
Stéarate de magnésium 2g  Magnesium stearate 2g
L'agitation est maintenue à 50 t/min pendant 10 minutes. La poudre de pesticide récupérée est prête à être utilisée pour la fabrication de tablettes comprimées obtenues 13 Stirring is maintained at 50 rpm for 10 minutes. The recovered pesticide powder is ready to be used for the manufacture of compressed tablets obtained 13
selon la procédure de l'exemple n°3. On obtient des tablettes pesant 2,36 g dosées à 0.3 g de Dicamba permettant chacune de préparer 1 litre de solution aqueuse. according to the procedure of Example No. 3. Tablets weighing 2.36 g are obtained, dosed with 0.3 g of Dicamba, each of which makes it possible to prepare 1 liter of aqueous solution.
Exemple 8 : Vitesse de dispersion dans l'eau Example 8: Dispersion rate in water
On reprend une tablette selon l'exemple 4 dans laquelle le mélange A des agents solubles le mannitol et le sucrose avec les agents de désagrégation rapide l'acide malique, l'acide citrique et l'hydrogénocarbonate de sodium, n'a pas été réalisé préalablement. Using a tablet according to Example 4 in which the mixture A soluble agents mannitol and sucrose with the fast disintegrating agents malic acid, citric acid and sodium hydrogencarbonate, was not realized previously.
La durée de désagrégation complète selon l'exemple 3 passe de 45 secondes à 52 secondes.  The complete disintegration time according to Example 3 goes from 45 seconds to 52 seconds.

Claims

14 14
REVENDICATIONS
1) Traitement pour végétaux sous forme solide protégée à dispersion et/dissolution ultra-rapide dans l'eau permettant d'obtenir une préparation aqueuses pré-dosée tout en supprimant le contact de l'utilisateur avec les actifs et caractérisé en ce qu'il comprend au moins : 1) Plant treatment in solid form protected dispersion and / ultra-fast dissolution in water to obtain a pre-metered aqueous preparation while removing the contact of the user with the assets and characterized in that it includes at least:
- un actif ou un mélange d'actifs de traitement des végétaux sous forme de poudre ou de micro-granules pouvant être enrobées  an active ingredient or a mixture of plant treatment active agents in the form of powder or micro-granules which can be coated
- un agent ou un mélange d'agents de désagrégation rapide  an agent or a mixture of fast disintegrants
- un mélange de deux agents solubles à dissolution rapide de poids moléculaire inférieur à 1000 daltons  a mixture of two fast-dissolving soluble agents of molecular weight less than 1000 daltons
- un agent de glissement  - a slip agent
- un film hydrosoluble entourant le solide  a water-soluble film surrounding the solid
et que la masse du solide soit comprise entre 0.1 et 100 grammes. and that the mass of the solid is between 0.1 and 100 grams.
2) Traitement pour végétaux selon la revendication n°1 dans lequel l'agent de désagrégation rapide est un mélange effervescent au contact de l'eau, constitué d'un acide et d'un carbonate ou d'hydrogénocarbonate ou de leurs sels de métal alcalin ou alcalino-terreux ou ammonium ou organo-ammonium ou potassium ou sodium et l'agent de glissement est du talc 2) Plant treatment according to claim 1 wherein the rapid disintegrating agent is an effervescent mixture in contact with water, consisting of an acid and a carbonate or hydrogencarbonate or their metal salts alkaline or alkaline earth or ammonium or organoammonium or potassium or sodium and the slip agent is talc
3) Traitement pour végétaux selon les revendications n°1 et n°2, dans lequel l'agent de désagrégation rapide est un mélange effervescent constitué d'acide citrique et d'hydrogénocarbonate de sodium  3) Plant treatment according to claims 1 and 2, wherein the fast disintegrant is an effervescent mixture of citric acid and sodium hydrogencarbonate
4) Traitement pour végétaux selon l'une quelconque des revendications 1 à 3 caractérisé en ce que le ou les agents désagrégeants et le ou les agents solubles sont mélangés ensemble préalablement en mélangeur à poudre pendant une durée au moins égale à 10 minutes avant d'être ajoutés aux autres composants.  4) Treatment for plants according to any one of claims 1 to 3 characterized in that the disintegrating agent (s) and the soluble agent (s) are mixed together beforehand in a powder mixer for a duration at least equal to 10 minutes before to be added to the other components.
5) Traitement pour végétaux selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'un agent soluble est choisi parmi un oligoside, un diholoside, un mélange de diholosides, les saccharides, les mono et disaccharides, les oligosaccharides, le glucose, le galactose le maltose, le sucrose, le thréalose, le lactose.  5) Treatment for plants according to any one of claims 1 to 4, characterized in that a soluble agent is selected from an oligoside, a diholoside, a mixture of diholosides, saccharides, mono and disaccharides, oligosaccharides, glucose, galactose, maltose, sucrose, threalose, lactose.
6) Traitement pour végétaux selon l'une des revendications 1 à 5 caractérisée en ce qu'un des deux agent solubles est choisi parmi les polyols, le mannitol, le xylitol, le sorbitol, le maltitol, le lactitol, l'isomaltitol, le glycerol, l'erythritol, l'arabitol, le ribitol, le volemitol 15 6) Treatment for plants according to one of claims 1 to 5 characterized in that one of the two soluble agent is chosen from polyols, mannitol, xylitol, sorbitol, maltitol, lactitol, isomaltitol, glycerol, erythritol, arabitol, ribitol, volemitol 15
7) Traitement pour végétaux selon l'une quelconque des revendications 1 à 6 caractérisé en ce que l'actif qu'il contient est un actif ou un mélange d'actifs phytosanitaires choisis parmi les composés herbicides, insecticides, fongicides, nématocides, antibactériens, répulsifs et anti-mousse. 7) Treatment for plants according to any one of claims 1 to 6 characterized in that the asset it contains is an active ingredient or a mixture of phytosanitary active ingredients selected from herbicides, insecticides, fungicides, nematocides, antibacterials, repellents and antifoam.
8) Traitement pour végétaux selon l'une quelconque des revendications 1 à 7, caractérisé en ce qu'il contient un engrais et un actif ou un mélange d'actifs phytosanitaires choisis parmi les composés herbicides, insecticides, fongicides, nématocides, antibactériens, répulsifs et anti-mousse et que le film hydrosoluble est en polyvinylacool.  8) Treatment for plants according to any one of claims 1 to 7, characterized in that it contains a fertilizer and an active or a mixture of phytosanitary active ingredients selected from herbicides, insecticides, fungicides, nematocides, antibacterials, repellents and antifoam and that the water-soluble film is polyvinylacool.
9) Traitement pour végétaux selon l'une quelconque des revendications 1 à 8 caractérisé en ce que cette forme solide est protégée dans un film hydrosoluble de PVA et/ou un système de distribution unitaire hermétique.  9) Treatment for plants according to any one of claims 1 to 8 characterized in that this solid form is protected in a water-soluble PVA film and / or hermetic unitary distribution system.
PCT/FR2013/000336 2012-12-14 2013-12-12 Quick-dissolving treatment for plants in protected solid form WO2014091095A1 (en)

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FR1203403A FR2999384A1 (en) 2012-12-14 2012-12-14 TREATMENT FOR VEGETALS IN SOLID FORM PROTECTED WITH RAPID DISSOLUTION
FR12/03403 2012-12-14

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US20210323887A1 (en) * 2020-04-15 2021-10-21 Innovations for World Nutrition, LLC Plant growth enhancer using carbon dioxide to increase plant yield and method of increasing plant yield
WO2022137226A1 (en) * 2020-12-22 2022-06-30 Deshen Hazphon Active dissolving fertilizer tablets
US11787749B2 (en) 2020-04-15 2023-10-17 Innovations for World Nutrition, LLC Fertilizer and plant growth promoter to increase plant yield and method of increasing plant yield

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US11634366B2 (en) * 2020-04-15 2023-04-25 Innovations for World Nutrition, LLC Plant growth enhancer using carbon dioxide to increase plant yield and method of increasing plant yield
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