阅读说明：本技术 一种具有改善的稳定性的油分散组合物 (Oil dispersion composition with improved stability ) 是由 罗昌炎 詹姆斯.T.布里斯托 于 2020-06-02 设计创作，主要内容包括：本发明提供一种具有改善的稳定性的油分散组合物,其含有非极性有机溶剂、脂肪醇乙氧基化丙氧基化物、分散的农业化学活性物以及至少一种表面活性剂。本发明通过在油分散组合物中添加脂肪醇乙氧基化丙氧基化物,其能够使得农业化学活性物在非极性有机溶剂中稳定以防止发生颗粒聚集从而导致发生沉降的现象。(The present invention provides an oil dispersion composition with improved stability comprising a non-polar organic solvent, a fatty alcohol ethoxylated propoxylate, a dispersed agrochemical active and at least one surfactant. The present invention enables the agrochemical active to be stabilized in a non-polar organic solvent by adding a fatty alcohol ethoxylated propoxylate to an oil dispersion composition to prevent the occurrence of particle agglomeration leading to settling.)

1. Oil dispersion composition with improved stability, characterized in that it contains the following components:

(a) a nonpolar organic solvent in an amount of 200g/L to 800g/L relative to the weight of the oil-dispersed composition;

(b) a fatty alcohol ethoxylated propoxylate of from 5g/L to 150g/L by weight of the oil dispersion composition;

(c) a dispersed agrochemical active which is from 1g/L to 300g/L by weight of the oil dispersion composition;

(d) at least one surfactant in an amount of 1g/L to 300g/L relative to the weight of the oil dispersion composition.

2. Oil dispersion composition according to claim 1, wherein the weight ratio of fatty alcohol ethoxylated propoxylate to agrochemical active is from 150:1 to 1:60, preferably from 50:1 to 1:10, more preferably from 10:1 to 1: 5.

3. Oil dispersion composition according to claim 1, wherein the non-polar organic solvent is any one or a mixture of at least two of aromatic hydrocarbons, aliphatic hydrocarbons, vegetable oils or vegetable oil esterifiers.

4. Oil dispersion composition according to claim 1, characterised in that the fatty alcohol ethoxylated propoxylate is a C2-C20 fatty alcohol ethoxylated propoxylate having a number average molecular weight of 100-1,000,000, preferably a C4-C16 fatty alcohol ethoxylated propoxylate having a number average molecular weight of 200-100,000.

5. An oil dispersion composition according to claim 1, wherein the agrochemical active comprises at least one herbicide selected from: sulfonamides, sulfonylureas, and derivatives thereof.

6. Oil dispersion composition according to claim 5, wherein the herbicide is selected from at least one of the following: tribenuron-methyl, metsulfuron-methyl, thifensulfuron-methyl, flazasulfuron-methyl, iodosulfuron-methyl, rimsulfuron, nicosulfuron, cinosulfuron, bensulfuron-methyl, trifloxysulfuron, foramsulfuron, mesosulfuron-methyl, flucarbazone-methyl, metosulam, cloransulam-methyl, florasulam, flumetsulam, penoxsulam, pyroxsulam or diflufenican.

7. Oil dispersion composition according to claim 1, wherein the agrochemical active has a solubility in the non-polar organic solvent of less than 10g/L, preferably less than 5g/L, more preferably less than 1 g/L.

8. Oil dispersion composition according to claim 1, characterized in that it may further comprise a non-sulphonamide or sulphonylurea herbicide or herbicide safener dispersed or dissolved in the non-polar organic solvent.

9. The oil dispersion composition of claim 8, wherein the non-sulfonamide or sulfonylurea herbicide comprises any one or a mixture of at least two of clodinafop-propargyl, cyhalofop-butyl, fenoxaprop-ethyl, acetochlor, pretilachlor, metolachlor, fluroxypyr-meptyl, quizalofop-p-ethyl, picloram, quinclorac, pendimethalin, 2,4-D, mesotrione, pretilachlor, quizalofop-p-ethyl, butachlor, atrazine, metribuzin, pinoxaden or topramezone.

10. The oil dispersion composition of claim 8, wherein the herbicidal safener comprises any one or a mixture of at least two of cloquintocet-mexyl, benoxacor, oxabetrinil, isoxadifen-ethyl, mefenpyr-diethyl, or oxabetrinil.

11. The oil dispersion composition of claim 1, wherein the surfactant comprises at least one of an emulsifier, a dispersant, a wetting agent, an anti-foaming agent, a pH adjuster, a thickener, or a preservative.

12. A process for preparing an oil dispersion composition according to claim 1, comprising the steps of:

step 1: adding the agricultural chemical active substance and the surfactant into the nonpolar organic solvent, and stirring to be uniform;

step 2: fully grinding the mixture obtained in the step 1 to obtain an oil-based concentrated solution;

and step 3: adding the fatty alcohol ethoxylate into the oil-based concentrated solution in proportion, and stirring until the mixture is uniformly mixed to obtain the oil dispersion composition.

13. The method according to claim 12, wherein the grinding of step 2 is performed at a temperature of 0-50 ℃, preferably 15-45 ℃.

14. The method of claim 12, wherein the grinding of step 2 results in a particle size of D50 ≤ 5 μm, preferably D50 ≤ 3 μm.

15. A method of preventing the mutual aggregation of suspended particles of a sulfanilamide or sulfonylurea herbicidal active in an agricultural oil dispersion composition, comprising adding a sufficient amount of a fatty alcohol ethoxylated propoxylate to reduce the mutual aggregation of suspended particles of a sulfanilamide or sulfonylurea herbicidal active; the fatty alcohol ethoxylated propoxylate is selected from the group consisting of C2-C20 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 100-1,000,000, preferably C4-C16 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 200-100,000;

preferably, the sufficient amount of fatty alcohol ethoxylated propoxylate and sulfonamide or sulfonylurea herbicidal active is in a weight ratio of 150:1 to 1:60, preferably 50:1 to 1:10, more preferably 10:1 to 1: 5.

16. Use of a fatty alcohol ethoxylated propoxylate to inhibit or prevent aggregation of suspended particles of a sulfonamide or sulfonylurea herbicidal active in an oil-dispersed composition of claim 1 wherein the fatty alcohol ethoxylated propoxylate is selected from the group consisting of a C2-C20 fatty alcohol ethoxylated propoxylate having a number average molecular weight of 100-100,000,000, preferably a C4-C16 fatty alcohol ethoxylated propoxylate having a number average molecular weight of 200-100,000; the weight ratio of the fatty alcohol ethoxylated propoxylate to the sulfonamide or sulfonylurea herbicidal active is from 150:1 to 1:60, preferably from 50:1 to 1:10, more preferably from 10:1 to 1: 5.

17. A method for controlling harmful bio-organisms, which comprises applying the oil-dispersed composition according to any one of claims 1 to 11 to a place where harmful bio-organisms are grown.

18. A control method according to claim 17, characterized in that the oil dispersion composition is used in the form of a water spray dilution at the time of application.

19. A method of controlling according to claim 17 or 18, characterized in that the oil-dispersed composition contains a sulfanilamide or sulfonylurea herbicidal active to control the growth of harmful weeds.

Technical Field

The invention belongs to the technical field of agricultural chemistry, and particularly relates to an oil dispersion composition with improved stability and application of fatty alcohol ethoxylated propoxylate in controlling aggregation of suspended particles of an agricultural oil dispersion preparation composition, in particular to a stable agricultural chemical oil dispersion formed by inhibiting or preventing mutual aggregation of particles of an amide or sulfonylurea herbicide in the oil dispersion composition by using C2-C20 fatty alcohol ethoxylated propoxylate.

Background

Agricultural formulation products must be physically and chemically stable over a specified period of time in order to be commercially useful. However, there are a number of destabilizing factors such as active instability, phase separation and environmental factors. In today's agrochemical market, it is increasingly common to develop new formulations containing multiple actives and their required solvents, safeners and/or adjuvants etc. to achieve optimal spectrum, efficacy and delivery efficiency, which makes formulation stability increasingly challenging. Thus, techniques that can effectively isolate, interfere with, or eliminate adverse reactions or interactions between incompatible ingredients are often very important for successful products.

Agrochemical compositions such as herbicides, insecticides or fungicides or herbicidal safeners can rarely be used as they are originally manufactured. Agrochemicals are generally composed of two parts, namely the active and adjuvant components or inert ingredients, which are combined together in the formulation. Combining these two parts into the final product takes into account two main goals: firstly to maintain the stability of the product during storage and secondly to provide an easy and efficient way of spray application to the area to be treated after dilution of the product in a carrier such as water or oil.

Agrochemical formulations are generally designed based on the needs of the customer and the physicochemical properties of the active (e.g., solubility of the active ingredient in water or other non-aqueous solvents). There are mainly two main formulation categories, namely solid formulations and liquid formulations. Liquid formulations are generally preferred by the customer due to ease of handling in metering, pumping, diluting and spraying operations.

Oil Dispersions (OD) are a type of liquid formulation and are defined as stable suspensions of actives in water immiscible solvents, which may contain other dissolved actives and are intended to be diluted with water prior to use. Recently, oil dispersion formulations have become more important in current formulation research. As oil dispersion formulations are well suited for use in the following cases: (1) water sensitive actives, such as sulfonylurea herbicides, are highly susceptible to hydrolytic degradation, (2) compatibility issues with the active mixture, and (3) the need for intramolecular adjuvants (build-in adjuvant).

It is known that agricultural oil dispersions belong to thermodynamically unstable systems and more or less undergo sedimentation. The speed of sedimentation accords with the Stokes sedimentation speed theory w ═ 2g (rho)_s-ρ)gr²9 μ, formula (la): rho_sIs the particle density; ρ is the density of water; mu is the fluid viscosity; r is the particle radius; g is the acceleration of gravity. The addition of a fluid modifier to agricultural oil dispersion formulations is generally done to adjust the viscosity of the oil dispersion fluid to provide physical stability to the formulation. Various substances have been used as fluidics modifiers to stabilize oil dispersion against sedimentation, such as clays, organoclays, hydrophilic and hydrophobic silicas, xanthan gums, polyamides, polyvinylpyrrolidone, polyacrylates, and the like. From theoretical formula, it is known that the size of suspended particles in oil dispersion is also an important factor influencing sedimentation rate, and the growth of particle size of suspended particles during storage is another reason that the accelerated sedimentation influences physical stability of the preparation. There are generally two conditions for the particle size growth of the suspended particles, namely Ostwald ripening of the active by more or less dissolution of the active by polar solvents, and particle-to-particle agglomeration due to incompatibility between the active and adjuvants, solvents, surfactants, co-formulation components.

It is also reported in the current patent for controlling sedimentation delamination and particle growth of oil dispersions that the main protection in CN103118536A is to use a combination of clay or silica type rheology modifier and a polymer or oligomer capable of forming hydrogen bonds, preferably a combination of clay or silica type rheology modifier and polyethylene glycol or polypropylene glycol, to stabilize the oil dispersion against sedimentation delamination of particles. In CN107484767A, fatty acid ester solvent is selected as the dispersed phase of spirotetramat particles, and Ostwald ripening of suspended particles is reduced or inhibited, so as to control particle size growth and stabilize oil dispersion. However, to date, no relevant art has disclosed how to avoid the phenomenon of particles aggregating with each other in oil dispersions.

Disclosure of Invention

In order to solve the above technical problems, the present invention provides an oil dispersion composition having improved stability, in which suspended particles of an oil dispersion are relatively stable during long storage, are not aggregated and bound to each other, and the physical stability of the oil dispersion composition is significantly improved. The improvement is achieved by the addition of a specific fatty alcohol ethoxylated propoxylate. The present inventors have surprisingly found that these compounds with fatty alcohol ethoxylated propoxylates can significantly control the phenomenon of suspended particles aggregating with each other in oil dispersions.

In order to achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the present invention provides an oil dispersion composition with improved stability comprising the following components:

(a) a nonpolar organic solvent in an amount of 200g/L to 800g/L relative to the weight of the oil-dispersed composition;

(b) a fatty alcohol ethoxylated propoxylate of from 5g/L to 150g/L by weight of the oil dispersion composition;

(c) a dispersed agrochemical active which is from 1g/L to 300g/L by weight of the oil dispersion composition;

(d) at least one surfactant in an amount of 1g/L to 300g/L relative to the weight of the oil dispersion composition.

In the present invention, the weight ratio of the fatty alcohol ethoxylated propoxylate to the agrochemical active is from 150:1 to 1:60, such as 150:1, 120:1, 100:1, 80:1, 65:1, 50:1, 45:1, 30:1, 20:1, 10:1, 5:1, 2:1, 1:2, 1:5, 1:10, 1:20, 1:30, 1:40, 1:50, 1:55, 1:60, preferably from 50:1 to 1:10, more preferably from 10:1 to 1: 5.

The non-polar organic solvent used in the present invention is preferably one or more non-water miscible non-polar solvents, typically less than 0.5% by weight soluble in water, including one or more petroleum distillates such as aromatic hydrocarbons derived from benzene, e.g. toluene, xylene, mesitylene and the like, aliphatic hydrocarbons such as hexane, octane, cyclohexane and the like, vegetable, seed or animal oils such as soybean oil, rapeseed oil, olive oil, castor oil, sunflower oil, coconut oil, corn oil, cottonseed oil, linseed oil, palm oil, peanut oil, safflower oil, sesame oil and the like, and C1-C6 esters of vegetable or animal oils such as methyl oleate, epoxidized soybean oil, methyl palmitate, ethyl ricinoleate, C1-C6 alkyl esters of C6-C20 saturated and unsaturated aliphatic carboxylic acids.

Strongly polar organic solvents are not preferred in the present invention, and for example, ethers such as tetrahydrofuran and the like, alkylene glycol dialkyl ethers such as ethylene glycol diethyl ether and the like, amides such as dimethylacetamide or N-methylpyrrolidone and the like, ketones such as methylethylketone and the like, nitriles such as butyronitrile and the like, sulfoxides or sulfones such as dimethylsulfoxide or sulfolane and the like, and alkylene carbonates such as propylene carbonate or butyl carbonate and the like are exemplified. These strongly polar organic solvents have good solubility properties and have a certain solubility for most agricultural actives, such as sulfonamides and sulfonylurea herbicides. Active particles dispersed in such strongly polar organic solvents are prone to Ostwald ripening. Protic solvents, such as water, alcohols, polymeric polyols, may sometimes be incompatible with some of the active ingredients present in the oil dispersion formulation or the herbicidal safeners. In particular, some sulfonylurea herbicides have a degradation phenomenon by hydrolysis through cleavage at the sulfonylurea bridge in the presence of water. None of the above classes of organic solvents are selected for use in the present invention.

The non-polar organic solvent in the present invention is 200g/L to 800g/L, for example, 200g/L, 250g/L, 300g/L, 350g/L, 400g/L, 450g/L, 500g/L, 550g/L, 600g/L, 650g/L, 700g/L, 750g/L or 800g/L, preferably 300g/L to 750g/L, relative to the weight of the oil-dispersible composition.

The fatty alcohol ethoxylation propoxylate is an ether formed by copolymerizing saturated and/or unsaturated straight chain and/or branched chain monohydric alcohol with ethylene glycol and propylene glycol according to a certain molar ratio, wherein the fatty alcohol is selected from C2-C20 alcohol, such as C2, C6, C8, C9, C11, C14, C16 or C20, preferably C4-C16 saturated monohydric alcohol; the fatty alcohol ethoxylated propoxylate has a number average molecular weight in the range of 100-.

The fatty alcohol ethoxylated propoxylate of the present invention may be specifically selected from the group consisting of those sold under the tradenames TOXIMUL 8320(C4), EMULSOGEN MTP 070(C16-18), EMULSOGEN 3510(C4), ATLAS G-5000(C4), or Atplus 245 (C9-C11).

The fatty alcohol ethoxylated propoxylate of the present invention may be from 5g/L to 150g/L, such as 5g/L, 10g/L, 20g/L, 30g/L, 40g/L, 50g/L, 60g/L, 80g/L, 90g/L, 100g/L, 120g/L or 150g/L, relative to the weight of the oil dispersion composition, preferably from 10g/L to 120 g/L.

The inventors have found, unexpectedly, that the compounds of the fatty alcohol ethoxylated propoxylate are excellent in preventing aggregation of agrochemical actives, especially herbicidal sulfonamides, sulfonylurea actives, from the interaction of suspended particles, and serve to stabilize suspended particles in oil dispersions.

Suitable dispersed agrochemical active ingredients of the present invention may comprise one or more herbicides from the following classes, especially sulphonamides, sulphonylurea herbicides.

Herbicides that may be suitable for dispersion in the non-polar organic solvent of the present invention include, but are not limited to, triasulfuron (triasulfuron), tribenuron (tribenuron), metsulfuron (metasulfuron), thifensulfuron (thifensulfuron), flazasulfuron (flupyrsulfuron), iodosulfuron (iodosulfuron), rimsulfuron (rimsulfuron), nicosulfuron (nicosulfuron), cinosulfuron (cinosulfuron), bensulfuron (bensulfuron), trifloxysulfuron (trifloxysulfuron), triflusulfuron (mesosulfuron), triflusulfuron (sulfosulfuron), triflusulfuron (triflusulfuron-sodium trifluson (triflusulfuron), and derivatives of triflusulfuron (triflusulfuron-triflusulfuron), and flumetsulam (flumetum), flumetsulam (flumetsulam), flumetsulam (pyraoxysulfuron (triflusulfuron), and derivatives (triflusulfuron), penoxsulam (s (triflusulfuron (trifluson), penoxsulam), and the like.

For the oil dispersion composition of the present invention, the dispersible agrochemical active substance is from 1g/L to 300g/L, for example 1g/L, 10g/L, 30g/L, 40g/L, 50g/L, 60g/L, 70g/L, 80g/L, 100g/L, 150g/L, 180g/L, 220g/L, 250g/L or 300g/L, preferably from 10g/L to 250g/L, relative to the weight of the oil dispersion composition. It is known that such oil dispersion formulations can be diluted 1-2000 times at the time of use according to the amount of each herbicide used per mu.

In the present invention, the agrochemical active is less than 10g/L, for example 0.1g/L, 0.3g/L, 0.5g/L, 1g/L, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L or 9g/L, preferably less than 5g/L, more preferably less than 1g/L, soluble in the non-polar organic solvent.

Suitable second active ingredients which are soluble in or disperse in the oil phase may also be present in the oil dispersion composition of the present invention, including one or more non-sulphonamide or sulphonylurea herbicides, such as clodinafop-propargyl, cyhalofop-butyl, fenoxaprop-ethyl, acetochlor, pretilachlor, metolachlor, fluroxypyr, quinethazine (quizalofop-P), picloram, quinclorac, pendimethalin, 2,4-D, mesotrione, pretilachlor, quizalofop-P, quinclorac, butachlor, metribuzin, benzoxafen (topramezone), and the like.

The oil dispersion composition of the present invention may also have dissolved or dispersed herbicidal safeners present. Suitable herbicide safeners may include cloquintocet-mexyl, benoxacor, chloranil, isoxadifen ethyl, mefenpyr diethyl, oxabetrinil and their derivatives and analogues.

The at least one surfactant according to the present invention is a suitable functional surfactant commonly used for this purpose in oil dispersion formulations, such as emulsifiers, dispersants, wetting agents, defoamers, pH adjusters, thickeners, preservatives and the like.

Suitable emulsifiers are any substances used for this purpose in agrochemical formulations, preferably reactants of alkyl phenols with ethylene oxide and/or propylene oxide, ethoxylated nonyl phenols, castor oil ethoxylates, mixtures of polyalkoxylated alcohols (Atlox 4894), alkyl calcium salts, alkyl benzene sulphonic acid calcium salts, sorbitan derivatives or polyethylene oxide-sorbitan fatty acid esters, or combinations of any one or at least two thereof, where typical but non-limiting combinations are: a combination of ethoxylated nonylphenol and castor oil ethoxylate, a combination of ethoxylated nonylphenol and an alkyl calcium salt, a combination of ethoxylated nonylphenol and a calcium salt of alkylbenzene sulfonate, a combination of castor oil ethoxylate and an alkyl calcium salt, a combination of a calcium salt of alkylbenzene sulfonate and a sorbitan derivative, one or more of an alkyl calcium salt and a sorbitan derivative.

Suitable dispersants are any substances used for this purpose in agrochemical formulations, for example nonionic, amphoteric, cationic and anionic (polymeric) surfactants. Preferably such as one or more of naphthalene sulfonates, naphthalene sulfonate-formaldehyde condensates, alkyl sulfonates, lignosulfonates, polycarboxylates, fatty alcohol ethoxylates, fatty alcohol alkoxylates, EO/PO block copolymers, sulfonic acids of ethoxylated alcohols, sulfosuccinates, fatty acid methyl taurates, tristyrylphenol ethoxylates and alkoxylates, trissec-butylphenol ethoxylates, sulfated cresol-formaldehyde condensates, sulfated condensates of naphthalene and alkylnaphthalenes, phosphate esters of ethoxylated fatty alcohols, tristyrylphenol and trissec-butylphenol, and ethoxylated fatty alcohols, polyacrylic acids, polymethacrylic acids and acrylate copolymers, ether sulfates of tristyrylphenol and trissec-butylphenol, and polymeric dispersants.

Suitable wetting agents are any substances used for this purpose in agrochemical formulations, preferably anionic wetting agents, for example alkali metal, alkaline earth metal or ammonium salts of anionic wetting agents. Suitable wetting agents are naphthalenesulfonates (e.g. disodium methylenedinaphthalenesulfonate, sodium naphthalenesulfonate-formaldehyde condensates, ammonium naphthalenesulfonate-formaldehyde condensates), alkylnaphthalenesulfonates (e.g. sodium alkylnaphthalenesulfonate), benzenesulfonates, alkylbenzenesulfonates (e.g. sodium cumene sulfonate, potassium cumene sulfonate, sodium xylene sulfonate, sodium toluene sulfonate), alkanesulfonates (e.g. sodium tetradecene sulfonate), alpha-olefinsulfonates (e.g. sodium alpha-olefinsulfonate), sulfosuccinates (e.g. sodium dioctylsulfosuccinate), alkylphosphates (e.g. lauryl myristyl phosphate), alkylsulfates (e.g. sodium lauryl sulfate, sodium cetylstearyl sulfate, sodium cetyl sulfate, sodium myristyl sulfate, sodium cetylstearyl sulfate).

Suitable antifoams are any substances used for this purpose in agrochemical formulations, for example the salts of silicones, long-chain alcohols and fatty acids.

Suitable pH adjusters are any substances used for this purpose in agrochemical formulations, for example phosphoric acid, acetic acid, citric acid, sodium carbonate, sodium bicarbonate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate and the like which provide a protic acid or a protic base.

Suitable thickeners are any substances used for this purpose in agrochemical formulations, for example magnesium aluminium silicate, white carbon, diatomaceous earth, polyvinyl alcohol, polyvinylpyrrolidone.

Suitable preservatives are any substances which are used for this purpose in agrochemical formulations, for example alkylisothiazolinones and benzisothiazolinones.

The surfactant of the present invention is 1g/L to 300g/L, for example, 1g/L, 10g/L, 30g/L, 40g/L, 50g/L, 60g/L, 70g/L, 80g/L, 100g/L, 150g/L, 180g/L, 220g/L, 250g/L or 300g/L, preferably 10g/L to 200g/L, relative to the weight of the oil dispersion composition.

Further preferably, the oil dispersion composition of the present invention consists of:

(a) a non-polar organic solvent in an amount of 300g/L to 750g/L, relative to the weight of the oil-dispersed composition;

(b) a fatty alcohol ethoxylated propoxylate of 10g/L to 120g/L by weight of the oil dispersion composition;

(c) a dispersed agrochemical active which is 10g/L to 250g/L by weight of the oil dispersion composition;

(d) at least one surfactant in an amount of 10g/L to 200g/L relative to the weight of the oil dispersion composition.

The agricultural oil dispersion composition prepared according to the present invention can be stably stored even when stored at high temperatures or in cold conditions, and no phenomenon of mutual aggregation of particles or accelerated sedimentation of particles due to aggregation of particles is observed, and no phenomenon of aggregation is observed by microscopic observation, and no remarkable increase in particle size is observed by a malvern particle sizer test, and the preparation product shows excellent physical stability and does not cause quality problems for use after long-term storage.

The term "aggregation" as used herein refers to the phenomenon of mutual attraction, aggregation and accumulation between particles dispersed in an oil dispersion, and even more specifically, the particles are combined with each other to form a large particle, and thus cannot be easily separated again. The "growth" of particle size as referred to herein means that the suspended particles form large particles due to aggregation between the particles, and to the extent particle size growth is a thermodynamically further morphology of particle aggregation. The "sedimentation" is a phenomenon in which solid-liquid separation of an oil dispersion occurs due to particle aggregation, which increases the particle size to some extent.

The invention unexpectedly discovers that the addition of the fatty alcohol ethoxylated propoxylate can solve the problem of aggregation of suspended particles of the agricultural oil dispersion composition during storage, and also effectively avoids the problems of unstable preparation quality and inconvenient use caused by particle growth and sedimentation. The fatty alcohol ethoxylated propoxylate is unexpected and unexpected to those skilled in the art to control particle agglomeration in agricultural oil dispersion compositions.

In a second aspect, the present invention also provides a process for preparing the aforementioned oil-dispersed composition, comprising the steps of:

step 1: adding the agricultural chemical active substance and the surfactant into the nonpolar organic solvent, and stirring to be uniform;

step 2: fully grinding the mixture obtained in the step 1 to obtain an oil-based concentrated solution;

and step 3: adding the fatty alcohol ethoxylate into the oil-based concentrated solution in proportion, and stirring until the fatty alcohol ethoxylate and the oil-based concentrated solution are uniformly mixed to obtain the oil dispersion composition.

Preferably, the grinding of step 2 is performed at a temperature of 0-50 ℃, e.g., 0 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ or 50 ℃, preferably 15-45 ℃.

Preferably, the grinding described in step 2 results in a particle size D50 ≦ 5 μm, for example 0.4 μm, 0.8 μm, 1 μm, 2 μm, 3 μm, 4 μm, 4.5 μm, 4.8 μm, 5 μm, preferably D50 ≦ 3 μm, for the agrochemical active in the oil-based concentrate.

In a third aspect, the present invention also provides a method for preventing suspended particles of a sulfonamide or sulfonylurea herbicidal active in an agricultural oil-dispersible formulation composition from aggregating with each other.

The method comprises adding a sufficient amount of a fatty alcohol ethoxylated propoxylate to reduce the mutual aggregation of suspended particles of sulfonamide or sulfonylurea herbicidal actives; the fatty alcohol ethoxylated propoxylate is selected from the group consisting of C2-C20 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 100-1,000,000, preferably C4-C16 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 200-100,000;

preferably, the sufficient amount of fatty alcohol ethoxylated propoxylate and sulfonamide or sulfonylurea herbicidal active is in a weight ratio of 150:1 to 1:60, preferably 50:1 to 1:10, more preferably 10:1 to 1: 5.

In a method of preventing aggregation of suspended particles of an agricultural oil dispersion composition, a fatty alcohol ethoxylated propoxylate is added to an agricultural oil dispersion composition that forms an agricultural oil dispersion composition having the following components:

(I) a non-polar organic solvent;

(II) fatty alcohol ethoxylated propoxylates;

(III) a dispersed sulfonamide or sulfonylurea chemical active;

(IV) at least one surfactant.

The choice of the fatty alcohol ethoxylated propoxylate and the choice and proportions of the components and the like in preventing aggregation of suspended particles of the agricultural oil dispersion composition are consistent with those of the first aspect and will not be described in detail herein.

In a fourth aspect, the present invention also provides the use of a fatty alcohol ethoxylated propoxylate to inhibit or prevent the aggregation of suspended particles of a sulfonamide or sulfonylurea herbicidal active in an oil-dispersed composition as described in the first aspect with one another.

The fatty alcohol ethoxylated propoxylate is selected from the group consisting of C2-C20 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 100-1,000,000, preferably C4-C16 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 200-100,000; the weight ratio of the fatty alcohol ethoxylated propoxylate to the sulfonamide or sulfonylurea herbicidal active is from 150:1 to 1:60, preferably from 50:1 to 1:10, more preferably from 10:1 to 1: 5.

In inhibiting or preventing aggregation of the oil dispersion composition suspended particles, a fatty alcohol ethoxylated propoxylate is added to an agricultural oil dispersion composition that forms an agricultural oil dispersion composition containing the following components:

(I) a non-polar organic solvent;

(II) fatty alcohol ethoxylated propoxylates;

(III) a dispersed sulfonamide or sulfonylurea chemical active;

(IV) at least one surfactant.

The choice of the fatty alcohol ethoxylated propoxylate and the choice and proportions of the components and the like in inhibiting or preventing aggregation of suspended particles of an agricultural oil dispersion composition are consistent with those of the first aspect and are not described in detail herein.

In a fifth aspect, the present invention also provides a method for controlling pests, which comprises applying the oil-dispersed composition according to the first aspect to a locus where pests are growing.

The oil dispersion composition is applied as a water spray dilution.

The oil-dispersed composition comprises a sulfonamide or sulfonylurea herbicidal active to control the growth of harmful weeds.

The present invention provides a method of application of the oil dispersion composition as described in the first aspect, in particular an effective application amount often depending on, for example, the type of plant, the stage of plant growth, the severity of environmental conditions, the weeds to be controlled, the insect or fungal pathogen and the application conditions. Generally, plants which require protection from weeds or insects, or which require control or elimination of diseases or pathogens, are contacted with an amount of an oil dispersion formulation diluted in a carrier such as water which will provide the active ingredient in an amount of 1 to 40,000ppm, preferably 10 to 20,000 ppm. It is well known that such concentrated formulations can be diluted 1-2000 times at the time of use according to agricultural practice. The contacting can be in any effective manner. For example, any exposed part of the plant may be sprayed with the active ingredient mixed with an appropriate amount of a diluent or carrier, such as water, for example: leaves or stems.

The aforementioned compositions of the present invention may be applied to the foliage of the plant or to the soil or area adjacent to the plant. In addition, the compositions of the present invention may be mixed with or applied with any combination of agriculturally active ingredients such as herbicides, insecticides, bactericides, nematicides, miticides, biocides, termiticides, rodenticides, molluscicides, arthropodicides, fertilizers, growth regulators and pheromones.

Compared with the prior art, the invention has at least the following beneficial effects:

by adding the fatty alcohol ethoxylation propoxylate, the problem of aggregation of suspended particles of the agricultural oil dispersion composition in the storage process can be solved, and the problems of unstable preparation quality and inconvenient use caused by particle growth and sedimentation can be effectively avoided; after the oil dispersion composition added with the fatty alcohol ethoxylated propoxylate is subjected to heat storage at 54 ℃ for 14 days, the grain size growth rate can be controlled to be 3.10-5.50%, and the grains hardly aggregate.

Drawings

FIG. 1 is the observation result of the sample of example 1 under 400 times microscope after 3 months at normal temperature;

FIG. 2 is the observation result of the sample of example 4 under 400 times microscope after 3 months at normal temperature;

FIG. 3 is an observation result of a sample of comparative example 1 under a 400-fold microscope after 3 months at normal temperature;

FIG. 4 is the observation result of the sample of comparative example 4 under 400 times microscope after 3 months at normal temperature.

The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.

Detailed Description

The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.

For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.

The fatty alcohol ethoxylated propoxylates used in the present invention are commercially available. The fatty alcohol ethoxylated propoxylates used in the examples below are shown in table 1 with corresponding trade names.

TABLE 1

	Fatty alcohol ethoxylated propoxylates	Trade name
			Example 1	C4 fatty alcohol ethoxylated propoxylate	TOXIMUL 8320
Example 2	C4 fatty alcohol ethoxylated propoxylate	EMULSOGEN 3510
			Example 3	C4 fatty alcohol ethoxylated propoxylate	ATLAS G-5000
Example 4	Mixed C9-C11 fatty alcohol ethoxylated propoxylates	Atplus 245
			Example 5	Mixed C9-C11 fatty alcohol ethoxylated propoxylates	Atplus 245
Example 6	Mixed C16-18 fatty alcohol ethoxylated propoxylates	EMULSOGEN MTP 070

Example 1

Example 2

Example 3

Example 4

Example 5

Example 6

Comparative example 1

Comparative example 2

Comparative example 3

Comparative example 4

Comparative example 5

Comparative example 6

The samples of examples 1 to 6 and comparative examples 1 to 6 were subjected to accelerated storage tests, and after the samples were charged into measuring cylinders and placed in an oven at 54 ℃ for hot storage for 14 days, appearance microscopic observation and particle size measurement by a malvern laser particle sizer were performed and compared with the samples before hot storage, and the results of the measurements are shown in table 2 below.

TABLE 2

Note: judging the aggregation degree by using the microscope naked eye observation and the combination of the particle size test that the growth rate is more than 10 percent and more than 20 percent as a boundary, wherein the "-" indicates that the particles are not aggregated or are not obvious; "+" indicates particle aggregation; "+ +" indicates that the particles were heavily agglomerated.

As can be seen from the results shown in Table 2, the agricultural oil-dispersed composition of the present invention, the samples after heat storage, did not aggregate or became less noticeable, and the particle size increased less compared to comparative examples 1 to 6.

The particle size growth described in the present invention is mainly due to particle agglomeration. When the samples of example 1 and example 4 were observed under 400 times microscope after 3 months of storage at room temperature, as shown in fig. 1 and fig. 2, it was evident that the oil dispersion with the addition of the substance of fatty alcohol ethoxylated propoxylate according to the present invention had better particle dispersibility and was still uniformly distributed in the oil dispersion, while the oil dispersion without the addition of the substance of fatty alcohol ethoxylated propoxylate according to the present invention, when the samples of comparative example 1 and comparative example 4 were observed under 400 times microscope, as shown in fig. 3 and fig. 4, the originally dispersed particles aggregated and agglomerated and could not be uniformly distributed in the oil dispersion.

In conclusion, the problem of suspended particle aggregation of the agricultural oil dispersion composition in the storage process can be solved by adding the fatty alcohol ethoxylated propoxylate, and the problems of unstable preparation quality and inconvenient use caused by particle growth and sedimentation are effectively avoided.