WO2021244564A1 - Oil dispersion composition having improved stability - Google Patents

Abstract

The present invention provides an oil dispersion composition having improved stability, containing a non-polar organic solvent, a fatty alcohol ethoxylated propoxylate, dispersed agrochemical active matters, and at least one surfactant. In the present invention, the addition of the fatty alcohol ethoxylated propoxylate to the oil dispersion composition can stabilize the agrochemical active matters in the non-polar organic solvent, thereby preventing sedimentation due to particle aggregation.

Description

An oil dispersion composition with improved stability Technical field

The invention belongs to the technical field of agricultural chemistry, and specifically relates to an oil dispersion composition with improved stability, and the use of fatty alcohol ethoxylated propoxylate in controlling the aggregation of suspended particles of agricultural oil dispersion composition, especially It relates to a stable agrochemical oil dispersion formed by using C2-C20 fatty alcohol ethoxylated propoxylate to inhibit or prevent amide or sulfonylurea herbicide particles from agglomerating in an oil dispersion composition.

Background technique

Agricultural preparation products must be physically and chemically stable within a specific period of time to have commercial utility. However, there are many unstable factors, such as the instability of actives, phase separation and environmental factors. In today’s agrochemical market, it is increasingly common to develop new formulations containing multiple active substances and their required solvents, safeners and/or adjuvants to achieve the best pedigree, potency and delivery efficiency. The stability of formulations is facing more and more challenges. Therefore, technologies that can effectively isolate, interfere or eliminate adverse reactions or interactions between incompatible ingredients are often very important for successful products.

Agricultural chemical compositions such as herbicides, insecticides or fungicides or herbicide safeners are rarely used as they were originally manufactured. Agricultural chemicals generally consist of two parts, namely the active substance and the adjuvant component or inert ingredient combined together in the formulation. When combining these two parts into the final product, two main goals are considered: ① to maintain the stability of the product during storage, and ② to spray the product to the area to be treated after diluting the product in a carrier such as water or oil Provide an easy and effective way.

Agrochemical formulations are generally designed based on the needs of customers and the physicochemical properties of the active ingredients (for example, the solubility of the active ingredients in water or other non-aqueous solvents). There are mainly two main types of preparations, namely solid preparations and liquid preparations. Liquid formulations are generally preferred by customers due to their ease of handling during measurement, pumping, dilution and spraying operations.

Oil dispersion (OD) is a type of liquid formulation and is defined as a stable suspension of actives in water-immiscible solvents, which may contain other dissolved actives and are intended to be diluted with water before use. Recently, oil dispersion formulations have become more important in current formulation research. Because oil dispersion formulations are very suitable for the following situations: (1) water-sensitive actives, such as sulfonylurea herbicides, which are easily hydrolyzed and degraded, (2) compatibility issues with active mixtures, and (3) ) The need for an intramolecular adjuvant (build-in adjuvant).

It is now known that agricultural oil dispersions are thermodynamically unstable systems, and sedimentation will occur more or less. The speed of sedimentation accords with the Stokes sedimentation speed theory w=【2g(ρ _s -ρ)gr ² 】/9μ, where: ρ _s is the density of particles; ρ is the density of water; μ is the viscosity of the fluid; r is the particle Radius; g is the acceleration due to gravity. Generally, fluid modifiers are added to agricultural oil dispersion formulations to adjust the viscosity of the oil dispersion fluid to provide physical stability of the formulation. Many substances have been used as fluidics modifiers to stabilize oil dispersions to prevent sedimentation, such as clay, organoclay, hydrophilic silica and hydrophobic silica, xanthan gum, polyamide, polyethylene Pyrrolidone, polyacrylate, etc. It can be known from the theoretical formula that the size of the suspended particles in the oil dispersion is also an important factor affecting the sedimentation rate. The increase in the particle size of the suspended particles during storage is another reason that accelerates sedimentation and affects the physical stability of the formulation. There are generally two conditions for the increase of the particle size of suspended particles. One is the more or less dissolving effect of the polar solvent on the active material to cause Ostwald ripening; the other is the active material and additives, solvents, surfactants, The mutual agglomeration of particles caused by the incompatibility between the components of the formulation.

At present, there are also reports on the patents for controlling the sedimentation, stratification and particle growth of oil dispersions. The main protection in CN103118536A is to use a combination of clay or silica rheology modifiers and polymers or oligomers capable of forming hydrogen bonds. Preferably, a combination of a clay or silica type rheology modifier and polyethylene glycol or polypropylene glycol is preferred to stabilize the oil dispersion and prevent particle sedimentation and stratification. The main protection in CN107484767A is to select fatty acid ester solvents as the dispersed phase of spirotetramat particles to reduce or inhibit Ostwald ripening of suspended particles, so as to control the particle size growth and stabilize the oil dispersion. However, up to now, there is no relevant technology to disclose how to avoid the phenomenon of mutual aggregation of particles in the oil dispersion.

Summary of the invention

In order to solve the above technical problems, the present invention provides an oil dispersion composition with improved stability, wherein the suspended particles of the oil dispersion are relatively stable during a long storage process, and the particles do not aggregate or combine with each other. The physical stability of the oil dispersion composition is significantly improved. This improvement is achieved by adding a specific fatty alcohol ethoxylated propoxylate. The present invention has unexpectedly discovered that these compounds with fatty alcohol ethoxylated propoxylates can significantly control the mutual aggregation of suspended particles in the oil dispersion.

To achieve this goal, the present invention adopts the following technical solutions:

In the first aspect, the present invention provides an oil dispersion composition with improved stability, which contains the following components:

(a) Non-polar organic solvent, which is 200g/L-800g/L relative to the weight of the oil dispersion composition;

(b) Fatty alcohol ethoxylated propoxylate, which is 5g/L-150g/L relative to the weight of the oil dispersion composition;

(c) Dispersed agrochemical actives, which are 1g/L-300g/L relative to the weight of the oil dispersion composition;

(d) At least one surfactant, which is 1 g/L-300 g/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 substance is 150:1 to 1:60, for example 150:1, 120:1, 100:1, 80:1 65:1, 50:1, 45:1, 30:1, 20:1, 10:1, 5:1, 2:1, 1:1, 1:2, 1:5, 1:10, 1: 20, 1:30, 1:40, 1:50, 1:55, 1:60, preferably 50:1 to 1:10, more preferably 10:1 to 1:5.

The non-polar organic solvent used in the present invention is preferably one or more non-polar solvents that are immiscible with water, and generally have a solubility in water of less than 0.5% by weight, including one or more petroleum distillates such as those derived from benzene Aromatic hydrocarbons, such as toluene, xylene, mixed trimethylbenzene, etc., aliphatic hydrocarbons such as hexane, octane, cyclohexane, etc., vegetable oil, seed oil or animal oil 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, etc., as well as C1-C6 esters of vegetable oil or animal oil such as methyl oleate, epoxidized soybean oil, C1-C6 alkyl esters of methyl palmitate, ethyl castor oil, C6-C20 saturated and unsaturated aliphatic carboxylic acids.

In the present invention, strong polar organic solvents are not considered preferentially. For example, ethers such as tetrahydrofuran, alkylene glycol dialkyl ethers such as ethylene glycol diethyl ether, etc., amides such as dimethylacetamide or N-methyl Pyrrolidone and the like, ketones such as methyl ethyl ketone and the like, nitriles such as butyronitrile and the like, sulfoxides or sulfones such as dimethyl sulfoxide or sulfolane and the like, and alkylene carbonates such as propyl carbonate or butyl carbonate and the like. These strong polar organic solvents have good solubility properties, and have certain solubility for most agricultural active substances, such as sulfonamides and sulfonylurea herbicides. Active particles dispersed in such strong polar organic solvents are prone to Ostwald ripening. Protic solvents, such as water, alcohols, and polyols can sometimes be incompatible with some active ingredients or herbicide safeners present in oil dispersion formulations. Specifically, in the presence of water, some sulfonylurea herbicides have a degradation phenomenon of being hydrolyzed by breaking at the sulfonylurea bridge. None of the above categories of organic solvents are selected for use in the present invention.

In the present invention, the non-polar organic solvent is 200g/L-800g/L relative to the weight of the oil dispersion composition, such as 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-750g/L.

The fatty alcohol ethoxylated propoxylate of the present invention is an ether produced by the copolymerization of saturated and/or unsaturated linear and/or branched monohydric alcohol with ethylene glycol and propylene glycol in a certain molar ratio, wherein The fatty alcohol is selected from C2-C20 alcohols, such as C2, C6, C8, C9, C11, C14, C16 or C20, preferably C4-C16 saturated monohydric alcohols; the fatty alcohol ethoxylated propoxylate The number average molecular weight of the matrix is in the range of 100-1,000,000, for example, the number average molecular weight is 100, 200, 1000, 2200, 2500, 3000, 4500, 5200, 6300, 7000, 8600, 9500, 10,000, 30,000, 50,000, 100,000, 500,000 Or 1,000,000, preferably 200-100,000.

The fatty alcohol ethoxylated propoxylate described in the present invention can be specifically selected from the trade names TOXIMUL 8320 (C4), EMULSOGEN MTP 070 (C16-18), EMULSOGEN 3510 (C4), ATLAS G-5000 ( C4) or Atplus 245 (C9-C11), etc.

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

The inventors unexpectedly discovered that compounds such as fatty alcohol ethoxylated propoxylates can effectively prevent agrochemical active substances, especially herbicidal active substances, especially herbicidal sulfonamides and sulfonyl compounds in oil dispersions. Urea-based actives interact with suspended particles to cause aggregation to stabilize the suspended particles in the oil dispersion.

The suitable dispersed agrochemical active ingredients of the present invention may include one or more herbicides from the following categories, especially sulfonamides and sulfonylurea herbicides.

Herbicides suitable for dispersion in the non-polar organic solvents of the present invention include, but are not limited to, triasulfuron, tribenuron, metasulfuron, thifensulfuron, fluorine Flupyrsulfuron, iodosulfuron, rimsulfuron, nicosulfuron, cinosulfuron, bensulfuron, trifluorosulfuron (trifloxysulfuron), foramsulphuron, mesosulphuron, sulphosulphuron, flucarbazone-sodium tritosulphuron and derivatives, And flumetsulam, metosulam, chloransulam, florasulam, diclosulam, penoxsulam, penoxsulam, Pyroxsulam (pyroxsulam), diflufenican (diflufenican), fluopyram (thifluzamide) and derivatives, etc.

For the oil dispersion composition of the present invention, the dispersible agrochemical active material relative to the weight of the oil dispersion composition is 1g/L-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-250g/L. It is well known that this oil dispersion formulation can be diluted 1-2000 times during use according to the usage amount of each herbicide per mu.

In the present invention, the solubility of the agrochemical active substance in the non-polar organic solvent is less than 10g/L, such as 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.

The oil dispersion composition of the present invention may also contain a suitable second active ingredient that is soluble or dispersible in the oil phase, including one or more non-sulfonamide or sulfonylurea herbicides, such as clodinafop-propargyl , Cyhalofop-butyl, fenoxaprop-ethyl, acetochlor, pretilachlor, S-metolachlor, chlorofluoro Fluroxypyr, quizalofop-P, picloram, quinclorac, pendimethalin, 2,4-D, Mesotrione, pretilachlor, quizalofop-P, butachlor, atrazine, metribuzin, pinoxaden (pinoxaden), topramezone and so on.

The oil dispersion composition of the present invention may also contain a dissolved or dispersed herbicide safener. Suitable herbicide safeners may include cloquintocet-mexyl, benoxacor, cyometrinil, isoxadifen ethyl, and pyrazole mefenpyr diethyl), oxabetrinil and their derivatives and analogs.

The at least one surfactant described in the present invention is a suitable functional surfactant which is commonly used for this purpose in oil dispersion formulations, such as emulsifiers, dispersants, wetting agents, defoamers, pH adjuster, thickener, preservative, etc.

Suitable emulsifiers are any substances used for this purpose in agrochemical formulations, preferably reactants of alkylphenols with ethylene oxide and/or propylene oxide, ethoxylated nonylphenol, castor oil ethyl Oxygenates, mixtures of polyalkoxylated alcohols (Atlox 4894), alkyl calcium salts, alkyl benzene sulfonate calcium salts, sorbitan derivatives or polyethylene oxide-sorbitan fatty acid esters Any one or a combination of at least two, among which typical but non-limiting combinations are: ethoxylated nonylphenol and castor oil ethoxylate, ethoxylated nonylphenol and alkyl calcium Combination of salt, combination of ethoxylated nonylphenol and calcium salt of alkyl benzene sulfonate, combination of castor oil ethoxylate and alkyl calcium salt, combination of calcium salt of alkyl benzene sulfonate and sorbitan derivative One or more of the combination of alkyl calcium salt and sorbitan derivative.

Suitable dispersants are any substances used for this purpose in agrochemical formulations, such as nonionic, amphoteric, cationic and anionic (polymer) surfactants. Preferably such as naphthalene sulfonate, naphthalene sulfonate-formaldehyde condensation polymer, alkyl sulfonate, lignin sulfonate, polycarboxylate, fatty alcohol ethoxylate, fatty alcohol ethoxylate, fatty alcohol alkane Oxygenates, EO/PO block copolymers, ethoxylated alcohol sulfonic acids, sulfosuccinates, fatty acid methyl taurates, tristyrylphenol ethoxylates and alkoxylates, Tri-sec-butyl phenol ethoxylate, sulfated cresol-formaldehyde condensate, sulfated condensate of naphthalene and alkyl naphthalene, ethoxylated fatty alcohol, tristyryl phenol and tri-sec-butyl phenol phosphoric acid Esters, and one or more of ethoxylated fatty alcohols, polyacrylic acid, polymethacrylic acid and acrylate copolymers, ether sulfates of tristyryl phenol and tri-sec-butyl phenol, and polymer 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 naphthalene sulfonates (e.g., disodium methylene dinaphthalene sulfonate, sodium naphthalenesulfonate-formaldehyde condensate, ammonium naphthalenesulfonate-formaldehyde condensate), alkyl naphthalene sulfonates (e.g. Sodium alkyl naphthalene sulfonate), benzene sulfonate, alkyl benzene sulfonate (such as sodium cumene sulfonate, potassium cumene sulfonate, sodium xylene sulfonate, sodium toluene sulfonate), alkane sulfonate ( Such as sodium tetradecene sulfonate), α-olefin sulfonate (such as sodium α-olefin sulfonate), sulfosuccinate (such as sodium dioctyl sulfosuccinate), alkyl phosphate (such as laurel Myristyl phosphate), alkyl sulfates (e.g. sodium lauryl sulfate, sodium cetyl stearyl sulfate, sodium cetyl sulfate, sodium myristyl sulfate, sodium cetyl stearyl sulfate).

Suitable defoamers are any substances used for this purpose in agrochemical formulations, such as silicones, long-chain alcohols and salts of fatty acids.

Suitable pH regulators are any substances used for this purpose in agrochemical formulations, such as phosphoric acid, acetic acid, citric acid, sodium carbonate, sodium bicarbonate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, etc. Proton acid or proton base substance.

Suitable thickeners are any substances used for this purpose in agrochemical formulations, such as magnesium aluminum silicate, white carbon black, diatomaceous earth, polyvinyl alcohol, polyvinylpyrrolidone.

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

The surfactant of the present invention is 1g/L-300g/L relative to the weight of the oil dispersion composition, 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-200g/L.

Further preferably, the oil dispersion composition described in the present invention consists of the following components:

(a) A non-polar organic solvent, which is 300g/L-750g/L relative to the weight of the oil dispersion composition;

(b) Fatty alcohol ethoxylated propoxylate, which is 10g/L-120g/L relative to the weight of the oil dispersion composition;

(c) Dispersed agrochemical actives, which are 10g/L-250g/L relative to the weight of the oil dispersion composition;

(d) At least one surfactant, which is 10 g/L-200 g/L relative to the weight of the oil dispersion composition.

The agricultural oil dispersion composition prepared according to the present invention can be stored stably even if stored under high temperature or cold conditions. There is no phenomenon of mutual aggregation of particles, and no phenomenon of accelerated sedimentation due to particle aggregation. Through the microscope Observation did not find the phenomenon of aggregation, and the Malvern particle size analyzer test did not find a significant increase in particle size. The preparation product showed good physical stability and would not cause quality problems after long-term storage.

The “aggregation” in the present invention refers to the phenomenon that particles dispersed in the oil dispersion attract, move closer, gather, and accumulate. What's more, the interaction between the particles and the particles combine to form large particles. Was separated again. The "increase" of particle size in the present invention means that suspended particles form large particles due to the aggregation of particles. In terms of degree, particle size increase is a further thermodynamic form of particle aggregation. The "sedimentation" is a phenomenon in which the particle size increases to a certain extent due to the aggregation of particles, which causes the solid-liquid separation of the oil dispersion.

The present invention unexpectedly discovered that the addition of fatty alcohol ethoxylated propoxylate can solve the problem of the aggregation of suspended particles in the agricultural oil dispersion composition during storage, while also effectively avoiding particle growth and sedimentation that may cause poor formulation quality. The problem of stability and inconvenience. The fatty alcohol ethoxylated propoxylate is unpredictable for controlling particle aggregation in the agricultural oil dispersion composition, and has an unexpected control effect for those skilled in the art.

In the second aspect, the present invention also provides a method for preparing the aforementioned oil dispersion composition, which includes the following steps:

Step 1: Add agrochemical actives and surfactants to the non-polar organic solvent and stir to make them uniform;

Step 2: Thoroughly grind the mixture from Step 1 to obtain an oil-based concentrate;

Step 3: Add the fatty alcohol ethoxylate to the oil-based concentrate in proportion, and stir until the mixture is uniform to obtain the oil dispersion composition of the present invention.

Preferably, the grinding in step 2 is performed at a temperature of 0-50°C, for example, 0°C, 10°C, 15°C, 20°C, 25°C, 30°C, 35°C, 40°C, 45°C or 50°C, Preferably it is 15-45°C.

Preferably, the particle size D50 of the agrochemical active substance in the oil-based concentrate obtained by grinding in step 2 is less than or equal to 5 μm, such as 0.4 μm, 0.8 μm, 1 μm, 2 μm, 3 μm, 4 μm, 4.5 μm, 4.8 μm, 5 μm, preferably D50≤3μm.

In the third aspect, the present invention also provides a method for preventing the mutual aggregation of suspended particles of sulfonamide or sulfonylurea herbicidal actives in the agricultural oil dispersion composition.

The method includes adding a sufficient amount of fatty alcohol ethoxylated propoxylate to reduce the mutual aggregation of suspended particles of sulfonamides or sulfonylurea herbicidal actives; the fatty alcohol ethoxylated propoxylate is selected from several C2-C20 fatty alcohol ethoxylated propoxylate with an average molecular weight of 100-1,000,000, preferably C4-C16 fatty alcohol ethoxylated propoxylate with a number average molecular weight of 200-100,000;

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

In the method for preventing the aggregation of suspended particles of the agricultural oil dispersion composition, the fatty alcohol ethoxylated propoxylate is added to the agricultural oil dispersion composition, and the formed agricultural oil dispersion composition contains the following components:

(I) Non-polar organic solvents;

(II) Fatty alcohol ethoxylated propoxylate;

(III) Dispersed sulfonamide or sulfonylurea chemical active substances;

(IV) At least one surfactant.

When preventing the aggregation of suspended particles of the agricultural oil dispersion composition, the selection of the fatty alcohol ethoxylated propoxylate and the selection and ratio of each component are consistent with those in the first aspect. I won’t go into details here.

In a fourth aspect, the present invention also provides a fatty alcohol ethoxylated propoxylate in inhibiting or preventing the mutual aggregation of suspended particles of sulfonamide or sulfonylurea herbicidal actives in the oil dispersion composition of the first aspect. use.

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

When inhibiting or preventing the aggregation of the suspended particles of the oil dispersion composition, the fatty alcohol ethoxylated propoxylate is added to the agricultural oil dispersion composition, and the agricultural oil dispersion composition formed by it contains the following components:

(I) Non-polar organic solvents;

(II) Fatty alcohol ethoxylated propoxylate;

(III) Dispersed sulfonamide or sulfonylurea chemical active substances;

(IV) At least one surfactant.

When inhibiting or preventing the aggregation of suspended particles of the agricultural oil dispersion composition, the selection of the fatty alcohol ethoxylated propoxylate and the selection and ratio of each component are consistent with those in the first aspect. , I won’t repeat it here.

In the fifth aspect, the present invention also provides a pest control method, which is to use the oil dispersion composition as described in the first aspect in a place where pests grow.

When the oil dispersion composition is applied, it is used in the form of a water spray dilution.

The oil dispersion composition contains sulfonamide or sulfonylurea herbicidal actives to control the growth of harmful weeds.

The present invention provides an application method of the oil dispersion composition as described in the first aspect. Specifically, the effective application amount often depends on, for example, plant type, plant growth stage, harshness of environmental conditions, weeds, insects or fungi to be controlled Pathogens and application conditions. Generally, plants that need to be protected against weeds or insects, or need to control or eliminate diseases or pathogens, are contacted with a certain amount of an oil dispersion formulation diluted in a carrier such as water, and the formulation will provide 1-40,000 ppm, preferably Active ingredients in amounts of 10-20,000 ppm. It is well known that such concentrated formulations can be diluted 1-2000 times when used according to agricultural practice. The contact can be any effective way. For example, the active ingredient mixed with a suitable amount of a diluent or carrier such as water can be sprayed on any exposed part of the plant, such as leaves or stems.

The aforementioned composition of the present invention can be applied to plant leaves or the soil or area adjacent to the plant. In addition, the composition of the present invention can be combined with agricultural active ingredients such as herbicides, insecticides, fungicides, nematicides, acaricides, biocides, termiticides, rodenticides, molluscicides, and Any combination of arthropod agents, fertilizers, growth regulators, and pheromones is mixed or applied together with the combination.

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

In the present invention, by adding fatty alcohol ethoxylated propoxylate, the problem of the aggregation of suspended particles in the agricultural oil dispersion composition during storage can be solved, and at the same time, the problem of particle growth and sedimentation caused by poor formulation quality can be effectively avoided. The problem of stability and inconvenience; by storing the oil dispersion composition with fatty alcohol ethoxylated propoxylate at 54°C for 14 days, the growth rate of its particle size can be controlled at 3.10-5.50%, between particles Hardly gather.

Description of the drawings

Figure 1 is the observation result of the sample of Example 1 under a 400X microscope after 3 months at room temperature;

Figure 2 is the observation result of the sample of Example 4 under a microscope at 400 times after 3 months at room temperature;

Fig. 3 is the observation result of the sample of Comparative Example 1 under the microscope of 400 times after 3 months at room temperature;

Fig. 4 is the observation result of the sample of Comparative Example 4 under the microscope of 400 times after 3 months at room temperature.

The present invention will be described in further detail below. However, the following examples are only simple examples of the present invention, and do not represent or limit the protection scope of the present invention. The protection scope of the present invention is subject to the claims.

detailed description

The technical solutions of the present invention will be further described below in conjunction with the drawings and specific implementations.

In order to facilitate the understanding of the present invention, examples of the present invention are listed below. It should be understood by those skilled in the art that the described embodiments are only to help understand the present invention and should not be regarded as specific limitations to the present invention.

The fatty alcohol ethoxylated propoxylates used in the present invention can all be purchased on the market. The corresponding trade names of fatty alcohol ethoxylated propoxylates used in the following examples are shown in Table 1.

Table 1

To	Fatty alcohol ethoxylated propoxylate	Product 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 propoxylate	Atplus 245
Example 5	Mixed C9-C11 fatty alcohol ethoxylated propoxylate	Atplus 245
Example 6	Mixed C16-18 fatty alcohol ethoxylated propoxylate	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 the above-mentioned Examples 1-6 and Comparative Examples 1-6 were subjected to accelerated storage experiments. Each sample was put into a graduated cylinder and placed in an oven at 54°C for 14 days. After 14 days, the appearance of the sample was observed under a microscope and the particle size of the sample was passed through the Malvern laser. The particle size was tested by the instrument and compared with the sample before heat storage. The test results are shown in Table 2.

Table 2

Note: According to the microscope visual observation combined with the particle size test growth rate greater than 10% and greater than 20% as the limit to determine the degree of aggregation, where "-" means that the particles are not agglomerated or not obvious; "+" means that the particles are agglomerated; "++" means that the particles are agglomerated Seriously gather.

It can be seen from the results shown in Table 2 that in the agricultural oil dispersion composition of the present invention, the sample after heat storage does not aggregate or is not obvious, and the particle size increases less than that of Comparative Examples 1-6.

The increase in particle size described in the present invention is mainly caused by particle aggregation. After 3 months of storage at room temperature, the samples of Example 1 and Example 4 were observed under a 400X microscope. As shown in Figures 1 and 2, it was clearly found that the fatty alcohol ethoxylated propoxylate of the present invention was added. The oil dispersion of this type of material has good particle dispersibility and is still evenly distributed in the oil dispersion, and the oil dispersion of the fatty alcohol ethoxylated propoxylate of the present invention is not added, Observing the samples of Comparative Example 1 and Comparative Example 4 under a 400X microscope, as shown in Figs. 3 and 4, the originally dispersed particles aggregated and united with each other, and could no longer be evenly distributed in the oil dispersion.

In summary, by adding fatty alcohol ethoxylated propoxylate in the present invention, the problem of aggregation of suspended particles during storage of the agricultural oil dispersion composition can be solved, and particle growth and sedimentation can also be effectively avoided. It causes the problem of unstable quality of the preparation and inconvenience to use.

Claims (19)

1. The oil dispersion composition with improved stability is characterized in that it contains the following components:

   (a) Non-polar organic solvent, which is 200g/L-800g/L relative to the weight of the oil dispersion composition;

   (b) Fatty alcohol ethoxylated propoxylate, which is 5g/L-150g/L relative to the weight of the oil dispersion composition;

   (c) Dispersed agrochemical actives, which are 1g/L-300g/L relative to the weight of the oil dispersion composition;

   (d) At least one surfactant, which is 1 g/L-300 g/L relative to the weight of the oil dispersion composition.
2. The oil dispersion composition of claim 1, wherein the weight ratio of the fatty alcohol ethoxylated propoxylate to the agrochemical active substance is 150:1 to 1:60, preferably 50:1 to 1:10, more preferably 10:1 to 1:5.
3. The oil dispersion composition of 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 esters.
4. The oil dispersion composition of claim 1, wherein the fatty alcohol ethoxylated propoxylate is a C2-C20 fatty alcohol ethoxylated propoxylate with a number average molecular weight of 100-1,000,000, Preferred are C4-C16 fatty alcohol ethoxylated propoxylates having a number average molecular weight of 200-100,000.
5. The oil dispersion composition of claim 1, wherein the agrochemical active material comprises at least one selected from the group consisting of the following herbicides: sulfonamides, sulfonylureas and their derivatives.
6. The oil dispersion composition of claim 5, wherein the herbicide is selected from at least one of the following: tribensulfuron-methyl, metsulfuron-methyl, thifensulfuron-methyl, flufensulfuron-methyl, iodosulfuron-methyl, Rimsulfuron, nicosulfuron, metsulfuron-methyl, bensulfuron-methyl, trifluorosulfuron-methyl, formamisulfuron-methyl, mesosulfuron-methyl, fluazosulfuron-methyl, carfentrazone-ethyl, chlorfensulfuron , Fenoxsulam, flumetsulam, penoxsulam, methoxsulam or diflufenican.
7. The oil dispersion composition according to claim 1, wherein the solubility of the agrochemical active substance in the non-polar organic solvent is less than 10g/L, preferably less than 5g/L, more preferably less than 1g/L .
8. The oil dispersion composition according to claim 1, wherein the oil dispersion composition may further comprise a non-sulfonamide or sulfonylurea herbicide or a herbicide safe dispersed or dissolved in the non-polar organic solvent. Agent.
9. The oil dispersion composition according to claim 8, wherein the non-sulfonamide or sulfonylurea herbicide comprises clodinafop-propargyl, cyhalofop-butyl, fenoxaprop, acetochlor, and pretilachlor , Fine metolachlor, isooctyl fluroxypyr, quizalofop-ethyl, quinclorac, quinclorac, pendimethalin, 2,4-D, mesotrione, propionate Any one or a mixture of at least two of amines, quizalofop-p-ethyl, butachlor, atrazine, mefentrazone, pinoxaden, or mefentrazone.
10. The oil dispersion composition according to claim 8, wherein the herbicidal safener comprises chlorfenazone, chlorfenazone, chlorfenazone, ethyl fenoxaconate, fenpyrazone, or hydrochloride. Any one or a mixture of at least two of oxonitrile.
11. The oil dispersion composition of claim 1, wherein the surfactant comprises at least one of an emulsifier, a dispersant, a wetting agent, a defoamer, a pH adjuster, a thickener, or a preservative. kind.
12. A method for preparing the oil dispersion composition according to claim 1, characterized in that it comprises the following steps:

    Step 1: Add agrochemical actives and surfactants to the non-polar organic solvent and stir to make them uniform;

    Step 2: Thoroughly grind the mixture from Step 1 to obtain an oil-based concentrate;

    Step 3: Add the fatty alcohol ethoxylate to the oil-based concentrate in proportion, and stir until the mixture is uniform to obtain the oil dispersion composition.
13. The method according to claim 12, wherein the grinding in step 2 is performed at a temperature of 0-50°C, preferably 15-45°C.
14. The method according to claim 12, characterized in that the particle size D50 of the oil-based concentrate obtained by grinding in step 2 is less than or equal to 5 μm, preferably D50 less than or equal to 3 μm.
15. A method for preventing mutual aggregation of suspended particles of sulfonamide or sulfonylurea herbicidal actives in agricultural oil dispersion formulations, characterized in that the method includes adding a sufficient amount of fatty alcohol ethoxylated propoxylate to Reduce the mutual aggregation of suspended particles of sulfonamides or sulfonylurea herbicidal actives; the fatty alcohol ethoxylated propoxylate is selected from C2-C20 fatty alcohol ethoxylated propoxy groups with a number average molecular weight of 100-1,000,000 Compounds, preferably C4-C16 fatty alcohol ethoxylated propoxylates with a number average molecular weight of 200-100,000;

    Preferably, the weight ratio of the sufficient amount of fatty alcohol ethoxylated propoxylate to the sulfonamide or sulfonylurea herbicidal active is 150:1 to 1:60, preferably 50:1 to 1:10, more It is preferably 10:1 to 1:5.
16. Use of fatty alcohol ethoxylated propoxylates to inhibit or prevent the mutual aggregation of suspended particles of sulfonamides or sulfonylurea herbicidal actives in the oil dispersion composition of claim 1, characterized in that the fat Alcohol ethoxylated propoxylates are selected from C2-C20 fatty alcohol ethoxylated propoxylates with a number average molecular weight of 100-1,000,000, preferably C4-C16 fatty alcohol ethoxylates with a number average molecular weight of 200-100,000 The weight ratio of the fatty alcohol ethoxylated propoxylate and the sulfonamide or sulfonylurea herbicidal active substance is 150:1 to 1:60, preferably 50:1 to 1:10, more It is preferably 10:1 to 1:5.
17. A method for controlling pests, characterized in that the method is to use the oil dispersion composition according to any one of claims 1 to 11 in a place where pests grow.
18. The control method according to claim 17, wherein the oil dispersion composition is used in the form of a water spray dilution when applied.
19. The control method according to claim 17 or 18, wherein the oil dispersion composition contains sulfonamide or sulfonylurea herbicidal actives to control the growth of harmful weeds.

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