Herbicidal composition, preparation and application thereof

Abstract

The invention relates to the technical field of pesticides, in particular to a herbicidal composition, a preparation and an application thereof. A herbicidal composition including benzylazole and glyphosate; The weight ratio of the described benzylazole to glyphosate is 1: (10-100). The present invention also provides a dispersible oil suspension including the herbicidal composition, which optimizes the type and content of emulsifier, dispersant, synergist, viscosity regulator and dispersion medium by screening and optimizing the type and content of the dispersible oil suspension. The prepared dispersible oil suspension has stable quality and good performance, is more beneficial to the exertion of drug effect and also has excellent low temperature fluidity, dispersion stability, thermal storage stability and so on. Moreover, the raw material is easy to obtain, the preparation process is simple, and it is easy for industrial production, so it is suitable for the control of weeds in non-cultivated land.

Description

A herbicidal composition, preparation and application thereof Technical Field

[0001] The present invention relates to the technical field of pesticides, and in particular to a herbicidal composition, a preparation and applications thereof. Background Art

[0002] Benpyram, chemically known as 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylic acid ethyl ester, has a unique structure combining uracil and isoxazole. Compared to benpyram, it exhibits superior herbicidal activity and can effectively control annual and perennial weeds in gardens and non-arable land, but its cost is relatively high. Currently, herbicides containing a single active ingredient have varying degrees of drawbacks in agricultural weed control. These include the tendency to develop resistance with continuous use, a limited spectrum of weed control, and the ability to only control monocotyledonous or dicotyledonous weeds, or to control only emerging or pre-emerged weeds, with no ability to control multiple weeds. By compounding two or more active ingredients, the control effect can be improved, the use of active ingredients can be reduced, the control cost can be saved, the development of weed resistance can be delayed, the service life of the agent can be extended, and pollution to the environment can be reduced.

[0003] Dispersible oil suspension concentrates (DOSCs) are highly dispersed, long-term stable suspensions of the active ingredient (API) and adjuvants (such as emulsifiers, dispersants, and viscosity modifiers) in an oily carrier. At least one of the ingredients is insoluble in the non-aqueous medium and is used after dilution with water. Compared to other formulations, DDOs offer advantages such as safety, environmental friendliness, and superior efficacy. This is evident in the absence of dust pollution during production and the absence of flammable or explosive organic solvents. These advantages are relatively safe for manufacturers and users, convenient and safe for storage and transportation, and environmentally friendly, leading to their widespread international adoption. Due to the physicochemical properties of some active ingredients, or the lack of synergy between the active ingredient and adjuvants, such as poorly lipophilic APIs, which have difficulty penetrating the crop epidermis and entering the plant interior, their systemic effects are limited. Consequently, DDOs can enhance the efficacy of lipophilic APIs, particularly oil-insoluble herbicides. Due to the significant differences in the physical and chemical properties of different pesticide technicals, the performance of the various screened adjuvants, the interactions between the adjuvants, and their effects on the technicals vary greatly. Currently, dispersible oil suspension concentrates have problems such as poor low-temperature fluidity, poor dispersion stability, and poor thermal storage stability (oil separation, decomposition, discoloration, viscosity, and crystallization occur after thermal storage of the preparation). These problems easily lead to clogging of nozzles or filters during use, directly affecting the quality and application effect of dispersible oil suspension concentrates.

[0004] In response to the above technical problems, the present invention provides a herbicide composition containing benzylpyridamole and a dispersible oil suspension prepared therefrom, which solves the stability problem of the current dispersible oil suspension by selecting an auxiliary agent.

[0005] Summary of the Invention

[0006] In order to solve the above technical problems, the first aspect of the present invention provides a herbicidal composition, which comprises benzylpyridazone and glyphosate; the weight ratio of the benzylpyridazone to glyphosate is 1:(10-100).

[0007] The second aspect of the present invention provides a herbicidal composition formulation, which is composed of the above-mentioned herbicidal composition and pesticide-acceptable adjuvants.

[0008] As a preferred technical solution of the present invention, the formulation of the herbicidal composition is selected from one of a soluble concentrate, a microemulsion, a dispersible oil suspension, a wettable powder, and a water-dispersible granule.

[0009] As a preferred technical solution of the present invention, the weight percentage of the herbicidal composition in the herbicidal composition preparation is 5%-90%.

[0010] As a preferred technical solution of the present invention, the formulation of the herbicidal composition is a dispersible oil suspension; the pesticide-acceptable excipients include at least one of an emulsifier, a wetting agent, a dispersant, a stabilizer, a defoaming agent, a viscosity regulator, and a base oil.

[0011] As a preferred technical solution of the present invention, the emulsifier is selected from at least one of castor oil polyoxyethylene ether, calcium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, alkylphenol formaldehyde resin polyoxyethylene ether, sorbitan monostearate, sorbitan monostearate polyoxyethylene ether, phenethylphenol polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, alkoxy polyoxyethylene ether sulfonate, fatty alcohol sulfate, alkyl phosphate ester salt, fatty alcohol polyoxyethylene ether sulfate, EO-PO block copolymer and phenethylphenol polyoxyethylene ether sulfonate.

[0012] As a preferred technical solution of the present invention, the emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1: (0.1-0.5).

[0013] As a preferred technical solution of the present invention, the dispersant is selected from at least one of polycarboxylates, lignin sulfonates, EO-PO block copolymers, phosphates and their salts, sulfonates, alkylnaphthalene sulfonates, alkylphenol polyoxyethylene ethers and fatty alcohol polyoxyethylene ethers.

[0014] As a preferred technical solution of the present invention, the viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate, with a weight ratio of 1:(0.5-2).

[0015] The third aspect of the present invention provides the use of the herbicidal composition for controlling weeds in non-arable land. Beneficial effects

[0016] The present invention provides a herbicidal composition and a dispersible oil suspension containing the herbicidal composition, which have the following beneficial effects:

[0017] 1. The combination of benzylpyridamole and glyphosate has a unique mechanism of action and no cross-resistance, resulting in a synergistic effect. This broadens the weed control spectrum and improves control efficacy, compensating for the poor control of major weeds by using a single agent alone. It also improves the long-lasting effectiveness of each component of the combination, delays the development of weed resistance, reduces the number of repeated pesticide applications, and reduces usage and costs. It is primarily used to control weeds in non-arable land, especially glyphosate-resistant weeds such as Erigeron striata and Goosegrass.

[0018] 2. By screening and optimizing the types and contents of emulsifiers, dispersants, synergists, viscosity regulators and dispersion media, the prepared dispersible oil suspension has stable quality and good performance, which is more conducive to the efficacy of the drug. At the same time, it has excellent low-temperature fluidity, dispersion stability, thermal storage stability, etc.; and its raw materials are easily available, the preparation process is simple, and it is easy to industrialize. DETAILED DESCRIPTION

[0019] The present invention may be more readily understood by referring to the following detailed description of preferred embodiments of the present invention and the included Examples. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present invention pertains. In the event of a conflict, the definitions in this specification shall prevail.

[0020] As used herein, the term "prepared from" is synonymous with "comprising." As used herein, the terms "comprising," "including," "having," "containing," or any other variations thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises the listed elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

[0021] The conjunction "consisting of" excludes any unspecified element, step, or component. If used in a claim, this phrase renders the claim closed, excluding materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of" appears in a clause of the body of a claim, rather than immediately following the subject matter, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.

[0022] When amount, concentration or other value or parameter is represented with range, preferred range or the range that a series of upper preferred value and lower preferred value limit are expressed, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value and any range lower limit or preferred value, no matter whether this range is disclosed separately.For example, when disclosing scope "1 to 5", described scope should be interpreted as including scope "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5" etc.When numerical range is described in this article, unless otherwise stated, otherwise this scope is intended to include its end value and all integers and fractions within this range.

[0023] The singular includes plural references unless the context clearly dictates otherwise. "Optional" or "either" means that the subsequently described event or incident can or cannot occur, and that the description includes instances where the event occurs and instances where it does not.

[0024] Approximating terms in the specification and claims are used to modify a quantity to indicate that the invention is not limited to that specific quantity and includes acceptable modifications close to that quantity that do not result in a change in the relevant basic function. Accordingly, the use of "about," "approximately," or the like to modify a numerical value indicates that the invention is not limited to that exact numerical value. In some instances, approximating terms may correspond to the precision of the instrument used to measure the value. In the specification and claims of this application, range definitions may be combined and / or interchanged, and unless otherwise indicated, such ranges include all subranges contained therein.

[0025] In order to solve the above technical problems, the first aspect of the present invention provides a herbicidal composition, which comprises benzylpyridazone and glyphosate; the weight ratio of the benzylpyridazone to glyphosate is 1:(10-100).

[0026] In a preferred embodiment, the weight ratio of benzylpyridamole to glyphosate is 1:(20-60).

[0027] In a more preferred embodiment, the weight ratio of benzylpyridamole to glyphosate is 1:40.

[0028] The inventors have discovered that when benzylpyridamole and glyphosate are used in combination, a synergistic effect is produced due to the unique mechanism of action of the two active ingredients and the absence of cross-resistance. This expands the weed control spectrum, improves the control efficacy, and compensates for the poor control effect of single agents on major weeds. The long-lasting effect of each component of the combination is improved, delays the development of weed resistance, reduces the number of repeated pesticide applications, and reduces the usage amount and cost. The combination can be mainly used to control weeds in non-arable land, especially glyphosate-resistant weeds such as Erigeron striata and Goosegrass.

[0029] The second aspect of the present invention provides a herbicidal composition formulation, which is composed of the above-mentioned herbicidal composition and pesticide-acceptable adjuvants.

[0030] In a preferred embodiment, the herbicidal composition preparation is in the form of a soluble concentrate, a microemulsion, a dispersible oil suspension, a wettable powder, or a water-dispersible granule.

[0031] In a preferred embodiment, the herbicidal composition accounts for 5-90% by weight of the herbicidal composition formulation.

[0032] In a preferred embodiment, the herbicidal composition formulation is in the form of a dispersible oil suspension; the pesticide-acceptable excipients include at least one of an emulsifier, a wetting agent, a dispersant, a stabilizer, a defoaming agent, a viscosity regulator, and a base oil.

[0033] Dispersible oil suspension

[0034] In the present invention, the raw materials for preparing the herbicide dispersible oil suspension concentrate include at least the following components by weight: 5-50% of the herbicide composition, 5-20% of the emulsifier, 0-5% of the wetting agent, 1-5% of the dispersant, 0-5% of the defoaming agent, 2-10% of the viscosity regulator, and the base oil making up to 100%.

[0035] emulsifiers

[0036] Emulsifiers are compounds that can form a stable emulsion from a mixture of two or more immiscible components. Their mechanism of action is that during the emulsification process, the dispersed phase is dispersed in the continuous phase in the form of micron-sized droplets. The emulsifier reduces the interfacial tension between the components in the mixture and forms a relatively strong film on the droplet surface. Due to the charge imparted by the emulsifier, a double layer forms on the droplet surface, preventing the droplets from aggregating and maintaining a homogeneous emulsion. From a phase perspective, an emulsion is still a heterogeneous system. The dispersed phase in an emulsion can be either aqueous or oily, with the latter being the most common. The continuous phase can be either oily or aqueous, with the latter being the most common. An emulsifier is a surfactant with both hydrophilic and lipophilic groups in its molecules. The hydrophilicity or lipophilicity of an emulsifier is typically expressed in terms of its hydrophilic-lipophilic balance (HLB value). A lower HLB value indicates a more lipophilic nature, while a higher HLB value indicates a more hydrophilic nature. Various emulsifiers have different HLB values. In order to obtain a stable emulsion, a suitable emulsifier must be selected.

[0037] In the present invention, the emulsifier is selected from at least one of castor oil polyoxyethylene ether, calcium dodecylbenzenesulfonate, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, alkylphenol formaldehyde resin polyoxyethylene ether, sorbitan monostearate, sorbitan monostearate polyoxyethylene ether, phenethylphenol polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, alkoxy polyoxyethylene ether sulfonate, fatty alcohol sulfate, alkyl phosphate salt, fatty alcohol polyoxyethylene ether sulfate, EO-PO block copolymer and phenethylphenol polyoxyethylene ether sulfonate.

[0038] In a preferred embodiment, the emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1: (0.1-0.5).

[0039] In a more preferred embodiment, the weight ratio of the castor oil polyoxyethylene ether to the phenethylphenol polyoxyethylene ether sulfonate is 1:0.35.

[0040] Castor oil polyoxyethylene ether

[0041] In the present invention, the HLB value of the castor oil polyoxyethylene ether is 9-14.

[0042] In a preferred embodiment, the HLB value of the castor oil polyoxyethylene ether is 11-13.

[0043] In a preferred embodiment, the saponification value of the castor oil polyoxyethylene ether is 30-100 mgKOH / g.

[0044] In a more preferred embodiment, the saponification value of the castor oil polyoxyethylene ether is 50-70 mgKOH / g.

[0045] In the present invention, the source of the castor oil polyoxyethylene ether is not particularly limited, and may be Hai'an Petrochemical Plant, Jiangsu Province, with specifications of EL20, HEL20, EL30, HEL30, EL40, HEL40, etc.

[0046] Phenethylphenol polyoxyethylene ether sulfonate

[0047] In the present invention, the source of the phenylethylphenol polyoxyethylene ether sulfonate is not particularly limited, and the source may be Shandong Tiandao Bioengineering Co., Ltd., model #602.

[0048] The inventors have discovered that the system, which utilizes a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, can effectively prevent flocculation of the original drug particles, thereby improving the suspension stability and storage stability of the dispersible oil suspension concentrate. The inventors believe this may be due to the fact that the combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate significantly reduces the surface free energy of the original drug ions. On the one hand, the castor oil polyoxyethylene ether can adsorb on the particles, forming a thick adsorption layer; on the other hand, the phenethylphenol polyoxyethylene ether sulfonate can form a diffuse double layer on the particle surface, which not only repels the original drug ions but also increases the steric hindrance of interparticle aggregation, further improving the stability of the system. In particular, when the weight ratio of castor oil polyoxyethylene ether to phenethylphenol polyoxyethylene ether sulfonate is 1:(0.1-0.5), the suspension stability of the resulting dispersible oil suspension concentrate is optimal, and even after long-term storage, no particles will precipitate. During their research, the inventors unexpectedly discovered that the addition of an emulsifier can improve the dispersibility of the dispersible oil suspension concentrate after dissolving in water. The inventors believe this may be due to the presence of numerous interfaces in emulsions, making them thermodynamically unstable systems prone to spontaneous coalescence, stratification, and sedimentation. This reduces the number of interfaces, and the emulsifiers used in this system can produce a synergistic effect, effectively reducing the oil-water interfacial tension. This allows the original drug particles to remain dispersed in water, facilitating emulsification and improving the stability of the emulsion.

[0049] Wetting agent

[0050] Wetting agents, also known as wetting agents, are a type of pesticide adjuvant. They are substances that can make water-insoluble or non-wettable solid pesticides wettable. Their primary function is to reduce the surface tension or interfacial tension of water, allowing solid surfaces to become wettable. They can be used to create suspensions of water-insoluble pesticides, allowing the liquid to wet and spread on crops, insects, and pathogens, thereby improving pest control effectiveness and reducing the occurrence of pesticide damage.

[0051] In the present invention, the wetting agent is not particularly limited and is well known to those skilled in the art.

[0052] In a preferred embodiment, in order to further improve the ability of the original drug particles to remain dispersed into fine individual particles in water and at the same time improve the dispersibility of the original drug particles in water, the wetting agent is selected from at least one of alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylphenol polyoxyethylene ether phosphate, phenethylphenol polyoxyethylene ether phosphate, alkyl sulfate, alkyl sulfonate, and naphthalene sulfonate.

[0053] In the present invention, the weight ratio of the emulsifier to the wetting agent is 1:(0.05-0.5).

[0054] In a preferred embodiment, the weight ratio of the emulsifier to the wetting agent is 1:0.2.

[0055] dispersants

[0056] Dispersant is a surfactant that has two opposite properties, lipophilicity and hydrophilicity, in its molecule.

[0057] In the present invention, the dispersant is selected from at least one of polycarboxylates, lignin sulfonates, EO-PO block copolymers, phosphates and their salts, sulfonates, alkylnaphthalene sulfonates, alkylphenol polyoxyethylene ethers and fatty alcohol polyoxyethylene ethers.

[0058] In a preferred embodiment, the dispersant is a combination of sulfonate and phosphate, with a weight ratio of 1:(0.1-1.5).

[0059] In a more preferred embodiment, the weight ratio of the sulfonates to the phosphates is 1:0.85.

[0060] Sulfonates

[0061] In the present invention, the sulfonate is selected from at least one of naphthalenesulfonic acid formaldehyde condensates, alkylnaphthalenesulfonic acid formaldehyde condensates, lignin acid sulfonates, and aminosulfonates.

[0062] In a preferred embodiment, the sulfonates are preferably compounds with aromatic groups in their molecular structures, preferably naphthalenesulfonic acid formaldehyde condensates and alkylnaphthalenesulfonic acid formaldehyde condensates.

[0063] In the present invention, the sources of the naphthalenesulfonic acid formaldehyde condensate and the alkylnaphthalenesulfonic acid formaldehyde condensate are not particularly limited, and Jinan Hongboli Chemical Co., Ltd. can be mentioned.

[0064] Phosphates

[0065] In the present invention, the phosphate esters are preferably compounds having amino groups or amide groups in their molecular structures.

[0066] In a preferred embodiment, the phosphate esters may include alkylamide polyoxyethylene ether phosphate.

[0067] In the present invention, the source of the alkylamide polyoxyethylene ether phosphate is not particularly limited, and Guangzhou Bifeng Trading Co., Ltd. can be mentioned.

[0068] In the present invention, the weight ratio of the emulsifier to the dispersant is 1:(0.1-0.5).

[0069] In a preferred embodiment, the weight ratio of the emulsifier to the dispersant is 1:0.4.

[0070] The inventors have discovered that this system, which utilizes a sulfonate dispersant containing an aromatic group and a phosphate surfactant containing an amino or amide group, can effectively improve the stability of dispersible oil suspension concentrates after high- and low-temperature storage. The inventors believe this may be due to the relatively hydrophobic surface of the stock pesticide particles, particularly benzylpyridamole, which has a low melting point and is more prone to aggregation. The dispersant molecules employed in this invention interact synergistically with the pesticide surface through van der Waals attraction, hydrogen bonding, electrostatic repulsion, and steric hindrance, effectively dispersing the stock pesticide particles regardless of temperature. However, when the amount of the dispersant is less than 1%, the dispersant does not reach saturated adsorption on the surface of the original pesticide particles, and the pesticide particles cannot be fully coated by the dispersant molecules. Under the action of van der Waals forces and gravity fields, the particles aggregate and settle, increasing the viscosity of the preparation. When the amount of the dispersant is higher than 10%, the excess dispersant molecules in the system entangle with the coating layer on the surface of the active ingredient particles, causing bridging between the particles, resulting in flocculation, increasing the viscosity of the preparation, and deteriorating the fluidity, thereby affecting the appearance of the preparation.

[0071] Viscosity regulator

[0072] Viscosity regulators are mainly used to adjust the viscosity and consistency of the product. Generally, there are two types: viscosity reducers and viscosity increasers.

[0073] In the present invention, the viscosity modifier is not particularly limited and is well known to those skilled in the art.

[0074] In a preferred embodiment, in order to further improve the suspension stability of the system, inhibit the sedimentation of the technical particles, maintain the fluidity of the system, and ensure that the system does not stratify or undergo Ostwald ripening during thermal storage, the viscosity modifier may include gum arabic, xanthan gum, polyvinyl pyrrolidone, organic bentonite, hydroxymethyl cellulose, polyvinyl alcohol, silicon dioxide, magnesium aluminum silicate, and the like.

[0075] In a more preferred embodiment, the viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate in a weight ratio of 1:(0.5-2).

[0076] In a most preferred embodiment, the weight ratio of the organic bentonite to magnesium aluminum silicate is 1:0.76.

[0077] The inventors believe that this system, through the compounding of organic bentonite and magnesium aluminum silicate, absorbs water and expands in water to form a hydrogel network structure. At the same time, it can also expand the polymer chains to form a two-dimensional structure through covalent bonds and hydrogen bonds or repulsion between ions, thereby making the system thixotropic and increasing the structural strength of the suspension system.

[0078] base oil

[0079] In the present invention, the base oil is not particularly limited and is well known to those skilled in the art, and examples thereof include vegetable oil, vegetable oil ester compound, mineral oil, and the like.

[0080] In a preferred embodiment, the base oil is selected from at least one of soybean oil, corn oil, rapeseed oil, cottonseed oil, castor oil, turpentine, palm oil, coconut oil, sunflower oil, methyl oleate, diesel, motor oil, and mineral oil.

[0081] In a more preferred embodiment, the base oil comprises at least methyl oleate.

[0082] In a more preferred embodiment, the base oil is a combination of castor oil and methyl oleate in a weight ratio of 1:(0.1-10).

[0083] The inventors discovered that the combination of castor oil and methyl oleate in this system improves the dispersion stability of the emulsifier and dispersant in the base oil, thereby enhancing the suspension and stability of the system and its dispersion in water. It also reduces the oil separation rate of the system at room temperature and under hot storage conditions, further improving the suspension rate. The inventors believe this may be due to the fact that the organobentonite and magnesium aluminum silicate absorb oil and swell in methyl oleate, forming a network gel structure that encapsulates a large number of oily medium molecules within the network. As the organic carbon chains of the organobentonite increase the chance of overlapping and covering each other, the structure's resistance to damage increases, the system's yield value increases, the oil separation rate decreases, and the suspension rate increases.

[0084] In the present invention, the preparation method of the dispersible oil suspension is as follows: the herbicidal composition, emulsifier, wetting agent, dispersant, defoamer, viscosity regulator and base oil are mixed, and high-speed shear dispersion is performed for 10-60 minutes; and then grinding is performed until the D97 is 1-10 μm.

[0085] In a more preferred embodiment, the D97 is 3±1 μm.

[0086] D97 refers to the particle size value at which the cumulative percentage of particles from smallest to largest in a particle size distribution reaches 97%. This means that within a powder, 97% of the total particles have a particle size smaller than D97. It is often used to indicate the coarse end particle size of a powder and is a key indicator of concern in powder production and application.

[0087] The inventors found that controlling the D97 of the system to 1-10 μm can significantly improve the dispersibility and storage stability of the system.

[0088] The third aspect of the present invention provides the use of the herbicidal composition for controlling weeds in non-arable land.

[0089] In a preferred embodiment, the non-arable land may include woodlands, lawns, roads, railways, warehouses, ridges, ditches, forest fire prevention avenues, etc.

[0090] The present invention is described in detail below by way of examples. It is necessary to point out that the following examples are only used to further illustrate the present invention and are not to be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by professionals in this field based on the above-mentioned contents of the present invention still fall within the scope of protection of the present invention.

[0091] Example

[0092] Example 1

[0093] Example 1 provides a herbicide dispersible oil suspension concentrate, comprising at least the following components, by weight percentage: 30% of a herbicide composition, 10% of an emulsifier, 2% of a wetting agent, 4% of a dispersant, 6% of a viscosity modifier, and 100% of a base oil; the herbicide composition is a combination of benzylpyridamole and glyphosate, with a weight ratio of 1:40; the emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1:0.35; the castor oil polyoxyethylene ether was purchased from Hai'an Petrochemical Plant in Jiangsu Province, specification EL30; the phenethylphenol polyoxyethylene ether sulfonate was purchased from Shandong Tiandao Bioengineering Co., Ltd., model #602; The wetting agent is alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, purchased from Hai'an Petrochemical Plant in Jiangsu Province; the dispersant is a combination of alkylnaphthalenesulfonic acid formaldehyde condensate and alkylamide polyoxyethylene ether phosphate, with a weight ratio of 1:0.85; the alkylnaphthalenesulfonic acid formaldehyde condensate was purchased from Jinan Hongboli Chemical Co., Ltd.; the alkylamide polyoxyethylene ether phosphate was purchased from Guangzhou Bifeng Trading Co., Ltd.; the viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate, with a weight ratio of 1:0.76; the organic bentonite was purchased from Tuoyi New Materials (Guangzhou) Co., Ltd.; the base oil is a combination of castor oil and methyl oleate, with a weight ratio of 1:0.8.

[0094] The preparation method of the dispersible oil suspension is as follows: the herbicidal composition, emulsifier, wetting agent, dispersant, defoamer, viscosity regulator and base oil are mixed, and high-speed shear dispersion is performed for 30 minutes; and then grinding is performed until the D97 is 5 μm to obtain the product.

[0095] Example 2

[0096] Example 2 provides a herbicide dispersible oil suspension concentrate, comprising at least the following components, by weight percentage: 30% of a herbicide composition, 5% of an emulsifier, 1% of a dispersant, 2% of a viscosity modifier, and 100% of a base oil; the herbicide combination is a combination of benzylpyridamole and glyphosate, with a weight ratio of 1:40; the emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1:0.1; the castor oil polyoxyethylene ether was purchased from Hai'an Petrochemical Plant in Jiangsu Province, specification EL30; the phenethylphenol polyoxyethylene ether sulfonate was purchased from Shandong Tiandao Bioengineering Co., Ltd., model #602; The wetting agent is alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, purchased from Hai'an Petrochemical Plant in Jiangsu Province; the dispersant is a combination of alkylnaphthalenesulfonic acid formaldehyde condensate and alkylamide polyoxyethylene ether phosphate, with a weight ratio of 1:0.1; the alkylnaphthalenesulfonic acid formaldehyde condensate was purchased from Jinan Hongboli Chemical Co., Ltd.; the alkylamide polyoxyethylene ether phosphate was purchased from Guangzhou Bifeng Trading Co., Ltd.; the viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate, with a weight ratio of 1:0.5; the organic bentonite was purchased from Tuoyi New Materials (Guangzhou) Co., Ltd.; the base oil is a combination of castor oil and methyl oleate, with a weight ratio of 1:0.1.

[0097] The preparation method of the dispersible oil suspension concentrate is as follows: the herbicidal composition, emulsifier, wetting agent, dispersant, defoamer, viscosity regulator and base oil are mixed, and the mixture is dispersed at high shear for 30 minutes; and then ground until the D97 is 5 μm.

[0098] Example 3

[0099] Example 3 provides a herbicide dispersible oil suspension, which comprises at least the following components by weight: 50% of a herbicide composition, 20% of an emulsifier, 5% of a wetting agent, 5% of a dispersant, 10% of a viscosity modifier, and 100% of a base oil; the herbicide combination is a combination of benzylpyrazoline and glyphosate, with a weight ratio of 1:40; the emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1:0.5; the castor oil polyoxyethylene ether was purchased from Hai'an Petrochemical Plant in Jiangsu Province, specification EL30; the phenethylphenol polyoxyethylene ether sulfonate was purchased from Shandong Tiandao Bioengineering Co., Ltd., model 602 #; The wetting agent is alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, purchased from Hai'an Petrochemical Plant in Jiangsu Province; the dispersant is a combination of alkylnaphthalenesulfonic acid formaldehyde condensate and alkylamide polyoxyethylene ether phosphate, with a weight ratio of 1:1.5; the alkylnaphthalenesulfonic acid formaldehyde condensate was purchased from Jinan Hongboli Chemical Co., Ltd.; the alkylamide polyoxyethylene ether phosphate was purchased from Guangzhou Bifeng Trading Co., Ltd.; the viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate, with a weight ratio of 1:2; the organic bentonite was purchased from Tuoyi New Materials (Guangzhou) Co., Ltd.; the base oil is a combination of castor oil and methyl oleate, with a weight ratio of 1:10.

[0100] The preparation method of the dispersible oil suspension is as follows: the herbicidal composition, emulsifier, wetting agent, dispersant, defoamer, viscosity regulator and base oil are mixed, and high-speed shear dispersion is performed for 30 minutes; and then grinding is performed until the D97 is 1-10 μm.

[0101] Example 4

[0102] The difference between Example 4 and Example 1 is that the emulsifier does not include castor oil polyoxyethylene ether.

[0103] Example 5

[0104] The difference between Example 5 and Example 1 is that the emulsifier does not include phenethylphenol polyoxyethylene ether sulfonate.

[0105] Example 6

[0106] The difference between Example 6 and Example 1 is that the phenylethylphenol polyoxyethylene ether sulfonate in the emulsifier is replaced by alkylphenol polyoxyethylene ether.

[0107] Example 7

[0108] The difference between Example 7 and Example 1 is that the dispersant does not include alkylnaphthalenesulfonic acid formaldehyde condensate.

[0109] Example 8

[0110] The difference between Example 8 and Example 1 is that the dispersant does not include alkylamide polyoxyethylene ether phosphate.

[0111] Example 9

[0112] The difference between Example 9 and Example 1 is that the alkylnaphthalenesulfonic acid formaldehyde condensate in the dispersant is replaced by sodium lignin sulfonate.

[0113] Example 10

[0114] The difference between Example 10 and Example 1 is that the alkylamide polyoxyethylene ether phosphate in the dispersant is replaced by alkylphenol polyoxyethylene ether phosphate.

[0115] Example 11

[0116] The difference between Example 11 and Example 1 is that the viscosity regulator does not include magnesium aluminum silicate.

[0117] Example 12

[0118] The difference between Example 12 and Example 1 is that the base oil does not include methyl oleate.

[0119] Example 13

[0120] The difference between Example 13 and Example 1 is that the herbicidal combination is a combination of benzylpyridamole and glyphosate, with a weight ratio of 1:30.

[0121] Performance Testing

[0122] 1. Thermal storage stability:

[0123] Use a pipette to draw approximately 10g of the oil suspension concentrate sample into a clean ampoule. Seal the sample at high temperature and place it in a constant temperature (54 ± 2°C) incubator. After 14 days of hot storage, remove the sample and test various indicators such as the suspension rate and viscosity of the dispersible oil suspension concentrate. If all indicators before and after hot storage meet national standards, the hot storage is qualified. The sample is considered qualified after 2 years of room temperature storage. "√" indicates qualified; "×" indicates unqualified.

[0124] 2. Cold storage stability:

[0125] Use a pipette to draw approximately 80 mL of the oil suspension concentrate into a 100 mL beaker. Refrigerate in a refrigerator at (0±2°C) for one hour, stirring every 15 minutes for 15 seconds each time. Observe changes in appearance. Place the beaker in the refrigerator for another 7 days. After 7 days, remove the beaker and return it to room temperature. Test various indicators of the oil suspension concentrate, such as suspension rate and viscosity. If all indicators before and after cold storage meet national standards, the cold storage is qualified. The sample is considered qualified after 2 years of storage at room temperature. "√" indicates qualified; "×" indicates unqualified.

[0126] 3. Viscosity: The viscosity of the dispersible oil suspension was measured at room temperature using a NDJ-1 rotary viscometer. Each sample was measured three times and the average value was taken.

[0127] 4. Suspension rate: Test reference HG / T 2467.5-2003.

[0128] The test results are shown in Table 1.

[0129] Table 1. Performance test results of the embodiments

[0130]

[0131] 5. Prevention efficacy test:

[0132] Test sample:

[0133] Benpyraclostrobin, glyphosate.

[0134] Test target:

[0135] Conyzacanadensis (L.) Cronq., glyphosate-resistant, collected from Baihe Mountain, Changde City, Hunan Province;

[0136] Eleusine indica (L.) Gaertn., which is resistant to glyphosate, was collected from Ma'an Town, Huizhou City, Guangdong Province.

[0137] Test method:

[0138] Indoor culture of target materials

[0139] Mix the seeds of Erigeron candidum and Goosegrass with soil and sow them in a seedling tray. Transplant the seedlings when they are about 10 cm tall, one plant per paper cup. Place them in a greenhouse for normal cultivation. Spray the stems and leaves about 15 days after transplanting.

[0140] Treatment method:

[0141] According to the designed dosage, the crops were sprayed on a crawler crop sprayer (designed and manufactured by Engineer Research Ltd., UK) (spray pressure 1.95 kg / cm 2 , spray volume 500L / hm 2 , crawler speed 1.48 km / h), with three replicates. After treatment, the test materials were placed in the operating hall. After the pesticide solution dried naturally, they were placed in the greenhouse and managed according to conventional methods. The response of the test weeds to the pesticide was observed and recorded. After treatment, the weed control efficacy of the test pesticide was regularly assessed by visual inspection or fresh weight.

[0142] Statistical analysis method of test results:

[0143] Test drug ED 50 / ED 90 Value Calculation

[0144] Calculation was performed using DPS statistical analysis software

[0145] Calculation of co-toxicity coefficient:

[0146]

[0147] Among them: PA is the proportion of agent A in the active ingredients of the mixture, PB is the proportion of agent B in the active ingredients of the mixture. If the co-toxicity coefficient is less than 80, it is an antagonistic effect; if the co-toxicity coefficient is greater than 120, it is a synergistic effect; if the co-toxicity coefficient is between 80-120, it is an additive effect.

[0148] The results are shown in Tables 2 and 3, where A is benzylpyridamole and B is glyphosate.

[0149] Table 2 The results of the control effect test of the mixed use of benzylpyraclostrobin and glyphosate on glyphosate-resistant Erigeron truncatum

[0150]

[0151]

[0152] Table 3 The results of the control effect test of the mixed use of benzylpyraclostrobin and glyphosate on glyphosate-resistant goosegrass

[0153]

[0154] 6. Field efficacy test:

[0155] Test agent:

[0156] The herbicide dispersible oil suspension control agent of Example 13:

[0157] 10% benzylpyraclostrobin emulsion in water (Nantong Jiangshan Pesticide Chemical Co., Ltd.), 30% glyphosate soluble concentrate (trade name: Roundup)

[0158] Trial Location:

[0159] The Yangtze River embankment in Chizhou

[0160] Targets:

[0161] The dominant weeds are mainly Bermuda grass and Erigeron dactylon, which grow vigorously and densely, with an average plant height of 10-30 cm when treated; there are also other weeds such as annual ferns, water celery, crabgrass, bermudagrass, lychee grass, motherwort, cnidium monnieri and other small amounts.

[0162] Test method:

[0163] Plot division: Each treatment was repeated 3 times, randomly arranged, and each plot was 20m 2 .

[0164] Usage: On May 23, 2020, the stem and leaf spray treatment was carried out. The spraying equipment was a 3WBD-20L electric sprayer with a fan-shaped nozzle. The working pressure was 0.2-0.4Mpa, the spray volume was 45kg / mu, and the spray was uniform.

[0165] (Conventional weed control on levees requires 2-3 rounds of prevention and control, and the main pesticide used is a mixture of glyphosate, dimethoate, and dicamba, which Erigeron spp. is highly resistant to.)

[0166] Survey, recording and measurement methods:

[0167] Weather data: The day of application was sunny, with an average temperature of 20.4°C and a maximum temperature of 25.3°C, and a light breeze. There were many rainy days during the test period, but no obvious adverse conditions.

[0168] Weed survey: Visually inspect the weed death symptoms and speed 3, 6, 9, 12, and 16 days after application; 16 days after application, sample 3 points in each plot, survey 0.25 m at each point 2 The number of remaining Erigeron spp. plants was counted and the control efficacy was calculated.

[0169] The control effect on Erigeron chinensis weeds (16 days after treatment) is as follows:

[0170]

[0171] The foregoing examples are merely illustrative and serve to illustrate some of the features of the method of the present invention. The appended claims are intended to claim the widest possible scope that can be envisioned, and the embodiments presented herein are merely illustrative of selected implementations according to a combination of all possible embodiments. Therefore, it is the applicant's intention that the appended claims are not limited by the selection of examples illustrating the features of the present invention. Some numerical ranges used in the claims also include subranges therein, and variations in these ranges should also be interpreted as being covered by the appended claims where possible.

Claims

1. A herbicidal composition, It is characterized in that The composition comprises benzylpyrazone and glyphosate; the weight ratio of the benzylpyrazone to glyphosate is 1:(10-100).

2. A herbicidal composition preparation, It is characterized in that The herbicidal composition is composed of the herbicidal composition according to claim 1 and an auxiliary material acceptable in pesticides.

3. The herbicidal composition formulation according to claim 2, It is characterized in that The dosage form of the herbicidal composition preparation is selected from one of a soluble agent, a microemulsion, a dispersible oil suspension, a wettable powder and a water-dispersible granule.

4. The herbicidal composition formulation according to claim 2, It is characterized in that The weight percentage of the herbicidal composition in the herbicidal composition preparation is 5%-90%.

5. The herbicidal composition formulation according to claim 2, It is characterized in that The dosage form of the herbicidal composition preparation is a dispersible oil suspension; the pesticide-acceptable adjuvants include at least one of an emulsifier, a wetting agent, a dispersant, a stabilizer, a defoaming agent, a viscosity regulator, and a base oil.

6. The herbicidal composition formulation according to claim 5, It is characterized in that The emulsifier is selected from at least one of castor oil polyoxyethylene ether, calcium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, alkylphenol formaldehyde resin polyoxyethylene ether, sorbitan monostearate, sorbitan monostearate polyoxyethylene ether, phenethylphenol polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, alkoxy polyoxyethylene ether sulfonate, fatty alcohol sulfate, alkyl phosphate salt, fatty alcohol polyoxyethylene ether sulfate, EO-PO block copolymer and phenethylphenol polyoxyethylene ether sulfonate.

7. The herbicidal composition formulation according to claim 6, It is characterized in that The emulsifier is a combination of castor oil polyoxyethylene ether and phenethylphenol polyoxyethylene ether sulfonate, with a weight ratio of 1: (0.1-0.5).

8. The herbicidal composition formulation according to claim 5, It is characterized in that The dispersant is selected from at least one of polycarboxylates, lignin sulfonates, EO-PO block copolymers, phosphates and their salts, sulfonates, alkylnaphthalene sulfonates, alkylphenol polyoxyethylene ethers and fatty alcohol polyoxyethylene ethers.

9. The herbicidal composition formulation according to claim 5, It is characterized in that The viscosity regulator is a combination of organic bentonite and magnesium aluminum silicate, with a weight ratio of 1:(0.5-2).

10. Use of the herbicidal composition according to claim 1, It is characterized in that Used to control weeds in non-cultivated land.