CN112155015B - Composition containing flufenacet and diflufenican as well as preparation method and application thereof - Google Patents
Composition containing flufenacet and diflufenican as well as preparation method and application thereof Download PDFInfo
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- CN112155015B CN112155015B CN202011086042.3A CN202011086042A CN112155015B CN 112155015 B CN112155015 B CN 112155015B CN 202011086042 A CN202011086042 A CN 202011086042A CN 112155015 B CN112155015 B CN 112155015B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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Abstract
The invention relates to the technical field of pesticides, in particular to a composition containing flufenacet and diflufenican, a preparation method and application thereof. The composition comprises flufenacet and diflufenican in a weight ratio of (5-30): (15-30). The invention provides a composition which has high control effect on annual weeds in wheat fields, such as barnyard grass, crab grass, green bristlegrass, eleusine pratense and the like, through the combined action of flufenacet and diflufenican. The applicant finds that the stability of flufenacet and diflufenican in water can be improved, the aggregation or precipitation of particles at long time or high temperature can be reduced, the storage stability and the fluidity of the composition can be improved, and the service life of the composition can be prolonged by selecting a proper wetting dispersant, a proper thickening agent and the like.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a composition containing flufenacet and diflufenican, a preparation method and application thereof.
Background
With the advancement and development of modern agriculture and the enlargement of planting scale, the demand of our country for pesticides is increasing, and among them, herbicides as necessities in agricultural production are receiving wide attention from people. However, the use of a large amount of pesticides brings about potential hazards such as soil structure destruction and weed drug resistance enhancement. In modern agricultural production, national policy leads to higher requirements on the safety and the reasonability of agricultural herbicides. Therefore, the development of new, highly effective, broad-spectrum, low-dose herbicides has become an urgent problem for the research and development personnel of agricultural chemicals.
Flufenacet is a herbicide variety discovered by bayer crop science, introduced in 1995 at the british brayton plant protection conference. The active ingredient belongs to an aryloxyacetamide compound as well as mefenacet, has a similar weed control spectrum as a chloroacetamide herbicide, and can be widely used for controlling annual gramineous weeds, nutgrass flatsedge and small-grain broadleaf weeds.
Diflufenican belongs to carotenoid biosynthesis inhibitors and is a broad-spectrum selective wheat field herbicide. The residual period in soil is longer. Is suitable for preventing and killing various broad-leaved weeds such as cleavers, polygonum convolvulus, purslane, black nightshade, chickweed, vetch, bindweed, weasel flower, polygonum cuspidatum, polygonum orientale, amaranthus retroflexus, dayflower, elsholtzia, Thalathus, vetch, descurainia sophia and Convolvulus in barley and wheat fields.
The method has the advantages that different raw medicines are compounded to improve the drug effect and reduce the drug resistance, and the water aqua is the current development direction due to small environmental pollution caused by using water as a carrier, but the low solubility of flufenacet and diflufenican in water causes difficulties in the stability, the flowability and the like of the water aqua.
Disclosure of Invention
In order to solve the problems, the invention provides a composition containing flufenacet and diflufenican, which comprises the following components in parts by weight (5-30): (15-30).
As a preferable technical scheme, the weight ratio of the flufenacet to the diflufenican is (10-25): (20-30).
As a preferable technical scheme, the weight ratio of flufenacet to diflufenican is (10-20): (20-25).
As a preferable technical scheme, the total weight of the flufenacet and the diflufenican accounts for 30-40 wt% of the weight of the composition.
As a preferable technical scheme, the formulation of the composition is selected from one or more of missible oil, microemulsion, water dispersible granules, wettable powder, water dispersible granules and suspending agents.
As a preferable technical scheme, the preparation raw material of the composition also comprises a wetting dispersant, and the wetting dispersant accounts for 2-8 wt% of the composition.
In a preferred embodiment of the present invention, the wetting dispersant comprises at least one anionic wetting dispersant and at least one nonionic wetting dispersant.
As a preferable technical scheme of the invention, the preparation raw materials of the composition also comprise at least one thickening agent, and the thickening agent accounts for 0.1-2 wt% of the weight of the composition.
In a second aspect, the present invention provides a process for the preparation of a composition containing flufenacet and diflufenican as described above, said process comprising the steps of:
mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
In a third aspect, the invention provides the application of the composition containing flufenacet and diflufenican for controlling plant weeds.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a composition which has high control effect on annual weeds in wheat fields, such as barnyard grass, crab grass, green bristlegrass, eleusine pratense and the like, through the combined action of flufenacet and diflufenican. The applicant finds that the stability of flufenacet and diflufenican in water can be improved, the aggregation or precipitation of particles at long time or high temperature can be reduced, the storage stability and the fluidity of the composition can be improved, and the service life of the composition can be prolonged by selecting a proper wetting dispersant, a proper thickening agent and the like.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of 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.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.
The applicant finds that the flufenacet and the diflufenican are compounded in a certain range, so that the weed control range and the weed control effect can be expanded, and the compound herbicide has high control effect on annual weeds in wheat fields, such as barnyard grass, crab grass, green bristlegrass, goosegrass herb and the like. The invention provides a composition containing flufenacet and diflufenican, which comprises the following components in parts by weight (5-30): (15-30). In a preferred embodiment, the weight ratio of flufenacet to diflufenican in the present invention is (10-25): (20-30); in a preferred embodiment, the weight ratio of flufenacet to diflufenican in the present invention is (10-20): (20-25); in a preferred embodiment, the weight ratio of flufenacet to diflufenican in accordance with the present invention is 15: 22.5.
flufenacet
Flufenacet is a herbicide variety discovered by bayer crop science, introduced in 1995 at the british brayton plant protection conference. The active ingredient belongs to an aryloxyacetamide compound as well as mefenacet, has a similar weed control spectrum as a chloroacetamide herbicide, and can be widely used for controlling annual gramineous weeds, nutgrass flatsedge and small-grain broadleaf weeds. Flufenacet is mainly used for soil treatment, and the solubility in water (mg/l,25 ℃) can be used before and after germination, namely 56(pH4, 7) and 54(pH 9). In one embodiment, the flufenacet of the present invention is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican
Diflufenican belongs to carotenoid biosynthesis inhibitors and is a broad-spectrum selective wheat field herbicide. The residual period in soil is longer. Is suitable for preventing and killing various broad-leaved weeds such as cleavers, polygonum convolvulus, purslane, black nightshade, chickweed, vetch, bindweed, weasel flower, polygonum cuspidatum, polygonum orientale, amaranthus retroflexus, dayflower, elsholtzia, Thalathus, vetch, descurainia sophia and Convolvulus in barley and wheat fields. Diflufenican belongs to carotenoid biosynthesis inhibitors. The treated plant plants have a reduced carotenoid content, which in turn leads to chlorophyll destruction, cell membrane rupture and weeds appearing as sprouts that are bleached or whitened. Before weed germination, a leaching-resistant pesticide soil layer can be formed on the upper surface, and the activity of the weed can be maintained in the whole growth period of crops. When the weeds germinate, the agent is absorbed by the sprouts or the root system and finally dies. The death rate is related to the intensity of light, which is fast and slow. In one embodiment, diflufenican of the present invention is available from dream biotechnology, ltd, north of hu.
In one embodiment, the composition of the invention has a dosage form selected from one or more of missible oil, microemulsion, water dispersible granule, wettable powder, water dispersible granule and suspending agent; in a preferred embodiment, the composition of the present invention is in the form of a suspension.
In one embodiment, the raw materials for preparing the composition of the present invention further comprise at least one thickener.
Thickening agent
In one embodiment, the thickener of the present invention comprises 0.1 to 2 wt% of the composition; in a preferred embodiment, the thickener of the present invention is 0.2 to 1 wt% of the composition; in one embodiment, the thickener of the present invention comprises 0.2 to 0.8 wt% of the composition.
The applicant finds that the composition provided by the invention contains more flufenacet and diflufenican, precipitates and precipitates can be caused by gravity or solubility difference in the storage process, the xanthan gum is added, the xanthan gum can be quickly dissolved in water, and the water and the flufenacet can form a gel-like network structure through hydrogen bond interaction to support particles such as the flufenacet and the diflufenican and reduce the precipitates or the precipitates. Preferably, the thickening agent is selected from one or more of xanthan gum, Arabic gum, magnesium aluminum silicate, chitosan and sodium alginate. Further, the thickener of the present invention comprises xanthan gum.
Xanthan gum (Xanthan gum), also known as Xanthan gum, is a microbial extracellular polysaccharide with wide action produced by Xanthomonas campestris (Xanthomonas campestris) by fermentation engineering with carbohydrate as main raw material (such as corn starch). The microbial polysaccharide has unique rheological property, good water solubility, stability to heat and acid and alkali, and good compatibility with various salts, can be widely applied to more than 20 industries such as food, petroleum, medicine and the like as a thickening agent, a suspending agent, an emulsifying agent and a stabilizing agent, and is the microbial polysaccharide which has the largest production scale and extremely wide application in the world at present; examples of xanthan gum include, but are not limited to, F-200F (mesh 200), F-80LD (mesh 80), F-40 (mesh 40) from Zibo sea billulans chemical Co., Ltd. In a preferred embodiment, the mesh number of the xanthan gum is 150-250 mesh.
The mesh count is the number of mesh holes per square inch.
The applicant has found that as the composition is stored for extended periods of time, or at elevated temperatures, the stretched xanthan chains entangle and curl with each other, causing a significant increase in viscosity, resulting in increased sheeting, flocculation or sedimentation, and as the chains interact, pseudoplasticity diminishes and flowability deteriorates. However, the applicant found that when a certain amount of acrylic acid copolymer and xanthan gum are used together as a thickener, the acrylic acid copolymer and xanthan gum can rapidly diffuse together in water to form a cross-linked network with water to increase the hydration volume due to the action of the hydrophilic carboxylate ions in the acrylic acid copolymer, and the anion in the acrylic acid copolymer and the anion at the end of the xanthan gum branched chain can favorably repel each other to improve the viscosity increase and promote the stability and fluidity during long-term or high-temperature storage. More preferably, the thickener of the present invention further comprises an acrylate copolymer.
Acrylate copolymer thickeners, dispersions of lightly crosslinked acrylic polymers, provide excellent stability and thickening properties to surfactant systems and provide excellent suspensibility even in low viscosity formulations. Examples of acrylate copolymers include, but are not limited to, T-251 of Shenzhen Haihun chemical, ASE-60 of Rohm and Haas (solid content 28 wt%, distributed viscosity at 25 ℃ of 10cps), ACYSOLTMTT-935 (solid content 30 wt%, distributed viscosity at 25 ℃ of 0-25 cps), and Dow TT-615 (solid content 30 wt%, distributed viscosity at 25 ℃ of 20 cps). In a preferred embodiment, the acrylate copolymer of the present invention has a solid content of 25 to 35 wt% and a Brookfield viscosity of 8 to 15cps at 25 ℃.
The solid content is the mass percentage of the dried residual part in the total amount. Can be tested by drying in an oven at 103 degrees for four hours.
Brookfield viscosity is the viscosity obtained by Brookfield viscometer test.
And the applicant found that the amount of xanthan gum and acrylic copolymer needs to be controlled in a certain ratio, when the amount of acrylic copolymer is small, entanglement and curling between xanthan gums cannot be suppressed, and when the amount of acrylic copolymer is too large, too much anion easily causes counter ion to enter an electric double layer, compresses the thickness of the double electrode layer, and affects stability. The applicant finds that when a certain mesh of xanthan gum and acrylic copolymer are mixed, the xanthan gum and the acrylic copolymer are more conveniently and uniformly distributed in a cross network, and the gel or paste phenomena of the xanthan gum and the like caused by the acrylic copolymer are favorably improved. Further preferably, the weight ratio of xanthan gum to acrylate copolymer according to the invention is 1: (0.2-0.8); in a preferred embodiment, the weight ratio of xanthan gum to acrylate copolymer according to the invention is 1: (0.2-0.4).
In one embodiment, the raw materials for preparing the composition of the present invention further comprise a wetting dispersant.
Wetting and dispersing agent
In one embodiment, the wetting and dispersing agent of the present invention comprises 2 to 8 wt% of the composition; in a preferred embodiment, the wetting and dispersing agent accounts for 3-8 wt% of the composition; in a preferred embodiment, the wetting and dispersing agent comprises 4 to 7 wt% of the composition.
Preferably, the wetting and dispersing agents of the present invention include at least one anionic wetting and dispersing agent and at least one nonionic wetting and dispersing agent. More preferably, the nonionic wetting dispersant of the present invention is selected from one or more of phenethyl phenol polyoxyethylene polyoxypropylene ether, castor oil polyoxyethylene ether, sorbitan fatty acid ester, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, polyethylene glycol, and alkylolamide polyoxyethylene ether.
The applicant found that at higher temperatures, the forces between the carboxylate ions in the acrylic copolymer and water are reduced, so that the forces of the cross-network are reduced, and the active ingredients and the like may be precipitated or separated out, and the movement of the xanthan gum molecular chains is increased at high temperatures, and the entanglement and the like are also increased, so that the viscosity of the composition is greatly improved. Applicants have found that by using a polyhydroxy sorbitan mono fatty acid ester as the non-ionic wetting dispersant, a certain amount of water-bound thickener and wetting dispersant interact to promote cross-network stabilization and thus storage stability at high temperatures, since more of the alcoholic hydroxyl groups in the sorbitan fatty acid ester can form relatively more stable hydrogen bonds with the acrylic acid copolymer, xanthan gum, and the like. Further preferably, the non-ionic wetting dispersant of the present invention comprises a sorbitan fatty acid ester.
The sorbitan fatty acid ester is oil-soluble liquid or wax, can be dissolved in hot oil and various organic solvents, is insoluble in water, and has excellent emulsifying capacity and dispersing power. Examples of the sorbitan fatty acid ester include, but are not limited to, S-20 (hydroxyl value: 330 to 360mgKOH/g), S-40 (hydroxyl value: 255 to 290mgKOH/g), S-60 (hydroxyl value: 240 to 270mgKOH/g), S-80 (hydroxyl value: 190 to 220mgKOH/g), and S-85 (hydroxyl value: 60 to 80mgKOH/g) of Hainan petrochemical plant of Jiangsu province. In a preferred embodiment, the hydroxyl value of the sorbitan fatty acid ester is 255-360 mgKOH/g.
The applicant has found that as the composition is stored for extended periods of time, or at elevated temperatures, the stretched xanthan chains entangle and curl with each other, causing a significant increase in viscosity, resulting in increased sheeting, flocculation or sedimentation, and as the chains interact, pseudoplasticity diminishes and flowability deteriorates. However, the applicant found that when a certain amount of acrylic acid copolymer and xanthan gum are used together as a thickener, the acrylic acid copolymer and xanthan gum can rapidly diffuse together in water to form a cross-linked network with water to increase the hydration volume due to the action of the hydrophilic carboxylate ions in the acrylic acid copolymer, and the anion in the acrylic acid copolymer and the anion at the end of the xanthan gum branched chain can favorably repel each other to improve the viscosity increase and promote the stability and fluidity during long-term or high-temperature storage. Still more preferably, the non-ionic wetting dispersant of the present invention further comprises polyethylene glycol.
Polyethylene glycol is a compound with a chemical formula of HO (CH2CH2O) nH, and the series of products have no irritation, slightly bitter taste, good water solubility and good compatibility with a plurality of organic matter components. They have excellent lubricity, moisture retention, dispersibility, adhesives, antistatic agents, softeners and the like, and are widely applied in the industries of cosmetics, pharmacy, chemical fibers, rubber, plastics, papermaking, paint, electroplating, pesticides, metal processing, food processing and the like. As examples of polyethylene glycol, there may be mentioned, but not limited to, PEG-400 (number average molecular weight of 400), PEG-600 (number average molecular weight of 600), PEG-800 (number average molecular weight of 800); in a preferred embodiment, the polyethylene glycol of the present invention has a number average molecular weight of 400 to 600.
And the applicant found that the ratio of the two molecular wetting dispersants needs to be controlled, when the polyethylene glycol is less, agglomeration, precipitation and the like between the active ingredients are easily caused due to the weaker bit group and the higher lipophilicity of the sorbitan mono-fatty acid ester, and when the polyethylene glycol is more, the probability of entanglement between the flexible polyethylene glycol extending outside the electric double layer and the thickening agent is increased, pseudoplasticity is reduced, and the fluidity of the composition is affected. In a preferred embodiment, the weight ratio of the sorbitan fatty acid ester to the polyethylene glycol is (2-3): 1.
applicants have found that while the addition of a nonionic wetting dispersant containing a polyhydroxy group reduces the entanglement of xanthan gum at high temperatures and promotes fluidity, it also results in a reduced hydration volume for interaction with the thickener, weakening the interaction with the aqueous phase, and especially when a small alcohol antifreeze is added, because of the action of the thickener and antifreeze, further reduces the hydration volume while increasing viscosity, resulting in increased drainage, and applicants have found that when a certain amount of a sulfonate anionic surfactant is added, because of the higher sulfonate dosage form, competitive adsorption with the thickener promotes stabilization of the hydration volume. Preferably, the anionic wetting dispersant of the present invention is selected from one or more of sulfonate, sulfate, carboxylate, and examples of sulfonate include, but are not limited to, alkyl naphthalene sulfonate, dodecylbenzene sulfonate, lignin sulfonate, sodium naphthalene sulfonate formaldehyde condensate; as examples of carboxylates, including, but not limited to, dioctyl sodium sulfosuccinate and acrylic acid homopolymer sodium salt; as examples of sulfates, there are included, but not limited to, alkyl sulfates. Preferably, the anionic wetting dispersant of the present invention is a sulfonate. The sulfonate is not particularly limited in the present invention, and may be a sodium salt, a potassium salt, an ammonium salt, etc. of sulfonic acid.
And the applicant finds that when the sulfonate containing the aryl and the alkyl is adopted to act together, the sulfonate and the flufenacet and the diflufenican are strongly adsorbed, on one hand, the aryl, the flufenacet and the diflufenican have similar structures and are favorable for solubility in water, and on the other hand, the alkyl is wound on the outer side of an inner layer of an electric double layer formed by the aryl and the sulfonic acid group and can interact with a nonionic wetting agent to increase the stability of the electric double layer. And the sulfonate, the polyhydroxy nonionic wetting agent, water and the like act to promote a high-elasticity hydrated film to be formed outside the double-electrode layer, so that the storage stability is promoted while the bit group is further improved, and the water separation is improved. More preferably, the anionic wetting dispersants of the present invention are alkyl naphthalene sulfonates and dodecyl sulfonates. In a preferred embodiment, the alkyl naphthalene sulfonate and the dodecyl sulfonate of the present invention are present in a weight ratio of 1: (0.5 to 1).
Further preferably, the alkyl naphthalene sulfonate of the present invention is a C8-C14 alkyl naphthalene sulfonate. In a preferred embodiment, the alkylnaphthalene sulfonates of the present invention are available from C8-C14 as research institute of Shaoxing Homopolimus organic chemistry.
The applicant found that in order to improve the stability of the composition, it is necessary to ensure the structural stability of the electric double layer and a certain range of viscosity, when the viscosity is low, the precipitation is easy due to gravity and the like, and when the viscosity is too high, the phenomena of aggregation increase, fluidity increase, even shear thickening and no flowing are caused, and when a certain amount of the thickening agent is used, a proper amount of initial viscosity is achieved, and a certain stability of the electric double layer and the viscosity is maintained through the combined action with other preparation raw materials, so that the service life is prolonged, and the use of the composition is promoted. More preferably, the weight ratio of the anionic wetting dispersant to the nonionic wetting dispersant is (2-3): (2-3).
In one embodiment, the starting material for the preparation of the composition of the present invention comprises the balance water.
In one embodiment, the composition of the present invention further comprises one or more of a stabilizer, an anti-freeze agent, an anti-foam agent, a ph adjusting agent. Examples of defoaming agents include, but are not limited to, silicones, C8-C10 fatty alcohols, C10-C20 saturated aliphatic carboxylic acids and their esters and ester-ether type compounds, in one embodiment, the defoaming agent of the present invention comprises 0 to 1 wt% of the composition; as examples of anti-freeze agents, including, but not limited to, ethylene glycol, propylene glycol, and glycerin, in one embodiment, the anti-freeze agent of the present invention comprises 1 to 10 wt% of the composition; examples of the pH adjusting agent include, but are not limited to, those selected from acetic acid, hydrochloric acid, sodium hydroxide, potassium hydroxide, ammonium hydroxide and ammonium salts and triethanolamine, and in one embodiment, the pH adjusting agent of the present invention is 0 to 2 wt% of the composition.
In a second aspect, the present invention provides a process for the preparation of a composition containing flufenacet and diflufenican as described above, said process comprising the steps of:
mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
In a third aspect, the invention provides the use of a composition containing flufenacet and diflufenican as described above for controlling plant weeds.
Examples
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
Example 1
This example provides a composition prepared from, by weight percent, 15 wt% flufenacet, 22.5 wt% diflufenican, 0.3 wt% thickener, 7 wt% wetting and dispersing agent, 5 wt% antifreeze agent, and the balance water; the thickening agent comprises xanthan gum and acrylate copolymer thickening agent, and the weight ratio of the xanthan gum to the acrylate copolymer thickening agent is 1: 0.3, wherein the wetting dispersant comprises a non-ionic wetting dispersant and an anionic wetting dispersant, and the weight ratio of the non-ionic wetting dispersant to the anionic wetting dispersant is 1: 1, the non-ionic wetting dispersant comprises polyethylene glycol, and the anionic wetting dispersant comprises sodium dodecyl sulfate; the antifreezing agent is glycerol; the composition is in the form of a suspension.
The flufenacet is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican is available from Hubei Yuanmeng Biotech limited.
The xanthan gum is purchased from F-200F of Zibo sea wave chemical Co.
The acrylate copolymer was purchased from ASE-60 of Rohm and Haas.
The polyethylene glycol was purchased from PEG-400.
This example also provides a method of preparing a composition as described above, comprising the steps of: mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
Example 2
This example provides a composition prepared from, by weight percent, 15 wt% flufenacet, 22.5 wt% diflufenican, 0.3 wt% thickener, 7 wt% wetting and dispersing agent, 5 wt% antifreeze agent, and the balance water; the thickening agent comprises xanthan gum and acrylate copolymer thickening agent, and the weight ratio of the xanthan gum to the acrylate copolymer thickening agent is 1: 0.3, wherein the wetting dispersant comprises a non-ionic wetting dispersant and an anionic wetting dispersant, and the weight ratio of the non-ionic wetting dispersant to the anionic wetting dispersant is 1: 1, the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol, and the weight ratio is 3: 1, the anionic wetting dispersant comprises sodium dodecyl sulfate; the antifreezing agent is glycerol; the composition is in the form of a suspension.
The flufenacet is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican is available from Hubei Yuanmeng Biotech limited.
The xanthan gum is purchased from F-200F of Zibo sea wave chemical Co.
The acrylate copolymer was purchased from ASE-60 of Rohm and Haas.
The sorbitan fatty acid ester is purchased from S-40 of the Haian petrochemical plant of Jiangsu province.
The polyethylene glycol was purchased from PEG-400.
This example also provides a method of preparing a composition as described above, comprising the steps of: mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
Example 3
This example provides a composition prepared from, by weight, 10 wt% flufenacet, 20 wt% diflufenican, 0.8 wt% thickener, 3 wt% wetting and dispersing agent, 5 wt% antifreeze agent, and the balance water; the thickening agent comprises xanthan gum and acrylate copolymer thickening agent, and the weight ratio of the xanthan gum to the acrylate copolymer thickening agent is 1: 0.8, wherein the wetting dispersant comprises a non-ionic wetting dispersant and an anionic wetting dispersant, and the weight ratio of the non-ionic wetting dispersant to the anionic wetting dispersant is 2: 3, the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol, and the weight ratio is 2: 1, the anionic wetting dispersant comprises alkyl naphthalene sulfonate and sodium dodecyl sulfate, and the weight ratio of the alkyl naphthalene sulfonate to the sodium dodecyl sulfate is 1: 0.5; the antifreezing agent is glycerol; the composition is in the form of a suspension.
The flufenacet is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican is available from Hubei Yuanmeng Biotech limited.
The xanthan gum is purchased from F-200F of Zibo sea wave chemical Co.
The acrylate copolymer was purchased from ASE-60 of Rohm and Haas.
The sorbitan fatty acid ester is purchased from S-20 of the Haian petrochemical plant of Jiangsu province.
The polyethylene glycol was purchased from PEG-600.
The alkylnaphthalene sulfonates were purchased from C8-C14, institute of Shaoxing Shangymo organic chemistry.
This example also provides a method of preparing a composition as described above, comprising the steps of: mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
Example 4
This example provides a composition prepared from, by weight percent, 15 wt% flufenacet, 25 wt% diflufenican, 0.6 wt% thickener, 7 wt% wetting and dispersing agent, 5 wt% antifreeze agent, and the balance water; the thickening agent comprises xanthan gum and acrylate copolymer thickening agent, and the weight ratio of the xanthan gum to the acrylate copolymer thickening agent is 1: 0.4, wherein the wetting dispersant comprises a non-ionic wetting dispersant and an anionic wetting dispersant, and the weight ratio of the non-ionic wetting dispersant to the anionic wetting dispersant is 1: 1, the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol, and the weight ratio is 3: 1, the anionic wetting dispersant comprises alkyl naphthalene sulfonate and sodium dodecyl sulfate, and the weight ratio of the alkyl naphthalene sulfonate to the sodium dodecyl sulfate is 1: 1; the antifreezing agent is glycerol; the composition is in the form of a suspension.
The flufenacet is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican is available from Hubei Yuanmeng Biotech limited.
The xanthan gum is purchased from F-200F of Zibo sea wave chemical Co.
The acrylate copolymer was purchased from ASE-60 of Rohm and Haas.
The sorbitan fatty acid ester is purchased from S-40 of the Haian petrochemical plant of Jiangsu province.
The polyethylene glycol was purchased from PEG-400.
The alkylnaphthalene sulfonates were purchased from C8-C14, institute of Shaoxing Shangymo organic chemistry.
This example also provides a method of preparing a composition as described above, comprising the steps of: mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
Example 5
This example provides a composition prepared from, by weight percent, 15 wt% flufenacet, 22.5 wt% diflufenican, 0.3 wt% thickener, 7 wt% wetting and dispersing agent, 5 wt% antifreeze agent, and the balance water; the thickening agent comprises xanthan gum and acrylate copolymer thickening agent, and the weight ratio of the xanthan gum to the acrylate copolymer thickening agent is 1: 0.3, wherein the wetting dispersant comprises a non-ionic wetting dispersant and an anionic wetting dispersant, and the weight ratio of the non-ionic wetting dispersant to the anionic wetting dispersant is 1: 1, the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol, and the weight ratio is 3: 1, the anionic wetting dispersant comprises alkyl naphthalene sulfonate and sodium dodecyl sulfate, and the weight ratio of the alkyl naphthalene sulfonate to the sodium dodecyl sulfate is 1: 0.8; the antifreezing agent is glycerol; the composition is in the form of a suspension.
The flufenacet is purchased from Jiangsu photobiology technologies, Inc.
Diflufenican is available from Hubei Yuanmeng Biotech limited.
The xanthan gum is purchased from F-200F of Zibo sea wave chemical Co.
The acrylate copolymer was purchased from ASE-60 of Rohm and Haas.
The sorbitan fatty acid ester is purchased from S-40 of the Haian petrochemical plant of Jiangsu province.
The polyethylene glycol was purchased from PEG-400.
The alkylnaphthalene sulfonates were purchased from C8-C14, institute of Shaoxing Shangymo organic chemistry.
This example also provides a method of preparing a composition as described above, comprising the steps of: mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
Example 6
This example provides a composition, which is specifically illustrated in example 1, except that the acrylate copolymer thickener is replaced with sodium alginate, available from Shanghao Hay seaweed industries, Inc.
This example also provides a method for preparing the composition, which is the same as that described in example 1.
Example 7
This example provides a composition, which is specifically described in example 1, except that the thickening agent comprises xanthan gum and an acrylate copolymer thickening agent in a weight ratio of 1: 0.01.
this example also provides a method for preparing the composition, which is the same as that described in example 1.
Example 8
This example provides a composition, which is specifically described in example 1, except that the thickening agent comprises xanthan gum and an acrylate copolymer thickening agent in a weight ratio of 1: 1.
this example also provides a method for preparing the composition, which is the same as that described in example 1.
Example 9
This example provides a composition which is specifically embodied in the same manner as example 1 except that the acrylate copolymer thickener is available from Dow TT-615.
This example also provides a method for preparing the composition, which is the same as that described in example 1.
Example 10
This example provides a composition, which is similar to example 2, except that the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol in a weight ratio of 0.5: 1.
this example also provides a method for preparing the composition, which is described in example 2.
Example 11
This example provides a composition, which is similar to example 2, except that the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol in a weight ratio of 6: 1.
this example also provides a method of preparing a composition, as embodied in example 11.
Example 12
This example provides a composition, which is similar to example 2, except that the sorbitan fatty acid ester is obtained from S-85 of Haian petrochemical plant of Jiangsu province.
This example also provides a method for preparing the composition, which is described in example 2.
Example 13
This example provides a composition which is similar to example 2, except that the polyethylene glycol is available from PEG-800.
This example also provides a method for preparing the composition, which is described in example 2.
Example 14
This example provides a composition as in example 5, except that the anionic wetting dispersant comprises sodium salt of naphthalene sulfonic acid and sodium lauryl sulfate in a weight ratio of 1: 0.8.
this example also provides a method for preparing the composition, which is described in example 5.
Example 15
This example provides a composition, which is specifically described in example 5, except that the anionic wetting dispersant comprises alkyl naphthalene sulfonate and sodium dodecyl sulfate in a weight ratio of 1: 0.2.
this example also provides a method for preparing the composition, which is described in example 5.
Example 16
This example provides a composition, which is specifically described in example 5, except that the anionic wetting dispersant comprises alkyl naphthalene sulfonate and sodium dodecyl sulfate in a weight ratio of 1: 1.5.
this example also provides a method for preparing the composition, which is described in example 5.
Evaluation of Performance
1. Storage stability at normal temperature: the compositions provided in the examples were placed in a glass container, sealed at (23 ± 2) ° c for 6 months, 9 months, and 12 months, and observed whether solid matter was deposited on the side wall of the container or whether precipitation occurred on the bottom of the container, wherein grade 1 showed no wall deposition and precipitation, grade 2 showed slight wall deposition and no precipitation, grade 3 showed wall deposition, slight precipitation, grade 4 showed wall deposition and precipitation, and grade 5 showed wall deposition and precipitation, and the results are shown in table 1.
Table 1 performance characterization test
2. Heat storage stability: after the compositions provided in the examples were placed in a glass container and sealed at (54 ± 2) ° c for 7 days, 14 days, 28 days and 35 days, whether solid matter was adhered to the side wall of the container or whether precipitation occurred at the bottom of the container was observed, wherein grade 1 shows no wall adhesion and precipitation, grade 2 shows slight wall adhesion and no precipitation, grade 3 shows general wall adhesion and slight precipitation, grade 4 shows general wall adhesion and precipitation, and grade 5 shows remarkable wall adhesion and precipitation, and the results are shown in table 2.
Table 2 characterization test of properties
3. Heat storage fluidity: placing the composition provided in the example in a glass container, sealing at (54 + -2) ° c, storing for 28 days, shaking the container, and observing the flow state, wherein grade 1 is that the composition can recover the flow by slightly shaking the container, the container is vertical, and the bottom is free from caking; grade 2, slightly shaking the container, the composition can flow again, the container is vertical, and a small amount of lumps are on the bottom; grade 3, shaking the container with force to recover the flow of the composition, making the container vertical and having a small amount of lumps at the bottom; the 4-stage is that the container is shaken vigorously, and the composition can not flow again and is in a flocculation state. The results are shown in Table 3.
Table 3 performance characterization test
4. Water separation rate: after the composition provided in the example was stored at (54 ± 2) ° c for 14 days, 5m was taken out after centrifugation at 3000r/min for 30min, and the water separation volume (mL) was recorded, and the water separation rate was 100% per 5mL, wherein the water separation rate was less than 0.5% in stage 1, less than 1.5% in stage 2, 0.5% or more in stage 2, less than 3% in stage 3, 1.5% or more in stage 4, less than 5% in stage 4, 3% or more in stage 2, and 5% or more in stage 2, and the results are shown in table 4.
Table 4 characterization test of properties
| Examples | Water separation rate |
| 1 | Stage 2 |
| 2 | Grade 3 |
| 3 | Stage 2 |
| 4 | Level 1 |
| 5 | Level 1 |
| 11 | 4 stage |
| 14 | 4 stage |
| 15 | Stage 2 |
| 16 | Stage 2 |
As can be seen from the test results in tables 1 to 4, the composition provided by the invention has good weeding performance, and particularly has high control effect on annual weeds in wheat fields, such as barnyard grass, large crabgrass, green bristlegrass, eleusine pratense, and the like; the composition provided by the invention has high storage and fluidity and can meet the requirement of long-term use.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (6)
1. The composition containing flufenacet and diflufenican is characterized by comprising the following components in parts by weight (5-30): (15-30);
the raw materials for preparing the composition also comprise a wetting dispersant, wherein the wetting dispersant accounts for 2-8 wt% of the composition, and the wetting dispersant comprises at least one anionic wetting dispersant and at least one nonionic wetting dispersant;
the nonionic wetting dispersant comprises sorbitan fatty acid ester and polyethylene glycol in a weight ratio of (2-3): 1, the hydroxyl value of the sorbitan fatty acid ester is 255-360 mgKOH/g; the anionic wetting dispersant is C8-C14 alkyl naphthalene sulfonate and dodecyl sulfonate in the weight ratio of 1: (0.5 to 1); the number average molecular weight of the polyethylene glycol is 400-600;
the raw materials for preparing the composition also comprise at least one thickening agent, wherein the thickening agent accounts for 0.1-2 wt% of the weight of the composition, the thickening agent comprises a xanthan gum and an acrylate copolymer, the solid content of the acrylate copolymer is 25-35 wt%, the Brookfield viscosity at 25 ℃ is 8-15 cps, the weight ratio of the xanthan gum to the acrylate copolymer is 1: (0.2 to 0.4);
the total weight of the flufenacet and the diflufenican accounts for 30-40 wt% of the weight of the composition.
2. The composition containing flufenacet and diflufenican according to claim 1, wherein the weight ratio of flufenacet to diflufenican is (10-25): (20-30).
3. The composition containing flufenacet and diflufenican according to claim 2, wherein the weight ratio of flufenacet to diflufenican is (10-20): (20-25).
4. The composition containing flufenacet and diflufenican according to claim 1, wherein the composition is in a dosage form selected from one or more of emulsifiable concentrate, microemulsion, water dispersible granules, wettable powder, water dispersible granules and suspending agents.
5. A method for preparing a composition containing flufenacet and diflufenican according to any of claims 1-4, comprising the steps of:
mixing, grinding and filtering the preparation raw materials of the composition to obtain the composition.
6. Use of a composition containing flufenacet and diflufenican according to any one of claims 1-4 for controlling plant weeds.
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| JP5563773B2 (en) * | 2008-12-17 | 2014-07-30 | バイエル・クロップサイエンス・アーゲー | Herbicidal composition |
| WO2017134446A1 (en) * | 2016-02-05 | 2017-08-10 | Agform Limited | Herbicidal combination |
| CN107743360A (en) * | 2015-04-27 | 2018-02-27 | 拜耳作物科学股份公司 | Purposes of some Herbicidal combinations in root crop plant |
| CN107743966A (en) * | 2017-10-20 | 2018-03-02 | 南京农业大学 | A kind of flufenacet diflufenican binary built agent for preventing and kill off wheat paddock resistant weed |
| CN109197879A (en) * | 2018-08-22 | 2019-01-15 | 四川利尔作物科学有限公司 | A kind of suspending agent containing flufenacet and diflufenican |
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2020
- 2020-10-12 CN CN202011086042.3A patent/CN112155015B/en active Active
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|---|---|---|---|---|
| JP5563773B2 (en) * | 2008-12-17 | 2014-07-30 | バイエル・クロップサイエンス・アーゲー | Herbicidal composition |
| CN107743360A (en) * | 2015-04-27 | 2018-02-27 | 拜耳作物科学股份公司 | Purposes of some Herbicidal combinations in root crop plant |
| WO2017134446A1 (en) * | 2016-02-05 | 2017-08-10 | Agform Limited | Herbicidal combination |
| CN107743966A (en) * | 2017-10-20 | 2018-03-02 | 南京农业大学 | A kind of flufenacet diflufenican binary built agent for preventing and kill off wheat paddock resistant weed |
| CN109197879A (en) * | 2018-08-22 | 2019-01-15 | 四川利尔作物科学有限公司 | A kind of suspending agent containing flufenacet and diflufenican |
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