CN114903051A - Herbicide composition containing flumioxazin and application thereof - Google Patents

Herbicide composition containing flumioxazin and application thereof Download PDF

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Publication number
CN114903051A
CN114903051A CN202110185565.1A CN202110185565A CN114903051A CN 114903051 A CN114903051 A CN 114903051A CN 202110185565 A CN202110185565 A CN 202110185565A CN 114903051 A CN114903051 A CN 114903051A
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herbicide
composition
glufosinate
glyphosate
flumioxazin
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Inventor
殷勇
罗小娟
罗杰
李双阳
杨志兰
刘晓伟
谌俊旭
梁灵
左元明
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Sichuan Lier Crop Science Co Ltd
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Sichuan Lier Crop Science Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N57/00Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/18Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, 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
    • A01N43/84Biocides, 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 six-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,4

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention provides a herbicide composition containing flumioxazin and application thereof. The herbicide composition comprises a herbicide A, a herbicide B and a herbicide C, wherein the herbicide A is at least one of glyphosate and glufosinate-ammonium, the herbicide B is at least one of halauxifen and halauxifen, and the herbicide C is flumioxazin. The herbicide composition is suitable for preventing and controlling weeds in uncultivated areas and orchards, has good safety and plays a positive role in protecting the ecological environment.

Description

Herbicide composition containing flumioxazin and application thereof
Technical Field
The application relates to the technical field of herbicides, in particular to a herbicide composition containing flumioxazin and application thereof.
Background
The land is wide in China, the non-cultivated land and orchard area is large, and the distribution is wide. The current weed control in non-cultivated lands and orchards often has the following problems: the weeds with big age and maturity are taken as main materials, and the difficulty of preventing and removing the weeds is large. Moreover, the emergence time of the weeds is uneven, so that the long-acting weed control is difficult to realize. Herbicide application is one of the main means of controlling non-cultivated land weeds and orchard weeds, but current herbicides are mainly concerned with the small-age weeds of the crop field.
Although glyphosate and glufosinate belong to biocidal herbicides, with the annual use of the herbicide, many resistant or tolerant weeds such as buttercup, annual fleabane, dayflower, ragweed and the like are often left. The weeds in the non-cultivated land can be bred due to underground tubers, rhizomes, bulbs and seeds, so that the difficulty in preventing and removing the weeds is high, for example, cyperus rotundus, cattail, wild garlic and the like.
In addition, orchards are distributed in all regions of the country, the environment difference among the regions is large, a plurality of places have the habit of weeding in early spring by opening the orchard and weeding in late autumn by clearing the orchard, and common uncultivated areas and orchards in the market have large influence of low temperature, so that the pesticide effect cannot be well exerted. The photoactivatable herbicide has a good weed control effect under the action of sufficient illumination, but the illumination conditions of places such as orchards, woodlands and the like are generally poor, particularly in the vigorous growth period of trees, the application effect is obviously poor under the condition, and for example, PPO, PS II and photosynthesis inhibitor herbicides have a good effect. At present, few reports have been made on herbicides having excellent effects on malignant weeds, aged weeds, and weeds in low-temperature, arid and low-irradiance environments.
In view of the above, in actual production, there is an urgent need to develop a herbicide that can effectively control old weeds, aged weeds, and malignant weeds and has a stable effect in special environments such as low temperature, poor sunlight, and drought.
Disclosure of Invention
To solve the above problems, the present application provides a herbicide composition which has an excellent effect on controlling older weeds, mature weeds and malignant weeds, is not limited by a particular environment, and is particularly suitable for weed control in uncultivated areas and orchards.
In one aspect, the present application provides a flumioxazin-containing herbicide composition comprising herbicidally effective ingredients: herbicide A, herbicide B and herbicide C,
the herbicide A is: the herbicide A is: at least one of glyphosate, glyphosate salt, glufosinate, and glufosinate salt;
the herbicide B is: at least one of chlorofluoropyridine ester and chlorofluoropyridine ester; and
the herbicide C is: flumioxazin;
wherein the mass ratio of the herbicide A to the herbicide B to the herbicide C is (15-80): (0.05-4): (1-20).
In some embodiments, the herbicide A is glyphosate or a salt of glyphosate, the herbicide B is halauxifen, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (30-80): 0.05-3): 1-20), such as (40-60): 0.1-1.5): 2-15, such as (45-55): 0.2-0.6): 5-10.
In some embodiments, the herbicide A is glyphosate or a salt of glyphosate, the herbicide B is a fluroxypyridine ester, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (30-80): 0.1-4): 1-20, such as (40-60): 0.3-3): 2-15, and such as (45-55): 0.6-1.5): 5-10.
In some embodiments, the herbicide A is glufosinate-ammonium or a salt of glufosinate-ammonium, the herbicide B is halauxifen, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): 0.05-3): 1-20, such as (20-35): 0.1-1.5): 2-15, such as (25-30): 0.2-0.6): 5-10.
In some embodiments, the herbicide A is a salt of glufosinate-ammonium and the herbicide B is a fluroxypyr meptyl, the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): 0.1-4): 1-20, such as (20-35): 0.3-3): 2-15, and such as (25-30): 0.6-1.5): 5-10.
In some embodiments, the herbicidal active ingredient is present in the herbicidal composition in a mass percentage of 6 to 80% based on the total mass of the herbicidal composition.
In some embodiments, the herbicidal active ingredient is present in the herbicidal composition in a mass percentage of 34 to 80% based on the total mass of the herbicidal composition.
In some embodiments, the herbicidal active ingredient is present in the herbicidal composition in a mass percentage of 32 to 80% based on the total mass of the herbicidal composition.
In some embodiments, the herbicidal active ingredient is present in the herbicidal composition in a mass percentage of 10% to 80% based on the total mass of the herbicidal composition.
In some embodiments, the herbicidal active ingredient is present in the herbicidal composition in a mass percentage of 6 to 80% based on the total mass of the herbicidal composition.
In some embodiments, the herbicidal composition further comprises a pesticidally acceptable adjuvant.
In some embodiments, the herbicidal composition is an oil suspension, a wettable powder, or a water dispersible granule.
The invention also provides the application of the herbicide composition, and the herbicide composition is used for controlling weeds in non-cultivated land and/or orchards.
In some embodiments, the herbicidal composition is applied at a dose of 300-1200 g (a.i.)/ha.
In some embodiments, the weeds are one or more of glyphosate/glufosinate-ammonium-tolerant goosegrass, glufosinate-ammonium-tolerant annual fleabane, glufosinate-ammonium-tolerant ranunculus, glyphosate-tolerant ambrosia trifida, glyphosate-tolerant dayflower, bluegrass, gnawing, smartweed, nettle, typha, alfalfa, bromegrass, wheatgrass, and chloranthus glauca.
Has the beneficial effects that:
the herbicide composition containing flumioxazin provided by the invention comprises at least one of glyphosate, glyphosate salt, glufosinate-ammonium and glufosinate-ammonium salt, at least one of halauxifen-ethyl and halauxifen-ethyl, and flumioxazin. By compounding the weeding active ingredients in a specific ratio, the purpose of preventing and removing weeds can be achieved, the weeding spectrum is wide, the influence of adverse weather environments such as low temperature and poor illumination can be overcome, and the herbicide composition can still keep a good weed preventing and removing effect under the conditions of low temperature and insufficient illumination. The herbicide composition has excellent effects of preventing and removing old weeds, aged weeds and malignant weeds, is low in dosage, delays the generation of drug resistance of the weeds, saves cost, can also play a role in sealing soil and inhibiting weed germination after the weeds die and leaves fall on the ground, is particularly suitable for preventing and treating weeds in non-cultivated lands and orchards, and is high in safety.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a flumioxazin-containing herbicide composition, which comprises the following effective herbicidal components: herbicide A, herbicide B and herbicide C,
the herbicide A is: the herbicide A is: at least one of glyphosate, glyphosate salt, glufosinate, and glufosinate salt;
the herbicide B is: at least one of chlorofluoropyridine ester and chlorofluoropyridine ester; and
the herbicide C is: flumioxazin;
wherein the mass ratio of the herbicide A to the herbicide B to the herbicide C is (15-80): (0.05-4): (1-20).
In some embodiments, the herbicide A is glyphosate or a salt of glyphosate, the herbicide B is halauxifen, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (30-80): 0.05-3): 1-20), such as (40-60): 0.1-1.5): 2-15, such as (45-55): 0.2-0.6): 5-10.
In some embodiments, the herbicide A is glyphosate or a salt of glyphosate, the herbicide B is a fluroxypyridine ester, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (30-80): 0.1-4): 1-20, such as (40-60): 0.3-3): 2-15, and such as (45-55): 0.6-1.5): 5-10.
In some embodiments, the herbicide A is glufosinate-ammonium or a salt of glufosinate-ammonium, the herbicide B is halauxifen, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): 0.05-3): 1-20, such as (20-35): 0.1-1.5): 2-15, such as (25-30): 0.2-0.6): 5-10.
In some embodiments, the herbicide A is glufosinate-ammonium or a salt of glufosinate-ammonium and the herbicide B is fluroxypyridine ester, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): 0.1-4): 1-20, such as (20-35): 0.3-3): 2-15, such as (25-30): 0.6-1.5): 5-10.
In the present invention, the mass ratio of the herbicide a, the herbicide B and the herbicide C represents a ratio of the masses of the three components, and the range of the corresponding ratio includes all mass ratios falling within the range of the ratio of the present invention after multiplying or dividing by any coefficient, for example, 90:7:34 divided by a coefficient 2 is 45:3.5:17, falling within (15 to 80): (0.05-4): (1-20). The mass ratio of the three substances is not limited to the listed examples, and the other mass ratios are within the scope of the present invention as long as the mass ratio of the three substances is multiplied or divided by any coefficient.
The "glufosinate" of the present invention includes a mixed racemate of D-glufosinate and L-glufosinate (DL-glufosinate). The glufosinate-ammonium can be DL-glufosinate-ammonium or L-glufosinate-ammonium. Because only L-glufosinate-ammonium in glufosinate-ammonium has weeding activity, the glufosinate-ammonium accounts for 50 percent of the total. Thus, when glufosinate is L-glufosinate, the weight in the composition is in terms of glufosinate: and the ratio of L-glufosinate-ammonium is 2: 1.
The glyphosate provided by the invention comprises various glyphosate salts. However, the glyphosate has the problems of toxic symptoms and slow death of weeds, great influence of air temperature and illumination on the drug effect, drug resistance of weeds and the like in the application. The chlorofluoropyridine ester or chlorofluoropyridine ester may be a formate, acetate, propionate, benzyl ester or other herbicidally active ester compounds known in the art. Fluroxypyridine esters or fluroxypyridine esters are synthetic auxin herbicides and are known to be applied to crop fields to control young weeds and to have poor effects on older and mature weeds.
The chlorofluoropyridine ester disclosed by the invention is a compound shown as the following structural formula (I) or an agriculturally acceptable salt thereof, or a combination of one or more of the compounds and the ester thereof. Wherein the agricultural ester of the compound shown in the formula (I) comprises an alkyl ester shown as C1-4 in the formula (I) or a benzyl ester shown in the formula (I). In some embodiments, the chlorofluoropyridine esters include methyl, ethyl or benzyl esters of the compounds of formula (I).
Figure BDA0002942931800000051
The fluorochloropyridinates described herein are 4-amino-3-chloro-6- (4-chloro-2-fluoro-3-methoxyphenyl) pyridine-2-carboxylic acid (fluorochloropyridinate), halauxifen) and combinations of one or more of its salts or esters, e.g., in some embodiments, 4-amino-3-chloro-6- (4-chloro-2-fluoro-3-methoxyphenyl) -2-picolinate, ethyl 4-amino-3-chloro-6- (4-chloro-2-fluoro-3-methoxyphenyl) -2-picolinate, or 4-amino-3-chloro-6- (4-chloro-2-fluoro-3-methoxyphenyl) carboxylate ) -2-pyridinecarboxylic acid benzyl ester.
Flumioxazin is a protoporphyrinogen oxidase inhibitor and is known to be used primarily as a dry farming soil-blocking herbicide. When the herbicide is used for treating stems and leaves in early postemergence, old weeds cannot be effectively prevented and removed.
The herbicidal compositions described herein may also include any pesticidally acceptable adjuvants.
The herbicide composition can be prepared into any one of oil suspending agent, wettable powder or water dispersible granules according to the requirement, and the aim of the invention can be achieved.
In some embodiments, the herbicide a is glyphosate or a salt of glyphosate, the herbicide B is halauxifen, and the herbicidal composition is present in the formulation in an amount of 30% to 80% by weight, specifically 35% to 75% by weight, 50% to 60% by weight, such as 34%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80% by weight, and the like, it being understood that the above proportions are merely exemplary, and in other embodiments of the present application, the herbicidal composition may be present in the formulation in other ranges, such as 41% by weight.
As an exemplary technical scheme, the herbicide composition is prepared into an oil suspending agent, wherein the mass percentage of the herbicide active ingredients is 34-51% of the total mass of the oil suspending agent.
As an exemplary technical scheme, the herbicide composition is prepared into wettable powder, wherein the mass percentage of the herbicide active ingredient is 34-80%, for example 51-73% based on the total mass of the wettable powder.
As an exemplary technical scheme, the herbicide composition is prepared into water dispersible granules, and the mass percentage of the weeding active ingredients is 34-80% of the total mass of the water dispersible granules.
In some embodiments, the herbicide a is glufosinate or a salt of glufosinate-ammonium, the herbicide B is halauxifen-ethyl, and the herbicidal composition is present in the formulation in an amount of 10% to 80% by weight, specifically 15% to 75% by weight, 50% to 60% by weight, for example 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80% by weight, and the like, it being understood that the above proportions are merely exemplary, and in other embodiments of the present application, the herbicidal composition may be present in the formulation in other proportions, for example 10%.
As an exemplary technical scheme, the herbicide composition is prepared into an oil suspending agent, and the mass percentage of the herbicide active ingredients is 10-51% of the total mass of the oil suspending agent.
As an exemplary technical solution, the herbicide composition is prepared into wettable powder, and the mass percentage of the herbicidal active ingredients is 10% to 80%, for example 51% to 73%, based on the total mass of the wettable powder.
As an exemplary technical scheme, the herbicide composition is prepared into water dispersible granules, and the mass percentage of the weeding active ingredients is 10-80% of the total mass of the water dispersible granules.
In some embodiments, the active ingredient a is glyphosate or a salt of glyphosate, the active ingredient B is fluroxypyr-meptyl, and the herbicidal composition is present in the formulation in a mass percentage of 30% to 80%, specifically 45% to 75%, 50% to 60%, such as 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, etc., it being understood that the above proportions are merely examples, and in other embodiments of the present application, the herbicidal composition may be present in the formulation in other proportions, such as 43%.
As an exemplary technical solution, the herbicide composition is prepared into an oil suspension, wherein the mass percentage of the herbicidal active ingredient A, B, and C is 32-51% based on the total mass of the oil suspension.
As an exemplary technical scheme, the herbicide composition is prepared into wettable powder, wherein the mass percentage of the herbicidal active ingredients A, B and C is 32-80%, for example 59-76%, based on the total mass of the wettable powder.
As an exemplary technical scheme, the herbicide composition is prepared into water dispersible granules, wherein the mass percent of the herbicide active ingredients A, B and C is 32-80% based on the total mass of the water dispersible granules.
In some embodiments, the active ingredient a is glufosinate or a salt of glufosinate-ammonium, the active ingredient B is a fluroxypyridine ester, and the herbicidal composition is present in the formulation in an amount of 5% to 80% by weight, specifically 15% to 75% by weight, 50% to 60% by weight, such as 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80% by weight, and the like, it is understood that the above proportions are merely examples, and in other embodiments of the present application, the herbicidal composition may be present in the formulation in other proportions, such as 10%.
As an exemplary technical scheme, the herbicide composition is prepared into an oil suspending agent, and the mass percentage of the herbicidal active ingredients is 6-52% of the total mass of the oil suspending agent.
As an exemplary technical scheme, the herbicide composition is prepared into wettable powder, and the mass percentage of the herbicide active ingredient is 6-80%, for example 52-78% based on the total mass of the wettable powder.
As an exemplary technical scheme, the herbicide composition is prepared into water dispersible granules, and the mass percentage of the weeding active ingredients is 6-80% of the total mass of the water dispersible granules.
The herbicide composition can be applied to weed control in non-cultivated land/orchard. The orchard refers to a garden where fruit trees are planted and includes, but is not limited to, fields such as oranges, apples, pears, peaches, plums, apricots and the like.
The non-cultivated land refers to a region where crops are not planted, and includes but is not limited to the fields of front and back houses, railways, highways, warehouses, forest fire prevention, ditch edges, roadside, wasteland, forest lands and the like.
In some embodiments, the herbicidal composition may be formulated directly into a dosage form or tank-mixed with each herbicidal active ingredient, prepared as a herbicidal composition, dispersed in a solvent at the time of use to prepare a spray solution, and then sprayed directly onto the stems and leaves of the growing weeds. In other embodiments, the herbicidal active ingredients contained in the herbicide composition may be prepared as a spray solution by separately preparing the solutions and mixing the solutions at the time of use.
In some embodiments, the herbicide a in the herbicidal composition is glyphosate or a salt of glyphosate, and the herbicidal composition is used in an effective amount of 600 to 1200g (a.i.)/ha.
In some embodiments, the herbicide a is glufosinate or a salt thereof in the herbicide composition, and the effective amount of the herbicide composition is 300 to 600g (a.i.)/ha.
The following is a detailed description of the technical aspects of the present invention using examples.
Examples
In order to make the objects, technical solutions and advantages of the present invention more concise and clearer, the present invention is described with reference to the following specific examples, but the present invention is by no means limited to these examples. The following description is only a preferred embodiment of the present invention, and is only for the purpose of describing the present invention, and should not be construed as limiting the scope of the present invention. It should be understood that any modifications, equivalents and improvements made within the spirit and principle of the present invention are included within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
In these examples, all percentages are by weight unless otherwise indicated.
The structural formulas of the fluorochloropyridine ester and the chlorofluoropyridine ester related to the embodiment of the invention are respectively as follows:
chlorofluoropyridine ester:
Figure BDA0002942931800000081
chlorofluoropyridine esters:
Figure BDA0002942931800000082
the wettable powder of the embodiment and the comparative example of the invention comprises the following auxiliary materials: naphthalene sulfonate, sodium dodecyl sulfate, lignosulfonate, white carbon black and kaolin.
The auxiliary materials of the oil suspending agent of the embodiment and the comparative example comprise: vegetable oil and its derivatives (methyl oleate), calcium dodecylbenzenesulfonate, castor oil polyoxyethylene ether, polycarboxylate, alkylphenol polyoxyethylene ether, and organic bentonite.
The auxiliary materials of the water dispersible granules of the embodiment and the comparative example of the invention comprise: lignosulfonate, sodium dodecyl sulfate, alkyl naphthalene sulfonate, white carbon black and organic soil.
The auxiliary materials of the same dosage forms in the examples and the comparative examples have the same composition.
The proportion of each embodiment is as follows:
the application provides 84 embodiments of the weeding composition in total, and the specific mixture ratio of the component A, the component B and the component C in each embodiment is detailed in the following table 1:
table 1 formulation table of herbicidal compositions of examples 1 to 84, comparative examples 1 to 27
Figure BDA0002942931800000091
Figure BDA0002942931800000101
Figure BDA0002942931800000111
Figure BDA0002942931800000121
Figure BDA0002942931800000131
Test of drug efficacy 1: indoor proportioning screening
Raw materials of the test medicament: 98% ammonium glyphosate technical (PD 20082658: Jiangsu Haoying Wen agricultural chemical Co., Ltd.); 95% glufosinate (PD 20110578: rill chemical gmbh); 93% Fluoropicolinate bulk drug (PD 20161259: Yinong Dow USA); 91.4% chlorofluoropyridine ester bulk drug (PD 20171736: Yinong Dow, USA); 99.2% technical flumioxazin (PD 20160295: Lile chemical Co., Ltd.).
Test materials: the glyphosate-resistant grass seeds are collected from fields by researchers of Sichuan rill crop science limited company and stored in a storage warehouse.
Preparing a medicament: weighing a glyphosate ammonium salt raw drug, a glufosinate ammonium raw drug, a halauxifen raw drug, a chlorofluoropyridyl ester raw drug and a flumioxazin raw drug, adding acetone to the fluorochloraridine ester raw drug, fully dissolving the fluorochloraridine ester raw drug and the chlorofluoropyridyl ester raw drug, diluting the fluorochloran raw drug with 0.1% tween 80 aqueous solution, adding N-methylpyrrolidone to the flumioxazin raw drug, fully dissolving the fluorochloran raw drug, diluting the fluorochloran raw drug with 0.1% tween 80 aqueous solution, directly adding the glyphosate ammonium salt raw drug and the glufosinate ammonium raw drug to the 0.1% tween 80 aqueous solution for dilution, respectively preparing single-dose mother liquor, and setting 7-16 concentration gradients for each drug.
Control solution: 0.1% tween 80 in water.
The test method comprises the following steps: adopting a potted stem and leaf treatment method (NY/T1155.4-2006): the method comprises the steps of filling quantitative drying soil in plastic pots with different heights of 17cm and diameters of 20.5cm, sowing 25-30 weed seeds to be tested in the plastic pots, covering with fine soil with the thickness of 0.5-1 cm, absorbing water from the bottom, ensuring that the relative humidity of soil in each pot is 75% after sowing, placing the pots in a greenhouse for cultivation, properly replenishing water according to the dry and wet conditions of the soil, ensuring that weeds can grow normally, and ensuring that other conditions are consistent. And (3) setting 10 weeds per pot for standby when the weeds grow to 10-12 leaves, weighing every day after the relative humidity of the soil is reduced to 40%, supplementing water and keeping the relative humidity of the soil to be 40%. Then, spray treatment of stem and leaf was carried out, and the treatment was repeated 4 times, and the treatment containing no drug was set as a control.
The application method comprises the following steps: spraying stem and leaf. The spraying adopts a 3WPSH-500D type biological spraying tower produced by Nanjing agricultural mechanization research institute of agricultural department, the diameter of a disc is 50cm, the rotating speed of a main shaft is 6r/min, the aperture of a spray head is 0.3mm, the spraying pressure is 0.3MPa, the diameter of a fog drop is 100 mu m, and the flow rate of the spray head is 90 mL/min. And (3) placing the target weeds subjected to spray treatment on stems and leaves in an artificial climate chamber (20 ℃ in the day and 15 ℃ at night) for culturing, and keeping the relative humidity of soil at 40% until result investigation.
The investigation method comprises the following steps: after 35d of test treatment, the target damage symptoms and the growth inhibition condition are visually observed, the fresh weight of the overground part is weighed, and the toxicity of the weeding composition on the target weeds is evaluated according to the residual rate of the fresh weight of the weeds.
Wherein, the calculation formula of the weed fresh weight survival rate is shown as the following formula:
Figure BDA0002942931800000141
the combined action is evaluated by a Colby method, wherein the theoretical weed fresh weight survival rate of the weeding composition is calculated by the following formula:
Figure BDA0002942931800000151
in the formula: taking X as the multiplication number and the weed fresh weight survival rate of the herbicide A when the dosage is P;
y is the weed fresh weight residual rate of the herbicide B when the dosage is Q;
z is the weed fresh weight residual rate of the herbicide C when the dosage is W;
n is the number of chemicals to be mixed (n-3 in this test);
E 0 the theoretical weed fresh weight survival rate of the herbicide (A + B + C) when the dosage is (P + Q + W).
E is the actual weed fresh weight survival rate of the herbicide (A + B + C) when the dosage is (P + Q + W);
E 0 -E>10% of the composition has a synergistic effect; e 0 -E<-10% is antagonism; e 0 An E value of. + -. 10% is additive effect.
TABLE 2 indoor toxicity assay for glufosinate-ammonium, fluorochloropyridyl ester and flumioxazin
Figure BDA0002942931800000152
Figure BDA0002942931800000161
Figure BDA0002942931800000171
Figure BDA0002942931800000181
From Table 2E 0 E (%) distribution, the synergistic relationship of the glufosinate-ammonium, the halauxifen-methyl and the flumioxazin after being mixed is that the synergistic effect is achieved within the range of the mass ratio of (15-40) to (0.05-3) to (1-20), and the inventor of the invention unexpectedly finds that the glufosinate-ammonium: fluorochloropyridine ester: in the range of the mass ratio of the flumioxazin to (25-30): (0.2-0.6): 5-10), the synergistic effect is obviously better than other ratios.
TABLE 3 indoor toxicity assay for glufosinate, fluroxypyridine and flumioxazin
Figure BDA0002942931800000182
Figure BDA0002942931800000191
Figure BDA0002942931800000201
Figure BDA0002942931800000211
From Table 3E 0 E (%) distribution shows that the synergistic relationship of the glufosinate-ammonium, the fluroxypyr-meptyl and the flumioxazin after being mixed is that the synergistic effect is achieved within the mass ratio of (15-40) to (0.1-4) to (1-20), and the inventor of the invention unexpectedly finds that the glufosinate-ammonium: chlorofluoropyridine esters: in the range of the mass ratio of the flumioxazin to (25-30) to (0.6-1.5) to (5-10), the synergistic effect is obviously better than that of other ratios.
TABLE 4 indoor toxicity assay for Glyphosate, halauxifen and flumioxazin
Figure BDA0002942931800000212
Figure BDA0002942931800000221
Figure BDA0002942931800000231
Figure BDA0002942931800000241
Figure BDA0002942931800000251
From Table 4E 0 The E (%) distribution shows that the synergistic relationship of the glyphosate, the halauxifen and the flumioxazin after being mixed is that the synergistic effect is shown in the mass ratio of the glyphosate to the flumioxazin to be (30-80) to (0.05-3) to (1-20), and the inventor of the invention unexpectedly finds that the glyphosate: fluorochloropyridine ester: in the range of the mass ratio of flumioxazin to (45-55): (0.2-0.6): 5-10), the synergistic effect is obviously better than other ratios.
TABLE 5 indoor toxicity assay for Glyphosate, Clinopyridyl chloride and flumioxazin
Figure BDA0002942931800000252
Figure BDA0002942931800000261
Figure BDA0002942931800000271
Figure BDA0002942931800000281
From Table 5E 0 E (%) distribution shows that the synergistic relationship of the glyphosate, the fluroxypyridine ester and the flumioxazin after being mixed is that the synergistic effect is achieved within the mass ratio of (30-80) to (0.1-4) to (1-20), and the inventor of the invention unexpectedly finds that the glyphosate: chlorofluoropyridine esters: in the range of the mass ratio of flumioxazin to (45-55): (0.6-1.5): 5-10), the synergistic effect is obviously better than other ratios.
Pharmacodynamic test 2: field efficacy test with differential duration of action
The test method comprises the following steps: the test is carried out in a guava garden piled in sand in a new meeting area of Jiangmen city, Guangdong province, the test land is yellow loam at the temperature of about 30 ℃, the terrain is smooth, the soil is uniform, glyphosate is used all the year before 2010, glufosinate-ammonium is used all the year after 2011, the herbicide is used 3-4 times each year, and the eleusine indica has obvious resistance to glufosinate-ammonium and glyphosate. When the pesticide is applied, the resistant eleusine indica is in the flowering period, about 15-20 tillers are formed, xylem is formed, the density is high, and the pesticide liquid can not directly reach the ground when stem leaves are sprayed. Examples 1 to 42 and comparative examples 1 to 10, comparative examples 20 to 22 were applied at an amount of 525g (a.i.)/ha, examples 43 to 84 and comparative examples 11 to 19, and comparative examples 25 to 27 were applied at an amount of 1000g (a.i.)/ha, wherein comparative examples 23 to 24 were applied at glufosinate-ammonium, halauxifen-ethylOr the application rate of the chlorofluoropyridinate with the flumioxazin herbicide composition was 525g (a.i.)/ha, while comparative examples 23 to 24 applied the application rate of the glyphosate, the chlorofluoropyridinate or the chlorofluoropyridinate with the flumioxazin herbicide composition was 1000g (a.i.)/ha. Each treatment was repeated 4 times, each cell area being 30m 2 The herbicide composition is applied by diluting with water to a spray volume of 40L per mu and replacing the herbicide composition with water as a blank. Random block permutation. The pesticide spraying device is an AGROLEX HD400 electric sprayer of Singapore Linong, and adopts a stem leaf spraying method. The conditions were identical for each treatment area except that the herbicide was applied according to the above protocol.
The evaluation method comprises the following steps: after 30 days of medicine, 4 points of each treatment area are randomly sampled, and the area of the sample is 0.25m 2 The fresh weight of the overground part is called, and the control effect of the medicament on the target weeds is evaluated according to the control effect of the fresh weight. And then surveying the emergence conditions of the new weeds in each plot every 20 days (the main targets are digitaria sanguinalis, eleusine indica, barnyard grass, bidens bipinnata, wedeloa chinensis, purslane and guayule), the control effect is expressed by the total fresh weight control effect of the grass, and the fresh weight control effect is calculated according to the following formula:
Figure BDA0002942931800000291
2.1 field efficacy testing of herbicides (glufosinate-ammonium, chloropyridyl fluoride and flumioxazin) with differential duration
Reagent to be tested: the herbicidal compositions of examples 1 to 21 were prepared according to Table 1.
Comparison of the medicaments: 8 kinds of herbicidal compositions such as comparative examples 1 to 5, comparative example 20, comparative example 21 and comparative example 23, and single-dose herbicides in table 6:
TABLE 6 comparative agent information Table involved in field efficacy test of difference in effective period
Contrast agent Source Trade name
200g/L glufosinate-ammonium aqua Is commercially available Baikudun (quick action)
7.5g/L chlorofluoropyridine ester emulsifiable concentrate Self-matching \
51% flumioxazin water dispersible granule Commercial purchase Feng Qing
And (3) test results:
TABLE 7 efficacy of glufosinate-ammonium, fluorochloropyridyl ester and flumioxazin at different times after application of different herbicidal compositions
Figure BDA0002942931800000292
Figure BDA0002942931800000301
Figure BDA0002942931800000311
From the data analysis in table 7, it can be seen that:
(1) compared with the control effect of 30 days after single-agent treatment, the control effects of the three-element herbicide composition of glufosinate-ammonium, halauxifen-ethyl and flumioxazin are obviously better than those of single-agent treatment on the resistant eleusine indica in the flowering period of the old.
(2) Compared with the control effects of 30 days after the medicines are applied to the examples 1-21 and the comparative examples 1-5, 20, 21 and 23, the control effects of the examples 1-21 are obviously better than those of the comparative examples 1-5, 20, 21 and 23.
(3) Through comparison of the weed sealing effect of 50-110 days after the treatment of the herbicide in examples 1-21 and other comparative examples, the ternary weeding composition containing glufosinate-ammonium, halauxifen-methyl and flumioxazin is obviously superior to the single herbicide and the comparative examples in the aspect of inhibiting the germination of new weeds.
2.2 field efficacy testing of herbicides (glufosinate, fluroxypyridine and flumioxazin) with differential duration
Reagent to be tested: the herbicidal compositions of examples 22 to 42 were formulated as shown in Table 1.
Comparing the medicament: 8 herbicidal compositions of comparative examples 6 to 10, comparative example 20, comparative example 22 and comparative example 24, and the single-dose herbicides in Table 8:
TABLE 8 comparison drug information Table involved in field drug efficacy test of differences in terms of duration
Contrast agent Source Name of commodity
200g/L glufosinate-ammonium aqua Commercial purchase Hundred fast tons
3% chlorofluoropyridine ester emulsifiable concentrate Commercial purchase Lingsuke pill
51% flumioxazin water dispersible granule Commercial purchase Feng Qing
And (3) test results:
TABLE 9 drug effects of glufosinate-ammonium, fluroxypyridine-ester and flumioxazin in different combinations at different periods of time
Figure BDA0002942931800000321
Figure BDA0002942931800000331
From the data analysis in table 9, it can be seen that:
(1) compared with the control effect of 30 days after single-agent treatment, the three-element weeding composition containing glufosinate, fluroxypyr-meptyl and flumioxazin is obviously better than single-agent treatment in the effect of the three-element weeding composition on old goosegrass in the flowering period.
(2) By comparing the control effects of the examples 22-42 with those of the comparative examples 6-10, 20, 22 and 24 after 30 days of stem and leaf treatment, the control effects of the examples 22-42 are obviously better than those of the comparative examples 6-10, 20, 22 and 24.
(3) By comparing the weed blocking effects of the three herbicidal compositions in examples 22 to 42 with those of the three herbicidal compositions after being treated by other treatment agents for 50d to 110d, the three herbicidal compositions of glufosinate-ammonium, fluroxypyr-meptyl and flumioxazin are obviously superior to those of the single agent and the comparative example in the aspect of inhibiting the germination of the new weeds.
2.3 field efficacy testing of differential duration of herbicides (Glyphosate, Fluoropicolide and Fluroxyprophosamine)
Reagent to be tested: the herbicidal compositions of examples 43 to 63 were formulated according to Table 1.
Comparison of the medicaments: 8 herbicidal compositions of comparative examples 11 to 15, comparative example 23, comparative example 25 and comparative example 26, and the single-dose herbicides in Table 10:
TABLE 10 comparison drug information Table involved in field efficacy test of differences in terms of duration
Contrast agent Source Name of commodity
41% glyphosate isopropylamine salt aqueous solution Commercial purchase Nongda (agricultural chemical)
7.5g/L chlorofluoropyridine ester emulsifiable concentrate Self-matching \
51% flumioxazin water dispersible granule Is commercially available Feng Qing
And (3) test results:
TABLE 11 efficacy of glyphosate, fluroxypyridine and flumioxazin at different times after application of different herbicidal compositions
Figure BDA0002942931800000341
Figure BDA0002942931800000351
From the data analysis in table 11, it can be seen that:
(1) compared with the control effect of 30 days after single-agent treatment, the three-element weeding composition containing glyphosate, halauxifen-methyl and flumioxazin has obviously better effect on old goosegrass in flowering period than single-agent treatment in the embodiments 43-63.
(2) Compared with the control effects of 30 days after the treatment of stems and leaves of the comparative examples 43 to 63, 11 to 15, 23, 25 and 26, the control effects of the examples 43 to 63 are obviously superior to those of the comparative examples 11 to 15, 23, 25 and 26.
(3) By comparing the weed sealing effect of the three herbicidal compositions of glyphosate, halauxifen-methyl and flumioxazin after being treated by the three herbicides in examples 43-63 with that of the herbicide after being treated by other herbicides for 50 d-110 d, the three herbicidal compositions of glyphosate, halauxifen-methyl and flumioxazin are obviously superior to the single herbicide and the comparative herbicide in the aspect of inhibiting the germination of new weeds.
2.4 field efficacy testing of herbicides (Glyphosate, Chlorofluoropyridyl ester and flumioxazin) with differential duration
Reagent to be tested: the herbicidal compositions of examples 64 to 84 were formulated according to Table 1.
Comparing the medicament: 8 kinds of herbicidal compositions of comparative examples 16 to 19, comparative example 24, comparative example 25 and comparative example 27, and single-dose herbicides in table 12:
TABLE 12 comparative agent information Table involved in field efficacy testing of differences in terms of duration
Contrast agent Source Trade name
41% glyphosate isopropylamine salt aqueous solution Commercial purchase Nongda (agricultural chemical)
3% chlorofluoropyridine ester emulsifiable concentrate Commercial purchase Lingsuke pill
51% flumioxazin water dispersible granule Is commercially available Feng Qing
And (3) test results:
TABLE 13 efficacy of glyphosate, fluroxypyridine and flumioxazin at different times after application to different herbicidal compositions
Figure BDA0002942931800000361
Figure BDA0002942931800000371
From the data analysis in table 13, it can be seen that:
(1) compared with the control effect of 30 days after single-agent treatment, the examples 64-84 show that the effect of the ternary weeding composition containing glyphosate, fluroxypyr-meptyl and flumioxazin on the old goosegrass in the flowering period is obviously better than that of single-agent treatment.
(2) Compared with the control effects of 30 days after the treatment of stems and leaves of the comparative examples 64 to 84, 16 to 19, 24, 25 and 27, the control effects of the examples 64 to 84 are obviously superior to those of the comparative examples 16 to 19, 24, 25 and 27.
(3) Through comparison of the weed sealing effects of the three herbicides of glyphosate, fluroxypyr and flumioxazin after being treated by the three herbicides in examples 64-84 and other treatments for 50 d-110 d, the ternary herbicide composition of glyphosate, fluroxypyr and flumioxazin is obviously superior to a single agent and a comparative example in the aspect of inhibiting the germination of new weeds.
In summary, the experiment proves that the weeding composition can obviously improve the drug effect on the old and the aged weeds under a specific proportion. And through the mode of stem leaf treatment, not only solve the problem of weeds on the ground, but also can effectively inhibit the germination of new weeds, and achieve the long-acting weeding effect of 'killing one by one'.
Pharmacodynamic test 3: indoor pharmacodynamic test of temperature on pharmacodynamic effect
Reagent to be tested: examples 1 to 84, comparative examples 1 to 27.
Test targets: 8-10 tillered bluegrass and 15-20 leaf stage Gnaphalium affine are stored in a field-collected weed seed storage by scientific researchers of Sichuan rill crop science Limited company.
The test method comprises the following steps: a potted stem and leaf treatment method (NY/T1155.4-2006) is adopted, namely quantitative soil is filled in a plastic pot with the height of 17cm and the diameter of 20.5cm, 15-20 weed seeds to be tested are sown in the plastic pot, the plastic pot is covered with fine soil with the thickness of 0.5-1 cm and then placed in a greenhouse for culture, plants are fixed after weeds emerge, and only 10 weeds are reserved in each pot. And (3) carrying out stem and leaf spraying treatment when the early-maturing rice grows to 8-10 tillers and the Gnaphalium affine grows to 15-20 leaf stages, repeating the treatment for 4 times, and taking the treatment without the medicament as a control. Each set of experiments was individually provided with a single dose control.
The application method comprises the following steps: spraying stem and leaf. The spraying is carried out by using 3WPSH-500D type biological spraying tower produced by Nanjing agriculture mechanization research institute of Ministry of agriculture, the diameter of a disc is 50cm, and the rotation speed of a main shaft is 6 r.min -1 The aperture of the nozzle is 0.3mm, the spraying pressure is 0.3MPa, the diameter of the fog drop is 100 mu m, and the flow rate of the nozzle is 90mL/min -1 . After treatment, 1 group of the test materials are placed in a climatic chamber at 25 ℃ in the day and 30-night, and the other 1 group of the test materials are placed in a climatic chamber at 10 ℃ in the day and 15-night for continuous culture. The illumination intensity is 0LX to 7500LX in the daytime.
The evaluation method comprises the following steps: the weed control effect of each treatment is regularly observed, the fresh weight of each treated weed is weighed after 30 days, and the control effect of the agent on the target weeds is evaluated according to the fresh weight control effect.
Figure BDA0002942931800000381
And (3) test results:
TABLE 14 herbicidal effect of glufosinate-ammonium, fluorochloropyridine ester and flumioxazin in different herbicidal compositions in 30 days after application
Figure BDA0002942931800000382
Figure BDA0002942931800000391
As shown in Table 14, the test results show that the compound preparation of glufosinate-ammonium, halauxifen-methyl and flumioxazin is prepared by the following steps: under the condition of 30 ℃ in the day to 25 ℃ at night, the control effect of the medicines of the examples 1 to 21 after 30 days has certain advantages compared with the control effects of the comparative examples 1 to 5, 20, 21 and 23, and the control effect difference is 6.17 to 53.76 percent.
Under the condition of 15 ℃ in the day to 10 ℃ at night, the control effect of the example 1 to 21 after 30 days is obviously expanded compared with the control effects of the comparative examples 1 to 5, 20, 21 and 23, and the control effect difference of the two is expanded to 23.79 to 60.11%.
The above data show that: glufosinate-ammonium, fluorochloropyridine ester and flumioxazin (15-40): (0.05-3): the (1-20) weight ratio is compounded, so that the weeding composition has an obvious coordination and synergism effect, the weeding spectrum is expanded, and the using effect is better under a low-temperature condition.
TABLE 15 herbicidal effects of glufosinate-ammonium, fluroxypyridine-ester and flumioxazin in different herbicidal compositions for 30 days
Figure BDA0002942931800000401
Figure BDA0002942931800000411
As shown in Table 15, the test results show that the compound of glufosinate-ammonium, fluroxypyr-meptyl and flumioxazin is as follows:
under the condition of 30-25 ℃ in the daytime and 25 ℃ at night, the control effect of the embodiment 22-42 after the drug is applied for 30 days has certain advantages compared with the control effects of the comparative examples 6-10, 20, 22 and 24, and the control effect difference value is 6.04-33.27%.
Under the condition of 15-10 ℃ in the day and 10-night, compared with the control effects of the comparative examples 6-10, the comparative example 20, the comparative example 22 and the comparative example 24, the control effect of the examples 22-42 after the drug is applied for 30 days is obviously expanded in the efficacy advantage, and the difference value of the control effects of the two is expanded to 19.67-42.04%.
The above data show that: glufosinate-ammonium, fluroxypyridine-ester and flumioxazin in an amount of (15-40): (0.1-4): the (1-20) weight ratio is compounded, so that the weeding composition has an obvious coordination and synergism effect, the weeding spectrum is expanded, and the using effect is better under a low-temperature condition.
TABLE 16 after application of glyphosate, fluorochloropyridine ester and flumioxazin in different herbicidal compositions, the efficacy of the compositions in different environments is 30 days
Figure BDA0002942931800000421
Figure BDA0002942931800000431
As shown in Table 16, the test results show that the glyphosate, the halauxifen and the flumioxazin are compounded:
under the condition of 30 ℃ in the day to 25 ℃ at night, the control effect of the example 43-63 after the drug is applied for 30 days has certain advantages compared with the control effects of the comparative examples 11-15, 23, 25 and 26, and the control effect difference is 4.92-33.27%.
Under the condition of 15 ℃ in the day to 10 ℃ at night, the control effect of the example 43-63 after the drug is used for 30 days is obviously enlarged in the advantages of the drug effect compared with the control effects of the comparative examples 11-15, 23, 25 and 26, and the difference value of the control effects of the two is enlarged to 17.76-45.97%.
The above data show that: glyphosate, halauxifen-methyl and flumioxazin are mixed by the following ratio (30-80): (0.05-3): the (1-20) weight ratio is compounded, so that the weeding composition has an obvious coordination and synergism effect, the weeding spectrum is expanded, and the using effect is better under a low-temperature condition.
TABLE 17 efficacy of glyphosate, fluroxypyridine ester and flumioxazin in different herbicidal compositions after 30 days of application
Figure BDA0002942931800000432
Figure BDA0002942931800000441
Figure BDA0002942931800000451
As shown in Table 17, the test results show that after the glyphosate, the fluroxypyr-meptyl and the flumioxazin are compounded, the components:
under the condition of 30-25 ℃ in the daytime and 25 ℃ at night, the control effect of the embodiment 64-84 after the pesticide is applied for 30 days has certain advantages compared with the control effects of the comparative examples 16-19, the comparative example 24, the comparative example 25 and the comparative example 27, and the control effect difference value is 5.06-22.49%.
Compared with the control effects of the comparative examples 16 to 19, 24, 25 and 27, the control effect of the examples 64 to 84 after the application for 30 days is obviously expanded under the condition of 15 ℃ in the day and 10 ℃ at night, and the control effect difference value of the two is expanded to 14.60 to 40.28%.
The above data show that: glyphosate, fluroxypyridine ester and flumioxazin are mixed in a ratio of (30-80): (0.1-4): the (1-20) weight ratio is compounded, so that the weeding composition has an obvious coordination and synergism effect, the weeding spectrum is expanded, and the using effect is better under a low-temperature condition.
Pharmacodynamic test 4: field efficacy test of Urtica dioica and Typha
Reagent to be tested: the herbicidal compositions of examples 1 to 84 were prepared according to Table 1.
Comparison of the medicaments: herbicidal compositions of comparative examples 1 to 27 were formulated according to table 1, and the single-dose herbicides in table 18:
TABLE 18 control agent information table related to field efficacy test of Urtica dioica and Typha
Contrast agent Source Name of commodity
200g/L glufosinate-ammonium aqua Commercial purchase Hundred fast tons
7.5g/L chlorofluoropyridine ester emulsifiable concentrate Self-matching \
51% flumioxazin water dispersible granule Commercial purchase Feng Qing
3% chlorofluoropyridinate emulsifiable concentrate Commercial purchase Lingsuke pill
41% glyphosate isopropylamine salt aqueous solution Commercial purchase Nongda (agricultural chemical)
Primary targets: nettle with a height of 1-1.2m, and typha with a height of 1.2-1.5 m.
The test method comprises the following steps: the test is carried out on a barren land with rich paddy and town in Mianyang city, Sichuan province, the test land is yellow loam and the topography is flat. Other herbicides are not applied before and after the test, and the weed population is stable and uniformly distributed. Wherein the application amount of the herbicide compositions of examples 1 to 42 and comparative examples 1 to 10, comparative examples 20 to 21 was 525g (a.i.)/ha, the application amount of the herbicide compositions of examples 43 to 84 and comparative examples 11 to 19, comparative examples 25 to 27 was 1000g (a.i.)/ha, and the application amount of comparative examples 23, 24 was 525/1000g (a.i.)/ha as the case may be. Each treatment was repeated 4 times, each cell area being 30m 2 When the herbicide composition is applied, the herbicide composition is diluted by water until the water consumption of each mu of spray is 40L, and the water is used for replacing the herbicide composition to be used as a blank treatment, and the water is randomly arranged in blocks. The pesticide spraying device is an AGROLEX HD400 electric sprayer of Singapore Lingnong, and adopts a stem and leaf spraying method. The conditions were identical for each treatment area except that the herbicide was applied according to the above protocol.
The evaluation method comprises the following steps: after spraying herbicide for 35 days, 4-point random sampling is carried out on weeds in each plot of the treatment area, and the area of the sample is 1m 2 And weighing the fresh weight of the overground part, and evaluating the control effect of the medicament on the target weeds by using the fresh weight control effect. The fresh-weight control effect is calculated according to the following formula, and the results are shown in tables 19 to 22.
Figure BDA0002942931800000461
TABLE 19 control efficacy of various herbicidal compositions of glufosinate-ammonium, halauxifen-methyl and flumioxazin against nettle, cattail for 35 days after application
Figure BDA0002942931800000462
Figure BDA0002942931800000471
As can be seen from Table 19, the herbicidal compositions of examples 1 to 21 have a significant advantage in controlling urtica fissa and typha compared to the control agents and comparative examples 1 to 5, 20, 21 and 23. The glufosinate-ammonium single agent has poor control effect on the nettle with fissured leaves and the cattail. The single dose of halauxifen is poor in prevention effect of nettle and cattail. The flumioxazin single agent has poor effect on urtica fissa and cattail.
The herbicidal compositions of comparative examples 1 to 5 contain the same components as those of the examples, but have obvious differences in control effect due to different proportions of the components.
In summary, when glufosinate-ammonium, halauxifen-methyl and flumioxazin are mixed in the ratio of (15-40): (0.05-3): (1-20), the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the compound pesticide has ideal control effect on the urtica fissa and the typha.
TABLE 20 control efficacy of various herbicidal compositions of glufosinate-ammonium, fluroxypyr-meptyl and flumioxazin against Urtica foliorum and Typha after 35 days
Figure BDA0002942931800000472
Figure BDA0002942931800000481
Figure BDA0002942931800000491
As can be seen from Table 20, the herbicidal compositions of examples 22 to 42 have significant advantages in controlling urtica fissa and typha compared to the control agents and comparative examples 6 to 10, 20, 22 and 24. The glufosinate-ammonium single agent has poor prevention effect on nettle and cattail. The chloropyridyl ester single agent of the urtica fissa and the cattail has poor prevention effect. The flumioxazin single agent has poor effect on urtica fissa and cattail.
Although the components contained in the herbicidal compositions of comparative examples 6 to 10 are the same as those in the examples, the control effects are obviously different because the proportions of the components are different.
In summary, when glufosinate-ammonium, fluroxypyridine-ester and flumioxazin are mixed in the ratio of (15-40): (0.1-4): (1-20), the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the compound pesticide has ideal control effect on the urtica fissa and the typha.
TABLE 21 controlling effect of different herbicidal compositions of glyphosate, halauxifen-methyl and flumioxazin against urtica foliosa and cattail after 35 days
Figure BDA0002942931800000492
Figure BDA0002942931800000501
As can be seen from Table 21, the herbicidal compositions of examples 43 to 63 have a significant advantage in controlling urtica fissa and typha compared with the control agents and comparative examples 11 to 15, 23, 25 and 26. The single glyphosate preparation has poor control effect on nettle and typha. The single dose of halauxifen is poor in prevention effect of nettle and cattail. The flumioxazin single agent has poor effect on nettle schizophyllum and cattail.
Although the components contained in the herbicidal compositions of comparative examples 11 to 15 are the same as those in examples, the control effects are obviously different because the proportions of the components are different.
In summary, when glyphosate, halauxifen and flumioxazin are mixed in the ratio of (30-80): (0.05-3): when the components (1-20) are compounded in a weight ratio, the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the composition has ideal control effect on the urtica fissa and the cattail.
TABLE 22 controlling effect of different herbicidal compositions of glyphosate, fluroxypyr-meptyl and flumioxazin against urtica foliosa and cattail after 35 days
Figure BDA0002942931800000502
Figure BDA0002942931800000511
Figure BDA0002942931800000521
As can be seen from Table 22, the herbicidal compositions of examples 64 to 84 have significant advantages in controlling urtica fissa and typha compared to the control agents and comparative examples 16 to 19, 24, 25 and 27. The single glyphosate preparation has poor control effect on nettle and typha. The chloropyridyl ester single agent of the urtica fissa and the cattail has poor prevention effect. The flumioxazin single agent has poor effect on urtica fissa and cattail.
The herbicidal compositions of comparative examples 16 to 19 contain the same components as those of the examples, but the control effects are remarkably different because the proportions of the components are different.
In summary, when glyphosate, fluroxypyridine ester and flumioxazin are mixed in the ratio of (30-80): (0.1-4): (1-20), the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the compound pesticide has ideal control effect on the urtica fissa and the typha.
Pharmacodynamic test 5: the pesticide effect test reagent under the condition of fruit tree shading and under the condition of drought and weak illumination in a specific scene simultaneously: the herbicidal compositions of examples 1 to 42 were prepared according to Table 1.
Comparing the medicament: herbicidal compositions of comparative examples 1 to 10, comparative examples 20 to 24, and single-dose herbicides in table 23 were prepared according to table 1:
TABLE 23 comparison medicament information table related to field efficacy test under shady condition of fruit tree
Contrast agent Source Name of commodity
200g/L glufosinate-ammonium aqua Commercial purchase Hundred fast tons
7.5g/L chlorofluoropyridine ester emulsifiable concentrate Self-matching \
51% flumioxazin water dispersible granule Commercial purchase Feng Qing
3% chlorofluoropyridine ester emulsifiable concentrate Commercial purchase Lingsuke pill
Primary targets: alfalfa at 8-10 leaf stage, and bromus awkeotsang at 10-12 leaf stage.
The test method comprises the following steps: the test is carried out in a pear garden in Shijiazhuang city in Hebei province, the test land is sandy soil, sloping land, dry soil and the relative humidity is about 39 percent. Other herbicides are not applied before and after the test, and the weed population is stable and uniformly distributed. Carrying out manual treatment on a test field, dividing the test field into two parts, setting 2 tests with different soil humidity types, and setting a normal management group when one part is irrigated by sprinkling till the soil is completely wet; half of the solution still remains dry and is shaded by 50% (transmittance is 50%)Sunshade net) set as drought, shade or oligoillumination group. Each treatment was repeated 4 times, each cell area being 30m 2 The application is carried out by diluting with water until the spray quantity per mu is 40L, and replacing the herbicide composition with water as a blank treatment, wherein the test treatments are arranged in random blocks. The pesticide spraying device is an AGROLEX HD400 electric sprayer of Singapore Linong, and adopts a stem leaf spraying method. The conditions were identical for each treatment area except that the herbicide was applied according to the above protocol.
The evaluation method comprises the following steps: the weed control effect of each treatment was observed periodically, and after 30 days, 4 samples were taken per plot, 1m each 2 Weighing the fresh weight of the overground part of the target weeds in the sample prescription, and expressing the control effect of the medicament on the target weeds by using the fresh weight control effect.
Figure BDA0002942931800000531
And (3) test results:
TABLE 24 control efficacy of different herbicidal compositions of glufosinate-ammonium, fluorochloropyridyl ester and flumioxazin against alfalfa and awnless brome 30 days after application
Figure BDA0002942931800000532
Figure BDA0002942931800000541
As can be seen from Table 24, the herbicidal compositions of examples 1 to 21 have significant advantages in controlling weeds under drought and under poor sunlight conditions, as compared with the control agents and comparative examples 1 to 5, comparative example 20, comparative example 21 and comparative example 23.
The herbicidal compositions of comparative examples 1 to 5 contain the same components as those of the examples, but have obvious differences in control effect due to different proportions of the components.
In summary, when glufosinate-ammonium, halauxifen-methyl and flumioxazin are mixed in the ratio of (15-40): (0.05-3): when the components (1-20) are compounded in weight ratio, the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the herbicide composition has ideal control effect on specific scenes such as drought and poor illumination.
TABLE 25 control efficacy of various herbicidal compositions of glufosinate, fluroxypyridine esters and flumioxazin against alfalfa, bromegrass for 30 days
Figure BDA0002942931800000542
Figure BDA0002942931800000551
Figure BDA0002942931800000561
As can be seen from Table 25, the herbicidal compositions of examples 22 to 42 have a significant advantage in controlling weeds under drought, shade or low sunlight conditions, as compared to the control agents and comparative examples 6 to 10, comparative example 20, comparative example 22 and comparative example 24.
The herbicidal compositions of comparative examples 6 to 10 contain the same components as those of the examples, but the control effects are remarkably different because the proportions of the components are different.
In summary, when glufosinate-ammonium, fluroxypyridine-ester and flumioxazin are mixed in the ratio of (15-40): (0.1-4): when the components (1-20) are compounded in a weight ratio, the three components have obvious coordination and synergism, the weed control spectrum is effectively expanded, and the herbicide composition has ideal control effect on specific scenes such as drought and poor illumination.
Pharmacodynamic test 6: under the non-cultivated land shading condition, the drug effect test reagent under the specific scene of drought and short illumination simultaneously: the herbicidal compositions of examples 43 to 84 were formulated according to Table 1.
Comparison of the medicaments: the herbicidal compositions of comparative examples 11 to 19, comparative examples 23 to 27, and the single-dose herbicides in table 26 were formulated according to table 1:
TABLE 26 reference chemical information sheet for field efficacy test under non-cultivated land shading condition
Contrast agent Source Name of commodity
7.5g/L chlorofluoropyridine ester emulsifiable concentrate Self-matching \
51% flumioxazin water dispersible granule Commercial purchase Feng Qing
3% chlorofluoropyridine ester emulsifiable concentrate Commercial purchase Lingsuke pill
41% glyphosate isopropylamine salt aqueous solution Commercial purchase Nongda (agricultural chemical)
Primary targets: wheatgrass at the 8-10 leaf stage and floret mustard at the 8-10 leaf stage.
The test method comprises the following steps: the test is carried out in non-cultivated land of Lin \27950, Gansu province, and the test land is sandy soil, sloping land, dry soil and relative humidity of about 42 percent. Other herbicides are not applied before and after the test, and the weed population is stable and uniformly distributed. The test field is manually processed and divided into two parts, 2 different soil humidity types are set for testing,setting a normal management group when half of the spray irrigation is carried out till the soil is completely wet; half of the plants still kept dry and shaded by 50% (shading net with 50% of light transmittance) were set as a dry and shaded oligophotogroup. Each treatment was repeated 4 times, each cell area being 30m 2 The application was carried out by diluting with water to a spray volume of 40L per acre and replacing the herbicide composition with water as a blank treatment, the test treatments being arranged in random blocks. The pesticide spraying device is an AGROLEX HD400 electric sprayer of Singapore Linong, and adopts a stem leaf spraying method. The conditions were identical for each treatment area except that the herbicide was applied according to the above protocol.
The evaluation method comprises the following steps: the weed control effect of each treatment was observed periodically, and after 30 days, 4 samples were taken per plot, 1m each 2 Weighing the fresh weight of the overground part of the target weeds in the sample prescription, and expressing the control effect of the medicament on the target weeds by using the fresh weight control effect.
Figure BDA0002942931800000571
TABLE 27 control of different herbicidal compositions of glyphosate, halauxifen and flumioxazin against wheatgrass and chloranthus japonicus after 30 days
Figure BDA0002942931800000572
Figure BDA0002942931800000581
As is apparent from Table 27, the herbicidal compositions of examples 43 to 63 have a significant advantage in controlling the effects of Bingcao and Smallanthus sonchifolius as compared with the control agents and comparative examples 11 to 15, comparative example 23, comparative example 25 and comparative example 26.
The herbicidal compositions of comparative examples 11 to 15 contain the same components as in the examples, but have significant differences in control effects due to the different proportions of the components.
In conclusion, when the glyphosate, the halauxifen and the flumioxazin are compounded according to the weight ratio of (30-80) to (0.05-3) to (1-20), the three have obvious coordination and synergism, effectively expand the weed control spectrum and have ideal control effects under drought, shade-shading and low-lighting conditions.
TABLE 28 control efficacy of different herbicidal compositions of glyphosate, fluroxypyr and flumioxazin against wheatgrass and chloranthus glauca
Figure BDA0002942931800000582
Figure BDA0002942931800000591
Figure BDA0002942931800000601
As can be seen from Table 28, the herbicidal compositions of examples 64 to 84 have significant advantages in controlling the effects of Bingcao and Thellungiella asiatica, as compared with the control agents and comparative examples 16 to 19, comparative example 24, comparative example 25 and comparative example 27.
The herbicidal compositions of comparative examples 16 to 19 contain the same components as those of the examples, but the control effects are remarkably different because the proportions of the components are different.
In conclusion, when the glyphosate, the fluroxypyr-meptyl and the flumioxazin are compounded according to the weight ratio of (30-80) to (0.1-4) to (1-20), the three components have obvious coordination and synergism, effectively expand the weed control spectrum and have ideal control effects under the conditions of drought, shade and little illumination.
The herbicide composition containing flumioxazin, and the preparation, application and application method thereof provided by the application are described in detail above. The principle and the implementation of the present application are explained by applying specific examples, and the above description of the embodiments is only used to help understanding the technical solution and the core idea of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the scope of the embodiments of the present application.

Claims (15)

1. A flumioxazin-containing herbicide composition is characterized by comprising herbicide active ingredients, wherein the herbicide active ingredients comprise a herbicide A, a herbicide B and a herbicide C,
the herbicide A is: at least one of glyphosate, glyphosate salt, glufosinate, and glufosinate salt;
the herbicide B is: at least one of chlorofluoropyridine ester and chlorofluoropyridine ester; and
the herbicide C is: flumioxazin;
wherein the mass ratio of the herbicide A to the herbicide B to the herbicide C is (15-80): (0.05-4): (1-20).
2. The herbicide composition as claimed in claim 1, wherein the herbicide A is glyphosate or a salt of glyphosate, the herbicide B is halauxifen-methyl, and the mass ratio of the herbicide A to the herbicide B to the herbicide C is (30-80): (0.05-3): 1-20);
preferably, the mass ratio of the herbicide A to the herbicide B to the herbicide C is (40-60): (0.1-1.5): 2-15).
3. The herbicide composition as claimed in claim 1, wherein the herbicide A is glyphosate or glyphosate salt, the herbicide B is fluroxypyr meptyl, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (30-80): (0.1-4): (1-20);
preferably, the mass ratio of the herbicide A to the herbicide B to the herbicide C is (40-60): (0.3-3): 2-15).
4. A herbicide composition as claimed in claim 1, wherein the herbicide A is glufosinate or a salt of glufosinate, the herbicide B is halauxifen-ethyl, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): (0.05-3): (1-20);
preferably, the mass ratio of the herbicide A to the herbicide B to the herbicide C is (20-35): (0.1-1.5): (2-15).
5. A herbicide composition as claimed in claim 1, wherein the herbicide A is glufosinate-ammonium or a salt of glufosinate-ammonium, the herbicide B is fluroxypyridine ester, and the mass ratio of the herbicide A, the herbicide B and the herbicide C is (15-40): (0.1-4): (1-20);
preferably, the mass ratio of the herbicide A to the herbicide B to the herbicide C is (20-35): (0.3-3): 2-15).
6. The herbicide composition as claimed in claim 1, wherein the herbicidal active ingredient is present in an amount of 6 to 80% by mass based on the total mass of the herbicide composition.
7. The herbicide composition as claimed in claim 2, wherein the herbicidal active ingredient is present in an amount of 34 to 80% by mass based on the total mass of the herbicide composition.
8. A herbicidal composition according to claim 3, characterized in that the mass percentage of the herbicidally active components in the herbicidal composition is 32% to 80% based on the total mass of the herbicidal composition.
9. The herbicide composition as claimed in claim 4, wherein the herbicidal active ingredient is present in an amount of 10 to 80% by mass based on the total mass of the herbicide composition.
10. The herbicide composition as claimed in claim 5, wherein the herbicidal active ingredient is present in an amount of 6 to 80% by mass based on the total mass of the herbicide composition.
11. A herbicidal composition according to any one of claims 1 to 10, characterized in that it further comprises a pesticidally acceptable adjuvant.
12. The herbicide composition as claimed in claim 11, wherein the herbicide composition is any one of oil-based suspension, wettable powder or water dispersible granule.
13. Use of a herbicidal composition according to any one of claims 1 to 10, characterized in that it is used for controlling weeds in non-cultivated lands and/or orchards.
14. The use as claimed in claim 13, wherein the herbicidal composition is applied at a dose of 300 to 1200g (a.i.)/ha.
15. The use of claim 13, wherein the weeds are one or more of glyphosate/glufosinate-resistant eleusine indica, glufosinate-resistant annual fleabane, glufosinate-resistant ranunculus, glyphosate-resistant ambrosia trifida, glyphosate-resistant commelina communis, bluegrass, gnawing kojira, nettle, cattail, alfalfa, awnless brome, wheatgrass, and chloranthus parvifolia.
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CN109380272A (en) * 2018-12-07 2019-02-26 利尔化学股份有限公司 Herbicidal combinations and its application containing L-glufosinate-ammonium and flumioxazin
CN109392946A (en) * 2017-08-15 2019-03-01 海利尔药业集团股份有限公司 A kind of Herbicidal combinations containing glufosinate-ammonium and flumioxazin
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Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104661521A (en) * 2012-07-24 2015-05-27 美国陶氏益农公司 Herbicidal compositions comprising 4-amino-3-chloro-5-fluoro-6-(4-chloro-2-fluoro-3-methoxyphenyl) pyridine-2-carboxylic acid
CN105813460A (en) * 2013-12-12 2016-07-27 美国陶氏益农公司 Selective weed control with halauxifen
CN108782597A (en) * 2017-04-26 2018-11-13 四川利尔作物科学有限公司 A kind of suspending agent containing glyphosate and flumioxazin
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