Ternary weeding composition containing ALS enzyme inhibitor and application thereof

Abstract

The invention provides a ternary weeding composition containing an ALS enzyme inhibitor and application of the ternary weeding composition, the herbicide composition comprises three active components, the active component A is flazasulfuron and salt thereof, the active component B is quinclorac and salt thereof, and the active component C is a mixture of the active component A and the active component B. The active ingredient C is selected from one of fluroxypyr, trichlopyr, halauxic, halauxic and salts and esters thereof, the weight part ratio of the active ingredients is 1: (1-50): (1-50), and the total weight of the active ingredients accounts for 1-80% of the total weight of the weeding composition. The ternary weeding composition can be used for preventing and removing various gramineous weeds, broadleaf weeds and cyperaceae weeds in warm-season lawns, has an obvious synergistic effect compared with a single component, can improve the prevention and treatment effect, and particularly has a good effect on flazasulfuron weeds; in addition, the weeding composition also has a very good control effect on older weeds, and is long in lasting period and high in safety.

Description

Technical Field

[0001] The invention belongs to the field of pesticides, and specifically relates to a ternary herbicidal composition of flazsulfuron-methyl, quinclorac and clofopyralid and application thereof. Background Art

[0002] With the continuous acceleration of urbanization, warm-season lawns are widely used in various fields because of their beautification of the environment and purification of the air. They are not only widely used in urban green belts and park lawns, but also in football fields, golf courses and other sports venues.

[0003] In lawn maintenance, weed control is an important task. At present, the use of selective herbicides is the most convenient and effective method. However, with the extensive use of herbicides, weed resistance has also increased, and the control effect has become increasingly poor. In addition, some older weeds are also difficult to control. These highly resistant and older weeds need to be effectively controlled.

[0004] Currently, the main herbicide for controlling warm-season lawn weeds on the market is fluazifop-methyl, but it has serious resistance and is basically ineffective against older weeds. Dichloroquine is a hormone-type quinoline carboxylic acid herbicide used to control grass weeds such as barnyard grass in lawns, but with the continuous increase in barnyard grass resistance in recent years, the control effect has been significantly weakened. Clofopyralid is a systemic hormone-type herbicide used to control broadleaf weeds in lawns, but it is ineffective against grass weeds and sedge weeds.

[0005] Patent EP3664609A4 discloses at least two hormone herbicides and at least one ALS inhibitor herbicide, of which only fluroxypyr and quinclorac are mentioned among the many hormone herbicides, and only flazasulfuron is mentioned among the many ALS inhibitor herbicides. However, there is no data showing that a synergistic effect is achieved, and there is no specific application method.

[0006] Patent CN103281899A discloses that a composition of quinclorac and fluroxypyra has a synergistic effect on barnyardgrass (Echinochloa crus-galli; ECHCG), Leptochloa chinensis (LEFCH) and Brachiaria platyphylla (BRAPP) within a certain ratio range. The present invention adds an ALS enzyme inhibitor herbicide flazasulfuron-methyl to quinclorac and fluroxypyra, and the synergistic effect is more significant under the cooperation of different action mechanisms, and it also has outstanding performance in preventing and controlling flazasulfuron-methyl-resistant weeds and older weeds.

[0007] In order to solve the above technical problems, the present invention provides a ternary herbicide composition containing an ALS enzyme inhibitor, which has a significant synergistic effect on grass weeds, broadleaf weeds and sedge weeds through the combination of herbicides with different action mechanisms, and is particularly effective against weeds resistant to flazasulfuron-methyl; in addition, it also has a good control effect on older weeds, has a long lasting effect and is highly safe. Summary of the invention

[0008] The object of the present invention is to provide a ternary herbicidal composition containing an ALS enzyme inhibitor.

[0009] Another object of the present invention is to provide a weed control application of the herbicidal composition in warm-season lawns.

[0010] The herbicidal composition of the present invention has a synergistic effect, and is particularly effective against weeds resistant to flazasulfuron-methyl; in addition, it also has a good control effect on older weeds, has a long lasting effect, and is highly safe.

[0011] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0012] The invention provides a ternary herbicidal composition containing an ALS enzyme inhibitor. The composition comprises three active ingredients, wherein the active ingredient A is flazasulfuron-methyl and its salt, the active ingredient B is quinclorac and its salt, and the active ingredient C is selected from one of clofopyralid, triclopyralid, clofopyralid, haloxyfop and its salt and ester, the weight ratio of the active ingredients A, B and C is 1:(1-50):(1-50), and the total weight percentage of the active ingredients accounts for 1-80% of the total weight of the herbicidal composition.

[0013] In a further preferred embodiment, the weight ratio of active ingredients A, B and C is 1:(3-30):(3-30), and the total weight of the active ingredients accounts for 10-70% of the total weight of the herbicidal composition.

[0014] The salts covered by the active ingredients Compound A, Compound B and Compound C in the present invention may be any agriculturally acceptable salts, including sodium salts, potassium salts, ammonium salts, magnesium salts, calcium salts, monomethyl salts, dimethyl salts, triethyl salts, inorganic acid salts, organic acid salts, etc.

[0015] The esters included in the active ingredient compound C of the present invention may be any agriculturally acceptable esters, including methyl ester, ethyl ester, propyl ester, isooctyl ester and the like.

[0016] The invention also provides application of the herbicidal composition in preventing and controlling grass weeds, broadleaf weeds and / or sedge weeds.

[0017] The grass weeds include barnyard grass (Echinochloa crus-galli), crabgrass (Digitariasanguinalis), foxtail grass (Setaria viridis), goosegrass (Eleusine indica), foxtail grass (Alopecurus aequalis), Japanese foxtail grass (Alopecurus japonicus), wild oats (Avena fatua) and the like.

[0018] The broadleaf weeds include Polygonum, Portulaca oleracea, Capsella bursa-pastoris, Abutilon theophrasti, Amaranthus spinosus, Amaranthus retroflexus, Chenopodium album, Rumexcrispus, Commelina communis, Xanthium strumarium, Solanum nigrum, Cassia tora, Stellaria media, Stellaria aguatica, Cerastium arvense, Galium aparine, Veronica didyma, etc.

[0019] The sedge weeds include Cyperus rotundus, Cyperus iria, Cyperus difformis and the like.

[0020] Furthermore, the present invention also provides the use of the herbicidal composition in controlling grass weeds, broadleaf weeds and / or sedge weeds in warm-season lawns. In particular, the herbicidal composition of the present invention has a significant effect on controlling resistant weeds and older weeds.

[0021] Wherein, the resistance index RI of the resistant weeds is ≥10.

[0022] The older weeds have more than 5 leaves and a plant height of more than 5 cm.

[0023] The varieties of the warm-season lawn include Cynodon dactylon, Zoysia japonica Steud. and Eremochloa ophiuroides.

[0024] Furthermore, the herbicidal composition provided by the present invention can be used to act on harmful plants, crops, plant seeds or areas where plants grow.

[0025] The ternary herbicidal composition of the present invention can be formulated into solid preparations such as powders, wettable powders, water-dispersible granules, dry suspensions or effervescent tablets, etc.; liquid preparations such as suspensions, dispersible oil suspensions, etc. The definition, development method, application technology, quality indicators and detection methods of the above-mentioned formulations are referred to Xu Yan, Liu Guangwen et al. [Pesticide Liquid Preparations, (2018, Chemical Industry Press)], Liu Guangwen et al. [Pesticide Solid Preparations, (2018, Chemical Industry Press)].

[0026] The ternary herbicidal composition of the present invention also contains common adjuvants required for preparing pesticide preparations, wherein solid preparations include dispersants, wetting agents, defoaming agents, complexing agents, pH regulators and fillers, etc., and liquid preparations include dispersants, emulsifiers, wetting agents, stabilizers, thickeners, pH regulators, defoaming agents and antifreeze agents, etc.

[0027] The wetting agent is selected from one or more of EO / PO block polyether, fatty alcohol polyoxyethylene ether, fatty alcohol ethoxylate, tallow ethoxylate ammonium salt, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, and acyl glutamate.

[0028] The dispersant is selected from one or more of EO / PO block polyether, condensed naphthalene sulfonate, phenol sulfonic acid condensate sodium salt, methyl naphthalene sulfonate sodium formaldehyde condensate, sodium lignin sulfonate, sodium methylene dinaphthalene sulfonate, acrylic acid homopolymer sodium salt, high molecular weight polycarboxylate, dioctyl sulfosuccinic acid sodium salt, and maleic acid-acrylic acid copolymer sodium salt.

[0029] The emulsifier is selected from one or more of alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, castor oil ethylene oxide adduct and its derivatives, alkyl sulfonates, alkyl biphenyl ether sulfonates, naphthalenesulfonic acid formaldehyde condensates, alkylphenol polyoxyethylene ether formaldehyde condensates, polyoxyethylene polyoxypropylene block copolymers, alkylnaphthalenesulfonic acid formaldehyde condensates, quaternary ammonium salts, tallow ethoxylated ammonium salts, amino acids, amine oxides, betaines and acyl glutamates.

[0030] The application of these auxiliary materials is to achieve the stability of the physical properties of the dosage form and achieve the field application effect. For the types, functions, and application techniques of auxiliary materials, please refer to Zhang Xiaojun, Liu Guangwen, et al. [Pesticide Adjuvants, (2018, Chemical Industry Press)].

[0031] Those skilled in the art know that the herbicide currently on the market for controlling warm-season lawn weeds is mainly fluazifop-methyl, but it has serious resistance and is basically ineffective against older weeds. Quinclorac, as a hormone-type quinoline carboxylic acid herbicide, is commonly used to control grass weeds such as barnyard grass in lawns, but with the increase in the dosage in recent years, the resistance of barnyard grass has been continuously improved, and the control effect has been significantly weakened. Flupyralid, as a systemic hormone-type herbicide, is used to control broadleaf weeds in lawns, but it is ineffective against grass weeds and sedge weeds.

[0032] After a large number of tests, the applicant unexpectedly found that when a combination of herbicides with different mechanisms of action is used, especially a combination of an ALS enzyme inhibitor herbicide flazasulfuron-methyl with a hormone herbicide dichloroquine and a systemic hormone herbicide clofopyralid, it has a significant synergistic effect on warm-season lawn weeds, further expanding the weed control spectrum and improving the control effect. In particular, it has a significant effect on the control of flazasulfuron-methyl-resistant weeds; in addition, the composition of the present invention can achieve good control of grass weeds, broad-leaved weeds and sedge weeds, and has a control effect on older weeds, has significant control effect, a long lasting effect, is highly safe for lawns, and is not prone to resistance.

[0033] Compared with the prior art, the advantages of the present invention are:

[0034] The ternary herbicidal composition provided by the present invention is composed of active ingredients with different action mechanisms. Furthermore, the composition of the present invention has good control effects on gramineous weeds, broadleaf weeds and sedge weeds in a specific ratio, can effectively control weeds resistant to fluazifop-methyl, maintains good weed control effects, has obvious synergistic effects, can significantly reduce the use of pesticides, has control effects on older weeds, and is highly safe for warm-season lawns.

[0035] The herbicidal composition provided by the invention can expand the control spectrum, effectively delay the generation of resistance, reduce the use cost and alleviate the pollution to the environment, and has great application value in controlling warm-season lawn weeds. DETAILED DESCRIPTION

[0036] In order to better understand the essence of the present invention, the content of the present invention is further described below in conjunction with the examples, but it cannot be regarded as limiting the present invention. The content mentioned in the examples is not limiting the present invention. The material formula selection can be adapted to local conditions and has no substantial effect on the results. In these examples, unless otherwise specified, all percentages are weight percentages.

[0037] Indoor activity measurement example 1:

[0038] After a large number of target tests, the inventors took the toxicity test of fennel as an example to conduct indoor activity determination demonstration.

[0039] The test was conducted with reference to the Agricultural Industry Standard of the People's Republic of China NY / T 1155.4-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Herbicides Part 4: Activity Determination Test Stem Spray Method" and the Agricultural Industry Standard of the People's Republic of China "NY / T1155.7-2006 Guidelines for Indoor Bioassay Tests of Pesticides - Herbicides Part 7: Determination of Combined Action of Mixtures" for testing:

[0040] 1. Purpose of the test

[0041] The fresh weight control effects of flazasulfuron-methyl, quinclorac, clofopyralid and their different mixed compositions on weeds were determined, and their combined effects were evaluated, providing a scientific basis for the formulation development of mixed agents and field efficacy trials for pesticide registration.

[0042] 2. Test conditions

[0043] 2.1. Test target: Anise

[0044] 2.2. Instruments and equipment: 3WPSH-500E biological testing spray tower, electronic balance (sensitivity 0.1 mg), basin, beaker, pipette.

[0045] 3. Experimental design

[0046] 3.1 Test soil: The test soil used was air-dried soil with an organic matter content of <3%, neutral pH and good permeability that could pass through sieve.

[0047] 3.2 Test method: The test soil was quantitatively filled to 4 / 5 of the pot. The bottom of the pot was infiltrated to make the soil completely wet. The pre-treated test weed seeds were evenly sown on the soil surface, covered with soil about 1.0 cm, and moved into the greenhouse for conventional cultivation after sowing. Water was replenished to saturation by infiltration irrigation at the bottom of the pot. After the weeds emerged, thinning and determining the weeds to ensure the same density (total density of 120 to 150 plants per square meter). When the weeds emerged and grew to 2 to 4 leaves, the 3WPSH-500E bio-test spray tower produced by Nanjing Agricultural Machinery Research Institute was used for stem and leaf spray treatment, with a liquid volume of 20 mL and a working pressure of 0.15 MPa. Each treatment group was repeated 3 times, and the treatment without the agent was set as the control. The growth of the target weeds was observed regularly.

[0048] 4. Absolute value (numerical measurement) survey method

[0049] After treatment, the growth status of the tested weeds was observed and recorded regularly. The herbicidal activity was investigated and recorded by the absolute value (number measurement) survey method 30 days after treatment, and the damage symptoms were described at the same time. The main symptoms were: color change (yellowing, etc.); morphological change (curved new leaves, etc.); growth change (dehydration, withering, dwarfing, clustering, etc.).

[0050] According to the survey data, the fresh weight control effect of the treatment is calculated according to the formula. The unit is percentage (%). The calculation result is retained to 2 decimal places. According to the survey results, the fresh weight inhibition rate is calculated according to the following formula:

[0051] Fresh weight inhibition rate (%) = (CK fresh weight - treatment fresh weight) / CK fresh weight × 100

[0052] The herbicidal activity after mixing was tested by the Colby method, that is, E0 = XYZ / 10000, where X is the weed survival rate of herbicide A at a dosage of P; Y is the weed survival rate of herbicide B at a dosage of Q; Z is the weed survival rate of herbicide C at a dosage of W; E0 is the theoretical weed survival rate of herbicide (A+B+C) at a dosage of (P+Q+W); and E is the actual weed survival rate of each treatment. According to the Colby method, when E0-E>10%, it means that the mixed herbicide has a synergistic effect; when E0-E<-10%, it means that the mixed herbicide has an antagonistic effect; when the E0-E value is between ±10%, it means that the mixed herbicide has an additive effect.

[0053] 5. Test results and conclusions

[0054] According to the present invention, a large number of mixing tests were conducted to verify the toxicity of the following ratios. After preliminary tests, the combined toxicity of different ratios of flazasulfuron, quinclorac and clofopyralid on fennel is shown in Table 1:

[0055] Table 1: The combined toxicity of the herbicide combination to fennel (spray method)

[0056]

[0057] It can be seen from the results in Table 1 that when flazasulfuron-methyl and quinclorac are compounded, at 2:10 and 4:20, E0-E is between ±10%, showing an additive effect, and at 1:0 and 2:40, E0-E>10%, showing a certain synergistic effect; when flazasulfuron-methyl and clofopyralid are compounded, at 2:10 and 4:10, E0-E is between ±10%, showing an additive effect, and at 1:20 and 2:20, E0-E>10%, showing a certain synergistic effect; when quinclorac and clofopyralid are compounded, at 10:40 and 40:10, E0-E is between ±10%, showing an additive effect, and at 20:10 and 10:10, E0-E>10%, showing a certain synergistic effect. When the three components of flazasulfuron, quinclorac and clofopyralid are compounded, compared with the use of each pesticide component alone or in combination of two, they have excellent control effects on broadleaf weeds such as fennel. When the weight ratio of flazasulfuron, quinclorac and clofopyralid is 4:20:20, 2:20:40, 2:20:10, 2:40:40, 1:10:10, 1:20:40, E0-E>10%, further, when the weight ratio is 4:20:20, 2:20:40, 2:20:10, 2:40:40, 1:10:10, E0-E>15%, when the weight ratio is 2:40:40 and 1:10:10, E0-E exceeds 20%, and the theoretical survival rate of fennel is significantly higher than the actual survival rate of fennel, showing a synergistic effect.

[0058] The weed control test after compounding the above three ingredients of fluazifop-butyl, quinclorac and clofopyralid showed that the activity of the three-ingredient compound was significantly increased, which was significantly better than the effect of the two-ingredient compound.

[0059] Indoor resistance grass activity determination example 2:

[0060] The inventors conducted a large number of target tests and took the toxicity test of Echinochloa crus-galli (L.) P.Beauv. as an example to demonstrate indoor activity determination. The Echinochloa crus-galli is obtained by culturing Echinochloa crus-galli seeds indoors until the leaves reach more than 5 pieces and the plant height reaches more than 5 cm.

[0061] The test was conducted with reference to the Agricultural Industry Standard of the People's Republic of China NY / T 1155.4-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Herbicides Part 4: Activity Determination Test Stem Spray Method" and the Agricultural Industry Standard of the People's Republic of China "NY / T1155.7-2006 Guidelines for Indoor Bioassay Tests of Pesticides - Herbicides Part 7: Determination of Combined Action of Mixtures" for testing:

[0062] 1. Purpose of the test

[0063] The fresh weight control effects of flazasulfuron-methyl, quinclorac, clofopyralid and their different mixed compositions on weeds were determined, and their combined effects were evaluated, providing a scientific basis for the formulation development of mixed agents and field efficacy trials for pesticide registration.

[0064] 2. Test conditions

[0065] 2.1. Test target: Old barnyard grass

[0066] 2.2. Instruments and equipment: 3WPSH-500E biological testing spray tower, electronic balance (sensitivity 0.1 mg), basin, beaker, pipette.

[0067] 3. Experimental design

[0068] 3.1 Test soil: The test soil used was air-dried soil with an organic matter content of <3%, neutral pH and good permeability that could pass through sieve.

[0069] 3.2 Test method: The test soil was quantitatively filled to 4 / 5 of the pot. The bottom of the pot was infiltrated to make the soil completely wet. The pre-treated resistant barnyard grass seeds were evenly sown on the soil surface, covered with soil about 1.0 cm, and moved into the greenhouse for conventional cultivation after sowing. Water was replenished to saturation by infiltration irrigation at the bottom of the pot. After the weeds emerged, thinning and determining the weeds to ensure the same density (total density of 120 to 150 plants per square meter). When the weeds emerged and grew to 2 to 4 leaves, the 3WPSH-500E bio-test spray tower produced by Nanjing Agricultural Machinery Research Institute was used for stem and leaf spray treatment. The liquid volume was 20 mL, the working pressure was 0.15 MPa, and each treatment group was repeated 3 times, and the treatment without the drug was set as the control. The growth of the target weeds was observed regularly.

[0070] 4. Absolute value (numerical measurement) survey method

[0071] After treatment, the growth status of the tested weeds was observed and recorded regularly. The herbicidal activity was investigated and recorded by the absolute value (number measurement) survey method 30 days after treatment, and the damage symptoms were described at the same time. The main symptoms were: color change (yellowing, etc.); morphological change (curved new leaves, etc.); growth change (dehydration, withering, dwarfing, clustering, etc.).

[0072] According to the survey data, the fresh weight control effect of the treatment is calculated according to the formula. The unit is percentage (%). The calculation result is retained to 2 decimal places. According to the survey results, the fresh weight inhibition rate is calculated according to the following formula:

[0073] Fresh weight inhibition rate (%) = (CK fresh weight - treatment fresh weight) / CK fresh weight × 100

[0074] The herbicidal activity after mixing was tested by the Colby method, that is, E0 = XYZ / 10000, where X is the weed survival rate of herbicide A at a dosage of P; Y is the weed survival rate of herbicide B at a dosage of Q; Z is the weed survival rate of herbicide C at a dosage of W; E0 is the theoretical weed survival rate of herbicide (A+B+C) at a dosage of (P+Q+W); and E is the actual weed survival rate of each treatment. According to the Colby method, when E0-E>10%, it means that the mixed herbicide has a synergistic effect; when E0-E<-10%, it means that the mixed herbicide has an antagonistic effect; when the E0-E value is between ±10%, it means that the mixed herbicide has an additive effect.

[0075] 5. Test results and conclusions

[0076] According to the present invention, a large number of mixing tests were conducted to verify the toxicity of the following ratios. After preliminary tests, the combined toxicity of different ratios of flazasulfuron, quinclorac and clofopyralid on old barnyard grass is shown in Table 2:

[0077] Table 2: Combined toxicity of herbicidal combinations to old barnyard grass (spray method)

[0078]

[0079]

[0080] It can be seen from the results in Table 2 that when flazasulfuron-methyl and dichloroquine are compounded, at 2:10 and 4:20, E0-E is between ±10%, showing an additive effect, and at 1:10 and 2:40, E0-E>10%, showing a certain synergistic effect; when flazasulfuron-methyl and clofopyralid are compounded, at 2:10 and 4:10, E0-E is between ±10%, showing an additive effect, and at 1:20 and 2:20, E0-E>10%, showing a certain synergistic effect; when dichloroquine and clofopyralid are compounded, at 10:40 and 40:10, E0-E is between ±10%, showing an additive effect, and at 20:10 and 10:10, E0-E>10%, showing a certain synergistic effect. When the three components of flazasulfuron-methyl, quinclorac and clofopyralid are compounded, compared with the use of each pesticide component alone or in combination of two, they have excellent control effects on grass weeds such as old barnyard grass. When the weight ratio of flazasulfuron-methyl, quinclorac and clofopyralid is 4:20:20, 2:20:40, 2:20:10, 2:40:40, 1:10:10, 1:20:40, E0-E>10%, further, when the weight ratio is 4:20:20, 2:20:40, 2:20:10, 2:40:40, 1:10:10, E0-E>15%, when the weight ratio is 2:40:40, 1:10:10, E0-E exceeds 20%, and the theoretical survival rate of old barnyard grass is significantly higher than the actual survival rate of old barnyard grass, showing a synergistic effect.

[0081] The weed control test after compounding the above three ingredients of fluazifop-butyl, quinclorac and clofopyralid showed that the activity of the three-ingredient compound was significantly increased, which was significantly better than the effect of the two-ingredient compound.

[0082] Preparation excipient example 1: 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules (1:30:3)

[0083] The composition of 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules is shown in Table 3:

[0084] Table 3 Component details of 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules

[0085]

[0086] According to the detailed components in Table 3, active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, the above materials are subjected to air flow pulverization to D90≤25μm, the above pulverized materials are mixed with water (150-180kg of deionized water is used per ton of materials) by a mixer to make the materials plastic, the mixed materials are extruded into columnar particles with a diameter of 1.0mm and dried with 80-90℃ hot air until the moisture is less than 3%, and the ternary herbicidal composition 34% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention can be prepared. After testing, the ternary herbicidal composition 34% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention meet various product standards and are qualified products.

[0087] Preparation excipient example 2: 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules (1:3:30)

[0088] The composition of 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules is shown in Table 4:

[0089] Table 4 Component details of 34% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules

[0090]

[0091] According to the detailed components in Table 4, active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, the above materials are subjected to air flow pulverization to D90≤25μm, the above pulverized materials are mixed with water (150-180kg of deionized water is used per ton of materials) by a mixer to make the materials plastic, the mixed materials are extruded into columnar particles with a diameter of 1.0mm and dried with 80-90℃ hot air until the moisture is less than 3%, and the ternary herbicidal composition 34% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention can be prepared. After testing, the ternary herbicidal composition 34% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention meet various product standards and are qualified products.

[0092] Preparation excipient example 3: 11% flazasulfuron-methyl·quinclorac·clofopyralid suspension (1:5:5)

[0093] The composition of 11% flazasulfuron-methyl·quinclorac·clofopyralid suspension is shown in Table 5:

[0094] Table 5 Component details of 11% flazasulfuron-methyl·quinclorac·clofopyralid suspension

[0095]

[0096] According to the details of each component in Table 5, the original drug, dispersing wetting agent, antifreeze agent, preservative and part of thickener, defoamer, stabilizer and water are weighed in proportion and mixed evenly, and ground. When the particle size is 5 μm, the grinding is stopped, and the remaining thickener and defoamer are added and adjusted evenly to obtain a suspension product. The ternary herbicidal composition 11% flazasulfuron-methyl·quinclorac·clofopyralid suspension of the present invention meets all product standards and is a qualified product.

[0097] Preparation excipient example 4: 21% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules (1:10:10)

[0098] The composition of 21% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules is shown in Table 6:

[0099] Table 6 Component details of 21% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules

[0100]

[0101]

[0102] According to the detailed components in Table 6, active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, the above materials are subjected to air flow pulverization to D90≤25μm, the above pulverized materials are mixed with water in a mixer (120-150kg of deionized water is used per ton of materials) to make the materials plastic, the mixed materials are extruded into columnar particles with a diameter of 1.0mm and dried with 80-90℃ hot air to a moisture content of less than 3%, and the ternary herbicidal composition 21% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention can be obtained. After testing, the ternary herbicidal composition 21% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention meet various product standards and are qualified products.

[0103] Preparation excipient example 5: 32% flazasulfuron-methyl·quinclorac·clofopyralid wettable powder (1:10:5)

[0104] The composition of 32% flazasulfuron-methyl·quinclorac·clofopyralid wettable powder is shown in Table 7:

[0105] Table 7 Components of 32% flazasulfuron-methyl·quinclorac·clofopyralid wettable powder

[0106]

[0107] According to the detailed components in Table 7, the active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, and the above materials are subjected to air flow crushing to D90≤30μm to obtain the ternary herbicidal composition 32% flazasulfuron-methyl·quinclorac·clofopyralid wettable powder of the present invention. After testing, the ternary herbicidal composition 32% flazasulfuron-methyl·quinclorac·clofopyralid wettable powder of the present invention meets various product standards and is a qualified product.

[0108] Preparation excipient example 6: 41% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules (1:20:20)

[0109] The composition of 41% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules is shown in Table 8:

[0110] Table 8 Component details of 41% flazasulfuron-methyl·quinclorac·clofopyralid water dispersible granules

[0111]

[0112] According to the detailed components in Table 8, active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, the above materials are subjected to air flow pulverization to D90≤25μm, the above pulverized materials are mixed with water in a mixer (120-150kg of deionized water is used per ton of materials) to make the materials plastic, the mixed materials are extruded into columnar particles with a diameter of 1.0mm and dried with 80-90℃ hot air to a moisture content of less than 3%, and the ternary herbicidal composition 41% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention can be obtained. After testing, the ternary herbicidal composition 41% flazsulfuron-methyl·quinclorac·clofopyralid water dispersible granules of the present invention meet various product standards and are qualified products.

[0113] Preparation excipient example 7: 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder (1:10:20)

[0114] The composition of 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder is shown in Table 9:

[0115] Table 9 Component details of 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder

[0116]

[0117] According to the details of each component in Table 9, the active ingredient 1, active ingredient 2, active ingredient 3, dispersant, wetting agent and carrier are put into a mixing kettle and mixed for 10 minutes, and the above materials are subjected to air flow crushing to D90≤30μm, so as to obtain the ternary herbicidal composition 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder of the present invention. After testing, the ternary herbicidal composition 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder of the present invention meets various product standards and is a qualified product.

[0118] Preparation excipient example 8: 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder (1:20:10)

[0119] The composition of 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder is shown in Table 9:

[0120] Table 10 Component details of 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder

[0121]

[0122] According to the details of each component in Table 10, the active ingredient 1, the active ingredient 2, the active ingredient 3, the dispersant, the wetting agent and the carrier are put into a mixing kettle and mixed for 10 minutes, and the above materials are subjected to air flow crushing to D90≤30μm, so as to obtain the ternary herbicidal composition 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder of the present invention. After testing, the ternary herbicidal composition 31% flazasulfuron-methyl·quinclorac sodium·clofopyralid wettable powder of the present invention meets various product standards and is a qualified product.

[0123] Product field efficacy method:

[0124] According to the product formulation excipient example, the present invention conducts field efficacy tests on the above formulations. The standard description is as follows:

[0125] Field efficacy example 1

[0126] Field trials of flazsulfuron-methyl, quinclorac and clofopyralid to control weeds in warm-season Bermudagrass turf

[0127] The test was conducted with reference to the National Standard of the People's Republic of China GB / T 17980.148-2004 "Guidelines for Field Efficacy Tests of Pesticides (II) Part 148: Herbicides for Control of Lawn Weeds":

[0128] 1. Experimental purpose: To investigate the field control effects of different compound combinations on weeds in warm-season lawns.

[0129] 2. Targets of prevention and control: broadleaf weeds, grass weeds and sedge weeds.

[0130] 3. Test agents: product formulation excipients of Examples 3 to 7, 25% flazasulfuron WG (commercially available), 50% quinclorac WP (commercially available), 20% clofopyralid EC (commercially available).

[0131] 4. Application method: normal amount of foliar spray.

[0132] 5. Plot arrangement, area and repetition:

[0133] Area of ​​the cell: 4 to 10 m 2 , leave 1m of protection row interval between each small room, and repeat 4 times.

[0134] 6. Experimental investigation and calculation method:

[0135] 6.1. Weed survey: record the weed population in the plot, including indicators such as weed number, coverage or weed weight, etc., and absolute numbers can be used;

[0136] 6.2. Investigation time: observe once a week after application and record the rating for 15 consecutive days, and investigate the results on the 30th day;

[0137] 6.3. Survey method: Investigate the total number or fresh weight of each weed, randomly select 4 points in each plot, 1m 2 Conducting sample surveys;

[0138] 6.4. Calculation method of drug efficacy

[0139] The efficacy is calculated according to the formula: Control effect (%) = [1-(CK-PT) / CK] × 100

[0140] Where: PT – number or fresh weight of remaining grass in the pesticide-treated area;

[0141] CK——number of live grass or fresh weight in blank control area.

[0142] 6. Test results and conclusions

[0143] This experiment was conducted in Suqian, Jiangsu Province, where the terrain is flat and the management is normal. The density and growth of weeds in all experimental plots are relatively uniform.

[0144] Based on the above conditions, the present invention is designed to spray once on April 26, 2023 according to Table 11 (A represents flazasulfuron, B represents quinclorac, and C represents clofopyralid), and conduct a final weed survey and statistics on May 25, 2023. The experimental design is shown in Table 11:

[0145] Table 11 Field trial design

[0146]

[0147]

[0148] According to the design in Table 11, on May 28, 2023, the present invention identified and counted weeds according to the above test survey results and calculation method, and analyzed the control effect. The results are shown in Table 12:

[0149] Table 12 Field efficacy test results

[0150]

[0151] As can be seen from Table 12, Formulation Examples 3 to 7 have good control effects on broadleaf weeds, grass weeds and sedge weeds in warm-season lawns. The formulations were sprayed once according to the dosage in Table 11, and the control effects on broadleaf weeds, grass weeds and sedge weeds in warm-season lawns reached more than 90% 30 days later, which was significantly better than the control effects of each control agent, especially Formulation Example 4, when the ratio of active ingredients was 1:10:10, the control effect could reach more than 95%.

[0152] Field efficacy example 2

[0153] Field trials of flazsulfuron-methyl, quinclorac and clofopyralid to control weeds in warm-season Bermudagrass turf

[0154] The test was conducted with reference to the National Standard of the People's Republic of China GB / T 17980.148-2004 "Guidelines for Field Efficacy Tests of Pesticides (II) Part 148: Herbicides for Control of Lawn Weeds":

[0155] 1. Experimental purpose: To investigate the field control effects of different compound combinations on weeds in warm-season lawns.

[0156] 2. Targets of prevention and control: broadleaf weeds, grass weeds and sedge weeds.

[0157] 3. Test agents: product formulation excipients of Examples 3 to 7, 25% flazasulfuron WG (commercially available), 50% quinclorac WP (commercially available), 20% clofopyralid EC (commercially available).

[0158] 4. Application method: normal amount of foliar spray.

[0159] 5. Plot arrangement, area and repetition:

[0160] Area of ​​the cell: 4 to 10 m 2 , leave 1m of protection row interval between each small room, and repeat 4 times.

[0161] 6. Experimental investigation and calculation method:

[0162] 6.1. Weed survey: record the weed population in the plot, including indicators such as weed number, coverage or weed weight, etc., and absolute numbers can be used;

[0163] 6.2. Investigation time: observe once a week after application and record the rating for 15 consecutive days, and investigate the results on the 30th day;

[0164] 6.3. Survey method: Investigate the total number or fresh weight of each weed, randomly select 4 points in each plot, 1m 2 Conducting sample surveys;

[0165] 6.4. Calculation method of drug efficacy

[0166] The efficacy is calculated according to the formula: Control effect (%) = [1-(CK-PT) / CK] × 100

[0167] Where: PT – number or fresh weight of remaining grass in the pesticide-treated area;

[0168] CK——number of live grass or fresh weight in blank control area.

[0169] 6. Test results and conclusions

[0170] This experiment was conducted in Changzhou, Jiangsu Province, where warm-season lawn weeds are highly resistant to flazasulfuron, the terrain is flat, and the management is normal. The weed density and growth of all experimental plots were relatively uniform.

[0171] Based on the above conditions, the present invention is designed to spray once on March 28, 2024 according to Table 11 (A represents flazasulfuron, B represents quinclorac, and C represents clofopyralid), and conduct a final weed survey and statistics on April 26, 2024. The experimental design is shown in Table 13:

[0172] Table 13 Field trial design

[0173]

[0174]

[0175] According to the design in Table 13, on May 6, 2024, the present invention identified and counted the weeds according to the above test survey results and calculation method, and analyzed the control effect. The results are shown in Table 14:

[0176] Table 14 Field efficacy test results

[0177]

[0178] As shown in Table 14, when 25% flazasulfuron WG (commercially available) is used at 15g, ai / ha (active ingredient), the control effect is only about 20%, and when it is used at 45g, ai / ha (active ingredient), the control effect is only about 40%, which is generally low, and the weeds in this area are highly resistant to flazasulfuron. However, formulation examples 3 to 7 have a good control effect on broadleaf weeds, grass weeds and sedge weeds in warm-season lawns. The formulations are sprayed once according to the dosage of Table 13, and the control effect on broadleaf weeds, grass weeds and sedge weeds in warm-season lawns after 30 days reaches more than 75%, which is significantly better than the control effect of each control agent, especially formulation example 4, when the active ingredient ratio is 1:10:10, the control effect can reach more than 85%.

[0179] In summary, the present invention adopts a ternary herbicidal composition for controlling a variety of broadleaf weeds, grass weeds and sedge weeds in warm-season lawns, and the optimal ratio thereof is between 1:(3-30):(3-30). Compared with the existing preparations, the present invention has an obvious synergistic effect, especially a good effect on weeds resistant to flazasulfuron-methyl. In addition, the present invention also has a good control effect on older weeds, and is worthy of promotion and application in agricultural production.

[0180] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A ternary herbicidal composition containing an ALS enzyme inhibitor, characterized in that: The herbicide composition comprises three active ingredients, wherein active ingredient A is flazasulfuron and its salts, active ingredient B is quinclorac and its salts, and active ingredient C is selected from one of clofopyralid, triclopyralid, clofopyralid, fluclopyralid and its salts and esters, the weight ratio of active ingredients A, B and C is 1:(1-50):(1-50), and the total weight percentage of the active ingredients accounts for 1-80% of the total weight of the herbicide composition.

2. The herbicidal composition according to claim 1, characterized in that The weight ratio of the active ingredients A, B and C is 1:(3-30):(3-30), and the total weight of the active ingredients accounts for 10-70% of the total weight of the herbicidal composition.

3. Use of the herbicidal composition according to claim 1 in controlling grass weeds, broadleaf weeds and / or sedge weeds.

4. The use according to claim 3, characterized in that: The herbicidal composition is used for preventing and controlling grass weeds, broadleaf weeds and / or sedge weeds in warm-season lawns.

5. The use according to claim 3, characterized in that: The grass weeds are barnyard grass and crabgrass, the broadleaf weeds are shepherd's purse and fennel, and the sedge weed is cyperus rotundus.

6. The use according to claim 4, characterized in that: The warm season lawn is a bermudagrass lawn and / or a zoysiagrass lawn.

7. The use according to claim 3, characterized in that: The herbicidal compositions act on harmful plants, crop plants, plant seeds or areas where plants grow.

8. The herbicidal composition according to claim 1, characterized in that The herbicidal composition can be formulated into one of wettable powder, granules, emulsifiable granules, water-dispersible granules, suspensions, suspoemulsions, dispersible oil suspensions and microcapsule suspensions.

9. The herbicidal composition according to claim 8, characterized in that The herbicidal composition also contains common adjuvants required for preparing pesticide formulations, and the common adjuvants are one or more of solvents, wetting agents, stabilizers, dispersants, thickeners, pH regulators, defoamers, antifreeze agents and fillers.

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