Sealing and killing type herbicide composition and preparation method thereof

Abstract

The invention provides a sealed herbicide composition, which comprises 5-40% of active components, 0-20% of a dispersant, 0-20% of an emulsifier, 1-2% of a stabilizer, 0-2% of a viscosity modifier, 0-20% of a carrier and the balance of a dispersion medium, the active components comprise saflufenacil and pyroxasulfone, and the mass ratio of the saflufenacil to the pyroxasulfone is 1: (1-20). The herbicide composition provided by the invention is a compound combination of herbicides with different action mechanisms and has no cross resistance, so that the herbicidal characteristics of the herbicides with various components are well complementary in advantages, and the generation and progress of resistance of weeds to a single agent can be effectively delayed.

Description

Technical Field

[0001] The invention relates to a herbicide composition and a preparation method thereof, belonging to the technical field of pesticide preparations. Background Art

[0002] The chemical name of Saflufenacil is: N′-{2-chloro-4-fluoro-5-[1,2,3,6-tetrahydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)pyrimidin-1-yl]benzoyl}-N-isopropyl-N-methanesulfonamide, and the structural formula is:

[0003] Safensulfuron is a protoporphyrinogen oxidase (PPO) inhibitor. It prevents the conversion of protoporphyrinogen IV to protoporphyrin IV during chlorophyll biosynthesis, destroys chlorophyll synthesis, causes chloroplast pigment bleaching, tissue necrosis, and ultimately inhibits growth until plant death. Safensulfuron can be used for more than 30 crops such as soybeans, corn, cereals, sugarcane, fruits and vegetables, rice, cotton, sorghum, etc., and controls more than 90 broadleaf weeds such as velvetleaf, purslane, field bindweed, ragweed, Xanthium sibiricum, Solanum nigrum, etc.

[0004] The chemical name of pyroxasulfone is: 3-(((5-(difluoromethoxy)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-4-yl)methyl)sulfonyl)-5,5-dimethyl-4,5-dihydroisoxazole. Pyroxasulfone belongs to the class of very-long-chain fatty acid elongase inhibitor herbicides. It inhibits the biosynthesis of very-long-chain fatty acid elongase (VLCFAE) and causes the construction of fatty acid precursors, which can inhibit the early growth of seedlings, destroy meristems and coleoptiles, and exert its efficacy. It is a new, broad-spectrum, highly active, low-dosage and safe pre-emergence soil treatment herbicide. It can be safely used on a variety of major crops such as soybeans, corn, cotton, peanuts, wheat, sunflowers, potatoes, etc., and can effectively control grass weeds such as Setaria, Crabgrass, and Echinochloa. Summary of the invention

[0005] The object of the present invention is to provide a herbicide composition having a broad weed control spectrum and significant weed control effect and its application.

[0006] The inventor of the present invention has rich experience in formulation development and strong product registration skills, and uses saflufenacil and pyraclostrobin, which have different structural types and mechanisms of action, in combination. Saflufenacil is a post-emergence broad-spectrum herbicide, and pyraclostrobin is a pre-emergence blocking herbicide. The combination of the two not only has no cross-resistance, but also has a synergistic effect, and can also expand the use of pyraclostrobin. One-time use of the drug can solve the problem of drug use throughout the life cycle, achieving the effect of reducing dosage and increasing efficiency, and is also highly safe for crops.

[0007] The first object of the present invention is to provide a herbicide composition, wherein the active ingredients of the herbicide composition contain saflufenacil and pyraclostrobin.

[0008] The second object of the present invention is to provide the use of the above-mentioned herbicide composition in controlling annual and perennial grass weeds and broad-leaved weeds.

[0009] The third object of the present invention is to provide the use of the above-mentioned herbicide composition in controlling crop weeds throughout their life cycle.

[0010] The fourth object of the present invention is to provide the above-mentioned herbicide composition to reduce the amount of pesticides and increase their efficiency, thereby providing farmers with a new weed control solution.

[0011] Specifically, the herbicide composition provided by the present invention has the following advantages: The herbicide composition provided by the present invention exhibits an excellent synergistic effect. The mixed composition significantly improves the weed control effect compared with its single agent and double agent, reduces the dosage of pesticides used, and thus reduces the pesticide cost for farmers and the impact on the environment.

[0012] The herbicide composition provided by the present invention expands the weed control spectrum of the herbicide. The herbicide composition provided by the present invention can control multiple weeds at the same time, is convenient and efficient to use, and has a good control effect on annual and perennial grass weeds and broad-leaved weeds.

[0013] The herbicide composition provided by the present invention is a compound combination of herbicides with different action mechanisms without cross-resistance, so that the herbicides of each component have good complementary advantages and can effectively delay the generation and development of weed resistance to a single agent.

[0014] Other features and advantages of the present invention will be described in detail in the following detailed description. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is the laser particle size distribution instrument diagram of the finished product of Example 3.

[0016] Figure 2 This is the SEM image of the finished product of Example 3. DETAILED DESCRIPTION

[0017] The specific embodiments of the present invention are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0018] The active ingredients of the herbicide composition provided by the invention contain saflufenacil and pyraclostrobin.

[0019] In the present invention, the active ingredient is 5-40%, the dispersant is 0-20%, the emulsifier is 0-20%, the stabilizer is 1-2%, the viscosity modifier is 0-2%, the carrier is 0-20% and the dispersion medium is supplemented to 100%, wherein the active ingredient contains saflufenacil and pyraclostrobin, and the mass ratio of pyraclostrobin to saflufenacil is 1:1-20.

[0020] The present invention preferably uses one or more of an emulsifier, a dispersant, a stabilizer, a dispersion medium, a viscosity modifier and.

[0021] The emulsifier can be any emulsifier known in the field of pesticide formulations. Specifically, the emulsifier is selected from one or more of pine base oil and hydrogenated lecithin.

[0022] The above-mentioned dispersant can be various dispersants known in the field of pesticide formulations. Specifically, the dispersant is selected from one or more of calcium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene polyoxypropylene ether, fatty amine, fatty acid polyoxyethylene ester, sodium dodecyl sulfate, secondary alkyl sodium sulfate, sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, alkylnaphthalene sulfonate, alkylphenol polyoxyethylene ether sulfate, alkylnaphthalene sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, phenethylphenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, fatty amine salt, ethanol ammonium salt, glycerol fatty acid ester polyoxyethylene ether, and polycarboxylate.

[0023] The stabilizer may be any stabilizer known in the field of pesticide formulations. Specifically, the stabilizer may be an organic acid (citric acid), an organic base, an ester, an antioxidant, epoxidized soybean oil, a surfactant, and the like.

[0024] In a preferred embodiment, the stabilizer is selected from one or more of WD01, citric acid, urea, and epoxidized soybean oil.

[0025] The WDO1 is a mixture of polycarboxylate + sulfate + EO-PO block polyether in a mass ratio of 3:2:1, wherein the polycarboxylate is GY-D800 (a polycarboxylate product of Beijing Guangyuan Yinong Chemical Co., Ltd.); and the sulfate is magnesium sulfate.

[0026] The viscosity regulator is selected from organic bentonite and white carbon black.

[0027] The carrier is selected from attapulgite and diatomaceous earth.

[0028] The above-mentioned dispersion medium can be various dispersion media known in the field of pesticide formulations. Specifically, the dispersion medium can be vegetable oils (soybean oil, corn oil, rapeseed oil, etc.), mineral oils (white oil, mineral oil, higher fatty hydrocarbon oil, etc.) and chemical synthetic oils (methyl oleate, fatty acid methyl ester, etc.). The above-mentioned viscosity modifier can be various viscosity modifiers known in the field of pesticide formulations. Specifically, the dispersion medium viscosity modifier is mainly used to obtain a long-term stable suspension system and prolong the suspension time of solids in liquids. The main principle is the Stockes formula (V=2r²(ρ1-ρ2)g / 9η), that is, the sedimentation rate is inversely proportional to the viscosity of the system. The higher the viscosity of the system, the slower the sedimentation rate. However, if it exceeds a certain threshold, it will increase the difficulty of production and packaging, and it is easier to agglomerate and precipitate. The viscosity of this formula product is controlled to be 400-500mPa·s (20℃). Commonly used thickeners are generally organic bentonite, white carbon black, etc.

[0029] According to the present invention, the herbicide composition may be in any of the commonly used formulations in the art, for example, the herbicide composition may be in the form of an oil suspension, a wettable powder, a water dispersible granule, etc. Preferably, the herbicide composition is in the form of an oil suspension.

[0030] The present invention provides a method for preparing a dispersible oil suspension, which adopts a solid-solid-liquid method to replace the traditional solid-liquid one-pot method, which is beneficial to improving the solubility of benzylpyraclostrobin and pyraclostrobin, avoiding agglomeration, and improving the stability and suspension rate of the product. The method specifically includes the following steps: 1) adding attapulgite and benzylpyraclostrobin and auxiliary agents with ultra-high surface, high adsorption capacity, easy suspension, good affinity and chemical stability to a high-efficiency mixer in a certain proportion and fully mixing for 2-6 hours to obtain a stable semi-finished product; 2) then sending the semi-finished product to a rotary crusher through an air conveying system, and then transporting it to a powder sand mill through a tubular hinge, and the particle size is controlled by D 90 10-30μm, to obtain a micron-sized semi-finished product; 3) add the semi-finished product and an appropriate amount of methyl oleate into the preparation kettle 1, start the stirring and high-speed shearing device, and stir and shear for 1-3h; 4) add methyl oleate, sulfone pyraclostrobin, additives, dispersants, stabilizers, wetting agents, etc. into the preparation kettle 2, stir and shear for 1-3h to make a homogeneous suspension; 5) respectively pass step 4) and step 5) through the first-level grinder into the mixing kettle, stir and shear for 1-3h, and then go through the second-level grinding (multi-level grinding is required according to needs) to control the granule D 90 1-100μm. After testing by high performance liquid chromatography, particle size analyzer, electron microscope, etc., all indicators meet the industry standards.

[0031] The addition ratio of saflufenacil technical and carrier attapulgite is controlled at 15-25:1. Too much attapulgite will affect the fluidity of the product, while too little will affect the final compatibility with pyraclostrobin. At the same time, the particle size D90 is controlled at 100-300μm. Too large a particle size will affect the subsequent shearing effect.

[0032] The present invention also provides the use of the herbicide composition in preventing and controlling annual and perennial grass weeds and broadleaf weeds. The weeds may be barnyard grass, horsetail grass, foxtail grass, velvetleaf, purslane and field bindweed.

[0033] According to the present invention, the specific application method of the herbicide composition is generally to apply the herbicide composition of the present invention to crops and places where crops grow in a conventional manner before or after weeds germinate. The application method can be, for example, soil sealing, stem and leaf spraying, etc., and the application method is simple.

[0034] The herbicide composition of the present invention is preferably used for soil sealing treatment after sowing and before seedlings emerge, and can simultaneously prevent and kill both emerged and unemerged weeds. The application amount of the herbicide composition provided by the present invention depends on weather conditions or crop status, and is usually applied at a concentration of 3-40 g / mu of active ingredient content. The application amount of the herbicide composition provided by the present invention is also related to external factors such as climate.

[0035] The present invention is further described below by means of specific examples, but the present invention is not limited to the following examples.

[0036] Example 1 The components were fully mixed according to the following formula to obtain an oil suspension concentrate A1, wherein the mass ratios of sulfamethoxazole and saflufenacil as active ingredients were as follows. In addition, the active ingredient ratios are also shown in the following Table 3.

[0037]

[0038] In the stabilizer, the mass ratio of WDO1+citric acid+urea is 2:1:1.

[0039] Example 2 The components were fully mixed according to the following formula to obtain an oil suspension A2, wherein the mass ratios of sulfamethoxazole and saflufenacil as active ingredients were as follows. In addition, the active ingredient ratios were also shown in the following Table 4.

[0040]

[0041] In the stabilizer, the mass ratio of WDO1+citric acid+urea is 2:1:1.

[0042] Example 3 The components were fully mixed according to the following formula to obtain an oil suspension concentrate A1, wherein the mass ratios of sulfamethoxazole and saflufenacil as active ingredients were as follows. In addition, the active ingredient ratios were also shown in the following Table 5.

[0043]

[0044] In the stabilizer, the mass ratio of WDO1+citric acid+urea is 2:1:1.

[0045] Taking Example 3 as an example, the composition of other raw materials is the same as that of this example, and the stabilizer formula (WDO1+citric acid+urea) is screened. The screening of stabilizers is the core of the research on dispersible oil suspension preparations. Stabilizers are usually divided into structural stabilizers, pH acid-base regulators, anti-base agents, etc., and the composition of the present invention is a compound preparation. Due to the particularity of the original drug, it has different physical and chemical properties and has great differences in stability in the system. Therefore, it is necessary to select suitable stabilizers for different original drugs so that the formula preparation can control the decomposition rate within 5% after thermal storage (60°C, thermal storage in an environment with a humidity of 30%). The specific screening results are shown in Table 6 below.

[0046] Table 1 Stabilizer formula screening

[0047] In the formulation of Example 3, the test data of the dispersible oil suspension formulation is as follows:

[0048] The formulated product was tested by liquid chromatography (HPLC), and the content of saflufenacil was 19.97%, and the content of sulfamethoxazole was 3.74%, which met the product standards. The particle size of the finished product was 0-100μm, D10=0.998, D50=13.99, and D90=53.89, as tested by laser particle size distribution instrument (GSL). The surface of the suspended particles was full, evenly dispersed, and non-aggregated as observed by scanning electron microscope (SEM).

[0049] Bio-test Drugs used: The above-mentioned preparation examples 1-3 can be dispersed in oil suspensions and single doses of each active ingredient.

[0050] Application method: The application method is to spray the stems and leaves during the weed-prone period.

[0051] Basic information of the test: The test was conducted in the company's own outdoor efficacy test base, which has 17 plots covering a total area of ​​1,500 square meters, which can be used for efficacy tests of both lethal and selective herbicides. There are grass and broad-leaved weeds in the field, which meet the conditions for applying pesticides.

[0052] Test targets: Echinochloa crusgalli, horsetail, Setaria viridis, Ramulus flavonoides, Purslane, and Bindweed.

[0053] Investigation method: The fresh weight of weeds was investigated 30 days after application and the control effect was calculated. The results are shown in Table 5.

[0054] Calculation formula: weed fresh weight control effect (%) = (weed fresh weight in the control area - weed fresh weight in the treatment area) / weed fresh weight in the control area × 100%.

[0055] Table 6: Weed fresh weight control effect

[0056] As can be seen from the above table, the herbicide composition provided by the present invention has good control effects on barnyard grass, horsetail, foxtail grass, velvetleaf, purslane, and field bindweed at a dosage of 20-40 g / mu. Among them, A3 has outstanding control effect and is better than the control effect of its single preparation, which conforms to the principle of product compounding. At the same time, the dosage is less than that of the single preparation under the same control effect, which conforms to the purpose of reducing dosage and increasing efficiency. Therefore, the formula combination has the necessity and economy of compounding and has great market prospects.

[0057] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0058] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0059] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A blocking herbicide composition, characterized in that: The active ingredient is 5-40%, the dispersant is 0-20%, the emulsifier is 0-20%, the stabilizer is 1-2%, the viscosity modifier is 0-2%, the carrier is 0-20% and the dispersion medium is supplemented to 100%, wherein the active ingredient contains saflufenacil and pyraclostrobin, and the mass ratio of pyraclostrobin to saflufenacil is 1:1-20.

2. The herbicide-blocking composition according to claim 1, characterized in that: The dispersant is selected from one or more of calcium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene polyoxypropylene ether, fatty amine, fatty acid polyoxyethylene ester, sodium dodecyl sulfate, secondary alkyl sodium sulfate, sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, alkylnaphthalene sulfonate, alkylphenol polyoxyethylene ether sulfate, alkylnaphthalene sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, phenethylphenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, fatty amine salt, ethanol ammonium salt, glycerol fatty acid ester polyoxyethylene ether, and polycarboxylate.

3. The herbicide-blocking composition according to claim 1, characterized in that: The emulsifier is selected from one or more of pine base oil and hydrogenated lecithin.

4. The herbicide-blocking composition according to claim 1, characterized in that: The stabilizer is selected from one or more of WD01, citric acid, urea, and epoxidized soybean oil.

5. The herbicide-blocking composition according to claim 1, characterized in that: The viscosity regulator is selected from bentonite and white carbon black.

6. The herbicide-blocking composition according to claim 1, characterized in that: The carrier is selected from attapulgite and diatomaceous earth.

7. The herbicide-blocking composition according to claim 1, characterized in that: The dispersion medium is selected from vegetable oils, mineral oils, or chemical synthetic oils; Among them, the vegetable oil is selected from soybean oil, corn oil, or rapeseed oil; the mineral oil is selected from white oil, mineral oil, or higher fatty hydrocarbon oil; the chemical synthetic oil is selected from methyl oleate or fatty acid methyl ester.

8. The method for preparing the block-type herbicide composition according to any one of claims 1 to 7, characterized in that: The steps include: (1) Add the carrier, saflufenacil and dispersant in a certain proportion into a high-efficiency mixer and mix them thoroughly for 2-6 hours to obtain a stable semi-finished product; (2) The semi-finished product is then sent to the rotary crusher through the air conveying system and then transported to the powder sand mill through the tubular hinge. The particle size is controlled by D 90 At 10-30μm, we get micron-sized semi-finished products; (3) Add the semi-finished product and an appropriate amount of stabilizer into the preparation kettle 1, turn on the stirring and high-speed shearing device, and stir and shear for 1-3 hours; (4) Add appropriate amounts of sulfonepyraclostrobin, emulsifier, viscosity regulator and dispersion medium into the preparation kettle 2, stir and shear for 1-3 hours to prepare a homogeneous suspension; (5) The mixtures of step (4) and step (5) are respectively put into a mixing kettle through a first-level grinder, stirred and sheared for 1-3 hours, and then ground to control the granule D 90 In the micrometer range of 5-15μm.

9. Use of the block-type herbicide composition according to any one of claims 1 to 7 in controlling annual and perennial grass weeds and broadleaf weeds.

10. Use of the block-type herbicide composition according to any one of claims 1 to 7 in controlling crop weeds throughout their life cycle.

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