Pesticide suspending agent containing pyroxsulam-flufenacet-isoproturon and application thereof

Abstract

The invention relates to the technical field of pesticides, in particular to a pesticide suspending agent containing pyroxsulam, flufenacet and isoproturon and application thereof.The pesticide suspending agent is prepared from, by mass, 7-10 parts of pyroxsulam, 4.4-7 parts of flufenacet, 4.6-8 parts of isoproturon, 5-13 parts of a weeding compound, 0.7-1.3 parts of a synergist, 10-15 parts of an organosilicon surfactant and 5.8-7.4 parts of a wetting dispersant. The coating is prepared from the following components in parts by weight: 0.3-0.8 part of a thickening agent, 0.4-0.7 part of an anti-freezing agent, 0.5-2 parts of a de-foaming agent, 0.5-1 part of a preservative and 30-40 parts of de-ionized water. On one hand, the hydrophobicity of the herbicide compound is enhanced through modification, on the other hand, the herbicide compound has a certain slow release performance through embedding of the biomass material and the polymer, and then the herbicide compound and the synergist have a synergistic effect, desorption and leaching are reduced, the utilization rate is increased, the action time is prolonged, and the herbicide compound has a wide application prospect.

Description

Technical Field

[0001] The invention relates to the technical field of pesticides, and in particular to a pesticide suspension containing formosulam-flufenacil-isoproturon and application thereof. Background Art

[0002] my country's annual wheat planting area is 350 million mu, second only to rice. In recent years, wheat field weeds have been seriously infested. The dominant weeds are mainly brome, knotweed, foxtail, Japanese foxtail, wild oats, bluegrass, shepherd's purse, sophora japonica, and cleaver. Weeds compete with wheat for growth nutrients and living space. Some weeds are also the transmission medium or overwintering carrier of wheat diseases and insect pests, which is one of the important factors affecting wheat yield and quality.

[0003] Wheat field weeds directly affect the yield of wheat crops and are a key factor restricting crop yields. Controlling wheat field weeds is an important task in developing wheat production. The use of chemical herbicides is one of the important signs of modern agriculture. Herbicides refer to agents that can kill weeds completely or selectively, also known as herbicides, a class of substances used to eliminate or inhibit plant growth.

[0004] At present, there are many varieties of herbicides available for the control of weeds in wheat fields. For example, sulfamethoxam is a sulfonamide systemic conduction type selective post-emergence herbicide for wheat fields. It is mainly absorbed through leaves, stems and roots, and translocated in the plant meristem, resulting in developmental retardation and chlorosis, necrosis and death. It is mainly used for the control of annual grass weeds and some broad-leaved weeds in wheat fields; isoproturon is a substituted urea herbicide, which is mainly absorbed by roots, stems and leaves to inhibit photosynthetic electron transfer. It is a selective pre-emergence and post-emergence herbicide and also has a selective systemic effect. Its application at the seedling stage will reduce the cold resistance of wheat crops. It is safer to apply the pesticide to wheat fields that have been tempered at low temperatures below 0°C before wintering and have enhanced cold resistance; flufenacet is an oxyacetanilide herbicide, which works mainly by inhibiting cell division and growth. It has the characteristics of high herbicidal activity, a wide spectrum of weed control, a wide range of applicable crops, and high safety. It has a good control effect on perennial grass weeds.

[0005] However, the use of single herbicides has made many weeds resistant to them and has had a negative impact on the environment. For example, pesticide residues and chemical herbicides are passed down the food chain and accumulate continuously, eventually accumulating in animals and humans at the top of the food chain, causing harm to humans and animals. Therefore, if herbicides are to develop sustainably, they must be coordinated with environmental protection.

[0006] At present, compounding of two or three herbicides and synergistic combination of herbicides and adjuvants are relatively common means of increasing the efficiency and reducing the dosage of herbicides. For example, patent technical document CN107751209A discloses a wheat herbicide composition with pyrimidine oxime, isoproturon and flufenacet as main active ingredients, the mass ratio of pyrimidine oxime, isoproturon and flufenacet is 5-40:0.1-10:3-45, and the sum of the three in the herbicide composition is 10%-80% by mass. The herbicide composition of the invention has the advantages of a wide spectrum of weed control and good efficacy, but isoproturon and flufenacet are both water-soluble and are easily lost in the soil when sprayed on the roots of weeds. The herbicide utilization rate is poor and cannot exert its effect for a long time.

[0007] Therefore, according to the above-mentioned related technologies, there is an urgent need to develop a pesticide suspension containing foramsulfuron-flufenacet-isoproturon and its application. Summary of the invention

[0008] In view of this, the object of the present invention is to provide a pesticide suspension containing formosulam-flufenacil-isoproturon and its application, so as to solve the problems of low herbicide utilization rate and short duration of herbicidal effect in the prior art.

[0009] Based on the above purpose, the present invention provides a pesticide suspension containing formosulam-flufenacil-isoproturon and application thereof.

[0010] A pesticide suspension containing formosulam-flufenacil-isoproturon is prepared from the following raw materials in parts by weight: 7-10 parts of formosulam, 4.4-7 parts of flufenacet, 4.6-8 parts of isoproturon, 5-13 parts of herbicide compound, 0.7-1.3 parts of synergist, 10-15 parts of silicone surfactant, 5.8-7.4 parts of wetting and dispersing agent, 0.3-0.8 parts of thickener, 0.4-0.7 parts of antifreeze agent, 0.5-2 parts of defoamer, 0.5-1 parts of preservative, 30-40 parts of deionized water; The herbicidal compound is obtained by mixing modified isoproturon and a microsphere composition; The mass ratio of the modified isoproturon to the microsphere composition is 9-15:22-27; The modified isoproturon is prepared from isoproturon and octadecyl acrylate; The microsphere composition is prepared from formosansulfuron, flufenacet, chitosan and pyrrole.

[0011] Preferably, the preparation method of the modified isoproturon is as follows: Isoproturon was placed in a centrifuge tube, N,N-dimethylformamide was added and ultrasonically mixed evenly, after standing at room temperature for 2 hours, octadecyl acrylate, 1-ethyl-3-methylimidazolium chloride and azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker. After heating for reaction, it was washed with methanol and deionized water in sequence, filtered and dried to obtain modified isoproturon.

[0012] Preferably, the usage ratio of isoproturon, N,N-dimethylformamide, octadecyl acrylate, 1-ethyl-3-methylimidazolium chloride and azobisisobutyronitrile is 2-5 g: 43-49 mL: 3-6 g: 0.23-0.35 mg: 0.1-0.15 mg; The temperature during the heating reaction is 60-70°C and the reaction time is 14-16h; The temperature during the drying is 58-63°C.

[0013] Preferably, the preparation method of the synergist is as follows: Grind the wheat straw and air dry it, pass it through a 2 mm sieve, add ultrapure water to the wheat straw, shake it at 180-210 r / min for 15-17 hours at 18-22°C, then centrifuge it at 5500-6000g for 15-18 minutes at 4-6°C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; The mass ratio of the wheat straw to ultrapure water is 1:4-6.

[0014] Preferably, the preparation method of the microsphere composition is as follows: Step A1. Add calcium chloride and ammonium persulfate to deionized water and stir to obtain a mixture A; Step A2. Add foramsulfuron and flufenacet to deionized water and stir evenly, then add chitosan, sodium alginate and pyrrole and stir evenly. After removing bubbles, add them dropwise into mixture A with a 5 mm syringe. After stirring at room temperature for 2-2.5 h, wash with deionized water 3 times to obtain a microsphere composition.

[0015] Preferably, the mass ratio of deionized water, calcium chloride and ammonium persulfate in step A1 is 8-10:0.25-0.3:0.1-0.15.

[0016] Preferably, the usage ratio of formosulam, flufenacet, deionized water, chitosan, sodium alginate, pyrrole and mixture A in step A2 is 4-7 g: 3-5 g: 10-15 mL: 0.2-0.3 g: 0.2-0.3 g: 0.56-0.7 mmol: 8-10 mL.

[0017] Preferably, the organosilicon surfactant is at least one of SilwetL77 and Silwet408; The wetting and dispersing agent is at least one of Morwet D-450 and Terwet 1004; The antifreeze agent is at least one of ethylene glycol and glycerol; The preservative is at least one of sodium benzoate and potassium sorbate; The thickener is at least one of xanthan gum and magnesium aluminum silicate; The defoaming agent is polydimethylsiloxane.

[0018] Preferably, the preparation method of the pesticide suspension is as follows: Step S1. The microsphere composition and modified isoproturon are mixed evenly to obtain a herbicide compound, and then deionized water, a wetting dispersant, a defoamer, an antifreeze agent and a synergist are mixed evenly, and then foramsulfuron, flufenacet and the herbicide compound are added, and the mixture is sheared for the first time, and then poured into a sand mill containing zirconium beads and sanded for 1.5-2.0 hours. After the particle size is sanded to less than 0.5 μm, the liquid medicine is filtered out to obtain a mixture B; Step S2. After isoproturon and the silicone surfactant are uniformly mixed, mixture B is added, and a second shearing is performed. After a thickener and a preservative are added, a third shearing is performed to obtain a pesticide suspension containing formosulfuron-flufenacet-isoproturon; The speed of the first shearing in step S1 is 3000-5000 r / min, and the time is 8-12 min; The speed of the second shearing in step S2 is 2500-3500 r / min, and the time is 10-13 min; The speed of the third shearing in step S2 is 3200-4000 r / min, and the time is 7-12 min.

[0019] Preferably, the pesticide suspension containing formosulam-flufenacil-isoproturon is used to remove annual weeds in winter wheat fields.

[0020] Beneficial effects of the present invention: The present invention provides a pesticide suspension containing foramsulfuron-flufenacet-isoproturon and an application thereof. The present invention uses three herbicides, foramsulfuron, flufenacet and isoproturon, in combination, and then adds other additives such as a herbicide complex and a synergist to obtain a winter wheat herbicide with high utilization rate and long-term effect. Among them, the herbicide complex is obtained by mixing modified isoproturon and a microsphere composition. On the one hand, the hydrophobicity of the complex is enhanced by modification, and on the other hand, it has a certain sustained release performance through biomass material and polymer encapsulation. It is synergistically enhanced with a synergist to improve the soil's adsorption of the active ingredients of the herbicide, reduce desorption and leaching, and increase the utilization rate and action time. Compared with the existing technology, it has broad application prospects. DETAILED DESCRIPTION

[0021] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0022] The sources and properties of some of the raw materials used in the present invention are as follows: 1-Ethyl-3-methylimidazole chloride was purchased from Shanghai Sane Chemical Technology Co., Ltd.; isoproturon was purchased from Jiangsu Kuaida Agrochemical Co., Ltd.; octadecyl acrylate was purchased from Shanghai Xige Biotechnology Co., Ltd.; azobisisobutyronitrile was purchased from Shandong Jinyueyuan New Materials Co., Ltd.; N,N-dimethylformamide was purchased from Shandong Qiangsen Chemical Co., Ltd.; flufenacet was purchased from Henan Jinxiuzhixing Crop Protection Co., Ltd.; foramsulfuron was purchased from Corteva, USA; chitosan was purchased from Zhengzhou Yuhe Food Additive Co., Ltd.; sodium alginate was purchased from Zhongshan Dixin Chemical Co., Ltd.; pyrrole was purchased from Shanghai Chuangsai Technology Co., Ltd.; Morwet D-450 was purchased from Akzo Nobel; Terwet 1004 was purchased from Huntsman; Silwet L77 was purchased from Beijing Solebold Technology Co., Ltd.; Silwet 408 was purchased from Nonon (Beijing) International Biotechnology Co., Ltd.

[0023] Example 1: A method for preparing a pesticide suspension containing formosulam-flufenacil-isoproturon, comprising the following steps: S1. 2 g of isoproturon was placed in a centrifuge tube, 43 mL of N,N-dimethylformamide was added and ultrasonically mixed, and after standing at room temperature for 2 h, 3 g of octadecyl acrylate, 0.23 mg of 1-ethyl-3-methylimidazolium chloride and 0.1 mg of azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker, heated at 60 ° C for 16 h, and then washed with methanol and deionized water in sequence, filtered, and dried at 58 ° C to obtain modified isoproturon; S2. Grind the wheat straw and air-dry it, pass it through a 2 mm sieve, add 4 g of ultrapure water to 1 g of wheat straw, shake it at 180 r / min for 15 h at 18 ° C, then centrifuge it at 5500 g for 15 min at 4 ° C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; S3. Add 0.25 g of calcium chloride and 0.1 g of ammonium persulfate to 8 g of deionized water and stir to obtain a mixture A; S4. 4 g of formosulfuron and 3 g of flufenacet were added to 10 mL of deionized water, stirred evenly, and then 0.2 g of chitosan, 0.2 g of sodium alginate and 0.56 mmol of pyrrole were added, stirred evenly, and after removing bubbles, the mixture was added dropwise to 8 mL of mixture A using a 5 mm syringe. After stirring at room temperature for 2 h, the mixture was washed three times with deionized water to obtain a microsphere composition; S5. 22 g of the microsphere composition and 9 g of modified isoproturon were mixed to obtain a herbicidal compound, and 30 g of deionized water, 5.8 g of Morwet D-450, 0.5 g of polydimethylsiloxane, 0.4 g of ethylene glycol and 0.7 g of a synergist were mixed to obtain a herbicidal compound, and 7 g of foramsulfuron, 4.4 g of flufenacet and 13 g of the herbicidal compound were added, and the mixture was sheared for the first time at a speed of 3000 r / min for 8 min, and then poured into a sand mill containing zirconium beads and sanded for 1.5 h. After the particle size was sanded to less than 0.5 μm, the drug solution was filtered out to obtain a mixture B; S6. After 4.6 g of isoproturon and 10 g of Silwet L77 are evenly mixed, the mixture B is added, and a second shearing is performed at a speed of 2500 r / min for 10 min. After adding 0.3 g of xanthan gum and 0.5 g of sodium benzoate, a third shearing is performed at a speed of 3200 r / min for 7 min to obtain a pesticide suspension containing foramsulfuron-flufenacil-isoproturon.

[0024] Example 2: A method for preparing a pesticide suspension containing formosulam-flufenacil-isoproturon, comprising the following steps: S1. 3 g of isoproturon was placed in a centrifuge tube, 45 mL of N,N-dimethylformamide was added and ultrasonically mixed, and after standing at room temperature for 2 h, 4 g of octadecyl acrylate, 0.25 mg of 1-ethyl-3-methylimidazolium chloride and 0.12 mg of azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker, heated at 62 ° C for 15.5 h, and then washed with methanol and deionized water in sequence, filtered, and dried at 60 ° C to obtain modified isoproturon; S2. Grind the wheat straw and air-dry it, pass it through a 2 mm sieve, add 5 g of ultrapure water to 1 g of wheat straw, shake it at 190 r / min for 16 h at 20 ° C, then centrifuge it at 5500 g for 16 min at 4 ° C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; S3. Add 0.25 g of calcium chloride and 0.12 g of ammonium persulfate to 8.5 g of deionized water and stir to obtain a mixture A; S4. 5 g of foramsulfuron and 4 g of flufenacet were added to 12 mL of deionized water and stirred evenly, and then 0.2 g of chitosan, 0.22 g of sodium alginate and 0.6 mmol of pyrrole were added and stirred evenly. After removing bubbles, the mixture was added dropwise to 9 mL of mixture A using a 5 mm syringe. After stirring at room temperature for 2 h, the mixture was washed three times with deionized water to obtain a microsphere composition; S5. 24 g of the microsphere composition and 10 g of modified isoproturon were mixed to obtain a herbicidal compound, and then 32 g of deionized water, 6.2 g of Morwet D-450, 0.8 g of polydimethylsiloxane, 0.5 g of ethylene glycol and 0.8 g of a synergist were mixed to obtain a herbicidal compound, and then 8 g of foramsulfuron, 5 g of flufenacet and 11 g of the herbicidal compound were added, and the mixture was sheared for the first time at a speed of 3500 r / min for 9 min, and then poured into a sand mill containing zirconium beads and sanded for 2 h. After the particle size was sanded to less than 0.5 μm, the drug solution was filtered out to obtain a mixture B; S6. After 5.2 g of isoproturon and 12 g of Silwet L77 are uniformly mixed, mixture B is added, and a second shearing is performed at a speed of 3000 r / min for 11 min. After adding 0.4 g of xanthan gum and 0.7 g of sodium benzoate, a third shearing is performed at a speed of 3400 r / min for 9 min to obtain a pesticide suspension containing foramsulfuron-flufenacil-isoproturon.

[0025] Example 3: A method for preparing a pesticide suspension containing formosulam-flufenacil-isoproturon, comprising the following steps: S1. 4 g of isoproturon was placed in a centrifuge tube, 47 mL of N,N-dimethylformamide was added and ultrasonically mixed, and after standing at room temperature for 2 h, 5 g of octadecyl acrylate, 0.28 mg of 1-ethyl-3-methylimidazolium chloride and 0.13 mg of azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker, heated at 64 ° C for 15 h, and then washed with methanol and deionized water in sequence, filtered, and dried at 62 ° C to obtain modified isoproturon; S2. Grind the wheat straw and air-dry it, pass it through a 2 mm sieve, add 5 g of ultrapure water to 1 g of wheat straw, shake it at 200 r / min for 16.5 h at 20 ° C, then centrifuge it at 5600 g for 17 min at 5 ° C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; S3. Add 0.27 g of calcium chloride and 0.13 g of ammonium persulfate to 9 g of deionized water and stir to obtain a mixture A; S4. 6 g of formosulfuron and 4 g of flufenacet were added to 13 mL of deionized water and stirred evenly, and then 0.25 g of chitosan, 0.25 g of sodium alginate and 0.63 mmol of pyrrole were added and stirred evenly. After removing bubbles, the mixture was added dropwise to 9 mL of mixture A using a 5 mm syringe. After stirring at room temperature for 2 h, the mixture was washed three times with deionized water to obtain a microsphere composition; S5. 25 g of the microsphere composition and 12 g of modified isoproturon were mixed to obtain a herbicidal compound, and 35 g of deionized water, 6.5 g of Morwet D-450, 1.3 g of polydimethylsiloxane, 0.6 g of ethylene glycol and 1.0 g of a synergist were mixed to obtain a herbicidal compound, and then 9 g of foramsulfuron, 5.7 g of flufenacet and 9 g of the herbicidal compound were added, and the mixture was sheared for the first time at a speed of 4000 r / min for 10 min, and then poured into a sand mill containing zirconium beads and sanded for 1.5 h. After the particle size was sanded to less than 0.5 μm, the drug solution was filtered out to obtain a mixture B; S6. After 6 g of isoproturon and 13 g of Silwet L77 are evenly mixed, mixture B is added, and a second shearing is performed at a speed of 3200 r / min for 12 min. After adding 0.6 g of xanthan gum and 0.8 g of sodium benzoate, a third shearing is performed at a speed of 3500 r / min for 10 min to obtain a pesticide suspension containing foramsulfuron-flufenacil-isoproturon.

[0026] Example 4: A method for preparing a pesticide suspension containing formosulam-flufenacil-isoproturon, comprising the following steps: S1. 5 g of isoproturon was placed in a centrifuge tube, 48 mL of N,N-dimethylformamide was added and ultrasonically mixed, and after standing at room temperature for 2 h, 5.5 g of octadecyl acrylate, 0.31 mg of 1-ethyl-3-methylimidazolium chloride and 0.14 mg of azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker, heated at 67 ° C for 14.5 h, and then washed with methanol and deionized water in sequence, filtered, and dried at 63 ° C to obtain modified isoproturon; S2. Grind the wheat straw and air-dry it, pass it through a 2 mm sieve, add 5 g of ultrapure water to 1 g of wheat straw, shake it at 210 r / min for 17 h at 22 ° C, then centrifuge it at 5800 g for 18 min at 5 ° C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; S3. Add 0.28 g of calcium chloride and 0.13 g of ammonium persulfate to 9.5 g of deionized water and stir to obtain a mixture A; S4. 6 g of formosulfuron and 4 g of flufenacet were added to 14 mL of deionized water, stirred evenly, and then 0.28 g of chitosan, 0.28 g of sodium alginate and 0.66 mmol of pyrrole were added, stirred evenly, and after removing bubbles, the mixture was added dropwise to 9 mL of mixture A with a 5 mm syringe. After stirring at room temperature for 2.5 h, the mixture was washed three times with deionized water to obtain a microsphere composition; S5. 26 g of the microsphere composition and 14 g of modified isoproturon were mixed to obtain a herbicidal compound, and 38 g of deionized water, 7 g of Morwet D-450, 1.7 g of polydimethylsiloxane, 0.7 g of ethylene glycol and 1.1 g of a synergist were mixed to obtain a herbicidal compound, and 10 g of foramsulfuron, 6 g of flufenacet and 7 g of the herbicidal compound were added, and the mixture was sheared for the first time at a speed of 4500 r / min for 11 min, and then poured into a sand mill containing zirconium beads and sanded for 2.0 h. After the particle size was sanded to less than 0.5 μm, the drug solution was filtered out to obtain a mixture B; S6. After 7 g of isoproturon and 15 g of Silwet L77 are evenly mixed, mixture B is added, and a second shearing is performed at a speed of 3500 r / min for 13 min. After adding 0.8 g of xanthan gum and 1 g of sodium benzoate, a third shearing is performed at a speed of 3900 r / min for 12 min to obtain a pesticide suspension containing foramsulfuron-flufenacil-isoproturon.

[0027] Example 5: A method for preparing a pesticide suspension containing formosulam-flufenacil-isoproturon, comprising the following steps: S1. 5 g of isoproturon was placed in a centrifuge tube, 49 mL of N,N-dimethylformamide was added and ultrasonically mixed, and after standing at room temperature for 2 h, 6 g of octadecyl acrylate, 0.35 mg of 1-ethyl-3-methylimidazolium chloride and 0.15 mg of azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker, heated at 70 ° C for 14 h, and then washed with methanol and deionized water in sequence, filtered, and dried at 63 ° C to obtain modified isoproturon; S2. Grind the wheat straw and air-dry it, pass it through a 2 mm sieve, add 6 g of ultrapure water to 1 g of wheat straw, shake it at 210 r / min for 17 h at 22 ° C, then centrifuge it at 6000 g for 18 min at 6 ° C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; S3. Add 0.3 g of calcium chloride and 0.15 g of ammonium persulfate to 10 g of deionized water and stir to obtain a mixture A; S4. 7 g of formosulfuron and 5 g of flufenacet were added to 15 mL of deionized water, stirred evenly, and then 0.3 g of chitosan, 0.3 g of sodium alginate and 0.7 mmol of pyrrole were added, stirred evenly, and after removing bubbles, the mixture was added dropwise to 10 mL of mixture A with a 5 mm syringe. After stirring at room temperature for 2.5 h, the mixture was washed three times with deionized water to obtain a microsphere composition; S5. 27 g of the microsphere composition and 15 g of modified isoproturon were mixed to obtain a herbicidal compound, and 40 g of deionized water, 7.4 g of Morwet D-450, 2 g of polydimethylsiloxane, 0.7 g of ethylene glycol and 1.3 g of a synergist were mixed to obtain a herbicidal compound, and then 10 g of foramsulfuron, 7 g of flufenacet and 5 g of the herbicidal compound were added, and the mixture was sheared for the first time at a speed of 5000 r / min for 12 min, and then poured into a sand mill containing zirconium beads and sanded for 2.0 h. After the particle size was sanded to less than 0.5 μm, the drug solution was filtered out to obtain a mixture B; S6. After 8 g of isoproturon and 15 g of Silwet L77 are evenly mixed, the mixture B is added, and a second shearing is performed at a speed of 3500 r / min for 13 min. After adding 0.8 g of xanthan gum and 1 g of sodium benzoate, a third shearing is performed at a speed of 4000 r / min for 12 min to obtain a pesticide suspension containing foramsulfuron-flufenacil-isoproturon.

[0028] Comparative Example 1: Compared with Example 1, the herbicidal compound was not added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacet-isoproturon was obtained.

[0029] Comparative Example 2: Compared with Example 1, modified isoproturon was not added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacet-isoproturon was obtained.

[0030] Comparative Example 3: Compared with Example 1, the microsphere composition was not added during the preparation process of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacet-isoproturon was obtained.

[0031] Comparative Example 4: Compared with Example 1, no synergist was added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacet-isoproturon was obtained.

[0032] Comparative Example 5: Compared with Example 1, pyrrole was not added during the preparation of the microsphere composition in this comparative example. The remaining steps and parameters were the same and will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacet-isoproturon was obtained.

[0033] Comparative Example 6: Compared with Example 1, this comparative example only replaces "22g of microsphere composition and 9g of modified isoproturon" with "22g of microsphere composition and 22g of modified isoproturon", and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, a pesticide suspension containing foramsulfuron-flufenacil-isoproturon is obtained.

[0034] Performance Test: Thermal storage stability: According to the determination method of GB / T19136-2003, the pesticide suspension containing foramsulfuron-flufenacet-isoproturon prepared in Examples 1 to 5 and Comparative Examples 1 to 6 was sealed in a thermostatic box at (54±2)°C for 14 days, then taken out and cooled to room temperature. The appearance, fluidity, dispersibility, active ingredient content, suspension rate and pourability and other technical indicators were analyzed, tested and recorded. If the indicators did not change significantly before and after hot storage, the hot storage stability was considered to be qualified; if the appearance and suspension rate did not change significantly before and after storage, the cold storage stability was considered to be qualified; Cold storage stability: According to the determination method of GB / T19137-2003, the pesticide suspension containing foramsulfuron-flufenacet-isoproturon prepared in Examples 1 to 5 and Comparative Examples 1 to 6 was placed in a refrigerator at (0±2)°C for 1 hour, and the appearance was observed for changes. Then, the suspension was further stored in a refrigerator at (0±2)°C for 7 days. If the appearance and suspension rate did not change significantly before and after storage, the cold storage stability was considered to be qualified. Suspension rate performance test: According to the GB / T14825-2006 test standard, weigh 5g of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon prepared in Examples 1-5 and Comparative Examples 1-6 respectively into a 200mL clean measuring cylinder, add standard hard water to the scale line, cover with a ground stopper, shake fully for 3min, open the stopper, place in a water bath and heat for 30min, and control the heating temperature to (30±2)℃. Use a pipette to suck out 9 / 10 of the liquid. Do not insert the pipette into the bottom of the measuring cylinder during this process, and ensure that the measuring cylinder is not shaken during the whole process. Transfer all the remaining contents in the measuring cylinder to a clean beaker for drying and weighing; Suspension rate calculation formula: Suspension rate (%) = ×100% Wherein, m is the weighed mass of the sample, g; w is the percentage of the active ingredient of the pesticide, %; m 1 —Mass of the beaker, g; m 2 —Total mass after drying, g.

[0035] Weed control effect: A winter wheat field with normal fertility and no other herbicides used before application was used. The pesticide suspension containing foramsulfuron-flufenacet-isoproturon prepared in Examples 1 to 5 and Comparative Examples 1 to 6 was divided into 11 groups to treat the winter wheat field. Each treatment was repeated 4 times, and the area of ​​each plot was 20 m 2 , randomized block arrangement, on a sunny day, directional spraying was used to spray the weeds on their stems and leaves once, and the water was diluted to 895.52 L·hm according to the experimental measurement. -2 , and a blank control group was set up to spray the same amount of water. Five points were randomly selected from each plot, with a 0.2 m 2 , investigate the plant control effect once at 15d, 30d and 70d after application; Calculation method of drug efficacy: plant protection effect / %= ×100% Table 1 project Thermal storage stability Cold storage stability Suspension rate / % Example 1 qualified qualified 93.8 Example 2 qualified qualified 94.5 Example 3 qualified qualified 92.6 Example 4 qualified qualified 96.1 Example 5 qualified qualified 95.8 Comparative Example 1 Failure Failure 72.1 Comparative Example 2 Failure Failure 79.4 Comparative Example 3 Failure Failure 77.3 Comparative Example 4 Failure Failure 75.5 Comparative Example 5 qualified qualified 83.8 Comparative Example 6 qualified qualified 86.5 Table 2 Data Analysis: It can be seen from Table 1 and Table 2 that the pesticide suspension containing foramsulfuron-flufenacet-isoproturon prepared by the present invention has a higher utilization rate and a longer action time. This may be because the present invention has a high-efficiency and broad-spectrum weed control effect through the combined use of three herbicides containing foramsulfuron, flufenacet and isoproturon; at the same time, the modified isoproturon in the herbicidal composite is copolymerized with acrylate to enhance its hydrophobicity, and can effectively avoid loss in the soil when applied to the roots of weeds; and the microsphere composition in the herbicidal composite has good stability due to the embedding of the biomass material chitosan and sodium alginate and the polymer polypyrrole, and can be slowly released after the herbicide is applied. , while improving the utilization rate of the herbicide, the action time is effectively extended; and the synergist used in the present invention is extracted from wheat straw, which is rich in organic carbon and may produce high concentrations of soluble organic matter in a short period of time after application, which can be adsorbed on the variable charge soil in the winter wheat field, thereby greatly improving the soil's adsorption capacity for the three main components of foramsulfuron, flufenacet and isoproturon and the herbicide complex, further reducing the soil's desorption and leaching of the herbicide, and improving the utilization rate of the herbicide; and foramsulfuron, flufenacet, isoproturon, the herbicide complex and the synergist are compounded in a specific ratio, the efficacy of the herbicide is further enhanced, and the utilization rate and duration are correspondingly improved; In Comparative Example 1, since the herbicide complex was not added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon, it can be seen from Tables 1 and 2 that its utilization rate is poor and the action time is short. This may be because the herbicide complex improves its hydrophobicity by modifying isoproturon with octadecyl acrylate to reduce the risk of soil leaching, and on the other hand, through the embedding effect of the microsphere composition, while playing a protective role on the original drug component, it also has a sustained release effect; in Comparative Example 2, since the modified isoproturon was not added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon, it can be seen from Tables 1 and 2 that its utilization rate is poor and the action time is short. This may be because octadecyl acrylate in the modified isoproturon is a long-chain alkane. The base acrylate contains a hydrophobic aliphatic long chain and can copolymerize with isoproturon, thereby enhancing its hydrophobicity, reducing the risk of soil leaching, and improving the utilization rate; since the microsphere composition was not added in the preparation process of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon in Comparative Example 3, and pyrrole was not added in the preparation process of the microsphere composition in Comparative Example 5, it can be seen from Tables 1 and 2 that its utilization rate is poor and the action time is short. This may be because the microsphere composition is prepared from foramsulfuron, flufenacet, chitosan, sodium alginate and pyrrole, among which chitosan and sodium alginate are two good embedding materials with good biocompatibility and can improve the stability of the material; pyrrole will generate a polymer polymer in the reaction. Pyrrole, the positive charge of oxidized polypyrrole may attract the negative charge of the sulfonamide group or amide group in the molecules of foramsulfuron and flufenacet, so that the sustained release effect is better and the duration of the drug effect is prolonged. In addition, polypyrrole itself is hydrophobic, and the stability of the microsphere composition is further improved, thereby improving the utilization rate. In Comparative Example 4, since no synergist was added during the preparation of the pesticide suspension containing foramsulfuron-flufenacet-isoproturon, it can be seen from Tables 1 and 2 that its utilization rate is poor and the action time is short. This may be because the synergist is extracted from wheat straw, which is rich in organic carbon and may produce a high concentration of soluble organic matter in a short period of time after application. It has good adsorption performance and can be mostly adsorbed on the pesticide suspension in the winter wheat field. On variable charge soil, the adsorption capacity of the soil for the three main components of foramsulfuron, flufenacet and isoproturon and the herbicide complex is greatly improved, the desorption and leaching of the herbicide by the soil is further reduced, and the utilization rate of the herbicide is improved; in Comparative Example 6, since "22g microsphere composition and 9g modified isoproturon" is replaced by "22g microsphere composition and 22g modified isoproturon", it can be seen from Tables 1 and 2 that its utilization rate is poor and the action time is short. This may be because excessive modified isoproturon will affect the overall hydrophobicity of the herbicide complex, reduce the wettability to weeds, make it difficult to be absorbed by weeds, and also reduce its mobility in the soil, thereby affecting the weed control effect, and it is easy to accumulate in the soil, which has a certain pollution effect on the soil.

[0036] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

[0037] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, 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 pesticide suspension containing formosulam-flufenacil-isoproturon, characterized in that: Prepared from the following raw materials in parts by weight: 7-10 parts of formosulam, 4.4-7 parts of flufenacet, 4.6-8 parts of isoproturon, 5-13 parts of herbicide compound, 0.7-1.3 parts of synergist, 10-15 parts of silicone surfactant, 5.8-7.4 parts of wetting and dispersing agent, 0.3-0.8 parts of thickener, 0.4-0.7 parts of antifreeze agent, 0.5-2 parts of defoamer, 0.5-1 parts of preservative, 30-40 parts of deionized water; The herbicidal compound is obtained by mixing modified isoproturon and a microsphere composition; The mass ratio of the modified isoproturon to the microsphere composition is 9-15:22-27; The modified isoproturon is prepared from isoproturon and octadecyl acrylate; The microsphere composition is prepared from formosansulfuron, flufenacet, chitosan and pyrrole.

2. The pesticide suspension containing formosulam-flufenacet-isoproturon according to claim 1, characterized in that: The preparation method of the modified isoproturon is as follows: Isoproturon was placed in a centrifuge tube, N,N-dimethylformamide was added and ultrasonically mixed evenly, after standing at room temperature for 2 hours, octadecyl acrylate, 1-ethyl-3-methylimidazolium chloride and azobisisobutyronitrile were added in sequence under nitrogen protection, and the sealed centrifuge tube was placed in a water bath shaker. After heating for reaction, it was washed with methanol and deionized water in sequence, filtered and dried to obtain modified isoproturon.

3. The pesticide suspension containing formosulam-flufenacil-isoproturon according to claim 2, characterized in that: The usage ratio of isoproturon, N,N-dimethylformamide, octadecyl acrylate, 1-ethyl-3-methylimidazolium chloride and azobisisobutyronitrile is 2-5 g: 43-49 mL: 3-6 g: 0.23-0.35 mg: 0.1-0.15 mg; The temperature during the heating reaction is 60-70°C and the reaction time is 14-16h; The temperature during the drying is 58-63°C.

4. The pesticide suspension concentrate containing formosulam-flufenacet-isoproturon according to claim 1, characterized in that: The preparation method of the synergist is as follows: Grind the wheat straw and air dry it, pass it through a 2 mm sieve, add ultrapure water to the wheat straw, shake it at 180-210 r / min for 15-17 hours at 18-22°C, then centrifuge it at 5500-6000g for 15-18 minutes at 4-6°C, and filter the supernatant through a 0.45 μm filter membrane to obtain the synergist; The mass ratio of the wheat straw to ultrapure water is 1:4-6.

5. The pesticide suspension containing foramsulfuron-flufenacet-isoproturon according to claim 1, characterized in that: The preparation method of the microsphere composition is as follows: Step A1. Add calcium chloride and ammonium persulfate to deionized water and stir to obtain a mixture A; Step A2. Add foramsulfuron and flufenacet to deionized water and stir evenly, then add chitosan, sodium alginate and pyrrole and stir evenly. After removing bubbles, add them dropwise into mixture A with a 5 mm syringe. After stirring at room temperature for 2-2.5 h, wash with deionized water 3 times to obtain a microsphere composition.

6. The pesticide suspension containing formosulam-flufenacet-isoproturon according to claim 5, characterized in that: The mass ratio of deionized water, calcium chloride and ammonium persulfate in step A1 is 8-10: 0.25-0.3: 0.1-0.

15.

7. The pesticide suspension containing formosulam-flufenacil-isoproturon according to claim 5, characterized in that: The usage ratio of formosulam, flufenacet, deionized water, chitosan, sodium alginate, pyrrole and mixture A in step A2 is 4-7 g: 3-5 g: 10-15 mL: 0.2-0.3 g: 0.2-0.3 g: 0.56-0.7 mmol: 8-10 mL.

8. The pesticide suspension containing formosulam-flufenacet-isoproturon according to claim 1, characterized in that: The organosilicon surfactant is at least one of SilwetL77 and Silwet408; The wetting and dispersing agent is at least one of Morwet D-450 and Terwet 1004; The antifreeze agent is at least one of ethylene glycol and glycerol; The preservative is at least one of sodium benzoate and potassium sorbate; The thickener is at least one of xanthan gum and magnesium aluminum silicate; The defoaming agent is polydimethylsiloxane.

9. The pesticide suspension containing formosulam-flufenacil-isoproturon according to claim 1, characterized in that: The preparation method of the pesticide suspension is as follows: Step S1. The microsphere composition and modified isoproturon are mixed evenly to obtain a herbicide compound, and then deionized water, a wetting dispersant, a defoamer, an antifreeze agent and a synergist are mixed evenly, and then foramsulfuron, flufenacet and the herbicide compound are added, and the mixture is sheared for the first time, and then poured into a sand mill containing zirconium beads and sanded for 1.5-2.0 hours. After the particle size is sanded to less than 0.5 μm, the liquid medicine is filtered out to obtain a mixture B; Step S2. After isoproturon and the silicone surfactant are uniformly mixed, mixture B is added, and a second shearing is performed. After a thickener and a preservative are added, a third shearing is performed to obtain a pesticide suspension containing formosulfuron-flufenacet-isoproturon; The speed of the first shearing in step S1 is 3000-5000 r / min, and the time is 8-12 min; The speed of the second shearing in step S2 is 2500-3500 r / min, and the time is 10-13 min; The speed of the third shearing in step S2 is 3200-4000 r / min, and the time is 7-12 min.

10. Use of a pesticide suspension containing formosulam-flufenacil-isoproturon according to any one of claims 1 to 9, characterized in that: The pesticide suspension containing formosulam-flufenacil-isoproturon is used for removing annual weeds in winter wheat fields.

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