Weeding composition containing diuron and preparation method thereof

Abstract

The invention discloses a diuron-containing weeding composition and a preparation method thereof, and belongs to the technical field of weeding compositions. The diuron-containing weeding composition is prepared from the following raw materials in parts by mass: 60 to 100 parts of diuron, 20 to 60 parts of voturon, 10 to 40 parts of oxyfluorfen, 5 to 15 parts of sugarcane polyphenol-zein / brassinolide, 2 to 8 parts of seaweed extract, 100 to 150 parts of filler and 5 to 10 parts of surfactant. Sugarcane polyphenol-zein / brassinolide is a sustained-release particle which is obtained by loading brassinolide by taking sugarcane polyphenol-zein as a nano carrier. According to the weeding composition, the formula is optimized, diuron is used as a main active component for weeding, the fumeturon and oxyfluorfen have a synergistic effect, and the sugarcane polyphenol-zein / brassinolide and the seaweed extract which are used for assisting in synergism are synchronously added, so that the application amount is reduced, the pesticide effect is guaranteed, and the harm of pesticide residues to ecology is reduced.

Description

Technical Field

[0001] This invention belongs to the field of herbicidal composition technology, specifically relating to a herbicidal composition containing diuron and its preparation method. Background Technology

[0002] Diuron is a phenylurea herbicide, belonging to the selective or non-selective herbicides, and can be used for weed control on a variety of crops. Its mechanism of action is essentially: after being absorbed by plant roots or leaves, it inhibits the Hill reaction in photosynthesis, causing chlorosis of the leaves, discoloration of the leaf tips and edges, and ultimately, plant death due to nutrient deficiency.

[0003] Although diuron is effective and fast-acting in weed control, large-scale use can lead to its deposition in the soil. Through rainwater leaching, it can seep into groundwater and pollute the groundwater, causing water pollution and posing certain risks to the ecosystem and human health. Therefore, reducing its usage while ensuring weed control can minimize environmental damage and benefit long-term crop cultivation. Summary of the Invention

[0004] This invention provides a herbicidal composition containing diuron and its preparation method, which can solve the problem of high diuron application rates in the prior art.

[0005] The objective of this invention can be achieved through the following technical solutions: A herbicidal composition containing diuron, comprising, by weight parts: Diuron 60-100 parts, fusulin 20-60 parts, ethoxyflufen 10-40 parts, sugarcane polyphenol-zein / brassinolide 5-15 parts, seaweed extract 2-8 parts, filler 100-150 parts, surfactant 5-10 parts. The sugarcane polyphenol-zein / brassinolide is a sustained-release particle obtained by loading brassinolide onto sugarcane polyphenol-zein as a nanocarrier.

[0006] Different herbicide components have different mechanisms of action and target organisms. Diuron is a systemic herbicide that primarily works by being absorbed by weeds through roots and leaves, then diffused, preventing them from photosynthesizing and causing them to gradually die, thus achieving weed control. Diuron's mechanism of action is the inhibition of photosynthesis. Combining diuron with fenuron (an inhibitor of acyl reductase) and ethoxyflufenoxam (an inhibitor of protoporphyrinogen oxidase), which both inhibit acyl reductase (ACCase) in plants, can delay the development of resistance and enhance weed control through the simultaneous action of their different mechanisms.

[0007] Brassinolide is a plant growth regulator whose mechanism of action is mainly through stimulating the activity of ATPase on the cell membrane, thereby promoting the secretion of H+ by the plasma membrane. +It reaches the cell wall, relaxes the cell wall, promotes cell elongation and division, and through the action of brassinolide, the active components of herbicides (such as diuron) sprayed on the root and leaf surface can enter the cells more quickly and be absorbed by weeds, thus ensuring efficacy at a lower concentration.

[0008] Herbicide active ingredients are easily washed away by rainwater after entering the soil. Applying seaweed extract to the soil can increase the proportion of water-stable macroaggregates in the soil. These water-stable macroaggregates intertwine to form a complex pore network, which improves the soil structure. This allows the active ingredients of the herbicide to be adsorbed and resisted from loss, so that they can be fully retained even at low concentrations, thus enhancing the efficacy of the herbicide.

[0009] Furthermore, the mass ratio of diuron, 2,4-D sodium salt and ethoxyflufenicol is 10:(3-7):(1-5).

[0010] Furthermore, the preparation method of the sugarcane polyphenol-zein / brassinolide includes the following steps: S1. Prepare a brassinolide ethanol solution with a concentration of 1-5 mg / mL; S2. After mixing the sugarcane polyphenol-zein concentrate and brassinolide ethanol solution, add the mixture to an ethanol aqueous solution and ultrasonically disperse it evenly to obtain the organic phase. S3. While stirring, add the organic phase to the deionized water and continue stirring to obtain a suspension; S4. After rotary evaporation and concentration, freeze-dry and grind to obtain sugarcane polyphenol-zein / brassinolide.

[0011] Brassinolide is hydrophobic, making it difficult to directly and evenly disperse and atomize it with water during the later stages of herbicide powder application. Sugarcane polyphenol-zein nanocarriers are composed of hydrophobic zein and hydrophilic polyphenol compounds. Brassinolide is encapsulated within the hydrophobic core of the zein, while the introduced hydrophilic sugarcane polyphenols ensure uniform dispersion in aqueous solution without precipitation or aggregation.

[0012] Furthermore, the concentration of zein in the sugarcane polyphenol-zein concentrate is 5-8% w / v.

[0013] Furthermore, the sugarcane polyphenol-zein concentrate and brassinolide are mixed at a mass ratio of zein to brassinolide of 100:6-10.

[0014] Further, in step S2, the volume ratio of ethanol to water in the ethanol-water solution is (7-8):(2-3).

[0015] Furthermore, in step S3, the deionized water is 8-10 times the volume of the organic phase.

[0016] Furthermore, the preparation method of the sugarcane polyphenol-zein concentrate includes the following steps: A1. Dissolve zein in an ethanol aqueous solution to obtain solution A, and dissolve sugarcane polyphenols in deionized water to obtain solution B; A2. Adjust the pH of solutions A and B to 9.0-9.5 respectively using sodium hydroxide solution; A3. Under light-protected conditions, the two solutions are stirred and mixed for 12-24 hours to obtain a mixture. After rotary evaporation and concentration, a sugarcane polyphenol-zein concentrate is obtained.

[0017] Zeatin has excellent self-assembly properties, enabling the preparation of spherical, uniformly sized nanoparticles. It can serve as a carrier for active components. By combining zeatin with polyphenols through hydrogen bonding, stable zeatin-based nanoparticles can be constructed, exhibiting strong biocompatibility and biodegradability, and enabling sustained release.

[0018] Furthermore, the concentration of zein in solution A is 20-30 mg / mL; and the concentration of sugarcane polyphenols in solution B is 40-50 mg / mL.

[0019] Furthermore, solution A and solution B are mixed at a mass ratio of zein to sugarcane polyphenols of 1:0.2-0.5.

[0020] Furthermore, in step A3, the deionized water is 3-5 times the volume of the mixed liquid.

[0021] Furthermore, the surfactant is one of sodium dodecylbenzenesulfonate and sodium lignosulfonate.

[0022] Furthermore, the filler is one of bentonite and kaolin.

[0023] The present invention also provides a method for preparing a herbicidal composition containing diuron, for preparing the herbicidal composition containing diuron as described above, comprising the following steps: Prepare the raw materials for the herbicidal composition according to the specified proportions, mix and stir all the raw materials evenly, and then crush them to obtain the finished product.

[0024] The beneficial effects of this invention are: This invention optimizes the formulation of a herbicidal composition containing diuron, using diuron as the main active herbicide component. It adds fenfluridine and ethoxyflufenoxam, which have different mechanisms of action, to synergistically delay the development of resistance in weeds and enhance the herbicidal effect. Simultaneously, sugarcane polyphenol-zein / brassinolide and seaweed extract are added to the herbicidal composition. Brassinolide relaxes plant cell walls, promoting the absorption of the active herbicide component. Sugarcane polyphenol-zein loads hydrophobic brassinolide, giving it hydrophilic slow-release properties, facilitating the formation of a uniform aqueous dispersion during subsequent application. Seaweed extract increases the proportion of water-stable macroaggregates in the soil, improving soil structure and reducing the loss of efficacy from the herbicide composition. By combining enhanced absorption of the active herbicide component and reduced efficacy loss, the herbicidal composition ensures full efficacy, reducing the amount of diuron required and avoiding ecological damage caused by excessive pesticide use. Detailed Implementation

[0025] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0026] Example 1

[0027] Preparation of sugarcane polyphenol-zein concentrate: A1. Prepare an ethanol-water solution with a volume ratio of 7:3. Weigh zein and add it to the ethanol-water solution at a concentration of 25 mg / mL. Stir until completely dissolved to obtain solution A. Weigh sugarcane polyphenols and add them to deionized water at a concentration of 45 mg / mL. Stir until completely dissolved to obtain solution B.

[0028] A2. Prepare a sodium hydroxide solution with a concentration of 0.1 mol / L. Add sodium hydroxide solution dropwise to solutions A and B respectively to adjust the pH of solutions A and B to 9.0.

[0029] A3. Under light-protected conditions, solution A and solution B were mixed at a mass ratio of zein to sugarcane polyphenol of 1:0.4 and stirred continuously for 12 hours to obtain a mixture. After rotary evaporation and concentration, a sugarcane polyphenol-zein concentrate was obtained, with a zein concentration of 6% w / v in the concentrate.

[0030] Preparation of sugarcane polyphenol-zein / brassinolide: S1. Prepare a 3 mg / mL brassinolide ethanol solution.

[0031] S2. Prepare an ethanol-water solution with a volume ratio of 7:3. Mix the sugarcane polyphenol-zeolite concentrate and the brassinolide ethanol solution with a mass ratio of 100:8 for zein and brassinolide. Add the mixture to an equal volume of the ethanol-water solution and sonicate for 30 minutes to obtain the organic phase.

[0032] S3. While stirring, add the organic phase to the deionized water. The volume of the deionized water should be 8 times the volume of the organic phase. Continue stirring for 10 minutes to obtain a suspension.

[0033] S4. After rotary evaporation and concentration, freeze-dry and grind to obtain sugarcane polyphenol-zein / brassinolide.

[0034] Preparation of herbicidal composition: Prepare the raw materials for the herbicidal composition according to the following mass proportions: 80 parts of diuron, 32 parts of fenuron, 24 parts of ethoxyflufenoxam, 10 parts of sugarcane polyphenol-zein / brassinolide, 6 parts of seaweed extract, 120 parts of bentonite, and 6 parts of sodium dodecylbenzenesulfonate. Mix all the raw materials evenly, pulverize them, and then obtain the finished product.

[0035] Example 2-Example 3

[0036] The only difference from Example 1 is that the proportions of diuron, fenuron, and ethoxyflufenicol in the raw materials of the herbicidal composition are different. The other steps and conditions are the same as in Example 1, and the specific proportions are shown in Table 1.

[0037] Table 1

[0038] Example 4

[0039] The only difference from Example 1 is that the mass fraction of sugarcane polyphenol-zein / brassinolide in the herbicidal composition is increased to 15 parts. Other conditions and steps are the same as in Example 1.

[0040] Example 5

[0041] The only difference from Example 1 is that the mass fraction of sugarcane polyphenol-zein / brassinolide in the herbicidal composition is reduced to 5 parts. All other conditions and procedures are the same as in Example 1.

[0042] Example 6

[0043] The only difference from Example 1 is that the mass fraction of seaweed extract in the herbicidal composition is increased to 8 parts. All other conditions and steps are the same as in Example 1.

[0044] Example 7

[0045] The only difference from Example 1 is that the mass fraction of seaweed extract in the herbicidal composition is reduced to 2 parts. All other conditions and steps are the same as in Example 1.

[0046] Comparative Example 1

[0047] This comparative example uses commercially available 25% diuron wettable powder.

[0048] Comparative Example 2

[0049] The only difference from Example 1 is that this comparative herbicidal composition does not contain fenfluridine and ethoxyflufenoxam.

[0050] Preparation of sugarcane polyphenol-zein concentrate: A1. Prepare an ethanol-water solution with a volume ratio of 7:3. Weigh zein and add it to the ethanol-water solution at a concentration of 25 mg / mL. Stir until completely dissolved to obtain solution A. Weigh sugarcane polyphenols and add them to deionized water at a concentration of 45 mg / mL. Stir until completely dissolved to obtain solution B.

[0051] A2. Prepare a sodium hydroxide solution with a concentration of 0.1 mol / L. Add sodium hydroxide solution dropwise to solutions A and B respectively to adjust the pH of solutions A and B to 9.0.

[0052] A3. Under light-protected conditions, solution A and solution B were mixed at a mass ratio of zein to sugarcane polyphenol of 1:0.4 and stirred continuously for 12 hours to obtain a mixture. After rotary evaporation and concentration, a sugarcane polyphenol-zein concentrate was obtained, with a zein concentration of 6% w / v in the concentrate.

[0053] Preparation of sugarcane polyphenol-zein / brassinolide: S1. Prepare a 3 mg / mL brassinolide ethanol solution.

[0054] S2. Prepare an ethanol-water solution with a volume ratio of 7:3. Mix the sugarcane polyphenol-zeolite concentrate and the brassinolide ethanol solution with a mass ratio of 100:8 for zein and brassinolide. Add the mixture to an equal volume of the ethanol-water solution and sonicate for 30 minutes to obtain the organic phase.

[0055] S3. While stirring, add the organic phase to the deionized water. The volume of the deionized water should be 8 times the volume of the organic phase. Continue stirring for 10 minutes to obtain a suspension.

[0056] S4. After rotary evaporation and concentration, freeze-dry and grind to obtain sugarcane polyphenol-zein / brassinolide.

[0057] Preparation of herbicidal composition: Prepare the raw materials for the herbicidal composition according to the following mass proportions: 136 parts of diuron, 10 parts of sugarcane polyphenol-zein / brassinolide, 6 parts of seaweed extract, 120 parts of bentonite, and 6 parts of sodium dodecylbenzene sulfonate. Mix all the raw materials evenly, pulverize them, and obtain the finished product.

[0058] Comparative Example 3

[0059] The only difference from Example 1 is that this comparative herbicidal composition does not contain sugarcane polyphenol-zein / brassinolide.

[0060] Preparation of herbicidal composition: Prepare the raw materials for the herbicidal composition according to the following mass proportions: 80 parts diuron, 32 parts fenuron, 24 parts ethoxyflufenoxam, 6 parts seaweed extract, 120 parts bentonite, and 6 parts sodium dodecylbenzenesulfonate. Mix all the raw materials evenly, pulverize them, and obtain the finished product.

[0061] Comparative Example 4

[0062] The only difference from Example 1 is that no seaweed extract is added to this comparative herbicidal composition.

[0063] Preparation of sugarcane polyphenol-zein concentrate: A1. Prepare an ethanol-water solution with a volume ratio of 7:3. Weigh zein and add it to the ethanol-water solution at a concentration of 25 mg / mL. Stir until completely dissolved to obtain solution A. Weigh sugarcane polyphenols and add them to deionized water at a concentration of 45 mg / mL. Stir until completely dissolved to obtain solution B.

[0064] A2. Prepare a sodium hydroxide solution with a concentration of 0.1 mol / L. Add sodium hydroxide solution dropwise to solutions A and B respectively to adjust the pH of solutions A and B to 9.0.

[0065] A3. Under light-protected conditions, solution A and solution B were mixed at a mass ratio of zein to sugarcane polyphenol of 1:0.4 and stirred continuously for 12 hours to obtain a mixture. After rotary evaporation and concentration, a sugarcane polyphenol-zein concentrate was obtained, with a zein concentration of 6% w / v in the concentrate.

[0066] Preparation of sugarcane polyphenol-zein / brassinolide: S1. Prepare a 3 mg / mL brassinolide ethanol solution.

[0067] S2. Prepare an ethanol-water solution with a volume ratio of 7:3. Mix the sugarcane polyphenol-zeolite concentrate and the brassinolide ethanol solution with a mass ratio of 100:8 for zein and brassinolide. Add the mixture to an equal volume of the ethanol-water solution and sonicate for 30 minutes to obtain the organic phase.

[0068] S3. While stirring, add the organic phase to the deionized water. The volume of the deionized water should be 8 times the volume of the organic phase. Continue stirring for 10 minutes to obtain a suspension.

[0069] S4. After rotary evaporation and concentration, freeze-dry and grind to obtain sugarcane polyphenol-zein / brassinolide.

[0070] Preparation of herbicidal composition: Prepare the raw materials for the herbicidal composition according to the following mass proportions: 80 parts of diuron, 32 parts of fenuron, 24 parts of ethoxyflufenoxam, 10 parts of sugarcane polyphenol-zein / brassinolide, 120 parts of bentonite, and 6 parts of sodium dodecylbenzenesulfonate. Mix all the raw materials evenly, pulverize them, and obtain the finished product.

[0071] Comparative Example 5

[0072] The only difference from Example 1 is that in this comparative example, sugarcane polyphenol-zeolite / brassinolide is replaced by the same mass of zeolite / brassinolide.

[0073] Preparation of zein / brassinolide: S1. Prepare a 3 mg / mL brassinolide ethanol solution. S2. Prepare an ethanol-water solution with a volume ratio of 7:3. Mix the ethanol solution of zein and brassinolide with a mass ratio of 100:8. Add the mixture to an equal volume of the ethanol-water solution and sonicate for 30 minutes to obtain the organic phase.

[0074] S3. While stirring, add the organic phase to the deionized water. The volume of the deionized water should be 8 times the volume of the organic phase. Continue stirring for 10 minutes to obtain a suspension.

[0075] S4. After rotary evaporation and concentration, freeze-dry and grind to obtain zein / brassinolide.

[0076] Preparation of herbicidal composition: Prepare the raw materials for the herbicidal composition according to the following mass proportions: 80 parts diuron, 32 parts fenuron, 24 parts ethoxyflufenoxam, 10 parts zein / brassinolide, 6 parts seaweed extract, 120 parts bentonite, and 6 parts sodium dodecylbenzenesulfonate. Mix all the raw materials evenly, pulverize them, and obtain the finished product.

[0077] Field efficacy tests were conducted on the herbicidal compositions prepared in Examples 1-7 and Comparative Examples 1-5, and the results are shown in Table 2.

[0078] Field efficacy trials: The herbicidal compositions prepared in Examples 1-7 and Comparative Examples 2-5 were used at a ratio of 100 g / 666.7 m³. 2 The dosage is 50 kg of water to prepare the solution. The 25% diuron wettable powder from Comparative Example 1 is prepared at a rate of 400 g / 666.7 m³. 2 The pesticide solution was prepared with 50 kg of water. After the sugarcane had grown to the 6-leaf stage, the weeds were sprayed in a directional manner with the nozzles lowered when they were at the 3-5 leaf stage. The plant control efficacy and fresh weight control efficacy were investigated 15 days and 30 days after application. The main weeds in the experimental field were crabgrass, goosegrass, foxtail grass, and purslane. The experimental field was divided into different areas, each with an area of ​​one mu. Each treatment was replicated 4 times, and an untreated area was set up as a control area.

[0079] The efficacy calculation is as follows: Control efficacy (%) = (Number of weeds in the control area - Number of weeds in the treatment area) / Number of weeds in the control area × 100; Fresh weight efficacy (%): (fresh weight of control area - fresh weight of treatment area) / fresh weight of control area × 100.

[0080] Table 2

[0081] As can be seen from Table 2, the herbicidal composition provided in this embodiment of the invention achieves a total plant control efficacy and total fresh weight control efficacy of over 94.5% after 30 days of application, which is significantly higher than the control efficacy of diuron alone in Comparative Example 1. In comparison, the amount of active ingredient per acre in the herbicidal composition of this embodiment is lower than that in Comparative Example 1, resulting in a reduction in the amount of herbicide used, but with improved efficacy.

[0082] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0083] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A herbicidal composition containing diuron, characterized in that, By weight, it includes the following raw materials: Diuron 60-100 parts, fusulin 20-60 parts, ethoxyflufen 10-40 parts, sugarcane polyphenol-zein / brassinolide 5-15 parts, seaweed extract 2-8 parts, filler 100-150 parts, surfactant 5-10 parts. The sugarcane polyphenol-zein / brassinolide is a sustained-release particle obtained by loading brassinolide onto sugarcane polyphenol-zein as a nanocarrier.

2. The herbicidal composition containing diuron according to claim 1, characterized in that, The mass ratio of diuron, 2,4-D sodium salt and ethoxyflufen is 10:(3-7):(1-5).

3. The herbicidal composition containing diuron according to claim 1, characterized in that, The preparation method of the sugarcane polyphenol-zein / brassinolide includes the following steps: S1. Prepare a brassinolide ethanol solution with a concentration of 1-5 mg / mL; S2. After mixing the sugarcane polyphenol-zein concentrate and brassinolide ethanol solution, add the mixture to an ethanol aqueous solution and ultrasonically disperse it evenly to obtain the organic phase. S3. While stirring, add the organic phase to the deionized water and continue stirring to obtain a suspension; S4. After rotary evaporation and concentration, freeze-dry and grind to obtain sugarcane polyphenol-zein / brassinolide.

4. The herbicidal composition containing diuron according to claim 3, characterized in that, The concentration of zein in the sugarcane polyphenol-zein concentrate is 5-8% w / v; The sugarcane polyphenol-zein concentrate and brassinolide were mixed at a mass ratio of zein to brassinolide of 100:6-10.

5. The herbicidal composition containing diuron according to claim 3, characterized in that, In step S3, the deionized water is 8-10 times the volume of the organic phase.

6. The herbicidal composition containing diuron according to claim 3, characterized in that, The preparation method of the sugarcane polyphenol-zein concentrate includes the following steps: A1. Dissolve zein in an ethanol aqueous solution to obtain solution A, and dissolve sugarcane polyphenols in deionized water to obtain solution B; A2. Adjust the pH of solutions A and B to 9.0-9.5 respectively using sodium hydroxide solution; A3. Under light-protected conditions, the two solutions are stirred and mixed for 12-24 hours to obtain a mixture. After rotary evaporation and concentration, a sugarcane polyphenol-zein concentrate is obtained.

7. The herbicidal composition containing diuron according to claim 6, characterized in that, The concentration of zein in solution A is 20-30 mg / mL; the concentration of sugarcane polyphenols in solution B is 40-50 mg / mL. Solution A and solution B are mixed at a mass ratio of zein to sugarcane polyphenols of 1:0.2-0.

5.

8. The herbicidal composition containing diuron according to claim 6, characterized in that, In step A3, the deionized water is 3-5 times the volume of the mixed liquid.

9. The herbicidal composition containing diuron according to claim 1, characterized in that, The surfactant is one of sodium dodecylbenzene sulfonate and sodium lignosulfonate; The filler is either bentonite or kaolin.

10. A method for preparing a herbicidal composition containing diuron, characterized in that, The preparation of the herbicidal composition containing diuron as described in any one of claims 1-9 comprises the following steps: Prepare the raw materials for the herbicidal composition according to the specified proportions, mix and stir all the raw materials evenly, and then crush them to obtain the finished product.

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