Tmbotrione-containing herbicide and preparation method thereof
By preparing cyclosulfone and syrupolamine compositions and using specific emulsifiers and stabilizers to combine, the problems of water dissipation, bottoming and demulsification during storage and use of herbicides are solved, and the good stability and high-efficiency performance of the herbicides are achieved.
Patent Information
- Application Number
- CN202411872532.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-18
- Publication Date
- 2025-05-13
AI Technical Summary
In the prior art, the thermal decomposition and stability of cyclosulfone and cyprolitholamine have not been effectively solved, resulting in problems such as water extraction, bottoming and demulsification during storage and use of herbicides.
By preparing the cyclic sulfone composition and the lysopylene composition, including cyclic sulfone, lysopylene, dispersant, water and lysopylene, emulsifier, colloid, preservative, stabilizer, and water, specific emulsifiers and stabilizers are used to avoid thermal storage of water, bottoming and demulsification problems.
The good stability of the herbicide containing cyclosulfone is achieved, and the problems of water dissipation, bottoming and demulsification are avoided, and the storage and use performance of the herbicide is improved.
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Abstract
Description
Technical Field
[0001] The present application relates to the technical field of herbicides, and in particular to a cyclosulfuron-containing herbicide and a preparation method thereof. Background Art
[0002] At present, corn field planting is becoming more and more large-scale and mechanized. Weed control advocates safety, efficiency, lightness and simplification. It is necessary to apply herbicides that can meet the weed control needs of the entire growth period at one time, that is, mixed products with both closed treatment activity and stem and leaf treatment activity. Cyclosulfuron is mainly used for stem and leaf treatment, and has a good control effect on both grass weeds and broad-leaved weeds. It is more resistant to rain erosion and has high activity. S-isopropylamine belongs to the chloroacetyl chloride compound, which is a type of optically active chiral pesticide and a closed treatment herbicide. It can be used to control annual grass weeds and some broad-leaved weeds in crop fields such as sorghum, sugarcane, corn, soybeans, and cotton. At present, the types of corn are constantly changing. For example, weeds in genetically modified corn fields have the problem of secondary weeds after application because glyphosate has no soil treatment activity. Some weeds are not sensitive to glyphosate and cannot be completely controlled. Glyphosate needs to be mixed with other agents to achieve the effect of double-effect blocking and simultaneous control of difficult-to-control and insensitive weeds at one time. At present, the use of cyclosulfuron or S-isopropylamine alone cannot completely solve the above problems.
[0003] A Chinese patent with a patent publication number of CN111436450A discloses a compound formulation of a post-emergence herbicide for corn fields and a preparation method thereof, and discloses a compound formulation composed of the following weight percentages: 1%-3% of nicosulfuron, 3%-8% of tembotrione, 5%-10% of S-metolachlor, 10%-25% of atrazine, 8%-10% of a synergist, 1%-2% of a safener, and 50%-70% of a solvent, but does not disclose a technical solution for solving the problems of thermal decomposition of tembotrione and S-metolachlor and changes in their stability.
[0004] Therefore, providing a cyclosulfone-containing herbicide with good stability is the main technical problem that needs to be solved at present. Summary of the invention
[0005] In order to solve the above problems, the first aspect of the present invention provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include a tembotrione composition and an S-metolachlor composition; the mass ratio of the tembotrione composition to the S-metolachlor composition is 1:(4-6);
[0006] The tembotrione composition comprises tembotrione, chlorpyrifos, a dispersant and water;
[0007] The S-metolachlor composition comprises S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0008] In one embodiment, the tembotrione composition comprises, by mass percentage, 16%-20% tembotrione, 15%-20% chlorpyrifos, 4.8%-6.0% dispersant, and the balance water.
[0009] In one embodiment, the water is deionized water.
[0010] In one embodiment, the pH of the dispersant is 8-10.
[0011] In one embodiment, the dispersant comprises a carboxylate dispersant.
[0012] In one embodiment, the dispersant can be purchased from Tangshan Bangxie Fine Additives Co., Ltd. and the model is Additive B.
[0013] In one embodiment, the S-metolachlor composition comprises, by mass percentage, 55%-65% of S-metolachlor, 5%-6% of emulsifier, 3.5%-6.75% of colloid, 0.1%-0.5% of preservative, 0.25%-0.5% of stabilizer, and the balance is water.
[0014] In one embodiment, the emulsifier includes emulsifier A and emulsifier monomer B, and the mass ratio of the emulsifier A to the emulsifier monomer B is (4.5-5.0): (0.5-1).
[0015] In one embodiment, the emulsifier consists of emulsifier A and emulsifier monomer B.
[0016] In one embodiment, the pH of the emulsifier A is 5-7.
[0017] In one embodiment, the emulsifier A includes a special lipophilic group and is a combined anionic and nonionic auxiliary agent.
[0018] In one embodiment, the pH of the emulsifier monomer B is 3-5.
[0019] In one embodiment, the emulsifier monomer B is a polymeric dispersant.
[0020] In one embodiment, the emulsifier A can be purchased from Tangshan Bangxie Fine Additives Co., Ltd., and the model number is Additive A.
[0021] In one embodiment, the emulsifier monomer B can be purchased from Tangshan Bangxie Fine Additives Co., Ltd., and the model is B material.
[0022] The technical obstacle encountered by the inventors during the experiment is that the obtained cyclohexane-containing herbicide will have the problem of thermal storage oil demulsification; in order to solve the above technical obstacle problem, the inventors found during the experiment that an emulsifier is used in the S-isopropylamine composition, and the emulsifier is composed of emulsifier A and emulsifier monomer B, and the mass ratio of emulsifier A to emulsifier monomer B is (4.5-5.0): (0.5-1), and the pH of emulsifier A is 5-7; the pH of emulsifier monomer B is 3-5; the S-isopropylamine composition obtained by using the emulsifier composed of the above-mentioned specific emulsifier A and emulsifier monomer B to cooperate with S-isopropylamine, colloid, preservative, stabilizer and water can avoid the problem of thermal storage oil demulsification of the obtained cyclohexane-containing herbicide. During the experiment, the inventors found that the problem of thermal storage oil demulsification of the obtained cyclosulfuron-containing herbicide can be avoided by using an emulsifier A containing a special lipophilic group and an emulsifier monomer B for cooperation; however, when an emulsifier monomer B280 or an emulsifier monomer 1602 is used in combination with an emulsifier A, the problem of thermal storage oil demulsification of the obtained cyclosulfuron-containing herbicide cannot be solved; the emulsifier monomer B280 is a fatty alcohol polyoxyethylene ether; the emulsifier monomer 1602 is an EOPO block polyether.
[0023] In one embodiment, the colloid includes xanthan gum, magnesium aluminum silicate, and ethylene glycol, and the mass ratio of the xanthan gum to magnesium aluminum silicate is (0.1-0.75):1; the mass ratio of the total mass of the xanthan gum and magnesium aluminum silicate to ethylene glycol is (0.55-1.75):(3-5).
[0024] In one embodiment, the colloid consists of xanthan gum, magnesium aluminum silicate, and ethylene glycol.
[0025] In one embodiment, the method for preparing the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0026] The technical obstacles encountered by the inventors during the experiment are that the obtained cyclohexane-containing herbicide will have the problem of large water precipitation and bottoming; the inventors found during the experiment that when xanthan gum is directly mixed with S-isopropylamine, emulsifier, preservative, stabilizer and water in the S-isopropylamine composition, the xanthan gum will be difficult to disperse. In order to better disperse the xanthan gum, the stirring time needs to be extended, but the inventors also found that even after the stirring time is extended, the obtained cyclohexane-containing herbicide will have the problem of water precipitation and bottoming; in order to solve the problem that the cyclohexane-containing herbicide will have a water precipitation of more than 2% and bottoming during storage, the inventors found during the experiment that S-isopropylamine When a colloid is mixed with S-isopropylamine, an emulsifier, a preservative, a stabilizer and water in a metolachlor composition, in particular, the colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol, and the mass ratio of the xanthan gum to the magnesium aluminum silicate is (0.1-0.75):1; when the mass ratio of the total mass of the xanthan gum and the magnesium aluminum silicate to the ethylene glycol is (0.55-1.75):(3-5), when the xanthan gum and magnesium aluminum silicate are added to ethylene glycol and mixed to obtain a colloid to obtain a transparent gel-like liquid, the colloid is mixed with S-isopropylamine, an emulsifier, a preservative, a stabilizer and water to obtain a tampron-containing herbicide without the problem of bottoming out, and the amount of water precipitation is less than 2%.
[0027] In one embodiment, the preservative is sodium benzoate.
[0028] In one embodiment, the stabilizer is a weak organic acid.
[0029] In one embodiment, the weak organic acid comprises citric acid.
[0030] In one embodiment, the weak organic acid is citric acid.
[0031] The technical obstacle encountered by the inventors during the experiment is that the obtained cyclosulfuron-containing herbicide will have the problem of decomposition of cyclosulfuron and S-isopropylamine in a hot storage environment. In order to solve the above technical obstacle, the inventors found during the experiment that when an organic weak acid is used as a stabilizer and the amount of the stabilizer added is 0.25%-0.5%, especially when citric acid is used as a stabilizer and is coordinated with S-isopropylamine, an emulsifier, a colloid, a preservative, and water to obtain an S-isopropylamine composition, the obtained cyclosulfuron-containing herbicide will avoid the problem of decomposition of cyclosulfuron and S-isopropylamine in a hot storage environment, and the thermal decomposition rate is greater than 5%; the inventors found during the experiment that when the amount of the stabilizer added is greater than 0.5%, the S-isopropylamine in the cyclosulfuron-containing herbicide will be thermally decomposed, and the thermal decomposition rate is greater than 5%; when no stabilizer is used, the cyclosulfuron in the cyclosulfuron-containing herbicide will be thermally decomposed, and the thermal decomposition rate is greater than 5%.
[0032] The second aspect of the present invention provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0033] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide.
[0034] In one embodiment, the stirring time is 60-120 min, the stirring speed is 200-400 r / min, and the stirring temperature is 10-40°C.
[0035] In one embodiment, the preparation method of the tembotrione-containing herbicide comprises the following steps:
[0036] The tembotrione, chlorpyrifos, a dispersant and water are mixed and then sand-milled to obtain a tembotrione composition;
[0037] The S-metolachlor composition is obtained by mixing and shearing S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water;
[0038] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide.
[0039] In one embodiment, tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min.
[0040] In one embodiment, tembotrione, chlorpyrifos, a dispersant and water are mixed and then sand-milled to obtain a tembotrione composition having a D90 particle size of 5-7 μm.
[0041] In one embodiment, S-methylpropionate, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-methylpropionate composition; the mixing and shearing is performed at a shear rate of 10,000 r / min, a shear time of 3 min, and the mixing and shearing is performed at 23° C. The D90 particle size of the obtained S-methylpropionate composition is 2.4-3.5 μm, and preferably the D90 particle size of the obtained S-methylpropionate composition is 3 μm.
[0042] In one embodiment, the tembotrione composition is added to the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 60-120 min, the stirring speed is 200-400 r / min, and the stirring temperature is 10-40°C.
[0043] In one embodiment, the tembotrione composition is added to the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 min, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0044] The technical resistance encountered by the inventors during the experiment is that in the process of preparing the cyclosulfone herbicide, the original drugs (cyclosulfone, chlorpyrifos, and metolachlor) will be dissolved and coated on the sand mill pick beads. Once the high-speed rotation speed and temperature are increased, the solubility of the original drugs will change, flocculation problems will occur, and there will also be problems of emulsion phase demulsification due to high speed. In order to solve the above technical resistance problems, the inventors found during the experiment that a cyclosulfone composition can be obtained by mixing cyclosulfone, chlorpyrifos, a dispersant, and water and then sand-milling. The sand milling is performed using a vertical sand mill for 1 hour, and the sand milling speed of the vertical sand mill is set to 3000r / min. S-isopropylamine, emulsifier, colloid, preservative, stabilizer, etc. are mixed. The invention discloses a method for preparing a cyclohexane-containing herbicide. The method comprises the steps of: mixing and shearing a cyclohexane-containing herbicide with water to obtain a cyclohexane-containing herbicide; mixing and shearing a cyclohexane-containing herbicide with a shearing speed of 10000 r / min and a shearing time of 3 min at 23° C. The cyclohexane-containing herbicide is prepared by mixing and shearing a cyclohexane-containing herbicide with water; the cyclohexane-containing herbicide is prepared by mixing and shearing a cyclohexane-containing herbicide with a shearing speed of 10000 r / min and a shearing time of 3 min at 23° C. The cyclohexane-containing herbicide is prepared by the method of the present invention.
[0045] Beneficial Effects
[0046] 1. In the present application, ethylene glycol is used to dissolve xanthan gum and magnesium aluminum silicate to prepare a transparent gel-like liquid, which can improve the problem of water precipitation and bottoming of cyclohexane-containing herbicides during storage or at high speed.
[0047] 2. In the present application, the thermal decomposition rate of tembotrione and S-isopropylamine can be reduced by using a specific stabilizer, and the problem of demulsification can be avoided.
[0048] 3. In the present application, the problem of oil droplets and demulsification during the hot storage of cyclohexane-containing herbicides can be avoided by using a specific emulsifier for coordination.
[0049] 4. The preparation method defined in the present application can avoid the flocculation problem that may occur during the preparation of cyclohexane-containing herbicides.
[0050] 5. The raw materials and process provided in this application can be used to obtain a cyclosulfuron-containing herbicide with good stability. BRIEF DESCRIPTION OF THE DRAWINGS
[0051] Figure 1 This is the water analysis state diagram.
[0052] Figure 2 This is the bottoming state diagram.
[0053] Figure 3 This is a diagram of the oil separation and demulsification state.
[0054] Figure 4 This is a diagram of the oil separation and demulsification state.
[0055] Figure 5 This is a diagram of the oil separation and demulsification state.
[0056] Figure 6 This is a flocculation state diagram.
[0057] Figure 7 This is a flocculation state diagram. DETAILED DESCRIPTION
[0058] The raw material information used in Examples 1-3 and Comparative Examples 1-13 is shown in Table 1.
[0059] Table 1
[0060]
[0061]
[0062] Example 1
[0063] In a first aspect, the present embodiment provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0064] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0065] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0066] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0067] The pH of the dispersant was 9.05.
[0068] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0069] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0070] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0071] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0072] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0073] The preservative is sodium benzoate.
[0074] The stabilizer is citric acid.
[0075] The second aspect of this embodiment provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0076] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0077] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C. The D90 particle size of the obtained S-metolachlor composition is 3 μm;
[0078] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0079] Example 2
[0080] In a first aspect, the present embodiment provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0081] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0082] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0083] Calculated by mass percentage, the tembotrione composition consists of 18.46% tembotrione, 17.45% chlorpyrifos, 4.8% dispersant and the balance water; the water is deionized water.
[0084] The pH of the dispersant was 9.05.
[0085] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5% of emulsifier, 3.55% of colloid, 0.1% of preservative, 0.3% of stabilizer, and the balance of water; the water is deionized water.
[0086] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5% emulsifier consists of 4.5% emulsifier A and 0.5% emulsifier monomer B.
[0087] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0088] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, 3.55% of the colloid is composed of 0.05% of xanthan gum, 0.5% of magnesium aluminum silicate and 3% of ethylene glycol.
[0089] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0090] The preservative is sodium benzoate.
[0091] The stabilizer is citric acid.
[0092] The second aspect of this embodiment provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0093] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0094] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C. The D90 particle size of the obtained S-metolachlor composition is 3 μm;
[0095] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0096] Example 3
[0097] In a first aspect, the present embodiment provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0098] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0099] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0100] Calculated by mass percentage, the tembotrione composition consists of 18.46% tembotrione, 17.45% chlorpyrifos, 6% dispersant and the balance water; the water is deionized water.
[0101] The pH of the dispersant was 9.05.
[0102] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 6% of emulsifier, 6.75% of colloid, 0.5% of preservative, 0.5% of stabilizer, and the balance of water; the water is deionized water.
[0103] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 6% emulsifier consists of 5% emulsifier A and 1% emulsifier monomer B.
[0104] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0105] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, 6.75% of the colloid is composed of 0.75% of xanthan gum, 1% of magnesium aluminum silicate and 5% of ethylene glycol.
[0106] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0107] The preservative is sodium benzoate.
[0108] The stabilizer is citric acid.
[0109] The second aspect of this embodiment provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0110] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0111] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C. The D90 particle size of the obtained S-metolachlor composition is 3 μm;
[0112] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0113] Comparative Example 1
[0114] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0115] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0116] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0117] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0118] The pH of the dispersant was 9.05.
[0119] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.06% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0120] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0121] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0122] The colloid is composed of xanthan gum and ethylene glycol. In terms of mass percentage, the colloid 4.06% is composed of 0.06% xanthan gum and 4% ethylene glycol.
[0123] The preparation method of the colloid comprises the following steps: adding xanthan gum into ethylene glycol and mixing them to obtain the colloid.
[0124] The preservative is sodium benzoate.
[0125] The stabilizer is citric acid.
[0126] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0127] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0128] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C. The D90 particle size of the obtained S-metolachlor composition is 3 μm;
[0129] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0130] Comparative Example 2
[0131] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0132] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0133] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0134] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0135] The pH of the dispersant was 9.05.
[0136] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.5% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0137] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0138] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0139] The colloid is composed of magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.5% is composed of 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0140] The preparation method of the colloid comprises the following steps: adding magnesium aluminum silicate into ethylene glycol and mixing them to obtain the colloid.
[0141] The preservative is sodium benzoate.
[0142] The stabilizer is citric acid.
[0143] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0144] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0145] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0146] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0147] Comparative Example 3
[0148] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0149] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0150] The S-metolachlor composition consists of S-metolachlor, an emulsifier, xanthan gum, magnesium aluminum silicate, ethylene glycol, a preservative, a stabilizer and water.
[0151] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0152] The pH of the dispersant was 9.05.
[0153] Calculated by mass percentage, the S-isopropylamine composition consists of 59.38% of S-isopropylamine, 5.55% of emulsifier, 0.06% of xanthan gum, 0.5% of magnesium aluminum silicate, 4% of ethylene glycol, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0154] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0155] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0156] The preservative is sodium benzoate.
[0157] The stabilizer is citric acid.
[0158] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0159] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0160] S-metolachlor, an emulsifier, xanthan gum, magnesium aluminum silicate, ethylene glycol, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0161] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0162] Comparative Example 4
[0163] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0164] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0165] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0166] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0167] The pH of the dispersant was 9.05.
[0168] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.75% of stabilizer, and the balance of water; the water is deionized water.
[0169] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0170] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0171] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0172] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0173] The preservative is sodium benzoate.
[0174] The stabilizer is citric acid.
[0175] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0176] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0177] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0178] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0179] Comparative Example 5
[0180] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0181] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0182] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative and water.
[0183] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0184] The pH of the dispersant was 9.05.
[0185] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative and the balance of water; the water is deionized water.
[0186] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0187] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0188] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0189] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0190] The preservative is sodium benzoate.
[0191] The stabilizer is citric acid.
[0192] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0193] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0194] S-metolachlor, an emulsifier, a colloid, a preservative, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0195] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0196] Comparative Example 6
[0197] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0198] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0199] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0200] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0201] The pH of the dispersant was 9.05.
[0202] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0203] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0204] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0205] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0206] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0207] The preservative is sodium benzoate.
[0208] The stabilizer is sodium dihydrogen phosphate.
[0209] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0210] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0211] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0212] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0213] Comparative Example 7
[0214] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0215] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0216] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0217] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0218] The pH of the dispersant was 9.05.
[0219] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.5% of stabilizer, and the balance of water; the water is deionized water.
[0220] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0221] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0222] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0223] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0224] The preservative is sodium benzoate.
[0225] The stabilizer is sodium dihydrogen phosphate.
[0226] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0227] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0228] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0229] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0230] Comparative Example 8
[0231] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0232] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0233] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0234] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0235] The pH of the dispersant was 9.05.
[0236] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.75% of stabilizer, and the balance of water; the water is deionized water.
[0237] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0238] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0239] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0240] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0241] The preservative is sodium benzoate.
[0242] The stabilizer is sodium dihydrogen phosphate.
[0243] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0244] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0245] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0246] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0247] Comparative Example 9
[0248] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0249] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0250] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0251] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0252] The pH of the dispersant was 9.05.
[0253] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0254] The emulsifier consists of emulsifier A and emulsifier monomer B280, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B280.
[0255] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B280 is 6.1.
[0256] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0257] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0258] The preservative is sodium benzoate.
[0259] The stabilizer is citric acid.
[0260] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0261] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0262] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0263] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0264] Comparative Example 10
[0265] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0266] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0267] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0268] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0269] The pH of the dispersant was 9.05.
[0270] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 5.55% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0271] The emulsifier is composed of emulsifier A and emulsifier monomer 1602 , and the 5.55% emulsifier is composed of 4.8% emulsifier A and 0.75% emulsifier monomer 1602 .
[0272] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer 1602 is 5.8.
[0273] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0274] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0275] The preservative is sodium benzoate.
[0276] The stabilizer is citric acid.
[0277] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0278] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0279] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0280] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0281] Comparative Example 11
[0282] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0283] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0284] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0285] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0286] The pH of the dispersant was 9.05.
[0287] Calculated by mass percentage, the S-metolachlor composition consists of 59.38% of S-metolachlor, 4.8% of emulsifier, 4.56% of colloid, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0288] The emulsifier is emulsifier A.
[0289] The pH of the emulsifier A is 6.43.
[0290] The colloid is composed of xanthan gum, magnesium aluminum silicate and ethylene glycol. In terms of mass percentage, the colloid 4.56% is composed of 0.06% xanthan gum, 0.5% magnesium aluminum silicate and 4% ethylene glycol.
[0291] The preparation method of the colloid comprises the following steps: adding xanthan gum and magnesium aluminum silicate into ethylene glycol and mixing them to obtain a colloid; the appearance of the colloid is a transparent gel-like liquid.
[0292] The preservative is sodium benzoate.
[0293] The stabilizer is citric acid.
[0294] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0295] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0296] S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer, and water are mixed and sheared to obtain a S-metolachlor composition; the mixing and shearing is performed at a shearing speed of 10000 r / min, a shearing time of 3 min, and the mixing and shearing is performed at 23° C.;
[0297] The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide; the stirring time is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C.
[0298] Comparative Example 12
[0299] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0300] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0301] The S-metolachlor composition consists of S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
[0302] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0303] The pH of the dispersant was 9.05.
[0304] Calculated by mass percentage, the S-isopropylamine composition consists of 59.38% of S-isopropylamine, 5.55% of emulsifier, 0.06% of xanthan gum, 0.5% of magnesium aluminum silicate, 4% of ethylene glycol, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0305] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0306] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0307] The preservative is sodium benzoate.
[0308] The stabilizer is citric acid.
[0309] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0310] Calculated by mass percentage, the raw materials in the 16.67% tembotrione composition and the raw materials in the 83.33% S-metolachlor composition were directly put into a sand mill for sand grinding, and then subjected to high-speed shearing to obtain a tembotrione-containing herbicide.
[0311] The sand grinding was performed using a vertical sand mill with a sand grinding speed of 3000 r / min and a sand grinding time of 1 h.
[0312] The high-speed shearing adopts a shearing speed of 10000 r / min, a shearing time of 3 min, and the shearing operation is performed at 23°C.
[0313] Comparative Example 13
[0314] The first aspect of the present comparative example provides a tembotrione-containing herbicide, wherein the raw materials for its preparation include 16.67% of a tembotrione composition and 83.33% of a S-metolachlor composition, by mass percentage;
[0315] The tembotrione composition consists of tembotrione, chlorpyrifos, a dispersant and water;
[0316] The S-metolachlor composition consists of S-metolachlor, an emulsifier, xanthan gum, magnesium aluminum silicate, ethylene glycol, a preservative, a stabilizer and water.
[0317] In terms of mass percentage, the tembotrione composition comprises 18.46% of tembotrione, 17.45% of chlorpyrifos, 5.6% of dispersant and the balance of water; the water is deionized water.
[0318] The pH of the dispersant was 9.05.
[0319] Calculated by mass percentage, the S-isopropylamine composition consists of 59.38% of S-isopropylamine, 5.55% of emulsifier, 0.06% of xanthan gum, 0.5% of magnesium aluminum silicate, 4% of ethylene glycol, 0.3% of preservative, 0.25% of stabilizer, and the balance of water; the water is deionized water.
[0320] The emulsifier consists of emulsifier A and emulsifier monomer B, and the 5.55% emulsifier consists of 4.8% emulsifier A and 0.75% emulsifier monomer B.
[0321] The pH of the emulsifier A is 6.43; the pH of the emulsifier monomer B is 4.3.
[0322] The preservative is sodium benzoate.
[0323] The stabilizer is citric acid.
[0324] The second aspect of this comparative example provides a method for preparing a tembotrione-containing herbicide, comprising the following steps:
[0325] The tembotrione, chlorpyrifos, a dispersant and water are mixed and sand-milled to obtain a tembotrione composition; the sand-milling is performed using a vertical sand mill for 1 hour, and the sand-milling speed of the vertical sand mill is set to 3000 r / min; the D90 particle size of the tembotrione composition is 5 μm;
[0326] A cyclosulfuron composition, S-isopropylamine, an emulsifier, xanthan gum, magnesium aluminum silicate, ethylene glycol, a preservative, a stabilizer and water are stirred and mixed, and then sheared to obtain a cyclosulfuron-containing herbicide; the stirring time used in the stirring is 80 minutes, the stirring speed is 200 r / min, and the stirring temperature is 23°C; the shearing speed used in the shearing is 10000 r / min, the shearing time is 3 minutes, and the shearing operation is performed at 23°C.
[0327] Performance Testing
[0328] 1. Stability test:
[0329] The tembotrione-containing herbicides provided in Examples 1-3 and Comparative Examples 1-3 were subjected to a thermal storage stability test. The thermal storage condition was (54±2)°C for 14 days to observe whether water precipitation and bottom formation would occur. The test results are shown in Table 2. Figure 1 The bottoming state is shown in Figure 2 .
[0330] The tembotrione-containing herbicides provided in Examples 1-3 and Comparative Examples 1-3 were subjected to a high-speed centrifugation stability test. The high-speed centrifugation conditions were a centrifugal speed of 3000 r / min and a centrifugal time of 30 min to observe whether water precipitation would occur. The test results are shown in Table 2.
[0331] The tembotrione-containing herbicides provided in Examples 1-3 and Comparative Examples 1-3 were stored at (20±5)°C for 14 days for stability testing to observe whether water precipitation would occur. The test results are shown in Table 2.
[0332] The tembotrione-containing herbicides provided in Examples 1-3 and Comparative Examples 1-3 were subjected to a cold storage stability test. The cold storage condition was (0±2)°C for 7 days to observe whether water precipitation would occur. The test results are shown in Table 2.
[0333] If the amount of water precipitated is less than 5%, it will be evaluated as unqualified; if the amount of water precipitated is greater than or equal to 5%, it will be evaluated as unqualified.
[0334] The amount of precipitated water = the volume of precipitated water / the total volume of the sample*100% (the hot and cold storage laboratory uses a 30mL cylindrical glass screw bottle with a scale line; while the high-speed centrifugal stability test uses a centrifuge tube with a scale line. The amount of precipitated water can be quickly and accurately calculated.)
[0335] Table 2
[0336]
[0337] The test results in Table 2 show that the use of ethylene glycol to dissolve xanthan gum and mix with magnesium aluminum silicate to prepare a transparent gel-like liquid can improve the problem of water precipitation and bottoming of cyclohexane-containing herbicides during storage or at high speeds.
[0338] 2. Thermal storage decomposition rate and thermal storage appearance test:
[0339] The cyclohexane-containing herbicides provided in Examples 1-3 and Comparative Examples 4-8 were subjected to heat storage at (54±2)°C for 14 days to test the appearance changes of the cyclohexane-containing herbicides and whether oil separation and demulsification would occur. The heat storage decomposition rates of cyclohexane and S-isopropylamine in the cyclohexane-containing herbicides were recorded. The test results are shown in Table 3.
[0340] Table 3
[0341]
[0342] It can be seen from the test results in Table 3 that the use of a specific stabilizer can reduce the thermal decomposition rate of tampronil and S-isopropylamine and avoid the problem of demulsification.
[0343] The thermal storage test showed oil separation and demulsification. Figure 3 , Figure 4 , Figure 5 .
[0344] 3. Thermal storage test:
[0345] The cyclohexane-containing herbicides provided in Examples 1-3 and Comparative Examples 9-11 were heat stored at (54±2)°C for 14 days to test the appearance changes of the cyclohexane-containing herbicides and whether oil separation and demulsification problems would occur. The test results are shown in Table 4.
[0346] Table 4
[0347] Example Thermal storage test Comprehensive evaluation Example 1 No oil separation or demulsification qualified Example 2 No oil separation or demulsification qualified Example 3 No oil separation or demulsification qualified Comparative Example 9 Oil separation and demulsification Failure Comparative Example 10 Oil separation and demulsification Failure Comparative Example 11 Oil separation and demulsification Failure
[0348] It can be seen from the test results in Table 4 that the use of a specific emulsifier for coordination can avoid the problems of oil droplets and demulsification of cyclohexane-containing herbicides during hot storage.
[0349] The thermal storage test showed oil separation and demulsification. Figure 3 , Figure 4 , Figure 5
[0350] 4. Preparation process stability test:
[0351] The tembotrione-containing herbicide was prepared according to the preparation method of the tembotrione-containing herbicide provided in Examples 1-3 and Comparative Examples 12-13, and whether flocculation problem would occur during the preparation process was observed. The test results are shown in Table 5. The flocculation state is shown in Table 5. Figure 6 , Figure 7 .
[0352] Table 5
[0353] Example Preparation process stability test Comprehensive evaluation Example 1 No flocculation qualified Example 2 No flocculation qualified Example 3 No flocculation qualified Comparative Example 12 Flocculation occurs Failure Comparative Example 13 Flocculation occurs Failure
[0354] It can be seen from the test results in Table 5 that the preparation method defined in the present application can avoid the flocculation problem that may occur during the preparation of the tembotrione-containing herbicide.
Claims
1. A tembotrione-containing herbicide, characterized in that: The preparation raw materials include a tembotrione composition and a S-metolachlor composition; the mass ratio of the tembotrione composition to the S-metolachlor composition is 1:(4-6); The tembotrione composition comprises tembotrione, chlorpyrifos, a dispersant and water; The S-metolachlor composition comprises S-metolachlor, an emulsifier, a colloid, a preservative, a stabilizer and water.
2. The tembotrione-containing herbicide according to claim 1, characterized in that: Calculated by mass percentage, the tembotrione composition comprises 16%-20% of tembotrione, 15%-20% of chlorpyrifos, 4.8%-6.0% of dispersant and the balance of water.
3. The tembotrione-containing herbicide according to claim 1, characterized in that: Calculated by mass percentage, the S-metolachlor composition comprises 55%-65% of S-metolachlor, 5%-6% of emulsifier, 3.5%-6.75% of colloid, 0.1%-0.5% of preservative, 0.25%-0.5% of stabilizer, and the balance is water.
4. The tembotrione-containing herbicide according to claim 1, characterized in that: The colloid comprises xanthan gum, magnesium aluminum silicate and ethylene glycol, wherein the mass ratio of the xanthan gum to magnesium aluminum silicate is (0.1-0.75):1; the mass ratio of the total mass of the xanthan gum and magnesium aluminum silicate to ethylene glycol is (0.55-1.75):(3-5).
5. The tembotrione-containing herbicide according to claim 1, characterized in that: The stabilizer is an organic weak acid.
6. The tembotrione-containing herbicide according to claim 5, characterized in that: The organic weak acid includes citric acid.
7. The tembotrione-containing herbicide according to claim 1, characterized in that: The emulsifier comprises an emulsifier A and an emulsifier monomer B, and the mass ratio of the emulsifier A to the emulsifier monomer B is (4.5-5.0):(0.5-1).
8. The tembotrione-containing herbicide according to claim 1, characterized in that: The pH of the emulsifier A is 5-7; the pH of the emulsifier monomer B is 3-5.
9. A method for preparing a tembotrione-containing herbicide according to any one of claims 1 to 8, characterized in that: The following steps are involved: The tembotrione composition is added into the S-isopropylamine composition and stirred to obtain a tembotrione-containing herbicide.
10. The method for preparing a tembotrione-containing herbicide according to claim 9, wherein: The stirring time is 60-120 min, the stirring speed is 200-400 r / min, and the stirring temperature is 10-40° C.
Citation Information
Patent Citations
Compound preparation of corn field post-emergence herbicide and preparation method thereof
CN111436450A