Suspending agent containing prothioconazole and preparation method thereof

Abstract

The invention discloses a suspending agent containing prothioconazole and a preparation method of the suspending agent. The suspending agent is prepared from the following components in percentage by mass: 20% of prothioconazole, 20% of tebuconazole, 1%-5% of an anti-freezing agent, 1%-15% of a dispersing agent, 0.1%-5% of a wetting agent, 0.1%-5% of a thickening agent, 0.2%-1.5% of a defoaming agent, 0.05%-0.9% of a preservative and the balance of water. The preparation method is simple, environment-friendly and low in cost, two carboxylate dispersants with different structures and two special sulfonate wetting dispersants with different structures are combined according to a certain proportion, a formula system is stable, when the 40% prothioconazole tebuconazole suspending agent and the 10% monopotassium phosphate solution are subjected to barrel mixing in a flight prevention scene, the stability of the emulsion is qualified, and the stability of the emulsion is good. When the prothioconazole tebuconazole suspending agent is used together with high-concentration monopotassium phosphate, time and labor are saved, precious water resources are saved, the expected purpose is achieved, the flocculation problem generated when the prothioconazole tebuconazole suspending agent and a high-salt solution are mixed in a barrel is effectively solved, and finally water, time and labor are saved, sterilization is achieved, and fertility is increased.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide preparations, in particular to a suspension concentrate containing prothioconazole and a preparation method thereof. Background Art

[0002] Prothioconazole chemical formula: C14H15Cl 2N3OS, solubility in water (20℃): 0.005g / L (pH4), 0.3g / L (pH8), 2.0g / L (pH9). Solubility in organic solvents (20℃): n-heptane <0.1g / L, xylene 8g / L, n-octanol 58g / L, acetonitrile 69g / L, isopropanol 87g / L, dichloromethane 88g / L, dimethyl sulfoxide 126g / L, acetone, ethyl acetate and polyethylene glycol are all >250g / L. It is stable at room temperature and stable to hydrolysis at pH 4-9. Prothioconazole is mainly used to control many diseases of cereal crops such as wheat, barley, rapeseed, peanuts, rice and legumes. It has a good control effect on almost all wheat diseases, such as powdery mildew, sheath blight, wilt, leaf spot, rust, sclerotinia, web spot, and moire of wheat and barley. It can also control soil-borne diseases of rapeseed and peanuts, such as sclerotinia, and major foliar diseases, such as gray mold, black spot, brown spot, black shank, sclerotinia, and rust.

[0003] Tebuconazole belongs to the triazole fungicide and is a thiol demethylation inhibitor. Its chemical formula is C16H22Cl N3O. Its solubility in water (20℃) is 32mg / L and in toluene is 50-100g / L. It can effectively prevent and treat various rusts, powdery mildew, web blotch, root rot, head blight, smut, seed-borne ring spot, tea cake disease, banana leaf spot, etc. of cereal crops. It is an inhibitor of ergosterol biosynthesis. It can be used to prevent and treat diseases caused by powdery mildew, rust, spore, pyrocoel and Septoria in cereal crops.

[0004] The commercially available combination containing prothioconazole has serious problems such as flocculation when mixed in a barrel with a high-concentration potassium dihydrogen phosphate solution, clogging the nozzle during spraying and making it unusable, and increased viscosity of samples when stored for a long time at room temperature. Summary of the invention

[0005] The invention aims to provide a suspension containing prothioconazole and a preparation method thereof. The preparation method is simple, environmentally friendly and low in cost. Two carboxylate dispersants with different structures and two special sulfonate wetting dispersants with different structures are combined in a certain proportion to make the formula system stable. When the suspension is mixed with a 10% potassium dihydrogen phosphate solution in a tank, the emulsion stability is qualified, and the flocculation problem when the prothioconazole tebuconazole suspension is mixed with a high-salt solution in a tank can be effectively solved. The suspension can save water, time and labor, and sterilize and increase fertility, so as to solve the problems raised in the above-mentioned background technology.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] The suspension containing prothioconazole contains the following components in percentage by mass: 20% of prothioconazole, 20% of tebuconazole, 1%-5% of antifreeze agent, 1-15% of dispersant, 0.1%-5% of wetting agent, 0.1%-5% of thickener, 0.2%-1.5% of defoamer, 0.05%-0.9% of preservative, and the balance is water.

[0008] Furthermore, the antifreeze agent is one or a combination of more than one of glycerol, propylene glycol, ethylene glycol and urea.

[0009] Furthermore, the dispersant is one or a combination of more than one of polycarboxylates, alkylnaphthalene sulfonates, sulfate anions, polymeric acidic dispersants, lignin sulfonates, and polyoxyethylene ether phosphates.

[0010] Furthermore, the wetting agent is one or a combination of more than one of fatty alcohol polyoxyethylene ether, EO / PO block copolymer and fatty alcohol polyoxyethylene ether sulfate.

[0011] Furthermore, the thickener is one or a combination of more than one of the polymer compound LT-908, carboxyalkyl cellulose, magnesium aluminum silicate, xanthan gum, and bentonite.

[0012] Furthermore, the defoaming agent is one or a combination of more than one of an organosilicon defoaming agent, a mineral oil, and a polyether defoaming agent.

[0013] Furthermore, the preservative is one or a combination of more than one of kason, sodium benzoate, isothiazolin, benzoic acid, formaldehyde, and polyhydroxypropyl benzoate of sorbic acid.

[0014] Furthermore, the preparation method of the suspension containing prothioconazole comprises the following steps:

[0015] Prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred into a uniform slurry by wet sand milling, and then the slurry is sand milled in three stages by a horizontal sand mill to obtain a suspension with a required particle size.

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] The preparation method of the present invention is simple, environmentally friendly, and has low cost. It aims to stabilize the formula system by combining two carboxylate dispersants with different structures and two special sulfonate wetting dispersants with different structures in a certain proportion. When 40% of prothioconazole tebuconazole suspension and 10% potassium dihydrogen phosphate solution are barrel mixed in the aerial spraying scenario, the emulsion stability is qualified, and it can be used together with high-concentration potassium dihydrogen phosphate to save time and labor, save precious water resources, and achieve the expected purpose. The flocculation problem when the prothioconazole tebuconazole suspension is barrel mixed with a high-content potassium dihydrogen phosphate solution can be effectively solved, water can be saved, time and labor can be saved, sterilization and fertility can be increased at the same time, and research in this regard is of great significance, and ultimately the utilization rate can be improved to ensure the efficacy of the product. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] Example 1: A suspension containing prothioconazole, comprising the following components in percentage by weight:

[0020]

[0021]

[0022] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0023] Example 2 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0024]

[0025] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0026] Example 3 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0027]

[0028]

[0029] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0030] Example 4 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0031]

[0032] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0033] Example 5 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0034]

[0035] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0036] Example 6 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0037]

[0038]

[0039] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0040] Example 7 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0041]

[0042] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0043] Example 8 The suspension containing prothioconazole is composed of the following components in percentage by weight:

[0044]

[0045] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0046] Comparative Example 1 contains a suspension concentrate of prothioconazole, which is composed of the following components in percentage by weight:

[0047]

[0048]

[0049] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0050] Comparative Example 2 contains a suspension concentrate of prothioconazole, which has the following components in percentage by weight:

[0051]

[0052] According to the above formula, the raw material components are weighed, and in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and then the slurry is sand milled by three-stage circulation of a horizontal sand mill to make the product particle size meet the requirements.

[0053] Sample flow states of the suspensions of Examples 1-8 of the present invention and Comparative Examples 1-2 during hot storage at 54° C. or after cold storage.

[0054] The thermal storage stability test shall be carried out in accordance with the provisions of GB / T 19136-2021, and the dispersion stability indicators shall meet the standard requirements.

[0055] The low temperature stability test is carried out in accordance with the provisions of GB / T 19137-2003. The dispersion stability index is qualified if it meets the standard requirements.

[0056] In the flying pest control barrel mix experiment, 40% prothioconazole tebuconazole SC and 10% potassium dihydrogen phosphate solution were mixed at a ratio of 4:100 and left at room temperature for 1 hour before observation.

[0057] Table 1

[0058]

[0059]

[0060] (Note 1. The hot storage samples in the table are stored at 54℃ for 14 days, 2. The low temperature stability is stored at 0℃ for 7 days, 3. The unqualified hot storage samples have the following phenomena: excessive water precipitation, bottoming, paste, poor fluidity, increased viscosity, wall adhesion, internal agglomeration, etc.)

[0061] As shown in Table 1, in Example 1 and Example 3-5, two carboxylate dispersants with different structures and two sulfonate wetting dispersants with different structures are combined in a certain proportion to stabilize the formula system. When the flying defense is mixed with 10% potassium dihydrogen phosphate solution, the emulsion stability is qualified, and it is used together with a high concentration of potassium dihydrogen phosphate solution to save time and effort, save precious water resources and achieve the desired purpose. The flying defense and 10% potassium dihydrogen phosphate solution barrel mix meet the requirements and the thermal storage stability meets the requirements. Although there is flocculation in the flying defense and 10% potassium dihydrogen phosphate solution barrel mix in Example 2, the thermal storage stability meets the requirements. There is flocculation and unqualified thermal storage stability in the examples 6-8 and the comparison examples 1-2. This shows that the present invention can effectively solve the above-mentioned quality deterioration problem, effectively solve the flocculation problem when 40% prothioconazole tebuconazole suspension is mixed with a high salt solution, and finally save water, save time and effort, sterilize and increase fertility at the same time, so it is of great practical value to study this aspect.

[0062] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A suspension concentrate containing prothioconazole, characterized in that: The invention contains the following components in percentage by mass: 20% of prothioconazole, 20% of tebuconazole, 1%-5% of antifreeze agent, 1-15% of dispersant, 0.1%-5% of wetting agent, 0.1%-5% of thickener, 0.2%-1.5% of defoamer, 0.05%-0.9% of preservative, and the balance is water.

2. The suspending agent containing prothioconazole as claimed in claim 1, characterized in that The antifreeze agent is one or a combination of glycerol, propylene glycol, ethylene glycol and urea.

3. The suspending agent containing prothioconazole as claimed in claim 1, characterized in that The dispersant is one or a combination of polycarboxylates, alkylnaphthalene sulfonates, sulfate anions, polymeric acidic dispersants, lignin sulfonates, and polyoxyethylene ether phosphates.

4. The suspending agent containing prothioconazole as claimed in claim 1, characterized in that The wetting agent is one or a combination of more than one of fatty alcohol polyoxyethylene ether, EO / PO block copolymer and fatty alcohol polyoxyethylene ether sulfate.

5. The suspension concentrate containing prothioconazole as claimed in claim 1, characterized in that The thickener is one or a combination of more than one of the polymer compound LT-908, carboxyalkyl cellulose, magnesium aluminum silicate, xanthan gum and bentonite.

6. The suspension concentrate containing prothioconazole as claimed in claim 1, characterized in that The defoaming agent is one or a combination of silicone defoaming agent, mineral oil, polyether defoaming agent.

7. The suspension concentrate containing prothioconazole as claimed in claim 1, characterized in that The preservative is one or a combination of more than one of kason, sodium benzoate, isothiazolin, benzoic acid, formaldehyde, and polyhydroxypropyl benzoate of sorbic acid.

8. A method for preparing a suspension concentrate containing prothioconazole, for preparing the suspension concentrate containing prothioconazole according to claim 1, characterized in that: Here are the steps: Prothioconazole, tebuconazole technical, antifreeze, dispersant, thickener, defoamer, preservative and carrier water are stirred into a uniform slurry by wet sand milling, and then the slurry is sand milled in three stages by a horizontal sand mill to obtain a suspension with a required particle size.

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