Tricyclazole-containing suspending agent and preparation method thereof

Abstract

The invention discloses a tricyclazole-containing suspending agent and a preparation method thereof, and is applicable to the technical field of pesticide preparations. The suspending agent containing tricyclazole comprises the following components in percentage by mass: 40% of tricyclazole, 1%-10% of an anti-freezing agent, 1%-10% 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, 0.1%-1% of a pH regulator and the balance of water. The preparation method is simple, environment-friendly and low in cost, the carboxylate dispersing agent and the sulfate wetting dispersing agent of different structures are combined according to a certain proportion, a formula system is stable, increase of the grain size of tricyclazole is inhibited, a system sample does not have an obvious color changing phenomenon, and finally the problems of aging stability and stability of the product in the storage process are solved. The utilization rate is improved and the efficacy of the product is ensured.

Description

Technical Field

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

[0002] Tricyclazole (Tricyclazole) is an organic compound with a molecular formula of C9H7N3S, a molecular weight of 189.237, and white, odorless needle-shaped crystals. Tricyclazole is a special fungicide for the prevention and treatment of rice blast, belonging to the thiazole class. The fungicidal mechanism is mainly to inhibit the formation of melanin in the attached spores, thereby inhibiting the germination and formation of attached spores, preventing the invasion of pathogens and reducing the production of rice blast fungus spores. The pure product is white crystals with a melting point of 187-188 degrees Celsius. The industrial original drug is orange crystals. It is stable to water, light and heat, and has a lasting effect of 7-10 days. Saturated vapor pressure (kPa): 0.267×10-7 (25°C), solubility: slightly soluble in water, soluble in methanol, ethanol, dichloromethane, and easily soluble in chloroform and acetone.

[0003] Tricyclazole has strong systemic properties and can be quickly absorbed by the roots, stems and leaves of rice and transported to various parts of the rice plants. Generally, the amount of drug absorbed by the rice plants can reach saturation 2 hours after spraying.

[0004] Tricyclazole disease prevention is mainly based on prevention and protection, and it is most effective when used before the onset of disease. The specific operation of the spray method is as follows: for seedling blight control, 50-75 grams of 20% wettable powder per mu is sprayed with water at the 3-4 leaf stage of the seedlings or 5 days before transplanting; for leaf blight and ear neck blight control, 75-100 grams of 20% wettable powder per mu is sprayed with water when leaf blight first occurs or from the late stage of ear formation to the beginning of ear stage; when ear neck blight is serious, apply the medicine once again after an interval of 10-14 days.

[0005] At present, the maximum increase in particle size of similar products after hot storage is between 100% and 200%. High-content tricyclazole suspension concentrates have the problems of excessive water precipitation, bottoming, poor fluidity, increased viscosity, wall sticking, large particle size increase, severe color change of samples, and easy color difference from khaki to reddish brown during hot storage. Summary of the invention

[0006] The purpose of the present invention is to provide a suspension containing tricyclazole, which has a simple and environmentally friendly preparation method and a low cost, and a preparation method thereof, so as to improve the utilization rate, ensure the efficacy of the product, and solve the problems in the prior art.

[0007] To achieve the above object, the present invention provides the following technical solutions:

[0008] A suspension containing tricyclazole comprises the following components in percentage by mass: 40% of tricyclazole, 1%-10% of antifreeze agent, 1-10% 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, 0.1%-1% of pH regulator, and the balance is water.

[0009] Furthermore, the antifreeze agent is one or a combination of more than one of glycerol, propylene glycol, ethylene glycol and urea.

[0010] Furthermore, the dispersant is one or a combination of more than one of polycarboxylates, alkylnaphthalene sulfonates, sulfate anions, polymeric acidic dispersants, and polyoxyethylene ether phosphates.

[0011] 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.

[0012] 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, bentonite, and polymer compound FG.

[0013] Furthermore, the defoaming agent is one or a combination of more than one of an organosilicon defoaming agent, a mineral oil defoaming agent, and a polyether defoaming agent.

[0014] Furthermore, the preservative is one or a combination of more than one of kason, sodium benzoate, isothiazolin, benzoic acid and formaldehyde.

[0015] Furthermore, the pH adjuster is one or a combination of more than one of citric acid, tartaric acid, glacial acetic acid, lactic acid, triethanolamine, and phosphoric acid.

[0016] Furthermore, the water is deionized water.

[0017] A method for preparing a suspension containing tricyclazole comprises the following steps:

[0018] The tricyclazole technical, antifreeze agent, dispersant, wetting agent, thickener, defoamer, preservative, pH regulator and carrier water weighed in percentage by mass are stirred into a uniform slurry by wet sand milling, and the slurry is sand milled in three stages by a horizontal sand mill to obtain a suspension containing tricyclazole with a required particle size.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The preparation method of the invention is simple, environmentally friendly and low in cost. It aims to stabilize the formulation system by combining two carboxylate dispersants with different structures and a sulfate hydrochloride wetting dispersant in a certain proportion, inhibit the growth of tricyclazole particle size, inhibit the discoloration of the sample during hot storage and room temperature storage, and ultimately solve the time stability of the product during storage, improve the utilization rate and ensure the efficacy of the product. DETAILED DESCRIPTION

[0021] 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.

[0022] The suspending agent containing tricyclazole provided by the present invention has been subjected to long-term and multiple tests, and is described in detail below in conjunction with specific examples.

[0023] Embodiment 1 A suspension containing tricyclazole, the following weight percentage components are composed:

[0024]

[0025] According to the above formula, in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster 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 achieve the required particle size.

[0026] Embodiment 2 A kind of suspension containing tricyclazole, the following weight percentage components are composed:

[0027]

[0028] According to the above formula, in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster 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 achieve the required particle size.

[0029] Embodiment 3 A suspension containing tricyclazole, the following weight percentage components are composed:

[0030]

[0031]

[0032] According to the above formula, in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster 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 achieve the required particle size.

[0033] Embodiment 4 A suspension containing tricyclazole, the following weight percentage components are composed:

[0034]

[0035] According to the above formula, in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster 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 achieve the required particle size.

[0036] Comparative Example 1 A suspension containing tricyclazole, composed of the following components in percentage by weight:

[0037]

[0038] According to the above formula, in a dispersion tank with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster and carrier water are stirred and sheared into a uniform slurry by wet sand milling, and the product particle size reaches the requirement through three-stage circulation sand milling by a horizontal sand mill.

[0039] Comparative Example 2 A suspension containing tricyclazole, composed of the following components in percentage by weight:

[0040]

[0041] According to the above formula, in a dispersion tank equipped with a high-speed stirrer, prothioconazole, tebuconazole technical, antifreeze, dispersant, wetting agent, thickener, defoamer, preservative, pH adjuster 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 achieve the required particle size.

[0042] Sample flow states of the suspensions of Examples 1-6 (including the control group) of the present invention during hot storage at 54° C. or after cold storage.

[0043] 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.

[0044] 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.

[0045] The particle size analyzer uses the OMEC LS-909 laser particle size analyzer, and the particle size is tested by the fully automatic detection method. The test items and test results are shown in Table 1 below:

[0046] Table 1 Particle size test items and results

[0047]

[0048]

[0049] 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 sticking, internal agglomeration, etc.

[0050] As shown in Table 1, in Examples 1 to 4 of the present invention, two carboxylate dispersants with different structures and sulfate wetting dispersants are combined in a certain proportion to stabilize the formulation system and inhibit the growth of tricyclazole particle size. The growth rates of the particle size after 14 days of hot storage are 0.3%, 0.8%, 1.3%, and 0.7%, respectively, and the color of the hot storage samples is normal. The growth rates of the tricyclazole particle size in Comparative Examples 1-2 are 2.4% and 135.3%, respectively, and the color of the hot storage samples is severely discolored, which shows that Comparative Examples 1- The dispersant combination of 2 has a poor ability to inhibit the growth of tricyclazole particle size. For the combination of comparative examples 1-2, there are phenomena such as excessive water precipitation, bottoming or paste formation, poor fluidity, increased viscosity, wall adhesion, and excessive particle size growth. The present invention can effectively solve the above-mentioned quality degradation problem. The particle size increases by 0.3%-2% after 14 days of hot storage. The formulation system is stable, effectively inhibits the growth of tricyclazole particle size, and inhibits the discoloration of the sample during hot storage and room temperature storage. Ultimately, the time-dependent stability of the product during storage is solved, the utilization rate is improved, and the efficacy of the product is guaranteed.

[0051] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A suspension concentrate containing tricyclazole, characterized in that: The invention comprises the following components in percentage by mass: 40% of tricyclazole, 1%-10% of antifreeze agent, 1-10% 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, 0.1%-1% of pH regulator, and the balance is water.

2. A suspending agent containing tricyclazole according to claim 1, characterized in that, The antifreeze agent is one or a combination of glycerol, propylene glycol, ethylene glycol and urea.

3. A suspending agent containing tricyclazole according to claim 1, characterized in that, The dispersant is one or a combination of polycarboxylates, alkylnaphthalene sulfonates, sulfate anions, polymeric acidic dispersants, and polyoxyethylene ether phosphates.

4. A suspending agent containing tricyclazole according to 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. A suspending agent containing tricyclazole according to claim 1, characterized in that, The thickener is one or a combination of the polymer compound LT-908, carboxyalkyl cellulose, magnesium aluminum silicate, xanthan gum, bentonite, and polymer compound FG.

6. A suspending agent containing tricyclazole according to claim 1, characterized in that, The defoaming agent is one or a combination of silicone defoaming agents, mineral oil defoaming agents, and polyether defoaming agents.

7. A suspending agent containing tricyclazole according to claim 1, characterized in that, The preservative is one or a combination of more than one of kason, sodium benzoate, isothiazolin, benzoic acid and formaldehyde.

8. A suspending agent containing tricyclazole according to claim 1, characterized in that, The pH adjuster is one or a combination of citric acid, tartaric acid, glacial acetic acid, lactic acid, triethanolamine, and phosphoric acid.

9. A suspending agent containing tricyclazole according to claim 1, characterized in that, The water is deionized water.

10. A preparation method for preparing the suspension concentrate containing tricyclazole according to any one of claims 1 to 9, characterized in that: The steps include: The tricyclazole technical, antifreeze agent, dispersant, wetting agent, thickener, defoamer, preservative, pH regulator and carrier water weighed in percentage by mass are stirred into a uniform slurry by wet sand milling, and the slurry is sand milled in three stages by a horizontal sand mill to obtain a suspension containing tricyclazole with a required particle size.

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