Microcapsule suspension-suspending agent containing clomazone and sulfentrazone as well as preparation method and application of microcapsule suspension-suspending agent

Abstract

The invention discloses a microcapsule suspension-suspending agent containing clomazone and sulfentrazone as well as a preparation method and application of the microcapsule suspension-suspending agent, and relates to the field of pesticides, the microcapsule suspension-suspending agent is prepared by mixing a clomazone microcapsule suspending agent and a sulfentrazone suspending agent according to a mass ratio of 1: (0.1-10); the clomazone microcapsule suspending agent comprises the following raw materials in parts by weight: 5-50 parts of clomazone, 2-10 parts of solvent oil, 0.4-5 parts of an oil phase wall material, 1-8 parts of a dispersing agent, 0.1-1 part of a water phase wall material, 25-80 parts of water and the like. The sulfentrazone suspending agent comprises the following raw materials in parts by weight: 5-50 parts of sulfentrazone, 1-8 parts of a dispersing agent, 45-96 parts of water and the like. The dispersing agent is at least one of sodium lignin sulfonate and polycarboxylate. On the premise that the clomazone and the sulfentrazone are compounded, the clomazone and the sulfentrazone can stably exist after being mixed, and meanwhile the defect of drifting phytotoxicity of the clomazone in use is overcome.

Description

Technical Field

[0001] The present invention relates to the technical field of pesticides, and in particular to a microcapsule suspension-suspension concentrate containing clomazone and sulfentrazone, and a preparation method and application thereof. Background Art

[0002] Microcapsule suspension is a new type of preparation that uses polymer film materials as wall materials to encapsulate the active ingredients of pesticides in a core-shell structure and evenly disperses the structure in water. The presence of the capsule wall, on the one hand, reduces the toxicity to non-target organisms, prolongs the efficacy, masks the unpleasant odor of most pesticides, and facilitates the use and cleaning of colored pesticides such as dimethoate, reduces the irritation of pesticides to applicators, and improves the distribution of pesticides in the soil. The use of special capsule wall materials can also achieve precise release of rapid release, sustained release, and controlled release to improve the utilization rate of pesticides and give pesticides some new ways of use. On the other hand, the presence of the capsule shell reduces the stability of the external environment, including the stability of the preparation before and after medication, and the environmental stability, making it possible to combine pesticides that cannot be compounded. Subsequently, microcapsule suspension-suspension concentrates, microcapsule suspension-water emulsions, microcapsule suspension-suspoemulsions, wettable powders based on spray drying technology, and water-dispersible granules and other dosage forms were derived.

[0003] At present, as a new herbicide, sulfentrazone herbicide has broad market prospects.

[0004] Sulfentrazone is a triazolinone herbicide developed by FMC. Sulfentrazone is a protoporphyrinogen oxidase inhibitor. Its mechanism of action is to inhibit protoporphyrinogen oxidase in the process of chlorophyll biosynthesis, causing cell membrane damage, causing leaves to dry up and die quickly. It has a good control effect on weeds that germinate in the soil before emergence.

[0005] Sulfonamide can effectively control most annual broadleaf weeds, grass and sedge weeds, such as morning glory, Amaranthus retroflexus, Amaranthus ferox, Chenopodium album, Datura, Polygonum pennsylvanicum, Digitaria, Setaria viridis, Xanthium sibiricum, Goosegrass, Cyperus oleifera, Cyperus rotundus, etc. It is effective against morning glory, Chenopodium album, Xanthium sibiricum, Cyperus rotundus, etc., which are difficult to control at present. Suitable crops include soybean, corn, sorghum, peanut, sunflower, etc. It has a long residual effect in the soil, with a half-life of 110 to 280 days. It is safe for the next crop of cereals, but has certain phytotoxicity to cotton and sugar beets.

[0006] Clomazone is a carotenoid biosynthesis inhibitor, with an unknown specific target enzyme. It is a selective pre-emergence herbicide. It inhibits the biosynthesis of carotene and chlorophyll by inhibiting the synthesis of pentadiene compounds. After the roots and young shoots of weeds absorb the agent, it is conducted upward and diffused to the leaves through the xylem, inhibiting the synthesis of weed pigments and causing them to whiten. This prevents the weeds from producing nutrients through photosynthesis, and eventually they die due to nutrient depletion. Soybeans have a specific metabolic effect that turns them into metabolites that have no weed effect and are selective and have a moderate degree of adhesion to the soil. They are mainly biodegraded by microorganisms in the soil. Sandy soils are more effective in rainy conditions, or when the temperature is low and the soil humidity is high. Clomazone has a wide spectrum of weed control and can control a variety of annual grass weeds and broad-leaved weeds.

[0007] After crops such as soybeans and sugarcane absorb the drug, they undergo a special metabolic process, converting the active ingredients of clomazone into non-toxic degradation products, making it safe. Clomazone is mainly used to control annual grass and leaf weeds such as barnyard grass, goosegrass, ramie, wilt, cocklebur, crabgrass, foxtail grass, ragweed, elsholtzia, water spiny needles, wild watermelon seedlings, quinoa, bluegrass, willow-leaf polygonum, sorrel-leaf polygonum, purslane, wolfsbane, Bidens pilosa, Commelina, etc. It also has a strong inhibitory effect on perennial thorns, thistle, sonchus, and horsetail. Soil treatment before and after sowing soybeans in soybean fields, or early stem and leaf treatment after seedlings. Clomazone has a long lasting effect, and a high dosage of more than 53g per mu not only has a good weed control effect, but also has a significant effect on promoting growth and increasing yields of soybeans. However, soybeans must continue to be planted in the second year, which has an impact on other crops. Similarly, soybeans are highly resistant to clomazone and have high selectivity, making it an optional agent for weed control in soybean fields.

[0008] Sulfonamide and isothiocarb have overlapping applicable crops and herbicidal spectra and can be used as combination agents, which is expected to achieve the purpose of synergistic enhancement.

[0009] However, the mixing of clomazone and sulfentrazone is currently mostly in the research and development stage, and there is no report on the combined microcapsule suspension-suspension concentrate of clomazone and sulfentrazone. The inventors analyzed that it may be because sulfentrazone has a large solubility in organic solvents, clomazone has a low vapor pressure and a low melting point. The preparation of microcapsule suspension-suspension concentrates can easily lead to Ostwald ripening of sulfentrazone, poor thermal storage stability, and great difficulty in development, which greatly increases the difficulty of preparing the combined microcapsule suspension-suspension concentrate of clomazone and sulfentrazone. Summary of the invention

[0010] Purpose of the Invention

[0011] In order to overcome the above-mentioned shortcomings, the purpose of the present invention is to provide a microcapsule suspension-suspension concentrate containing isocyanate and sulfentrazone, and a preparation method and application thereof. The present invention can provide a preparation process for a microcapsule suspension-suspension concentrate of isocyanate and sulfentrazone with stable quality. The process flow is simple, the equipment requirements are low, the industrialization is simple, and the market is broad.

[0012] Solution

[0013] To achieve the purpose of the present invention, the technical solution adopted by the present invention is as follows:

[0014] In a first aspect, the present invention provides a microcapsule suspension-suspension concentrate containing clomazone and sulfentrazone, comprising a mixture of a clomazone microcapsule suspension concentrate and a sulfentrazone suspension concentrate in a mass ratio of 1: (0.1-10); wherein,

[0015] The clomazone microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts by weight of clomazone, 2-10 parts by weight of solvent oil, 0.4-5 parts by weight of oil phase wall material, 1-8 parts by weight of dispersant, 0-5 parts by weight of thickener, 0-10 parts by weight of preservative, 0-5 parts by weight of antifreeze agent, 0.1-1 parts by weight of water phase wall material, 0-5 parts by weight of specific gravity regulator, 0-1 parts by weight of preservative and 25-80 parts by weight of water;

[0016] The sulfentrazone suspension comprises the following raw materials in parts by weight: 5 to 50 parts by weight of sulfentrazone, 1 to 8 parts by weight of a dispersant, 0 to 5 parts by weight of an antifreeze agent, and 45 to 96 parts by weight of water;

[0017] In the clomazone microcapsule suspension and / or sulfentrazone suspension, the dispersant is at least one of sodium lignin sulfonate and polycarboxylate.

[0018] Further, it comprises a mixture of a clomazone microcapsule suspension and a sulfentrazone suspension in a mass ratio of 1:(0.5-10), optionally in a mass ratio of 1:(0.5-9), optionally in a mass ratio of 1:(1-9);

[0019] And / or, the weight ratio of clomazone to sulfentrazone is (1-7):(1-40), optionally (1-7):

[0020] (1~9), optionally (1~2): (1~4).

[0021] Furthermore, the clomazone microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts by weight of clomazone, 2-10 parts by weight of solvent oil, 0.4-5 parts by weight of oil phase wall material, 1-6 parts by weight of polycarboxylate, 0-4 parts by weight of sodium lignin sulfonate, 0-5 parts by weight of thickener, 0-10 parts by weight of preservative, 0-5 parts by weight of antifreeze agent, 0.1-1 parts by weight of water phase wall material, 0-5 parts by weight of specific gravity regulator, 0-1 parts by weight of preservative and 25-80 parts by weight of water;

[0022] And / or, the sulfentrazone suspension concentrate comprises the following raw materials in parts by weight: 5 to 50 parts by weight of sulfentrazone, 1 to 6 parts by weight of polycarboxylate, 0 to 4 parts by weight of sodium lignin sulfonate, 0 to 5 parts by weight of antifreeze agent and 45 to 96 parts by weight of water;

[0023] And / or, in the clomazone microcapsule suspension and / or the sulfentrazone suspension, the mass fraction of polycarboxylate and sodium lignin sulfonate is ≤8%.

[0024] Furthermore, in the clomazone microcapsule suspension, the weight ratio of clomazone to the oil phase wall material is 1:(0.05-0.5), optionally 1:(0.08-0.5), optionally 1:(0.08-0.2).

[0025] Furthermore, in the clomazone microcapsule suspension, the clomazone is 5 to 45 parts by weight, and optionally 17 to 40 parts by weight (when the proportion of clomazone in the clomazone microcapsule suspension is 17 to 40%, it is a more suitable concentration).

[0026] and / or, in the clomazone microcapsule suspension, the dispersant is 3 to 8 parts by weight, optionally 4 to 6 parts by weight; optionally, the mass fraction of the dispersant is ≤ 8%;

[0027] and / or, in the clomazone microcapsule suspension, the oily wall material is 3-5%, optionally 3-4.5%,

[0028] And / or, in the clomazone microcapsule suspension, the oily wall material is aromatic isocyanate and its modified product; optionally, the oily wall material is selected from one or more of MDI, HDI, TDI, and IPDI;

[0029] and / or, in the clomazone microcapsule suspension, the aqueous wall material is 0.1 to 1.0 parts by weight;

[0030] And / or, in the clomazone microcapsule suspension, the aqueous phase wall material is a polyamine, and the aqueous phase wall material can be selected from one or more of hexamethylenediamine, triethylenetetramine, and tetraethylenepentamine.

[0031] Furthermore, in the clomazone microcapsule suspension, the solvent oil is 3 to 10 parts by weight, and optionally 3 to 5 parts by weight;

[0032] And / or, in the clomazone microcapsule suspension, the solvent is one or more of solvent oil 100#, solvent oil 150#, and solvent oil 200#;

[0033] and / or, in the clomazone microcapsule suspension, the thickener is 0.05 to 0.1 parts by weight;

[0034] and / or, in the clomazone microcapsule suspension, the thickener is xanthan gum;

[0035] and / or, in the clomazone microcapsule suspension, the preservative is 0.1 to 0.2 parts by weight;

[0036] and / or, in the clomazone microcapsule suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone;

[0037] and / or, in the clomazone microcapsule suspension, the specific gravity regulator is 3 to 5 parts by weight;

[0038] and / or, in the clomazone microcapsule suspension, the specific gravity regulator is anhydrous calcium chloride;

[0039] and / or, in the clomazone microcapsule suspension, the antifreeze agent is ethylene glycol;

[0040] And / or, the clomazone microcapsule suspension is supplemented with water to make up to 100 parts by weight.

[0041] Further, in the sulfentrazone aqueous suspension, sulfentrazone is 20 to 50 parts by weight, optionally 30 to 40 parts by weight;

[0042] and / or, in the aqueous suspension of sulfentrazone, the thickener is 0.05 to 0.1 parts by weight;

[0043] and / or, in the aqueous suspension of sulfentrazone, the thickener is xanthan gum;

[0044] and / or, in the aqueous suspension of sulfentrazone, the preservative is 0.1 to 0.2 parts by weight;

[0045] and / or, in the sulfentrazone aqueous suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone;

[0046] And / or, the antifreeze agent is 1 to 3% in the sulfentrazone aqueous suspension.

[0047] and / or, in the aqueous suspension of sulfentrazone, the antifreeze agent is ethylene glycol;

[0048] And / or, the sulfentrazone aqueous suspension concentrate is supplemented with water to make up to 100 parts by weight.

[0049] In a second aspect, a method for preparing the microcapsule suspension-suspension concentrate according to the first aspect is provided, characterized in that the method comprises the following steps:

[0050] 1) Preparation of clomazone microcapsule suspension:

[0051] The isothiocarb, solvent and oil phase wall material are mixed to form the oil phase;

[0052] Mixing a dispersant, a thickener and water as a water phase;

[0053] The oil phase is transferred into the water phase, and the emulsion is obtained by high-speed shearing and emulsification, and the water phase wall material is added and stirred continuously, and a specific gravity regulator and / or a preservative are added as required to obtain a clomazone microcapsule suspension; optionally, after adding tetraethylenepentamine, the emulsion is heated to 50-60° C. and then a specific gravity regulator and / or a preservative are added as required;

[0054] 2) Preparation of sulfentrazone aqueous suspension:

[0055] The terbuthiuron, dispersant, thickener, preservative, antifreeze agent and water are mixed and wet-grinded to a target particle size to obtain a sulfentrazone aqueous suspension;

[0056] 3) The materials of step 1) and step 2) are mixed to prepare a microcapsule suspension-suspension concentrate.

[0057] In a third aspect, there is provided an application of the microcapsule suspension-suspension concentrate described in the first aspect, or the microcapsule suspension-suspension concentrate prepared by the preparation method described in the second aspect, in controlling weeds in farmland before crop planting, before emergence after sowing, or during the crop growth period.

[0058] Further, the weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of Goosegrass, Digitaria, Chenopodium album, and Amaranthus retroflexus.

[0059] Beneficial Effects

[0060] (1) The present invention can provide a clomazone and sulfentrazone compounded microcapsule suspension-suspension concentrate with stable quality through the selection of auxiliary agents, with a simple preparation process, low equipment requirements, simple industrialization, and a broad market. The present invention can ensure that clomazone and sulfentrazone are compounded, and the two can be stably present after mixing, while solving the problem of drift phytotoxicity of clomazone during use.

[0061] (2) The advantages of the present invention include: ① the raw materials are common, and the purchase, storage and use are convenient and safe; ② the process operation is simple, and capsules can be formed in one step; ③ the difference between product batches is small, the stability is good, and the later storage stability is good; ④ after a large number of experiments, the auxiliary agent is screened to obtain a stable formulation and its product. The highlighted creativity is that the auxiliary agent selection of the sulfentrazone aqueous suspension must be consistent with the auxiliary agent system of the clomazone microcapsule suspension or the type of auxiliary agent used is selected from the auxiliary agent system of the clomazone microcapsule suspension. DETAILED DESCRIPTION

[0062] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are 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.

[0063] In addition, in order to better illustrate the present invention, numerous specific details are provided in the specific embodiments below. It should be understood by those skilled in the art that the present invention can be implemented without certain specific details. In some embodiments, raw materials, schemes, methods, means, etc. well known to those skilled in the art are not described in detail, so as to highlight the main purpose of the present invention.

[0064] Unless explicitly stated otherwise, throughout the specification and claims, the term “comprise” or variations such as “include” or “comprising”, etc., will be understood to include the stated elements or components but not to exclude other elements or components.

[0065] The above-mentioned fungicidal composition provides a new option for controlling weeds. The present disclosure is further illustrated by examples below, but the present disclosure is not limited thereto.

[0066] The clomazone and sulfentrazone compounded microcapsule suspension-suspension concentrate and the preparation method thereof of the present invention use a single-layer interface method to microencapsulate clomazone, and the required raw materials include: solvent, oil phase wall material, dispersant, thickener, preservative, specific gravity regulator, water phase wall material, etc. The present invention has been found through continuous research and development that the use of emulsifiers (generally commonly used additives in microcapsule suspension preparation) is abandoned in the auxiliary agent system, and only sodium lignin sulfonate and polycarboxylate are used as dispersants, and the dispersant system is used as an optional system for the sulfentrazone aqueous suspension concentrate, which can ensure that clomazone and sulfentrazone can be stably present after mixing under the premise of compounding, and at the same time solve the problem of drift phytotoxicity of clomazone during use.

[0067] In the following examples, clomazone and sulfentrazone are both commercially available, and other adjuvants are also commercially available products.

[0068] The present invention is further described in detail below by way of examples.

[0069] Example 1 (the weight ratio of clomazone to sulfentrazone is 1:1)

[0070] Preparation of (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0071] (I) Preparation of 35% Clomazone Microcapsule Suspension

[0072] A. Dissolve 36.46% clomazone technical (clomazone content 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0073] B. Take 5% polycarboxylate, 0.05% xanthan gum and 46.04% water and mix them evenly under shear homogenization conditions as the water phase for later use;

[0074] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.35% hexamethylenediamine and continue stirring;

[0075] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0076] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 35% clomazone microcapsule suspension. Discharge the material and set aside.

[0077] (II) Preparation of 35% sulfentrazone aqueous suspension

[0078] F. 36.84% sulfentrazone technical (including sulfentrazone content of 95%), 5% polycarboxylate, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water are put into the preparation apparatus and dispersed evenly.

[0079] G. The material system is ground to a target particle size using a wet grinding process to obtain a 35% sulfentrazone aqueous suspension.

[0080] H. Pass the 35% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0081] (III) Mixed (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate

[0082] I. The 35% clomazone microcapsule suspension prepared in step (i) and the 35% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a mass ratio of 1:1, and stirred evenly to obtain a (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0083] Example 2 (the weight ratio of clomazone to sulfentrazone is 2:1)

[0084] Preparation of (20% clomazone + 10% sulfentrazone) microcapsule suspension-suspension concentrate.

[0085] (I) Preparation of 30% Clomazone Microcapsule Suspension

[0086] A. Dissolve 31.25% clomazone technical (clomazone content 96%) in 5% solvent oil #100, then add 3% MDI and mix well to form the oil phase;

[0087] B. Take 4% polycarboxylate, 0.1% xanthan gum and 53.05% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0088] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.4% hexamethylenediamine and continue stirring;

[0089] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5 hours;

[0090] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C 30% to prepare the clomazone microcapsule suspension. Discharge the material and set aside.

[0091] (II) Preparation of 30% sulfentrazone aqueous suspension

[0092] F. 31.58% sulfentrazone technical (including sulfentrazone content of 95%), 4% polycarboxylate, 0.1% xanthan gum, 0.2% methylisothiazolinone, 3% ethylene glycol and 61.12% water are put into the preparation apparatus and dispersed evenly.

[0093] G. Grind the material system to the target particle size using a wet grinding process to obtain a 30% sulfentrazone aqueous suspension. H. Pass the 30% sulfentrazone aqueous suspension through a filter and store it in a transfer container for later use.

[0094] (III) Mixed (20% clomazone + 10% sulfentrazone) microcapsule suspension-suspension concentrate

[0095] I. The 30% clomazone microcapsule suspension prepared in step (i) and the 30% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a mass ratio of 2:1, and stirred evenly to obtain a (20% clomazone + 10% sulfentrazone) microcapsule suspension-suspension concentrate.

[0096] Example 3 (the weight ratio of clomazone to sulfentrazone is 1:3)

[0097] Preparation of (10% clomazone + 30% sulfentrazone) microcapsule suspension-suspension concentrate.

[0098] (I) Preparation of 40% Clomazone Microcapsule Suspension

[0099] A. Dissolve 41.67% clomazone technical (clomazone content 96%) in 4% 100# solvent oil, then add 4% MDI and mix well to form the oil phase;

[0100] B. Take 6% polycarboxylate, 0.05% xanthan gum and 38.88% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0101] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.3% hexamethylenediamine and continue stirring;

[0102] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 5% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0103] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to obtain the 40% clomazone microcapsule suspension. Discharge the material and set aside.

[0104] (II) Preparation of 40% sulfentrazone aqueous suspension

[0105] F. 42.11% sulfentrazone technical material (of which sulfentrazone content is 95%), 6% polycarboxylate used in the isoflurane microcapsule suspension, 0.05% xanthan gum, 0.1% methylisothiazolinone, 1% ethylene glycol and 50.74% water are put into the preparation apparatus and dispersed evenly.

[0106] G. The material system is ground to the target particle size by wet grinding process to obtain 40% sulfentrazone aqueous suspension.

[0107] H. Pass the 40% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0108] (III) Mixed (10% clomazone + 30% sulfentrazone) microcapsule suspension-suspension concentrate

[0109] I. The 40% clomazone microcapsule suspension prepared in step (i) and the 40% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 1:3, and stirred evenly to obtain a (10% clomazone + 30% sulfentrazone) microcapsule suspension-suspension concentrate.

[0110] Example 4 (the weight ratio of clomazone to sulfentrazone is 3:4)

[0111] Preparation of (15% clomazone + 20% sulfentrazone) microcapsule suspension-suspension concentrate.

[0112] (I) Preparation of 30% Clomazone Microcapsule Suspension

[0113] A. Dissolve 31.25% clomazone technical (clomazone content 96%) in 5% solvent oil #100, then add 3% MDI and mix well to form the oil phase;

[0114] B. Take 4% polycarboxylate, 0.1% xanthan gum and 53.05% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0115] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.4% hexamethylenediamine and continue stirring;

[0116] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5 hours;

[0117] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 30% clomazone microcapsule suspension. Discharge the material and set aside.

[0118] (II) Preparation of 40% sulfentrazone aqueous suspension

[0119] F. 42.11% sulfentrazone technical material (of which sulfentrazone content is 95%), 6% polycarboxylate used in the isoflurane microcapsule suspension, 0.05% xanthan gum, 0.1% methylisothiazolinone, 1% ethylene glycol and 50.74% water are put into the preparation apparatus and dispersed evenly.

[0120] G. The material system is ground to the target particle size by wet grinding process to obtain 40% sulfentrazone aqueous suspension.

[0121] H. Pass the 40% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0122] (III) Mixed (15% clomazone + 20% sulfentrazone) microcapsule suspension-suspension concentrate

[0123] I. The 30% clomazone microcapsule suspension prepared in step (i) and the 40% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a mass ratio of 1:1, and stirred evenly to obtain a (15% clomazone + 20% sulfentrazone) microcapsule suspension-suspension concentrate.

[0124] Example 5 (the weight ratio of clomazone to sulfentrazone is 4:3)

[0125] Preparation of (20% clomazone + 15% sulfentrazone) microcapsule suspension-suspension concentrate.

[0126] (I) Preparation of 40% Clomazone Microcapsule Suspension

[0127] A. Dissolve 41.67% clomazone technical (clomazone content 96%) in 4% 100# solvent oil, then add 4% MDI and mix well to form the oil phase;

[0128] B. Take 6% polycarboxylate, 0.05% xanthan gum and 38.88% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0129] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.3% hexamethylenediamine and continue stirring;

[0130] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 5% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0131] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 40% clomazone microcapsule suspension. Discharge the material and set aside.

[0132] (II) Preparation of 30% sulfentrazone aqueous suspension

[0133] F. 31.58% sulfentrazone technical (including sulfentrazone content of 95%), 4% polycarboxylate, 0.1% xanthan gum, 0.2% methylisothiazolinone, 3% ethylene glycol and 61.12% water are put into the preparation apparatus and dispersed evenly.

[0134] G. The material system is ground to the target particle size by wet grinding process to obtain 30% sulfentrazone aqueous suspension.

[0135] H. Pass the 30% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0136] (III) Mixed (20% clomazone + 15% sulfentrazone) microcapsule suspension-suspension concentrate

[0137] I. Mix 40% clomazone microcapsule suspension prepared in step (i) and 30% sulfentrazone aqueous suspension prepared in step (ii) in a ratio of 1:1, and stir evenly to obtain (20% clomazone + 15% sulfentrazone) microcapsule suspension-suspension concentrate.

[0138] Example 6 (the weight ratio of clomazone to sulfentrazone is 1:1)

[0139] Preparation of (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0140] (I) Preparation of 35% Clomazone Microcapsule Suspension

[0141] A. Dissolve 36.46% clomazone technical (clomazone content 96%) in 4.5% solvent oil 150#, then add 3.5% HDI and mix well to form the oil phase;

[0142] B. Take 2% polycarboxylate, 3% sodium lignin sulfonate, 0.05% xanthan gum, and 46.04% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0143] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.35% tetraethylenepentamine and continue stirring;

[0144] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0145] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 35% clomazone microcapsule suspension. Discharge the material and set aside.

[0146] (II) Preparation of 35% sulfentrazone aqueous suspension

[0147] F. 36.84% sulfentrazone technical (including sulfentrazone content of 95%), 2% polycarboxylate, 3% sodium lignin sulfonate, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water are put into the preparation apparatus and dispersed evenly.

[0148] G. The material system is ground to the target particle size by wet grinding process to obtain 35% sulfentrazone aqueous suspension.

[0149] H. Pass the 35% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0150] (III) Mixed (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate

[0151] I. The 35% clomazone microcapsule suspension prepared in step (i) and the 35% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a mass ratio of 1:1, and stirred evenly to obtain a (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0152] Example 7 (the weight ratio of clomazone to sulfentrazone is 2:3)

[0153] Preparation of (2% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate.

[0154] (I) Preparation of 5% clomazone microcapsule suspension

[0155] A. Dissolve 5.21% clomazone technical (clomazone content 96%) in 10% solvent oil 150#, then add 0.4% IPDI and mix well to form the oil phase;

[0156] B. Take 1% polycarboxylate, 1% sodium lignin sulfonate, 0.1% xanthan gum, and 78.99% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0157] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.1% triethylenetetramine and continue stirring;

[0158] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5 hours;

[0159] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 5% clomazone microcapsule suspension. Discharge the material and set aside.

[0160] (II) Preparation of 5% sulfentrazone aqueous suspension

[0161] F. Add 5.26% sulfentrazone technical (with sulfentrazone content of 95%), 1% polycarboxylate, 0.05% xanthan gum, 0.2% methylisothiazolinone, 1% ethylene glycol and 92.49% water into the preparation device and disperse evenly. G. Grind the material system to the target particle size using a wet grinding process to obtain a 5% sulfentrazone aqueous suspension. H. Pass the filter and store the 5% sulfentrazone aqueous suspension in a transfer container for later use.

[0162] (III) Mixed (2% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate

[0163] I. The 5% clomazone microcapsule suspension prepared in step (i) and the 5% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 2:3, and stirred evenly to obtain a (2% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate.

[0164] Example 8 (the weight ratio of clomazone to sulfentrazone is 1:9)

[0165] Preparation of (5% clomazone + 45% sulfentrazone) microcapsule suspension-suspension concentrate.

[0166] (I) Preparation of 50% Clomazone Microcapsule Suspension

[0167] A. Melt 52.08% clomazone technical (clomazone content 96%) at 50°C, then add 5% TDI and mix well to form the oil phase;

[0168] B. Take 4% polycarboxylate, 4% sodium lignin sulfonate, 0.05% xanthan gum, and 28.77% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0169] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an oil-in-water emulsion, and then slowly add 1% triethylenetetramine and continue stirring;

[0170] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 5% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0171] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 50% clomazone microcapsule suspension. Discharge the material and set aside.

[0172] (II) Preparation of 50% sulfentrazone aqueous suspension

[0173] F. Add 52.63% sulfentrazone technical (including sulfentrazone content of 95%), 8% polycarboxylate, 0.1% xanthan gum, 0.1% methylisothiazolinone, 3% ethylene glycol and 36.17% water into the preparation device and disperse evenly.

[0174] G. The material system is ground to the target particle size by wet grinding process to obtain 50% sulfentrazone aqueous suspension.

[0175] H. Pass the 50% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0176] (III) Mixed (5% clomazone + 45% sulfentrazone) microcapsule suspension-suspension concentrate

[0177] I. The 50% clomazone microcapsule suspension prepared in step (i) and the 50% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 1:9, and stirred evenly to obtain a (5% clomazone + 45% sulfentrazone) microcapsule suspension-suspension concentrate.

[0178] Example 9 (the weight ratio of clomazone to sulfentrazone is 1:40)

[0179] Preparation of (1% clomazone + 40% sulfentrazone) microcapsule suspension-suspension concentrate.

[0180] (I) Preparation of 5% clomazone microcapsule suspension

[0181] A. Dissolve 5.21% clomazone technical (clomazone content 96%) in 10% solvent oil 150#, then add 0.4% IPDI and mix well to form the oil phase;

[0182] B. Take 1% polycarboxylate, 1% sodium lignin sulfonate, 0.1% xanthan gum, and 78.99% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0183] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.1% triethylenetetramine and continue stirring;

[0184] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5 hours;

[0185] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 5% clomazone microcapsule suspension. Discharge the material and set aside.

[0186] (II) Preparation of 50% sulfentrazone aqueous suspension

[0187] F. Add 52.63% sulfentrazone technical (including sulfentrazone content of 95%), 8% polycarboxylate, 0.1% xanthan gum, 0.1% methylisothiazolinone, 3% ethylene glycol and 36.17% water into the preparation apparatus and disperse evenly.

[0188] G. The material system is ground to the target particle size by wet grinding process to obtain 50% sulfentrazone aqueous suspension.

[0189] H. Pass the 50% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0190] (III) Mixed (1% clomazone + 40% sulfentrazone) microcapsule suspension-suspension concentrate

[0191] I. The 5% clomazone microcapsule suspension prepared in step (i) and the 50% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 1:4, and stirred evenly to obtain a (4% clomazone + 40% sulfentrazone) microcapsule suspension-suspension concentrate.

[0192] Example 10 (the weight ratio of clomazone to sulfentrazone is 20:3)

[0193] Preparation of (20% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate.

[0194] (I) Preparation of 50% Clomazone Microcapsule Suspension

[0195] A. Melt 52.08% clomazone technical (clomazone content 96%) at 50°C, then add 5% TDI and mix well to form the oil phase;

[0196] B. Take 4% polycarboxylate, 4% sodium lignin sulfonate, 0.05% xanthan gum, and 28.77% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0197] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an oil-in-water emulsion, and then slowly add 1% triethylenetetramine and continue stirring;

[0198] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 5% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0199] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 50% clomazone microcapsule suspension. Discharge the material and set aside.

[0200] (II) Preparation of 5% sulfentrazone aqueous suspension

[0201] F. 5.26% sulfentrazone technical material (including sulfentrazone content of 95%), 1% of polycarboxylate used in isoflurane microcapsule suspension, 0.05% xanthan gum, 0.2% methylisothiazolinone, 1% ethylene glycol and 92.49% water are put into the preparation apparatus and dispersed evenly.

[0202] G. The material system is ground to the target particle size by wet grinding process to obtain 5% sulfentrazone aqueous suspension.

[0203] H. Pass the 5% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0204] (III) Mixed (20% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate

[0205] I. The 50% clomazone microcapsule suspension prepared in step (i) and the 5% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 2:3, and stirred evenly to obtain a (20% clomazone + 3% sulfentrazone) microcapsule suspension-suspension concentrate.

[0206] Comparative Example 1 (the weight ratio of clomazone to sulfentrazone is 1:1)

[0207] Preparation of (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0208] (I) Preparation of 35% Clomazone Microcapsule Suspension

[0209] A. Dissolve 36.46% clomazone technical (clomazone content 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0210] B. Take 5% sodium lignin sulfonate, 0.05% xanthan gum, and 46.04% water and mix them evenly under shear homogenization conditions as the aqueous phase for later use;

[0211] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.35% hexamethylenediamine and continue stirring;

[0212] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0213] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 35% clomazone microcapsule suspension. Discharge the material and set aside.

[0214] (II) Preparation of 35% sulfentrazone aqueous suspension

[0215] F. 36.84% sulfentrazone technical (including sulfentrazone content of 95%), 2% block polyether nonionic emulsifier, 3% phosphate dispersant, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water are put into the preparation device and dispersed evenly.

[0216] G. The material system is ground to the target particle size by wet grinding process to obtain 35% sulfentrazone aqueous suspension.

[0217] H. Pass the 35% sulfentrazone aqueous suspension through the filter and store it in a transfer container for later use.

[0218] (III) Mixed (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate

[0219] I. The 35% clomazone microcapsule suspension prepared in step (i) and the 35% sulfentrazone aqueous suspension prepared in step (ii) are mixed in a ratio of 1:1, and stirred evenly to obtain a (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0220] Comparative Example 2 (the weight ratio of clomazone to sulfentrazone is 1:1)

[0221] Preparation of (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0222] (I) Preparation of 35% Clomazone Microcapsule Suspension

[0223] A. Dissolve 36.46% clomazone technical (clomazone content 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0224] B. Take 5% polycarboxylate, 0.05% xanthan gum and 46.04% water and mix them evenly under shear homogenization conditions as the water phase for later use;

[0225] C. Transfer the oil phase into the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.35% hexamethylenediamine and continue stirring;

[0226] D. Heat the emulsion to 55°C under continuous stirring, keep the system warm for 4 hours, add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours;

[0227] E. Finally, keep the temperature for a certain period of time and then cool it down to 20-25°C to prepare 35% clomazone microcapsule suspension. Discharge the material and set aside.

[0228] (II) Preparation of 70% sulfentrazone wettable powder

[0229] F. After 73.68% sulfentrazone technical (including sulfentrazone content of 95%) and polycarboxylate (solid powder 26.32%) are uniformly mixed, the material system is pulverized by air flow pulverization to a target particle size, thereby obtaining 70% sulfentrazone wettable powder.

[0230] (III) Mixed (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate

[0231] I. The 35% clomazone microcapsule suspension prepared in step (i), the 70% sulfentrazone wettable powder prepared in step (ii) and water are mixed in a ratio of 2:1:1, and stirred evenly to obtain a (17.5% clomazone + 17.5% sulfentrazone) microcapsule suspension-suspension concentrate.

[0232] Test Example 1

[0233] The samples of Examples 1-10, Comparative Examples 1-2, and their hot storage and freeze-thaw samples were tested with reference to national standards.

[0234] The suspension rate is tested according to the GB / T14825-2023 method;

[0235] The persistent foaming property is tested according to the GB / T28137-2011 method;

[0236] The pH value is tested according to the GB / T 1601-2023 method;

[0237] The wet screening test is carried out according to the method of GB / T 16150-1995;

[0238] The dumping property is tested according to the GB / T31737-2015 method;

[0239] Hot storage stability is tested according to GB / T 19136-2021 method;

[0240] The freeze-thaw stability test was performed with 4 cycles between room temperature (20℃±2℃) and (-10℃±2℃), with each cycle consisting of 18 hours of freezing and 6 hours of thawing.

[0241] Spontaneous dispersion was determined by referring to MT160 in the CIPAC method.

[0242] The test results are shown in Table 1.

[0243] Table 1 Stability test results of sample preparations of Examples 1-10 and Comparative Examples 1-2

[0244]

[0245]

[0246] Note: In Table 1, the products of Comparative Examples 1 and 2 are flowable in appearance when they are just prepared; the hot storage stability of Comparative Examples 1 and 2 in Table 1 is unqualified, which is mainly reflected in the problem of sample paste after hot storage, and the detection significance is lost; the freeze-thaw stability of Comparative Examples 1 and 2 is also unqualified, and the unqualified items include: sulfentrazone suspension rate, spontaneous dispersibility, and isothiocarb encapsulation rate). Microscopic examination of freeze-thaw and room temperature samples shows that sulfentrazone has undergone severe Ostwald ripening, and the surface of the isothiocarb microcapsules has many depressions and obvious wrinkles, and it is no longer a smooth sphere.

[0247] As can be seen from Table 1, the clomazone + sulfentrazone microcapsule suspension-suspension concentrate prepared by the present invention is qualified in all indicators, and the sample is stable in quality after being subjected to heat storage and freeze-thaw accelerated storage treatment, indicating that the preparation process of the method has good reproducibility, stable product quality, and good freeze-thaw stability. Compared with comparative example 1-2, Example 1-10 shows that comparative example 1-2 is unqualified in freeze-thaw, and a large number of long radial rod-shaped crystals are found under microscopic examination, which are consistent with the surface properties of the room temperature comparative example sample, but slightly better than the room temperature sample, indicating that the stability of the comparative example product over time is poor, and low temperature can alleviate the trend of product deterioration. ② The specific reason for the deterioration of quality is that the adjuvant on the surface of the sulfentrazone particles in the microcapsule suspension-suspension concentrate desorbed and migrated to the water or the surface of the clomazone microcapsule (Comparative Example 1) or was not effectively adsorbed (Comparative Example 2) after being mixed into the microcapsule suspension-suspension concentrate. The loss of the auxiliary agent caused sulfentrazone to undergo obvious Ostschmatten ripening on the one hand, and on the other hand, sulfentrazone came into contact with the clomazone capsule skin, causing the microcapsule surface to deform and thus affecting the encapsulation rate of clomazone. Overall, the formula stability of the scheme of the present invention is good, which solves the disadvantage of unstable mixing of clomazone and sulfentrazone.

[0248] Test Example 2:

[0249] Field test example: Field test on annual weeds in sugarcane fields

[0250] This experiment was arranged in a sugarcane field in the suburbs of Yongning District, Nanning City, Guangxi Zhuang Autonomous Region. The terrain is flat, the land is level, the irrigation and drainage facilities are complete, the field management level is consistent, and the fertility is uniform and medium. The main weeds in the experimental field are goosegrass, crabgrass, quinoa, and Amaranthus retroflexus.

[0251] There are 5 treatments in total, namely: treatment 1: clean water spray, blank control; treatment 2: Example 1; treatment 3: Example 6; treatment 4: comparative example 1; treatment 5: comparative example 2. All samples are freshly prepared samples and can be diluted with water to meet the spraying requirements.

[0252] According to the field application registration data, the field dosage of each treatment was calculated to be 200g / mu.

[0253] Use Gongnong-16 backpack manual sprayer to apply the pesticide once, add 30L of water per mu of the preparation to prepare the liquid, and spray evenly. The weather was good during the test, with an average daily temperature of 18-23℃. There was no rain on the day of application, and no rain within 10 days after the application.

[0254] On the 30th day, when the experiment ended, four points were randomly selected from each plot, with a 0.25 m 2 , pull out annual weeds, classify them and weigh their fresh weight, and calculate the weed control effect by fresh weight.

[0255]

[0256] The results of the 30-day fresh weight control efficacy are shown in Table 2.

[0257] Table 2 Results of the 30-day fresh weight control test of annual weeds by each treatment agent

[0258]

[0259] According to Table 2, under the same dosage form and the same specifications, the embodiments are significantly better than the comparative examples. The (clomazone + sulfentrazone) microcapsule suspension-suspension concentrate prepared according to the method of the present invention has an overall control effect of more than 90% in use. Compared with the (clomazone + sulfentrazone) microcapsule suspension-suspension concentrate prepared in other conventional ways, the drug effect is more excellent. The reason for the analysis is that although the conventional physical and chemical indicators such as the appearance fluidity of the (clomazone + sulfentrazone) microcapsule suspension-suspension concentrate prepared in the comparative example meet the requirements of drug application, the internal effective ingredients are in an unstable state such as aggregation, and the dispersion effect is poor, especially for the herbicide for soil sealing, the original drug is in a "waiting for grass" state after spraying, and the distribution uniformity of the aggregated original drug is poor, resulting in poor control effect. Following up the growth of sugarcane in each treatment plot, no obvious abnormality was found, indicating that the drug combination covered by the present invention is highly safe for sugarcane and has a good application effect.

[0260] In summary, the (clomazone + sulfentrazone) microcapsule suspension-suspension concentrate preparation method protected by the present invention and the product prepared by the preparation method have higher stability, fewer types of processed raw materials, more stable efficacy, and obvious advantages.

[0261] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A microcapsule suspension-suspension concentrate containing clomazone and sulfentrazone, characterized in that: The invention comprises a mixture of a clomazone microcapsule suspension and a sulfentrazone suspension in a mass ratio of 1: (0.1-10); wherein: The clomazone microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts by weight of clomazone, 2-10 parts by weight of solvent oil, 0.4-5 parts by weight of oil phase wall material, 1-8 parts by weight of dispersant, 0-5 parts by weight of thickener, 0-10 parts by weight of preservative, 0-5 parts by weight of antifreeze agent, 0.1-1 parts by weight of water phase wall material, 0-5 parts by weight of specific gravity regulator, 0-1 parts by weight of preservative and 25-80 parts by weight of water; The sulfentrazone suspension comprises the following raw materials in parts by weight: 5 to 50 parts by weight of sulfentrazone, 1 to 8 parts by weight of a dispersant, 0 to 5 parts by weight of an antifreeze agent, and 45 to 96 parts by weight of water; In the clomazone microcapsule suspension and / or sulfentrazone suspension, the dispersant is at least one of sodium lignin sulfonate and polycarboxylate.

2. The microcapsule suspension-suspending agent according to claim 1, characterized in that The invention comprises a mixture of a clomazone microcapsule suspension and a sulfentrazone suspension in a mass ratio of 1:(0.5-10), optionally in a mass ratio of 1:(0.5-9), optionally in a mass ratio of 1:(1-9); And / or, the weight ratio of clomazone to sulfentrazone is (1-7):(1-40), optionally (1-7):(1-9), optionally (1-2):(1-4).

3. The microcapsule suspension-suspending agent according to claim 1 or 2, characterized in that: The clomazone microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts by weight of clomazone, 2-10 parts by weight of solvent oil, 0.4-5 parts by weight of oil phase wall material, 1-6 parts by weight of polycarboxylate, 0-4 parts by weight of sodium lignin sulfonate, 0-5 parts by weight of thickener, 0-10 parts by weight of preservative, 0-5 parts by weight of antifreeze agent, 0.1-1 parts by weight of water phase wall material, 0-5 parts by weight of specific gravity regulator, 0-1 parts by weight of preservative and 25-80 parts by weight of water; And / or, the sulfentrazone suspension concentrate comprises the following raw materials in parts by weight: 5 to 50 parts by weight of sulfentrazone, 1 to 6 parts by weight of polycarboxylate, 0 to 4 parts by weight of sodium lignin sulfonate, 0 to 5 parts by weight of antifreeze agent and 45 to 96 parts by weight of water; And / or, in the clomazone microcapsule suspension and / or the sulfentrazone suspension, the mass fraction of polycarboxylate and sodium lignin sulfonate is ≤8%.

4. The microcapsule suspension-suspending concentrate according to any one of claims 1 to 3, characterized in that: In the clomazone microcapsule suspension, the weight ratio of clomazone to the oil phase wall material is 1:(0.05-0.5), and can be optionally 1: (0.08~0.5), optionally 1:(0.08~0.2).

5. The microcapsule suspension-suspending concentrate according to any one of claims 1 to 4, characterized in that: In the clomazone microcapsule suspension, the clomazone is 5 to 45 parts by weight, and optionally 17 to 40 parts by weight; and / or, in the clomazone microcapsule suspension, the dispersant is 3 to 8 parts by weight, optionally 4 to 6 parts by weight; optionally, the mass fraction of the dispersant is ≤ 8%; and / or, in the clomazone microcapsule suspension, the oily wall material is 3-5%, optionally 3-4.5%, And / or, in the clomazone microcapsule suspension, the oily wall material is aromatic isocyanate and its modified product; optionally, the oily wall material is selected from one or more of MDI, HDI, TDI, and IPDI; and / or, in the clomazone microcapsule suspension, the aqueous phase wall material is 0.1 to 1.0 parts by weight; And / or, in the clomazone microcapsule suspension, the aqueous phase wall material is a polyamine, and the aqueous phase wall material can be selected from one or more of hexamethylenediamine, triethylenetetramine, and tetraethylenepentamine.

6. The microcapsule suspension-suspending concentrate according to any one of claims 1 to 5, characterized in that: In the clomazone microcapsule suspension, the solvent oil is 3 to 10 parts by weight, and optionally 3 to 5 parts by weight; And / or, in the clomazone microcapsule suspension, the solvent is one or more of solvent oil 100#, solvent oil 150#, and solvent oil 200#; and / or, in the clomazone microcapsule suspension, the thickener is 0.05 to 0.1 parts by weight; and / or, in the clomazone microcapsule suspension, the thickener is xanthan gum; and / or, in the clomazone microcapsule suspension, the preservative is 0.1 to 0.2 parts by weight; and / or, in the clomazone microcapsule suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone; and / or, in the clomazone microcapsule suspension, the specific gravity regulator is 3 to 5 parts by weight; and / or, in the clomazone microcapsule suspension, the specific gravity regulator is anhydrous calcium chloride; and / or, in the clomazone microcapsule suspension, the antifreeze agent is ethylene glycol; And / or, the clomazone microcapsule suspension is supplemented with water to make up to 100 parts by weight.

7. The microcapsule suspension-suspending concentrate according to any one of claims 1 to 6, characterized in that: In the sulfentrazone aqueous suspension, sulfentrazone is 20 to 50 parts by weight, and optionally 30 to 40 parts by weight; and / or, in the aqueous suspension of sulfentrazone, the thickener is 0.05 to 0.1 parts by weight; and / or, in the aqueous suspension of sulfentrazone, the thickener is xanthan gum; and / or, in the aqueous suspension of sulfentrazone, the preservative is 0.1 to 0.2 parts by weight; and / or, in the sulfentrazone aqueous suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone; and / or, in the aqueous suspension of sulfentrazone, the antifreeze agent is 1 to 3%; and / or, in the aqueous suspension of sulfentrazone, the antifreeze agent is ethylene glycol; And / or, the sulfentrazone aqueous suspension concentrate is supplemented with water to make up to 100 parts by weight.

8. A method for preparing a microcapsule suspension-suspension concentrate according to any one of claims 1 to 7, characterized in that: The steps include: 1) Preparation of clomazone microcapsule suspension: The isothiocarb, solvent and oil phase wall material are mixed to form the oil phase; Mixing a dispersant, a thickener and water as a water phase; The oil phase is transferred into the water phase, and the emulsion is obtained by high-speed shearing and emulsification, and the water phase wall material is added and stirred continuously, and a specific gravity regulator and / or a preservative are added as required to obtain a clomazone microcapsule suspension; optionally, after adding tetraethylenepentamine, the emulsion is heated to 50-60° C. and then a specific gravity regulator and / or a preservative are added as required; 2) Preparation of sulfentrazone aqueous suspension: The terbuthiuron, dispersant, thickener, preservative, antifreeze agent and water are mixed and wet-grinded to a target particle size to obtain a sulfentrazone aqueous suspension; 3) The materials of step 1) and step 2) are mixed to prepare a microcapsule suspension-suspension concentrate.

9. Use of the microcapsule suspension-suspension concentrate according to any one of claims 1 to 7, or the microcapsule suspension-suspension concentrate prepared by the preparation method according to claim 8, in preventing and controlling weeds in farmland before crop planting, before seedling emergence after sowing, or during the crop growth period.

10. The use according to claim 9, characterized in that: The weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of goosegrass, crabgrass, quinoa, and Amaranthus retroflexus.

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