Weeding composition containing clomazone and tebuthiuron, microcapsule suspension-suspending agent and preparation method and application of microcapsule suspension-suspending agent

Abstract

The invention discloses a weeding composition containing clomazone and tebuthiuron, a micro-capsule suspension-suspending agent and a preparation method and application of the weeding composition and the micro-capsule suspension-suspending agent, and relates to the field of pesticides, the weeding composition comprises the effective components of clomazone and tebuthiuron, and the weight ratio of clomazone to tebuthiuron is (0.1: 99)-(99: 0.1), optionally (40: 1)-(1: 40), and optionally (20: 1)-(1: 30). By compounding the composition, the prevention and treatment effect can be improved, the dosage is reduced, the phytotoxicity risk is reduced, and the occurrence of drug resistance is delayed.

Description

Technical Field

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

[0002] Pesticides are mainly divided into herbicides, insecticides, fungicides and plant growth regulators. Among them, herbicides account for the largest scale and the most types in the global pesticide market. In some years and statistical calibers, herbicides account for a considerable proportion of the total sales of pesticides. Due to the technical barriers of the herbicide industry, a stable pattern of six major pesticide companies, including Syngenta, Bayer, BASF, Dow, Monsanto and DuPont, has been formed worldwide. These companies dominate the herbicide market. This shows the important position of herbicides in the pesticide industry.

[0003] From an application perspective, weeds will compete with crops for nutrients in the soil, such as nitrogen fertilizer. For example, the ability of thistle to absorb nitrogen fertilizer is 1.5 times that of gramineous crops, and the water absorption of mugwort is also twice that of wheat. This will lead to limited growth of crops due to insufficient nutrients, which will affect yields. The lush growth of weeds will occupy a large amount of growth space, squeezing the growth space of crops. This will lead to a decrease in crop photosynthesis, thin and weak plants, and poor firmness, which will ultimately affect yields. For example, wheat may reduce yields by about 30% in fields with more weeds, and corn may reduce yields by about 50%. Weeds are not only breeding grounds for pests and diseases, but may also become a medium for the spread of pests and diseases. For example, cutworms like to lay eggs on field bindweed, so the probability of cutworms occurring in fields with more field bindweed is higher. This will increase the risk of crop damage, which will affect yields. In fields with more weeds, agricultural operations such as harvesting and tillage will be hindered. For example, if the Gynostemma pentaphyllum in the corn field is not properly controlled, it will affect the mechanized harvesting; wild reeds and paper mulberry shrubs in the Chinese medicinal materials field may create great obstacles to the harvesting of Chinese medicinal materials. These will increase the difficulty and cost of agricultural production, and indirectly lead to a reduction in production.

[0004] The use of herbicides is the most direct, effective and labor-saving means of weed control. However, with the long-term use of herbicides, weed resistance has gradually become prominent, and the resistance level has increased year by year. At present, 267 weeds in 96 crop fields in 72 countries around the world have developed resistance to herbicides, involving 513 herbicide-resistant biotypes. Even glyphosate, a non-selective broad-spectrum herbicide, currently has 56 weeds resistant to it worldwide, and 2 in my country. Mixing herbicides with different mechanisms of action can improve the weed control effect and reduce the risk of resistance.

[0005] Therefore, it is particularly important to develop reasonable compound herbicides and apply them reasonably.

[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 being absorbed by crops such as soybeans and sugarcane, clomazone undergoes special metabolism, converting the active ingredients of clomazone into non-toxic degradation products, making it safe. Clomazone is mainly used to control annual grass and 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 communis, etc. It also has a strong inhibitory effect on perennial plants such as prickly lettuce, thistle, sonchus, and horsetail. Soil treatment before and after sowing and before seedlings in soybean fields, or stem and leaf treatment in the early post-seedling period. Clomazone has a long lasting effect. When used at a high dosage of more than 53g per mu, it 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 be planted again 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. It can also be used as a herbicide for post-sowing and pre-emergence weed control in sugarcane fields.

[0008] Mechanism and characteristics of terbuthiuron: It is an inhibitor of photosynthetic electron transfer at the receptor site of photosynthetic system II. The specific mechanism is to inhibit the Hill reaction in photosynthesis, that is, to inhibit photosynthesis by forming hydrogen bonds between amino or carbonyl oxygen and the active center of chloroplasts. Terbuthiuron is a systemic soil herbicide with low selectivity. It is mainly absorbed by the root system and then conducted in the plant body. Terbuthiuron is a broad-spectrum herbicide used to control herbaceous and woody plants (dosage 0.6-4.5kg / hm2), annual weeds (dosage 1.3-4.5kg / hm2), and many perennial weeds and leaf weeds (dosage 2.2-4.5kg / hm2). Its uses include controlling undesirable woody plants and weeds in non-arable vegetation, grasslands and pastures, as well as grass weeds and broad-leaved weeds in sugarcane fields.

[0009] There are no reports on the combination of the two. 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 herbicidal composition containing clomazone and terbuthiuron, a microcapsule suspension-suspension concentrate, and a preparation method and application thereof. The compounding of the composition of the present invention can improve the control effect, reduce the dosage of the medicine, reduce the risk of pesticide damage, and delay the occurrence of drug resistance.

[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 herbicidal composition containing clomazone and terbuthiuron, wherein the active ingredients in the herbicidal composition include clomazone and terbuthiuron, and the weight ratio of clomazone to terbuthiuron is (0.1:99) to (99:0.1).

[0015] Furthermore, the weight ratio of clomazone and terbuthiop-methyl is (40:1) to (1:40), optionally (20:1) to (1:30), optionally (10:1) to (1:10), optionally (5:1) to (1:10), optionally (5:1) to (1:5), optionally 20:1, 10:1, 5:1, 1:1, 1:5, 1:10 or 1:20.

[0016] Furthermore, the active ingredient accounts for 1 to 99% of the total weight of the composition, optionally 6% to 80%, optionally 6% to 60%, optionally 30% to 40%.

[0017] The combination of the two agents within the above range can be prepared into dosage forms such as ZC, WG, WP, DF, EC, EW, GR, etc. by using auxiliary materials in combination with their physical and chemical properties, such as solvents, emulsifiers, dispersants, wetting agents, thickeners, fillers, preservatives, antifreeze agents, specific gravity regulators, defoaming agents, oil phase wall materials, water phase wall materials, water, etc.

[0018] Further, the formulation of the herbicidal composition is one or more of microcapsule suspension-suspension concentrate, emulsifiable concentrate, aqueous emulsion, dry suspension concentrate, wettable powder, water dispersible granule, granule, and seed treatment agent;

[0019] Furthermore, the herbicidal composition also includes an adjuvant, and optionally, the adjuvant is selected from one or more of a solvent, an emulsifier, a dispersant, a wetting agent, a thickener, a filler, a preservative, an antifreeze agent, a specific gravity regulator, a defoaming agent, an oil phase wall material, an aqueous phase wall material, and water.

[0020] Furthermore, the solvent is one or more of N,N-dimethylformamide, cyclohexanone, xylene, methylnaphthalene, and solvent oil;

[0021] Furthermore, the emulsifier is one or more of EOPO block polyether emulsifier, calcium dodecylbenzene sulfonate, Tween series, and Span series;

[0022] Further, the dispersant is one or more of polycarboxylates, lignin sulfonates, and naphthalene sulfonates;

[0023] Furthermore, the wetting agent is one or more of sodium dodecyl sulfate and sodium dodecylbenzene sulfonate;

[0024] Further, the thickener is one or more of xanthan gum and magnesium aluminum silicate;

[0025] Furthermore, the filler is one or more of calcined kaolin, bentonite, diatomaceous earth, attapulgite, fumed silica, corn starch or light calcium carbonate;

[0026] Further, the preservative is isomethylthiazolinone;

[0027] Furthermore, the antifreeze agent is one or more of ethylene glycol and glycerol;

[0028] Furthermore, the specific gravity regulator is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate; optionally, the specific gravity regulator can also be used as a spray drying aid for the DF dosage form and a disintegrant for the WG dosage form.

[0029] Further, the defoaming agent is a silicone emulsion;

[0030] Furthermore, the oil phase wall material is polyisocyanate; optionally, it is one or more of HDI, IPDI, MDI, and PAPI;

[0031] Further, the aqueous phase wall material is one or more of polyols and polyamines. Optionally, the aqueous phase wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine. Optionally, the average molecular weight of polyethylene glycol is 100 to 2000, optionally 200 to 800, optionally 300 to 500, optionally 300 to 400. Optionally, the polyethylene glycol is PEG400.

[0032] Furthermore, the granular carrier may be coal gangue.

[0033] In the second aspect, a microcapsule suspension-suspension concentrate comprising the herbicidal composition described in the first aspect is provided, comprising a microcapsule suspension of clomazone and a water suspension of terbuthiuron. Optionally, the weight ratio of the microcapsule suspension of clomazone and the water suspension of terbuthiuron is (1-3): (2-6).

[0034] Furthermore, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 5-60% clomazone, 2-20% solvent, 1-10% oil phase wall material, 1-10% dispersant, 50-70% water, 0.2-6.0% water phase wall material, 0-5% specific gravity regulator, and 0-1% preservative;

[0035] Furthermore, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 10-20% clomazone, 4-10% solvent, 1-6% oil phase wall material, 5-10% dispersant, 60-70% water, 0.25-4.0% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative;

[0036] Further optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15-20% clomazone, 5-10% solvent, 1-4% oil phase wall material, 5-10% dispersant, 65-70% water, 0.25-4.0% aqueous phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative.

[0037] Further optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 1-4% oil phase wall material, 5% dispersant, 65-70% water, 0.25-4.0% aqueous phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative.

[0038] Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 2-4% oil phase wall material, 5% dispersant, 65-70% water, 1-4% aqueous phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative.

[0039] Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 2-4% oil phase wall material, 5% dispersant, 65-70% water, 2-4% aqueous phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative.

[0040] Further optionally, the oil phase wall material is polyisocyanate, which may be one or more of HDI, IPDI, MDI, and PAPI.

[0041] Further optionally, the aqueous phase wall material is one or more of a polyol or a polyamine, optionally, the aqueous phase wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, hexamethylenediamine; optionally, the average molecular weight of the polyethylene glycol is 100-2000, optionally 200-800, optionally 300-500, optionally 300-400; optionally, the polyethylene glycol is PEG400.

[0042] Further optionally, the specific gravity regulator is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate;

[0043] Further optionally, the dispersant is one or more of polycarboxylate, lignin sulfonate, and naphthalene sulfonate; optionally, the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (3-6): (2-4);

[0044] Further optionally, the preservative is isomethylthiazolinone.

[0045] Furthermore, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 20-50%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5% and water 35-50%;

[0046] Further optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: 30-40% terbuthiuron, 5-15% dispersant, 0-1% thickener, 0-1% preservative, 0-5% antifreeze agent and 35-50% water;

[0047] Further optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 35-40%, dispersant 9-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5% and water 45-50%;

[0048] Further optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 35-40%, dispersant 9-15%, thickener 0.1-1%, preservative 0.15-1%, antifreeze 3-5% and water 45-50%;

[0049] Further optionally, the dispersant is one or more of polycarboxylates, lignin sulfonates, and naphthalene sulfonates; optionally, the dispersant comprises polycarboxylates and lignin sulfonates in a weight ratio of (3-9): (2-5); optionally, the dispersant comprises polycarboxylates and lignin sulfonates in a weight ratio of (6-8): (3-4);

[0050] Further optionally, the antifreeze agent is one or more of ethylene glycol and glycerol;

[0051] Further optionally, the preservative is isomethylthiazolinone;

[0052] Further optionally, the thickener is one or more of xanthan gum and magnesium aluminum silicate.

[0053] In a third aspect, a method for preparing the microcapsule suspension-suspension concentrate according to the first aspect is provided, comprising:

[0054] 1) Preparation of clomazone microcapsule suspension:

[0055] The isothiocarb, solvent and oil phase wall material are mixed to form the oil phase;

[0056] Mixing a dispersant, a thickener and water as a water phase;

[0057] 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 the water phase wall material, the emulsion is heated to 50-60° C. and then a specific gravity regulator and / or a preservative are added as required;

[0058] 2) Preparation of terbuthiuron aqueous suspension:

[0059] The terbuthiuron, dispersant, thickener, preservative, antifreeze agent and water are mixed and wet-grinded to a target particle size to obtain a terbuthiuron aqueous suspension;

[0060] 3) The materials of step 1) and step 2) are mixed to prepare a microcapsule suspension-suspension concentrate.

[0061] In a fourth aspect, there is provided a use of the herbicidal composition of the first aspect, or the microcapsule suspension-suspension concentrate of the second aspect, or the microcapsule suspension-suspension concentrate prepared by the preparation method of the third aspect in controlling farmland weeds before crop planting, before emergence after sowing, or during the crop growth period; optionally, the weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of crabgrass, goosegrass, and Amaranthus retroflexus.

[0062] Beneficial Effects

[0063] (1) The compounding of the composition of the present invention can improve the control effect, reduce the dosage of the drug, reduce the risk of drug damage, and delay the occurrence of drug resistance.

[0064] (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 easy to industrialize; 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 optimal compounding ratio of terbuthiuron and isothiocarb was screened; ⑤ After a large number of experiments, auxiliary agents were screened to obtain a stable formulation and its products. ⑥ It has a synergistic effect in weed control, which can improve the control effect of the agent on weeds, reduce the amount of medicine used, reduce costs, and delay the risk of weed resistance. DETAILED DESCRIPTION

[0065] 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.

[0066] 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.

[0067] 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.

[0068] The above herbicidal 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.

[0069] In the following examples, terbuthiuron and clomazone are both commercially available, and other adjuvants are also commercially available products.

[0070] The present invention is further described in detail below by way of examples.

[0071] Test Example 1 Indoor Toxicity Determination

[0072] The herbicidal synergistic effect of terbuthiuron and clomazone was determined by indoor toxicity test. According to the Sun Yunpei method, the co-toxicity coefficient (CTC) of the pesticides after compounding in a certain proportion was determined. CTC < 80 was antagonistic, 80 ≤ CTC ≤ 120 was additive, and CTC > 120 was synergistic.

[0073] All experimental reagents were provided by Shandong Weifang Runfeng Chemical Co., Ltd.

[0074] Experimental design: After the effective inhibitory concentration range of each agent is determined by preliminary test, a series of concentration treatments are set for each agent according to the content of the active ingredient, and a clear water control is set. The experiment is carried out in accordance with the "Guidelines for Indoor Bioassay of Pesticides and Herbicides", and the inhibitory concentration of the agent and the mixed agent is determined by soil spray, and the co-toxicity coefficient is calculated by the method of calculating the joint toxicity proposed by Sun Yunpei et al. (1960).

[0075] The calculation formula is as follows (taking terbuthiuron as the standard agent, its toxicity index is 100)

[0076] The toxicity index (TI) of clomazone = the ED of terbuthiuron 50 / ED of Clomazone 50 ×100.

[0077] Actual Toxicity Index (ATI) of M = ED of terbuthiuron 50 / M's ED 50 ×100.

[0078] Theoretical Toxicity Index (TTI) of M = clomazone TI × P 异噁草松 + terbuthiuron TI×P 特丁噻草隆 .

[0079]

[0080] Wherein: M is a mixture of clomazone and terbuthiuron in different proportions;

[0081] P 异噁草松 is the proportion of clomazone in the compound composition;

[0082] P 特丁噻草隆 It is the proportion of terbuthiuron in the compound composition.

[0083] The test results are shown in Table 1:

[0084] Table 1 The results of toxicity test of clomazone and terbuthiazol-methyl on Amaranthus retroflexus

[0085]

[0086]

[0087] As shown in Table 1, the ED of clomazone and terbuthiuron on Amaranthus retroflexus 50The mass ratios of clomazone and terbuthiuron are 48.45 mg / L and 191.85 mg / L respectively. When the mass ratio of clomazone and terbuthiuron is (40:1) to (1:40), an additive effect is exhibited. Preferably, the co-toxicity coefficient is greater than 120 at (20:1) to (1:30), showing an obvious synergistic effect. The more preferred mass ratio is (10:1) to (1:10), preferably (5:1) to (1:5), and 20:1, 10:1, 5:1, 1:1, 1:5, 1:10, and 1:20 all show a synergistic effect. Among them, when the mass ratio of clomazone and terbuthiuron is 1:5, the synergistic effect is most obvious.

[0088] Preparation Example

[0089] 1. EC

[0090] Example 1 (40% clomazone + 1% terbuthiuron) emulsifiable concentrate (mass ratio is 40:1)

[0091] Take 41.67% of clomazone technical drug (wherein the content of clomazone is 96%) and 1.04% of terbuthiuron technical drug (wherein the content of terbuthiuron is 96%), add 6% of EOPO block polyether emulsifier, 5% of calcium dodecylbenzene sulfonate as emulsifier, add 10% of cyclohexanone as cosolvent, make up solvent oil to 100%, and stir evenly. Then, (40% clomazone + 1% terbuthiuron) emulsifiable concentrate can be obtained.

[0092] Example 2 (5% clomazone + 1% terbuthiuron) emulsifiable concentrate (mass ratio is 5:1)

[0093] Take 5.21% of clomazone technical drug (of which the content of clomazone is 96%) and 1.04% of terbuthiuron technical drug (of which the content of terbuthiuron is 96%), add 6% Tween-80 and 4% Span-80 as emulsifiers, add 20% N,N-dimethylformamide as a cosolvent, and make up xylene to 100%, and stir evenly. You can get (5% clomazone + 1% terbuthiuron) emulsifiable concentrate.

[0094] 2. Water emulsion

[0095] Example 3 (1% clomazone + 1% terbuthiuron) aqueous emulsion (mass ratio is 1:1)

[0096] 1) Oil phase preparation

[0097] Take 1.04% of clomazone technical (including 96% of clomazone) and 1.04% of terbuthiuron technical (including 96% of terbuthiuron), add 4% of EOPO block polyether emulsifier and 4% of calcium dodecylbenzenesulfonate as emulsifiers, add 10% of cyclohexanone as co-solvent, add solvent oil to 40% and stir evenly to prepare the oil phase.

[0098] 2) EW preparation

[0099] Prepare 60% water as the aqueous phase, transfer the prepared oil phase into the aqueous phase and disperse it evenly by shearing, thereby obtaining a (1% clomazone + 1% terbuthiuron) aqueous emulsion.

[0100] 3. Granules

[0101] Example 4 (1% clomazone + 5% terbuthiuron) granules (mass ratio is 1:5)

[0102] Take 1.04% of clomazone technical (including 96% of clomazone) and 5.21% of terbuthiuron technical (including 96% of terbuthiuron), and dissolve them completely in N,N-dimethylformamide. Mix the solution with 93.75% of coal gangue, and dry them to obtain (1% clomazone + 5% terbuthiuron) granules.

[0103] 4 Dry suspension

[0104] Example 5 (30% clomazone + 30% terbuthiuron) dry suspension (mass ratio is 1:1)

[0105] (I) Preparation of 30% Clomazone Microcapsule Suspension

[0106] 31.25% of clomazone technical (including 96% of clomazone) was dissolved in 5.35% of solvent oil 100#, and then 3% of MDI was added and mixed evenly as the oil phase; 7% of polycarboxylate and 50% of water were mixed evenly under shear homogenization conditions as the water phase for standby use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 0.4% of hexamethylenediamine was slowly added with continuous stirring; under continuous stirring, the emulsion was heated to 55° C., the system was kept warm for 4 hours, and then 3% of calcium chloride was added; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and the preparation of 30% clomazone microcapsule suspension was completed.

[0107] (II) Preparation of 30% terbuthiuron aqueous suspension

[0108] 31.25% of terbuthiuron technical (including 96% of terbuthiuron content), 8.42% of polycarboxylate, 10% of lignin sulfonate and 50% of water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 30% terbuthiuron aqueous suspension. The 30% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0109] (III) Mixed isocyanate (15% isocyanate + 15% terbuthiuron) microcapsule suspension-suspension concentrate

[0110] The previously prepared 30% clomazone microcapsule suspension and 30% terbuthiuron aqueous suspension were mixed in a ratio of 1:1 and stirred evenly to obtain (15% clomazone + 15% terbuthiuron) microcapsule suspension-suspension concentrate, which was a slurry with a solid content of 50%.

[0111] (IV) Preparation of (30% clomazone + 30% terbuthiuron) dry suspension

[0112] The (15% clomazone + 15% terbuthiuron) microcapsule suspension-suspension concentrate (water content 50%) was spray-dried to obtain the (30% clomazone + 30% terbuthiuron) dry suspension concentrate.

[0113] 5. Wettable powder

[0114] Example 6 (10% clomazone + 40% terbuthiuron) wettable powder (mass ratio is 1:4)

[0115] (I) Preparation of 20% Clomazone Microcapsule Suspension

[0116] 20.83% of clomazone technical (with a clomazone content of 96%) was dissolved in 5.35% of xylene, and then 2% of PAPI was added and mixed evenly as the oil phase; 6% of polycarboxylate and 60% of water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 0.2% of hexamethylenediamine was slowly added with continuous stirring; under continuous stirring, the emulsion was heated to 55° C., the system was kept warm for 4 hours, and then 4% of calcium chloride was added; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and a 30% clomazone microcapsule suspension was prepared.

[0117] (II) Preparation of 50% Clomazone Microcapsule Dry Suspension

[0118] The 20% clomazone microcapsule suspension is spray-dried to obtain a 50% clomazone microcapsule dry suspension for later use.

[0119] (III) Preparation of 50% terbuthiuron wettable powder

[0120] Take 52.08% of terbuthiuron technical (including 96% terbuthiuron content), 4% polycarboxylate, 4% lignin sulfonate, 2% naphthalene sulfonate, 2% sodium dodecylbenzene sulfonate and calcined kaolin to make up to 100%, mix and grind by air flow to obtain 50% terbuthiuron wettable powder.

[0121] (IV) Preparation of (10% clomazone + 40% terbuthiuron) wettable powder

[0122] The 50% clomazone microcapsule dry suspension prepared earlier and the 50% terbuthiuron wettable powder were mixed in a ratio of 1:4 and stirred evenly to obtain a (10% clomazone + 40% terbuthiuron) wettable powder.

[0123] Example 7 (1% clomazone + 40% terbuthiuron) wettable powder (mass ratio is 1:40)

[0124] 2% fumed silica was used to absorb and melt 1.04% clomazone technical material (with a clomazone content of 96%), which was used as clomazone mother powder for standby use; the previously mixed clomazone mother powder and 41.67% terbuthiuron technical material (with a terbuthiuron content of 96%) were added into a mixer, and 5% polycarboxylate, 2% lignin sulfonate, 4% naphthalene sulfonate, 3% sodium dodecylbenzene sulfonate, and bentonite were added to make up to 100%, and after mixing, the mixture was subjected to air flow pulverization to collect and obtain a (1% clomazone + 40% terbuthiuron) wettable powder.

[0125] 6. Water dispersible granules

[0126] Example 8 (3% clomazone + 76% terbuthiuron) water dispersible granules (mass ratio is 3:76)

[0127] 3.125% clomazone technical drug (with clomazone content of 96%) melted by absorption with 3% fumed silica is used as clomazone mother powder for standby use; the clomazone mother powder mixed in the previous step and 80.20% terbuthiuron technical drug (with terbuthiuron content of 96%) are added into a mixer, and 4% lignin sulfonate, 3% naphthalene sulfonate, 1% sodium dodecylbenzene sulfonate, 0.2% defoamer (mixed into granulation liquid) and polycarboxylate dispersant are added to make up to 100%, and after mixing, the mixture is subjected to air flow pulverization to collect 3% clomazone + 76% terbuthiuron fine powder. According to the weight of the fine powder, 20% water is added as granulation liquid to mix into wet material. The wet material is subjected to extrusion granulation, and after granulation and drying, (3% clomazone + 76% terbuthiuron) water dispersible granules are obtained.

[0128] 7. Microcapsule suspension-suspension concentrate

[0129] Example 9 (30% clomazone + 1.5% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 30:1.5)

[0130] (I) Preparation of 35% Clomazone Microcapsule Suspension

[0131] Dissolve 36.46% clomazone stock (with a clomazone content of 96%) in 4.5% solvent oil, then add 3.5% MDI and mix well as the oil phase; take 5% polycarboxylate, 0.05% xanthan gum, and 46.04% water and mix well under shear homogenization conditions as the water phase for later use; C. Transfer the oil phase to the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.35% hexamethylenediamine and continue stirring; under continuous stirring, heat the emulsion to 55°C, keep the system warm for 4h, add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5h; finally, keep warm for a certain period of time and then cool to 20-25°C, and the 35% clomazone microcapsule suspension is ready. Discharge the material and set aside.

[0132] (II) Preparation of 10.5% terbuthiuron aqueous suspension

[0133] 10.94% terbuthiuron technical (including 96% terbuthiuron content), 4% polycarboxylate, 0.2% xanthan gum, 0.10% methylisothiazolinone, 3% ethylene glycol and 81.76% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 10.5% terbuthiuron aqueous suspension. The 10.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0134] (III) Mixed (30% clomazone + 1.5% terbuthiuron) microcapsule suspension-suspension concentrate

[0135] The previously prepared 35% clomazone microcapsule suspension and 10.5% terbuthiuron aqueous suspension were mixed in a ratio of 85.71:14.29 and stirred evenly to obtain a (30% clomazone + 1.5% terbuthiuron) microcapsule suspension-suspension.

[0136] Example 10 (25% clomazone + 5% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio of 5:1)

[0137] (I) Preparation of 40% Clomazone Microcapsule Suspension

[0138] 41.67% clomazone technical drug (clomazone content 96%) was dissolved in 4% xylene, and then 4% IPDI was added and mixed evenly as the oil phase; 6% polycarboxylate, 0.05% xanthan gum, and 38.88% water were mixed evenly under shear homogenization conditions as the water phase for standby use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 0.3% hexamethylenediamine was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55°C, the system was kept warm for 4h, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5h; finally, the temperature was lowered to 20-25°C after keeping warm for a certain period of time, and the 40% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0139] (II) Preparation of 13.33% terbuthiuron aqueous suspension

[0140] 13.89% terbuthiuron technical (including 96% terbuthiuron content), 3% polycarboxylate, 2% sodium lignin sulfonate, 1% sodium lauryl sulfate, 0.05% xanthan gum, 0.1% methylisothiazolinone, 2% ethylene glycol and 77.96% water were put into a preparation device and dispersed evenly. The material system was ground to a target particle size by a wet grinding process to obtain a 13.3% terbuthiuron aqueous suspension.

[0141] (III) Mixed (25% clomazone + 5% terbuthiuron) microcapsule suspension-suspension concentrate

[0142] The previously prepared 40% clomazone microcapsule suspension and 13.33% terbuthiuron aqueous suspension were mixed in a ratio of 62.5:37.5 and stirred evenly to obtain a (25% clomazone + 5% terbuthiuron) microcapsule suspension-suspension.

[0143] Example 11 (15% clomazone + 15% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:1)

[0144] (I) Preparation of 30% Clomazone Microcapsule Suspension

[0145] Dissolve 31.25% clomazone technical (clomazone content 96%) in 5% solvent oil, then add 3% MDI and mix well as oil phase; take 4% polycarboxylate, 0.1% xanthan gum and 53.05% water and mix well as water phase under shear homogenization conditions; transfer the oil phase to the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.4% hexamethylenediamine and continue stirring; under continuous stirring, heat the emulsion to 55°C, keep the system warm for 4h, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5h; finally keep warm for a certain period of time and then cool to 20-25°C, and the preparation of 30% clomazone microcapsule suspension is completed. Discharge and set aside.

[0146] (II) Preparation of 30% terbuthiuron aqueous suspension

[0147] 31.25% of terbuthiuron technical (including 96% of terbuthiuron content), 4% of polycarboxylate, 0.1% of xanthan gum, 0.2% of methylisothiazolinone, 3% of ethylene glycol and 61.45% of water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 30% terbuthiuron aqueous suspension. The 30% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0148] (III) Mixed isocyanate (15% isocyanate + 15% terbuthiuron) microcapsule suspension-suspension concentrate

[0149] The previously prepared 30% clomazone microcapsule suspension and 30% terbuthiuron aqueous suspension were mixed in a ratio of 1:1 and stirred evenly to obtain a (15% clomazone + 15% terbuthiuron) microcapsule suspension-suspension.

[0150] Example 12 (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:5)

[0151] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0152] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 2% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 68.93% water were mixed evenly under shear homogenization conditions as the water phase for standby use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 0.25% tetraethylene pentamine was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55°C, the system was kept warm for 4h, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5h; finally, the temperature was lowered to 20-25°C after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0153] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0154] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0155] (III) Mixed isocyanate (5% isocyanate + 25% terbuthiuron) microcapsule suspension-suspension concentrate

[0156] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:2 and stirred evenly to obtain a (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension.

[0157] Example 13 (3% clomazone + 30% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:10)

[0158] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0159] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 2% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 68.93% water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 0.25% tetraethylene pentamine was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55°C, the system was kept warm for 4h, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5h; finally, the temperature was lowered to 20-25°C after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0160] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0161] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0162] (III) Mixed isocyanate (3% isocyanate + 30% terbuthiuron) microcapsule suspension-suspension concentrate

[0163] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:4 and stirred evenly to obtain a (3% clomazone + 30% terbuthiuron) microcapsule suspension-suspension.

[0164] Example 14 (1% clomazone + 30% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:30)

[0165] (I) Preparation of 5% clomazone microcapsule suspension

[0166] Dissolve 5.21% clomazone technical (with clomazone content of 96%) in 5% solvent oil, then add 0.4% IPDI and mix well as oil phase; take 3% polycarboxylate, 1% sodium lignin sulfonate, 0.1% xanthan gum and 81.99% water and mix well as water phase under shear homogenization conditions; transfer the oil phase to the water phase, use a high-speed shear emulsifier to shear to obtain an emulsion, then slowly add 0.1% triethylenetetramine and continue stirring; under continuous stirring, heat the emulsion to 55°C, keep the system warm for 4h, add 3% calcium chloride and 0.2% methylisothiazolinone, and continue stirring for 0.5h; E. Finally, keep warm for a certain period of time and then cool to 20-25°C to complete the preparation of 5% clomazone microcapsule suspension. Discharge and set aside.

[0167] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0168] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 4% polycarboxylate, 4% sodium lignin sulfonate, 1% sodium dodecylbenzene sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0169] (III) Mixed isocyanate (1% isocyanate + 30% terbuthiuron) microcapsule suspension-suspension concentrate

[0170] I. The 5% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:4 and stirred evenly to obtain the (5% clomazone + 30% terbuthiuron) microcapsule suspension-suspension.

[0171] Example 15 (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:5)

[0172] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0173] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 2% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 67.18% water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 2% PEG 400 was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55° C., the system was kept warm for 4 hours, and then 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0174] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0175] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0176] (III) Mixed isocyanate (5% isocyanate + 25% terbuthiuron) microcapsule suspension-suspension concentrate

[0177] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:2 and stirred evenly to obtain a (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension.

[0178] Example 16 (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:5)

[0179] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0180] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 1% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 69.18% water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 1% PEG 400 was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55° C., and the system was kept warm for 4 hours, and then 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0181] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0182] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0183] (III) Mixed isocyanate (5% isocyanate + 25% terbuthiuron) microcapsule suspension-suspension concentrate

[0184] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:2 and stirred evenly to obtain a (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension.

[0185] Example 17 (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:5)

[0186] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0187] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 3% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 65.18% water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 3% PEG 400 was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55° C., and the system was kept warm for 4 hours, and then 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0188] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0189] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0190] (III) Mixed isocyanate (5% isocyanate + 25% terbuthiuron) microcapsule suspension-suspension concentrate

[0191] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:2 and stirred evenly to obtain a (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension.

[0192] Example 18 (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension concentrate (mass ratio is 1:5)

[0193] (I) Preparation of 15% Clomazone Microcapsule Suspension

[0194] 15.62% clomazone technical (with clomazone content of 96%) was dissolved in 5% xylene, and then 4% HDI was added and mixed evenly as the oil phase; 3% polycarboxylate, 2% sodium lignin sulfonate, 0.1% xanthan gum, and 63.18% water were mixed evenly under shear homogenization conditions as the water phase for later use; the oil phase was transferred to the water phase, and an emulsified liquid was obtained by shearing with a high-speed shear emulsifier, and then 4% PEG 400 was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55° C., and the system was kept warm for 4 hours, and then 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours; finally, the temperature was lowered to 20-25° C. after keeping warm for a certain period of time, and the 15% clomazone microcapsule suspension was prepared. The material was discharged and set aside.

[0195] (II) Preparation of 37.5% terbuthiuron aqueous suspension

[0196] 39.06% terbuthiuron technical (including 96% terbuthiuron content), 6% polycarboxylate, 3% sodium lignin sulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol and 48.69% water are put into a preparation device and dispersed evenly. The material system is ground to a target particle size by a wet grinding process to obtain a 37.5% terbuthiuron aqueous suspension. The 37.5% terbuthiuron aqueous suspension is stored in a transfer container through a filter for standby use.

[0197] (III) Mixed isocyanate (5% isocyanate + 25% terbuthiuron) microcapsule suspension-suspension concentrate

[0198] I. The 15% clomazone microcapsule suspension prepared earlier and the 37.5% terbuthiuron aqueous suspension were mixed in a ratio of 1:2 and stirred evenly to obtain a (5% clomazone + 25% terbuthiuron) microcapsule suspension-suspension.

[0199] Field test example: Field test on annual weeds in sugarcane fields

[0200] 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. There was no rainfall during the experiment, and the experiment was conducted in spring from March to April.

[0201] There are 21 treatments in total, namely: Treatment 1: clean water spray, blank control; Treatment 2: Example 1; Treatment 3: Example 2; Treatment 4: Example 3; Treatment 5: Example 4; Treatment 6: Example 5; Treatment 7: Example 6; Treatment 8: Example 7; Treatment 9: Example 8; Treatment 10: Example 9; Treatment 11: Example 10; Treatment 12: Example 11; Treatment 13: Example 12; Treatment 14: Example 13; Treatment 15: Example 14; Treatment 16: Example 15; Treatment 17: Example 16; Treatment 18: Example 17; Treatment 19: Example 18; Treatment 20: 360 g / L isoxazolidinone microcapsule suspension (commercially available); Treatment 21: 46% terbuthiuron aqueous suspension (commercially available).

[0202] The recommended dosage of clomazone per hectare is 300 g, and the recommended dosage of terbuthiuron per hectare is 1500 g. The dosage in the embodiment of the present invention is calculated according to the following formula:

[0203] The dosage of M (gai·hm -2 ) = recommended dosage of clomazone (gai·hm -2 )×P 异噁草松 +Recommended dosage of terbuthiuron (gai·hm -2 )×P 特丁噻草隆 .

[0204] Among them, P 异噁草松 , P 特丁噻草隆 and terbuthiuron respectively represent the proportion of the active ingredients of clomazone and terbuthiuron in the compound composition, i.e., P 异噁草松 +P 特丁噻草隆 =100%.

[0205] The pesticide was applied once with a Gongnong-16 backpack manual sprayer, and 450L of water was added to the dosage per hectare to prepare the liquid, and sprayed 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.

[0206] The weed control efficacy of each treatment was investigated 10, 20 and 30 days after application.

[0207] Weed control effectiveness survey method:

[0208] Ten, twenty and thirty days after application, refer to the estimated value survey method in the Pesticide Field Efficacy Test Guidelines (1): Control of Weeds in Sugarcane Fields by Herbicides (GB / T 17980.49-2000) to visually measure the weed coverage of each pesticide treatment area and the adjacent blank control area. The results are expressed as a simple percentage (0 means no control effect, 100% means complete control of weeds). The following grading standards can be used for the survey:

[0209] Level 1: No grass;

[0210] Level 2: Equivalent to 0-2.5% of the blank control area;

[0211] Grade 3: Equivalent to 2.6% to 5% of the vacuolar control area;

[0212] Level 4: Equivalent to 5.1% to 10% of the blank control area;

[0213] Level 5: Equivalent to 10.1% to 15% of the blank control area;

[0214] Level 6: Equivalent to 15.1% to 25% of the sky-day control area;

[0215] Level 7: Equivalent to 25.1% to 35% of the blank control area;

[0216] Level 8: Equivalent to 35.1% to 67.5% of the blank control area;

[0217] Level 9: Equivalent to 67.6% to 100% of the blank control area.

[0218] The formula for calculating the protective effect is as follows:

[0219] Prevention effect (%) = (10-number of treatment area grades) / 9×100%

[0220] The visual control effects 10 days, 20 days and 30 days after application are shown in Table 2.

[0221] Table 2. Results of visual control tests on annual weeds for each treatment agent at 10, 20 and 30 days

[0222]

[0223]

[0224] 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.

[0225]

[0226] The results of the 30-day fresh weight control efficacy are shown in Table 3.

[0227] Table 3 Results of the 30-day fresh weight control test of annual weeds by each treatment agent.

[0228]

[0229]

[0230] It can be seen from the above visual inspection and fresh weight control effect test results that: ① Under the same dosage form, the combination of clomazone and terbuthiuron has a good control effect on annual weeds. Example 15 (clomazone: terbuthiuron = 1:5) has the highest control effect, followed by Example 18 (clomazone: terbuthiuron = 1:5), Example 17 (clomazone: terbuthiuron = 1:5), Example 16 (clomazone: terbuthiuron = 1:5), and Example 12 (clomazone: terbuthiuron = 1:5), which are better than other examples, such as Example 1 (clomazone: terbuthiuron = 40:1), Example 9 (clomazone: terbuthiuron = 20:1), Example 10 (clomazone: terbuthiuron = 5:1), Example 11 (clomazone: terbuthiuron = 1:1), Example 6 (clomazone: terbuthiuron = 1:4), Example 13 (clomazone: terbuthiuron = 1:10), Example 8 (clomazone: terbuthiuron = 3:76), Example 14 (clomazone: terbuthiuron = 1:30), Example 7 (clomazone: terbuthiuron = 1:40) illustrate that reasonable ratios exhibit synergistic effects; from the comparison of the efficacy of each example and a single-dose application, it can be seen that within the ratio range of 40:1 to 1:40, field application has a synergistic effect in controlling annual weeds. ② In terms of dosage form, from the analysis of visual data, 10 days after the application, the difference between the treatments is not large, and the embodiment is slightly better than the comparative example. The reason for the analysis is that the weeds belong to the initial growth and germination stage, the gap is small, and the treatment effect is not obvious. As time goes by, under the same ratio, for example, the microcapsule suspension-suspension agent is better than other dosage forms, such as Example 10 vs. Example 2 (clomazone: terbuthiuron = 5:1), Example 11 vs. Example 3 (clomazone: terbuthiuron = 1:1), Example 12 vs. Example 4 (clomazone: terbuthiuron = 1:5) in 20 days. The visual control effect is better than other dosage forms, and the advantage is more obvious at 30 days. It shows that the microcapsule suspension-suspension agent has better effects than other dosage forms when applied in the field due to its unique sustained release effect and dispersion effect, and has a longer lasting effect. It can achieve the effect of long-term prevention and control with one-time medication, reduce the amount of medication, and reduce labor output. ③ In the test, we found that when Example 15 and Example 12 were compared with the same dosage form and the same ratio, the control effect of Example 15 was better than that of Example 12. The reason for this is that Example 15 uses polyol (PEG 400) as the aqueous phase wall material, and its capsule wall is more flexible. The flexible capsule wall is more conducive to the sustained and stable release of the active ingredient, and also reduces the leaching of microcapsule particles in the soil, thereby increasing the effect of sealing the soil to prevent weeds.④ In terms of the amount of water-phase wall material, among the samples with polyol as the water-phase wall material, when the amount of water-phase wall material is lower, the product has a higher 10-day protection effect and better quick-acting property, but the 30-day protection effect will deteriorate; when the amount of wall material is increased, the quick-acting property of the product deteriorates and the lasting property improves; from the 30-day visual data and fresh weight protection effect, the amount of wall material can affect the efficacy of the drug, and the effect is best when the amount is 2%. 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.

[0231] 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 herbicidal composition containing clomazone and terbuthiuron, characterized in that: The active ingredients in the herbicidal composition include clomazone and terbuthiuron, and the weight ratio of clomazone to terbuthiuron is (0.1:99) to (99:0.1).

2. The herbicidal composition according to claim 1, characterized in that The weight ratio of clomazone and terbuthiuron is (40:1) to (1:40), optionally (20:1) to (1:30), optionally (10:1) to (1:10), optionally (5:1) to (1:10), optionally (5:1) to (1:5), optionally 20:1, 10:1, 5:1, 1:1, 1:5, 1:10 or 1:

20.

3. The herbicidal composition according to claim 1 or 2, characterized in that The active ingredient accounts for 1-99% of the total weight of the composition, optionally 6%-80%, optionally 6%-60%, optionally 30%-40%.

4. The herbicidal composition according to any one of claims 1 to 3, characterized in that The herbicidal composition is in the form of one or more of microcapsule suspension-suspension concentrate, emulsifiable concentrate, aqueous emulsion, dry suspension concentrate, wettable powder, water dispersible granule, granule, and seed treatment agent; Optionally, the herbicidal composition further comprises an adjuvant, and the adjuvant is selected from one or more of solvents, emulsifiers, dispersants, wetting agents, thickeners, fillers, preservatives, antifreeze agents, specific gravity regulators, defoamers, oil phase wall materials, water phase wall materials, and water.

5. The herbicidal composition according to any one of claims 1 to 4, characterized in that The solvent is one or more of N,N-dimethylformamide, cyclohexanone, xylene, methylnaphthalene and solvent oil; And / or, the emulsifier is one or more of EOPO block polyether emulsifier, calcium dodecylbenzene sulfonate, Tween series, and Span series; and / or, the dispersant is one or more of polycarboxylates, lignin sulfonates, and naphthalene sulfonates; And / or, the wetting agent is one or more of sodium dodecyl sulfate and sodium dodecylbenzene sulfonate; And / or, the thickener is one or more of xanthan gum and magnesium aluminum silicate; And / or, the filler is one or more of calcined kaolin, bentonite, diatomaceous earth, attapulgite, fumed silica, corn starch or light calcium carbonate; and / or, the preservative is isomethylthiazolinone; And / or, the antifreeze agent is one or more of ethylene glycol and glycerol; And / or, the specific gravity regulator is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate; optionally, the specific gravity regulator is used as a spray drying aid or a disintegrant; And / or, the defoaming agent is a silicone emulsion; And / or, the oil phase wall material is polyisocyanate; optionally, it is one or more of HDI, IPDI, MDI, and PAPI; And / or, the aqueous phase wall material is one or more of polyamines and polyols. Optionally, the aqueous phase wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine; optionally, the average molecular weight of the polyethylene glycol is 100-2000, optionally 200-800, optionally 300-500, optionally 300-400; optionally, the polyethylene glycol is PEG400; And / or, the granular carrier may be coal gangue.

6. A microcapsule suspension-suspension concentrate comprising the herbicidal composition according to any one of claims 1 to 5, characterized in that: It comprises a clomazone microcapsule suspension and a terbuthiuron aqueous suspension. Optionally, the weight ratio of the clomazone microcapsule suspension to the terbuthiuron aqueous suspension is (1-3): (2-6).

7. The microcapsule suspension-suspending agent according to claim 6, characterized in that: The clomazone microcapsule suspension comprises the following raw materials in weight fractions: 5-60% clomazone, 2-20% solvent, 1-10% oil phase wall material, 1-10% dispersant, 50-70% water, 0.2-6.0% water phase wall material, 0-5% specific gravity regulator, and 0-1% preservative; Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 10-20% clomazone, 4-10% solvent, 1-6% oil phase wall material, 5-10% dispersant, 60-70% water, 0.25-4.0% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative; Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15-20% clomazone, 5-10% solvent, 1-4% oil phase wall material, 5-10% dispersant, 65-70% water, 0.25-4.0% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative; Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 1-4% oil phase wall material, 5% dispersant, 65-70% water, 0.25-4.0% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative; Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 2-4% oil phase wall material, 5% dispersant, 65-70% water, 1-4% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative; Optionally, the clomazone microcapsule suspension comprises the following raw materials in weight fractions: 15% clomazone, 5% solvent, 2% oil phase wall material, 5% dispersant, 65-70% water, 2-4% water phase wall material, 3-5% specific gravity regulator, and 0.1-1% preservative; Optionally, the oil phase wall material is polyisocyanate, which may be one or more of HDI, IPDI, MDI, and PAPI; Optionally, the aqueous phase wall material is one or more of a polyol or a polyamine, and optionally, the aqueous phase wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine; optionally, the average molecular weight of the polyethylene glycol is 100 to 2000, optionally 200 to 800, optionally 300 to 500, optionally 300 to 400; optionally, the polyethylene glycol is PEG400; Optionally, the specific gravity regulator is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate; Optionally, the dispersant is one or more of polycarboxylate, lignin sulfonate, and naphthalene sulfonate; Optionally, the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (3-6): (2-4); Optionally, the preservative is isomethylthiazolinone.

8. The microcapsule suspension-suspending agent according to claim 6 or 7, characterized in that: The terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 20-50%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5% and water 35-50%; Optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: 30-40% terbuthiuron, 5-15% dispersant, 0-1% thickener, 0-1% preservative, 0-5% antifreeze agent and 35-50% water; Optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 35-40%, dispersant 9-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5% and water 45-50%; Optionally, the terbuthiuron aqueous suspension comprises the following raw materials in weight fractions: terbuthiuron 35-40%, dispersant 9-15%, thickener 0.1-1%, preservative 0.15-1%, antifreeze 3-5% and water 45-50%; Optionally, the dispersant is one or more of polycarboxylates, lignin sulfonates, and naphthalene sulfonates; optionally, the dispersant comprises polycarboxylates and lignin sulfonates in a weight ratio of (3-9): (2-5); optionally, the dispersant comprises polycarboxylates and lignin sulfonates in a weight ratio of (6-8): (3-4); Optionally, the antifreeze agent is one or more of ethylene glycol and glycerol; Optionally, the preservative is isomethylthiazolinone; Optionally, the thickener is one or more of xanthan gum and magnesium aluminum silicate.

9. A method for preparing the microcapsule suspension-suspension concentrate according to claim 7 or 8, characterized in that: 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 the water phase wall material, 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 terbuthiuron aqueous suspension: The terbuthiuron, dispersant, thickener, preservative, antifreeze agent and water are mixed and wet-grinded to a target particle size to obtain a terbuthiuron aqueous suspension; 3) The materials of step 1) and step 2) are mixed to prepare a microcapsule suspension-suspension concentrate.

10. Use of the herbicidal composition according to any one of claims 1 to 5, or the microcapsule suspension-suspension concentrate according to any one of claims 6 to 8, or the microcapsule suspension-suspension concentrate prepared by the preparation method according to claim 9 for controlling weeds in farmland before crop planting, before seeding after sowing, or during the crop growth period; optionally, the weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of crabgrass, goosegrass, and Amaranthus retroflexus.

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