A topramezone·isopropylammonium sulfate suspension agent, a preparation method and application thereof

Abstract

The present application relates to the technical field of pesticides, in particular to a kind of mesopotamia · isopropylone suspending agent and its preparation method and application, by weight percentage, including: mesopotamia crude drug 5~10%, isopropylone crude drug 30~50%, wetting dispersant 10%~15%, anti-settling thickener 0.3%~1.5%, antifreeze 3~5%, antifoaming agent 0.01~0.5%, fungicide 0.01~0.2%, deionized water makes up the rest amount, while ensuring the sanding efficiency of product, thermal storage stability, cold storage stability, wetting spreading property, better satisfy the actual application demand.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of pesticides, in particular to a kind of sulfentrazone · isopropylol suspending agent and its preparation method and application. BACKGROUND

[0002] Sulfentrazone is a new type of broad-spectrum, high-activity pre-emergence soil treatment agent developed by Japan Combination Chemical Company, which belongs to isoxazole herbicide. After application, it is absorbed by weed seedling roots and young shoots, inhibits early growth of seedlings, destroys meristem and hypocotyl, and is a serious potential inhibitor in VLCFA (very long chain fatty acid) biosynthesis (C20-C30) in plant body. It mainly inhibits the activity of photosystem II by blocking the electron flow between primary acceptor (QB binding site of D1 protein) and secondary acceptor (plastoquinone) in photosystem II, leading to the production of reactive oxygen species (ROS) in plants, and then inhibiting the production of ATP and NADPH2. At present, the compound preparation of sulfentrazone and isopropylol mainly focuses on improving the weed control effect of crops. For example, Chinese patent (authorized publication number CN116158442B) discloses a composition containing sulfentrazone and isopropylol, and Chinese patent application (publication number CN108293988A) provides a herbicidal composition containing sulfentrazone and its use. Although the surface tension of the drug solution and the contact angle between the drug solution and the weed leaf surface can be effectively reduced to a certain extent by optimizing the adjuvant, the water dispersion effect of the preparation needs to be further improved in actual application, and the stability of the preparation under high and low temperature conditions also needs to be further improved. SUMMARY

[0003] In one aspect, the present application provides a kind of sulfentrazone · isopropylol suspending agent, by weight percentage, including: sulfentrazone 5-10%, isopropylol 30-50%, wetting dispersant 10%-15%, anti-settling thickener 0.3%-1.5%, antifreeze 3-5%, defoamer 0.01-0.5%, bactericide 0.01-0.2%, and the rest is deionized water.

[0004] As a preferred technical solution, the mass ratio of the sulfentrazone and isopropylol is 1: (4-6), preferably 1:5. Based on the system of the present application, sulfentrazone and isopropylol are used as effective active ingredients, and especially controlling the mass ratio of sulfentrazone and isopropylol to be 1: (4-6) has good synergistic effect. Under the action of a certain wetting dispersant, anti-settling thickener and other adjuvants, the sulfentrazone · isopropylol suspending agent provided has excellent weed control effect on crops, can meet the needs of annual weed control in winter wheat field, and the effect is less affected by the environment.

[0005] As a preferred technical solution, the wetting dispersant at least comprises a weak cationic polycarboxylic acid dispersant, a rosin ether modifier dispersant, and a block copolymer dispersant.

[0006] As a preferred technical solution, the weak cationic polycarboxylic acid dispersant is SP-SC3275 (a product of Qianyu Chemicals).

[0007] As a preferred technical solution, the rosin ether modifier dispersant is SP-SC3 (a product of Qianyu Chemicals).

[0008] As a preferred technical solution, the block copolymer dispersant at least comprises an EO / PO block polyether (a block copolymer composed of EO (oxyethylene ether) and PO (oxypropylene ether)) and a polyethylene / polypropylene block copolymer.

[0009] Preferably, the average molecular weight of the EO / PO block polyether is 2000-4000, and preferably Ethylan Ns-5001q (a product of Noligen).

[0010] Preferably, the polyethylene / polypropylene block copolymer is EZ TABS (a product of Nippon Shokubai).

[0011] As a preferred technical solution, the mass ratio of the weak cationic polycarboxylic acid dispersant, the rosin ether modifier dispersant, the EO / PO block polyether, and the polyethylene / polypropylene block copolymer is 3:3:2:(1-8), preferably 3:3:2:(3-6), and most preferably 3:3:2:5.

[0012] The suspension concentrate product provided by the present application, in order to ensure the prevention effect, optimizes the ratio of the raw material of pyroxasulfone and the raw material of isopropylol, and controls the total addition amount of the raw material of pyroxasulfone and the raw material of isopropylol in the product to be greater than or equal to 40 wt%, which greatly increases the difficulty of controlling the stability of the product, and to some extent, affects the sanding efficiency. In the early stage of the present application, the conventional carboxylate dispersant is used in combination with naphthalenesulfonate condensate and phosphate ester as an auxiliary system, although the heat storage and cold storage stability of the prepared product can be effectively controlled, the sanding efficiency is low, the wetting and spreading property is poor, the preparation enters water in a dispersed mass, and the dispersion effect is not good. In order to improve the above problems, and to provide a product with corresponding soil sealing effect, the product system is optimized to introduce synergist lignin and naphthalenesulfonate condensate in combination with phosphate ester, weak cationic polycarboxylic acid dispersant, rosin ether modifier dispersant, and block copolymer dispersant to prepare a suspension concentrate product, which can effectively improve the wetting and spreading property and the sanding efficiency of the product, but the heat storage stability of the product is destroyed, and after heat storage, the bottom is precipitated, the suspension rate is reduced, or the sieve analysis has the phenomenon of precipitate, which cannot meet the actual application requirements. Based on the unexpected discovery of a large number of auxiliaries in the screening process, by simultaneously introducing weak cationic polycarboxylic acid dispersant, rosin ether modifier dispersant, and block copolymer dispersant, especially the block copolymer dispersant at least including EO / PO block polyether and polyethylene / polypropylene block copolymer, under the combined action of other raw materials in the system, the sanding efficiency, heat storage stability, cold storage stability, and wetting and spreading property of the product are ensured, and the actual application requirements are better met.

[0013] As a preferred technical solution, the antifreeze agent at least includes ethylene glycol.

[0014] As a preferred technical solution, the anti-settling thickening agent at least includes magnesium aluminum silicate and xanthan gum.

[0015] Preferably, the mass ratio of the magnesium aluminum silicate and the xanthan gum is (8-12):1, preferably 10:1.

[0016] As a preferred technical solution, the defoaming agent at least includes silicone defoaming agent, and the silicone defoaming agent is preferably SAG 1572 (Maitian auxiliary).

[0017] Further, the present application controls the addition amount of the anti-settling thickening agent in the suspension concentrate product system and the selection and combination of the anti-settling thickening agent, especially uses magnesium aluminum silicate and xanthan gum with a mass ratio of (8-12):1 as the anti-settling thickening agent, and combines the wet dispersant system in the system, to obtain a suspension concentrate product with low viscosity, good water dispersibility, good heat storage stability, and good cold storage stability.

[0018] In addition, the suspension agent product provided by the application has excellent dispersion stability at a low dilution multiple, high suspension rate, and is resistant to volatilization and drift, and the mist droplet size is more uniform, can be uniformly dispersed in the soil after implementation of the prevention, and greatly enhances the application in the soil sealing effect with the aid of good adhesion and spreading properties.

[0019] As a preferred technical solution, the fungicide at least comprises 1,2-benzisothiazolin-3-one (BIT).

[0020] Another aspect of the application provides a preparation method of the metrafenone·isopropylthiolone suspension agent, at least comprising the following steps: adding deionized water, isopropylthiolone raw material, metrafenone raw material, wetting dispersant, antifreeze, anti-settling thickening agent, fungicide, and defoaming agent into a container, stirring and mixing, shearing and dispersing, and sand milling treatment to obtain the metrafenone·isopropylthiolone suspension agent.

[0021] As a preferred technical solution, the shearing and dispersing time is 3-8 min.

[0022] As a preferred technical solution, the sand milling treatment time is 2-2.5 h.

[0023] The suspension agent product provided by the application can control the sand milling particle size to be below 2.5 μm within 2-2.5 h by optimizing the combination of raw materials, greatly improving the production efficiency, and being easy to realize large-scale industrial production and popularization and application.

[0024] The third aspect of the application provides an application of the metrafenone·isopropylthiolone suspension agent, which is applied to the prevention and control of annual grass weeds and annual broadleaf weeds in winter wheat fields.

[0025] Beneficial effects

[0026] 1. Based on the system of the application, sulfentrazone and isopropylthiolone are used as effective active ingredients, and in particular, the combination of sulfentrazone and isopropylthiolone in a mass ratio of 1:(4-6) has good synergistic effect, under the action of a specific wetting dispersant, anti-settling thickening agent and other adjuvants, the metrafenone·isopropylthiolone suspension agent product provided by the application has excellent prevention effect on crop weeds, can meet the demand for prevention and control of annual weeds in winter wheat fields, and the prevention effect is less affected by the environment.

[0027] 2、The present application can ensure sanding efficiency, thermal storage stability, cold storage stability and wet spreading property of the product by simultaneously introducing weak cationic polycarboxylic dispersant, rosin ether modifier dispersant and block copolymer dispersant, especially the block copolymer dispersant comprising at least EO / PO block polyether and polyethylene / polypropylene block copolymer, and the cooperation of other raw materials in the system.

[0028] 3、The present application can obtain a suspension concentrate product with low viscosity, good water dispersion, good thermal storage stability and good cold storage stability by controlling the addition amount of anti-settling thickener in the product system and the selection and cooperation of the anti-settling thickener, especially by using magnesium aluminum silicate and xanthan gum with a mass ratio of (8-12) : 1 as the anti-settling thickener, and cooperating with the wet dispersant system in the system.

[0029] 4、The suspension concentrate product provided by the present application has excellent dispersion stability at a low dilution ratio, high suspension rate, and is resistant to volatilization and drift, and the droplet size is more uniform, and after implementation of the prevention and control, can be uniformly dispersed in the soil, and with good adhesion and spreading property, greatly enhances the application in soil sealing.

[0030] 5、The suspension concentrate product provided by the present application can control the sanding particle size to be below 2.5 μm within 2-2.5 h by optimizing the cooperation of raw materials, greatly improves the production efficiency, and is easy to realize large-scale industrial production and popularization and application. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 The suspension concentrate soil sealing effect comparison chart is provided for Example 1 and Comparative Example 1, wherein a corresponds to Example 1, and b corresponds to Comparative Example 1.

[0032] Figure 2 The suspension concentrate product state chart after thermal storage is provided for Comparative Example 2.

[0033] Figure 3 The suspension concentrate product wet spreading property comparison chart is provided for Example 1 and Comparative Example 4, wherein the left side corresponds to Example 1, and the right side corresponds to Comparative Example 4.

[0034] Figure 4 The suspension concentrate product state chart after thermal storage and screening is provided for Comparative Example 5.

[0035] Figure 5 The suspension concentrate product state chart after thermal storage is provided for Comparative Example 7. DETAILED DESCRIPTION

[0036] Example 1, Comparative Examples 1-7

[0037] Embodiment 1, Comparative Examples 1-7 of the present application provides a suspension concentrate of metalosate-methyl isopropyl amine, the formula is shown in Table 1.

[0038] Table 1

[0039]

[0040]

[0041] In Table 1: weak cationic polycarboxylic acid dispersant is SP-SC3275 (Qianyu Adjuvant). Rosin ether modifier dispersant is SP-SC3 (Qianyu Adjuvant). The average molecular weight of EO / PO block polyether is 4000, EthylanNs-500lq (Nuolong Adjuvant). Polyethylene / polypropylene block copolymer is EZ TABS (Ningbodi). Silicone defoamer is SAG 1572 (Meitu Adjuvant). Carboxylate dispersant is D900 (Fangzhong Adjuvant). Lignin is WG4 (Jieshi Adjuvant). Naphthalene sulfonate condensate is Morwet D-425 (Nuolong Adjuvant). Phosphate ester dispersant is DS505 (Fangzhong Adjuvant).

[0042] Embodiment 1, Comparative Examples 1-7 of the present application provides a preparation method of a suspension concentrate of metalosate-methyl isopropyl amine, which specifically comprises the following steps: adding deionized water, isopropyl amine technical material, metalosate-methyl technical material, wetting dispersant, antifreeze, anti-settling thickener, bactericide, defoamer into a container and stirring to mix, shearing and dispersing for 5 min, and then using a vertical sand mill for sand milling treatment for 2 h to obtain the suspension concentrate of metalosate-methyl isopropyl amine.

[0043] Performance test method

[0044] 1. The suspension concentrate product provided by Embodiment 1 is subjected to each physical and chemical performance test in Table 2, the test basis, test result index and test result are shown in Table 2.

[0045] Table 2

[0046]

[0047] 2. The suspension concentrate product provided by Embodiment 1, Comparative Examples 1-7 is subjected to each test in Table 3, and the test result is shown in Table 3. The product state diagram of the suspension concentrate product provided by Comparative Example 2 after heat storage appears creaming, which is shown in Figure 2 , the wetting and spreading property comparison of the suspension concentrate products provided by Embodiment 1 and Comparative Example 4 is shown in Figure 3 , the product state of the suspension concentrate provided by Comparative Example 5 after heat storage and screening appears precipitate, which is shown in Figure 4 , the product state of the suspension concentrate provided by Comparative Example 7 after heat storage appears bottoming, which is shown in Figure 5 .

[0048] Table 3

[0049]

[0050] Note: The sand milling efficiency in Table 3 is based on the particle size after sand milling for 2 hours according to the preparation process of Example 1 and Comparative Examples 1-7. The smaller the particle size, the higher the sand milling efficiency within the same time.

[0051] 3. The soil sealing effect test was conducted on the products provided by Example 1 and Comparative Example 1. The test method was as follows: the products provided by Example 1 and Comparative Example 1 were used in the soil before wheat germination (application method and water amount: conventional spraying method, water amount per mu was 30 liters, and the effective component amount was 576 grams per hectare). The weed situation in the wheat planting field was observed 35 days after application. The test results are shown in Table 2. Figure 1 Figure 1 It can be seen from the analysis that the sealing effect of the suspension concentrate provided by Example 1 was obvious after use, and there was basically no weed in the later period (preventing weed germination); while after using the suspension concentrate product provided by Comparative Example 1, part of the weeds in the trench section still germinated, and there were new weeds, and the sealing effect was worse than that of Example 1.

[0052] 4. Field efficacy test was conducted on the suspension concentrate product provided by Example 1.

[0053] In 2023, a field efficacy test of 48% metrafenone·isopropylthiolone suspension concentrate (Example 1) for controlling annual weeds in winter wheat field was conducted in Zhonglongxiao wheat planting field in Danfeng Street, Shizong County, Qujing City, Yunnan Province. Control object: annual grass weeds: Alopecurus aequalis Sobol., Poa annua L.; annual broadleaf weeds: Stellaria media (L.) Cyr.

[0054] The test agent is shown in Table 4.

[0055] Table 4

[0056]

[0057] Application method and water amount: conventional spraying method, water amount per mu was 30 liters.

[0058] The plant control efficiency of 48% metrafenone·isopropylthiolone suspension concentrate for controlling annual weeds in winter wheat field (35 days after application) is shown in Table 5.

[0059] Table 5

[0060]

[0061]

[0062] ​48% of pyroxasulfone · isopropylone suspension agent control winter wheat field annual weed fresh weight control effect (95 days after treatment) see table 6.

[0063] Table 6

[0064]

[0065]

Claims

1. A mixture of pyroxasulfone • isopropylolone suspension characterized in that, By weight percentage, include: mefenoxam technical 8%, isopropyl technical 40%, wetting dispersant 13%, anti-settling thickening agent 0.66%, anti-freezing agent 4%, defoaming agent 0.1%, bactericide 0.1%, deionized water to fill the balance; the wetting dispersant includes weak cationic polycarboxylic acid dispersant, rosin ether modifier dispersant and block copolymer dispersant, the block copolymer dispersant includes EO / PO block polyether and polyethylene / polypropylene block copolymer; the mass ratio of the weak cationic polycarboxylic acid dispersant, rosin ether modifier dispersant, EO / PO block polyether, polyethylene / polypropylene block copolymer is 3:3:2:5; the weak cationic polycarboxylic acid dispersant is SP-SC3275; the rosin ether modifier dispersant is SP-SC3; the anti-settling thickening agent includes magnesium aluminum silicate and xanthan gum with a mass ratio of 10:1; the anti-freezing agent is ethylene glycol; the bactericide is 1,2-benzisothiazolin-3-one; the defoaming agent is silicone defoaming agent.

2. A method for preparing the preparation of the sulfonylurea pyroxasulfone • ipro- lefone suspension according to claim 1, characterized in that, Deionized water, isopropyl technical, mefenoxam technical, wetting dispersant, anti-freezing agent, anti-settling thickening agent, bactericide, defoaming agent are added into a container and stirred to mix, then shearing dispersion, sand mill treatment to obtain mefenoxam•isopropyl suspension concentrate.

3. The use of the mefenoxam•isopropyl suspension concentrate according to claim 1 in the control of annual grass weeds and annual broadleaf weeds in winter wheat fields.

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