Nano suspending agent containing fluorine chlorine bisamide and chlorfenapyr

Abstract

The invention relates to the technical field of pesticides, and discloses a nanometer suspending agent containing fluorine chlorine bisamide and chlorfenapyr, and the nanometer suspending agent comprises 1%-30% of fluorine chlorine bisamide, 1%-30% of chlorfenapyr, and the balance of agriculturally acceptable auxiliary agents. The nano suspending agent prepared by the invention can obviously improve the stability of effective components, is high in wetting and infiltration capacity and high in activity to target crops, can obviously reduce the dosage, and is safe to the environment.

Description

Technical Field

[0001] This invention belongs to the field of pesticide technology, specifically relating to a nano-suspension containing chlorantraniliprole and bromonitrile. Background Technology

[0002] Fluroxyfenozide belongs to the benzamide class of insecticides. It can effectively activate ryanodine receptors in insects, leading to the excessive release of calcium ions from cellular calcium stores, resulting in paralysis and death of insects. This compound was independently developed by the group, and the compound patent (CN106977494B) has been granted.

[0003] Bromnifloxacin is a novel pyrrole compound that acts on the mitochondria of insect cells, exerting its effects through multifunctional oxidases within the insect body, primarily inhibiting the conversion of adenosine diphosphate (ADP) to adenosine triphosphate (ATP). Bromnifloxacin is characterized by its broad insecticidal spectrum, high efficacy, long-lasting effect, and safety, making it effective in controlling resistant pests.

[0004] CN111789123A discloses an insecticidal composition containing chlorantraniliprole, comprising active ingredient A (chlorantraniliprole) and active ingredient B (bromnifenac), and discloses the formulation and preparation method of a 30% chlorantraniliprole·bromnifenac suspension concentrate (1:2). CN114732022A discloses the use of an insecticidal composition containing chlorantraniliprole for controlling beet armyworm and aphids on crops, and discloses the formulation and preparation method of a 15% chlorantraniliprole·bromnifenac suspension concentrate (1:1). Pesticide suspension concentrates are one of the most important and high-performance water-based pesticide formulations, and their development has been rapid, earning them the title of a revolutionary new formulation in the domestic and international pesticide fields.

[0005] The existing suspension concentrates of flufenoxuron and brofenoxuron disclosed in the technology have problems such as poor dispersibility, easy occurrence of Austronesian ripening, and poor suspension stability during processing, preparation, production and sales. These problems are not conducive to the active ingredients entering the target to exert their efficacy, resulting in low biological activity and target utilization. In particular, when crop pests such as diamondback moth and beet armyworm have outbreaks, multiple applications of pesticides are required for control, leading to excessive pesticide residues in crops and causing environmental pollution.

[0006] To address the aforementioned issues, this application provides a nano-suspension containing chlorantraniliprole and bromuconazole, and its preparation method. This formulation can significantly improve the stability of the active ingredients, has strong wetting and penetration capabilities, high activity against target crops, can significantly reduce the amount of pesticide used, and is environmentally safe. Summary of the Invention

[0007] This invention addresses the shortcomings of existing technologies by providing a nano-suspension agent containing flufenoxuron and bromfenoxuron, which improves the stability of flufenoxuron and bromfenoxuron, has strong wetting and penetrating capabilities, high activity on target crops, can significantly reduce pesticide dosage, and is environmentally safe.

[0008] To achieve the above-mentioned objectives, the technical solution adopted in this invention is as follows: a nano-suspension agent containing chlorantraniliprole and bromfenac, characterized in that, calculated by weight percentage, it comprises: 1%–30% chlorantraniliprole, 1%–30% bromfenac, the remainder being 1%–20% agriculturally acceptable wetting and dispersing agent, 0.1%–2% thickener, 1%–10% antifreeze agent, 0.01%–0.3% preservative, 0.1%–5% defoamer, 0.5%–10% wetting and penetrating agent, and deionized water to make up to 100%;

[0009] Furthermore, the mass ratio of fluchlorfenapyr to bromuconazole is 1:5 to 5:1, such as 1:5, 1:4, 1:3, 1:2, 1:1, 2:1, 3:1 or any value between the above values;

[0010] Furthermore, the weight percentage of fluchlorfenapyr and brofenoxam in the nano-suspension is 10% to 40%, such as 10%, 15%, 20%, 30%, 35%, 40%, or any value between the above values;

[0011] Furthermore, the mass ratio of the wetting and dispersing agent is 4% to 15%, such as 4%, 5%, 6%, 9%, 10%, or any value between the above values;

[0012] Furthermore, the mass ratio of the wetting and dispersing agent is 6% to 9%;

[0013] A nano-suspension containing flufenoxuron and bromfenac, comprising, by weight percentage: 1%–30% flufenoxuron, 1%–30% bromfenac, with the remainder being 1%–20% agriculturally acceptable wetting and dispersing agents, 0.1%–2% thickeners, 1%–10% antifreeze agents, 0.01%–0.3% preservatives, 0.1%–5% defoamers, 0.5%–10% wetting and penetrating agents, and deionized water to bring the total to 100%.

[0014] A nano-suspension containing flufenoxuron and bromfenac, comprising, by weight percentage: 2%–20% flufenoxuron, 5%–30% bromfenac, with the remainder being agriculturally acceptable wetting and dispersing agents (6%–9%), thickeners (0.65%), antifreeze agents (5%), preservatives (0.03%), defoamers (0.5%), wetting and penetrating agents (5%–6%), and deionized water to bring the total to 100%.

[0015] A nano-suspension containing flufenoxuron and bromfenac, by weight percentage, comprises: 10% flufenoxuron, 20% bromfenac, with the remainder being 6%–9% agriculturally acceptable wetting and dispersing agent, 0.65% thickener, 5% antifreeze agent, 0.03% preservative, 0.5% defoamer, 5%–6% wetting and penetrating agent, and deionized water to bring the total to 100%.

[0016] A nano-suspension containing flufenoxuron and bromfenac, by weight percentage, comprises: 15% flufenoxuron, 15% bromfenac, the remainder being 6%–9% agriculturally acceptable wetting and dispersing agent, 0.65% thickener, 5% antifreeze agent, 0.03% preservative, 0.5% defoamer, 5%–6% wetting and penetrating agent, and deionized water to bring the total to 100%.

[0017] A nano-suspension containing flufenoxuron and bromfenac, comprising, by weight percentage: 7.5% flufenoxuron, 7.5% bromfenac, with the remainder being 6% agriculturally acceptable wetting and dispersing agent, 0.65% thickener, 5% antifreeze agent, 0.03% preservative, 0.5% defoamer, 5% wetting and penetrating agent, and deionized water to bring the total to 100%.

[0018] Further, the wetting and dispersing agent is selected from one or more of the following: alkylnaphthalene formaldehyde condensate sulfonate, alkylphenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether sulfonate, phenethylphenol polyoxyethylene ether phosphate, alkyl polyoxyethylene ether sulfonate, polyoxyethylene polyoxypropylene ether block copolymer, dodecyl polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, nonylphenol polyoxyethylene ether phosphate, naphthalene sulfonate formaldehyde condensate sodium salt block copolymer, polycarboxylate, sodium polycarboxylate, lignin sulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, phenethylphenol polyoxyethylene ether phosphate, alkyl sulfate, isopropyl alkyl sulfonate, alkylnaphthalene sulfonate, sulfonate anions, alkylphenol formaldehyde resin polyoxyethylene ether, triphenylethylphenol polyoxypropylene polyoxyethylene block polymer, sodium dodecyl sulfate, styrene-based phenol formaldehyde resin propylene oxide block polyether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, alkyl glycoside, and fatty alcohol polyoxyethylene ether sodium sulfonate.

[0019] In some embodiments, the wetting and dispersing agents are isopropyl naphthalene sulfonate ULTRASURGF4075 (Wuxi Yijingfeng), alkyl naphthalene sulfonate Morwet EFW (Nanjing Jierun), polycarboxylate 2700 (Kain Chemical), phosphate ester 7260-C (Nanjing Taihua), block copolymer dispersant D-800 (Dow Chemical), naphthalene sulfonate 2020 (Kain Chemical), lignin sulfonate YUS-WG4 (Shanghai Jieshi), and lignin sulfonate YUS-RXB (Shanghai Jieshi).

[0020] Furthermore, the wetting and dispersing agent is a mixture of block copolymer dispersant D-800, phosphate ester 7260-C, and polycarboxylate 2700;

[0021] Furthermore, the mass ratio of block copolymer dispersant D-800, phosphate ester 7260-C, and polycarboxylate 2700 is 1:3:2, 1:2:3, 1:1:1, 2:3:1, 2:1:3, 3:2:1, 3:1:2, and 4:1:1.

[0022] Furthermore, the thickener is selected from one or more of xanthan gum, magnesium aluminum silicate, silica, polyvinyl alcohol, carboxymethyl cellulose, carboxyethyl cellulose, and methyl cellulose;

[0023] Furthermore, the thickener is selected from one or more of xanthan gum, magnesium aluminum silicate, and organobentonite;

[0024] Furthermore, the thickener is a mixture of xanthan gum and magnesium aluminum silicate;

[0025] Furthermore, the antifreeze is selected from one or more of ethylene glycol, propylene glycol, glycerol, urea, polyethylene glycol, and sorbitol;

[0026] Furthermore, the antifreeze is selected from one or more of ethylene glycol, propylene glycol, and glycerol;

[0027] Furthermore, the antifreeze agent is propylene glycol;

[0028] Furthermore, the preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate, Kathon, and benzisothiazolinone;

[0029] Furthermore, the preservative is benzisothiazolinone;

[0030] Furthermore, the defoamer is selected from silicone compounds, silicone oils, and C. 10-20 Saturated fatty acid compounds, C 8-10 One or more of the following: fatty alcohols, hexanol, butanol, and octanol;

[0031] Furthermore, the defoamer is an organosilicone defoamer;

[0032] In some embodiments, the defoamer is silicone defoamer 0050 (Gutian Chemical);

[0033] Furthermore, the wetting and penetrating agent is selected from organosilicon wetting and penetrating agent 810 (Momentive), fatty alcohol ether wetting and penetrating agent CYAX (Solvay), nonionic wetting and penetrating agent EH-6 (Gutian Chemical), and alkyl sulfonate sodium salt anionic nonionic composite YUS-AN4 (Shanghai Jieshi).

[0034] In some embodiments, the wetting and penetrating agent is wetting and penetrating agent EH-6;

[0035] This invention also provides a method for preparing a nano-suspension containing chlorantraniliprole and bromfenac, characterized by the following steps: weighing chlorantraniliprole, bromfenac, wetting and dispersing agent, antifreeze, defoamer, and deionized water in proportion, homogenizing and mixing them by shearing, pouring the mixture into a milling jar, adding zirconia beads with a particle size of 0.2-0.6 mm, milling, and waiting for the particle size D... 50 After reaching a particle size of 0.1–0.6 μm, thickener, preservative, and wetting and penetrating agent are added, and the mixture is sheared and homogenized to obtain a nano-suspension.

[0036] Furthermore, the zirconium oxide beads have a particle size of 0.2–0.3 mm.

[0037] The use of a nano-suspension containing chlorantraniliprole and bromfenac, wherein the use is for the control of lepidopteran pests.

[0038] Furthermore, the aforementioned lepidopteran pests include: *Adoxophyes spp.*, *Adoxophyes orana*, *Agrotis spp.* (root cutter), *Agrotis ipsilon* (black cutworm), *Alabama argillacea* (cotton leafworm), *Amorbia cuneana*, *Amyelosis transitella* (navelorange worm), *Anacamptodes defectaria*, *Anarsia lineatella* (peach twig borer), *Anomis sabulifera* (jute looper), *Antica rsia g emma ta lis*, *Archi ps argyrospila* (fruittree leafroller), and *Archips rosana* (rose leafroller). The following are listed as leaf rollers, tortricid moths, orange tortrix, Autographa gamma, Bonagota cranaodes, rice leaf folder, cotton leaf perforator, leaf miners, Ca pua reticulana, peach fruit moth, Chilo spp., mango shoot borer, obliquebanded leafroller, and noctuid moths.The following species are listed: *Cnaphalocerus medinalis* (grass leafroller), *Colias* spp., *Conpomorpha cramerella*, *Cossus cossus* (carpenter moth), *Crambus* spp. (soil webworms), *Cydiafunebrana* (plum fruit moth), *Cydia molesta* (oriental fruit moth), *Cydia nignicana* (pea moth), *Cydiapomonella* (codling moth), *Darna diducta*, and *Diaphania* spp. (stem borer). *Diatraea* spp. (stalk borers), *Diatraeas accharalis* (sugarcane borer), *Diatraea graniosella* (southwester corn borer), *Earias* spp. (cotton bollworm), *Earias insulata* (Egyptian cotton bollworm), *Earias vitella* (rough northern bollworm), *Ecdytopopha aurantianum*, *Elasmopalpus lignosellus* (lesser cornstalk borer), *Epiphysias postruttana* (light brown apple moth), *Ephestia* spp. (flour moths), *Ephestia* cautella (almond moth), Tobacco moth (Ephestia elutella), Mediterranean flour moth (Ephestia kuehniella), and species of the genus Epimeces (Epimeces spp.).), Epinotia aporema, Erionotathrax (banana skipper), Eupoecilia ambiguella (grape leafroller), Euxoa auxiliaris (army cutworm), Feltia spp. (root cutter), Gortyna spp. (stemborers), Grapholitamolesta (oriental fruit borer).

[0039] (oriental fruit moth)), Hedylepta indicate (bean leaf webber), Helicoverpa sp p. (noctus moth), Helicoverpa armigera, Helicoverpa zea, Heliothis spp., Heliothis virescens, Hellula undalis (cabbage webworm), Indarbela spp. (root borers), Keiferia lycopersicella, Leucinodes orbonalis, Leucoptera malifoliella, Lithocollectis spp., Lobesia botrana (grape fruit moth) The following species are listed: fruitmoth, Loxagrotis spp., Loxagrotis albicosta (western bean cutworm), Lymantria dispar (gypsy moth), Lyonetia clerkella (apple leaf miner), Mahasena corbetti (oil palm bagworm), and Malacosoma spp.(tent caterpillars), cabbage armyworm (Mamestra brassicae), bean pod borer (Maruca testulalis), bagworm (Metisa plana), true armyworm (Mythimna unipuncta), elegantalis (Neoleucinodes elegantalis), depunctalis (Nymphula depunctalis), winter inchworm (Operophtherabrumata), European corn borer (Ostrinia nubilalis), Oxydiavesulia, common currant tortrix (Pandemis cerasana), brown apple tortrix (Pandemis heparana), African swallowtail butterfly (Papilio demodocus), pink bollworm (Pectinophora gossypiella). The following species are listed: bollworm, Peridroma saucia (variegated cutworm), Perileucoptera coffeella (white coffee leafminer), Phthorimaea operculella (potato tuber moth), and citrus leafminer.

[0040] Phyllostachysitis citrella, Phyllostachys spp., Pierisrapae, Platypena scabra, Plodia interpunctella, Plutella xylostella (diamondback moth), Polychrosis viteana (grape leafroller), Prays endocarpa, Prays oleae (olive moth), Pseudaletia spp. (noctus), Pseudaletia unipunctata (armyworm), Pseudoplusia includes (soybean noctus), Rachiplusia nu, Scirpophaga incertulas, Sesamia spp. (stemborers), pink rice stem borer (Sesamia inferens), nonagrioides, setora nitens, grain moth (Angoumois grain moth), grape pill roller (Sparganothis pilleriana), Spodoptera spp., beet armyworm (Spodoptera exigua), fall armyworm (Spodoptera fugiperda), southern armyworm (Spodoptera oridania), Synanthedon spp., Thecla basilides, Thermisia gemmatalis, clothes moth (Tineola bisselliella), cabbage worm (Trichoplusiani), tomato leafminer (Tuta absoluta);

[0041] Furthermore, the lepidopteran pest mentioned is the beet armyworm, and the effective ingredient dosage is 10–50 g / hm².2 The active ingredients are fluchlorfenapyr and brofenoxam.

[0042] Compared with the prior art, the beneficial effects of the technical solution of the present invention are as follows:

[0043] 1) The formulation prepared by this invention has a small particle size, with a particle size distribution between 0.2 and 0.6 μm. The active ingredients are highly dispersed, and the suspension rate reaches more than 99%, which can improve the rapid effect of the active ingredients.

[0044] 2) The formulation prepared by the present invention can significantly improve the surface tension and stability between various constituent phases in the aqueous suspension, form a uniform and stable dispersion system, promote the penetration and absorption of active ingredients at the target site, and improve the performance of pesticide active ingredients on leaf surface adhesion, deposition and distribution.

[0045] (3) The formulation prepared by the present invention improves the efficacy of the product, improves the safety of the suspension to organisms and the environment, improves the safety of food, reduces the risk of agricultural product residues and environmental pollution, and enhances the safety of the new pesticide formulation to the ecological environment. Detailed Implementation

[0046] This invention provides a nano-suspension containing chlorantraniliprole and bromfenac, comprising the following components by mass percentage:

[0047]

[0048]

[0049] Furthermore, the nano-suspension containing chlorantraniliprole and bromonitrile comprises the following components by mass percentage:

[0050] Components mass percentage Fluchlorfenapyr 10％～15％ bromfenoxam 15％～20％ wetting and dispersing agents 6％～9％ Thickener 0.65％ antifreeze 5％ preservative 0.03％ Defoamer 0.5％ Wetting and penetrating agents 5％～6％ Deionized water Replenish to 100%

[0051] Preparation Example 1:

[0052] 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20)

[0053] 10% Fluchlorfenapyr, 20% Bromnifenac, 1% Block Copolymer Dispersant (D-800), 3% Phosphate Ester (7260-C), 2% Polycarboxylate (2700), 5% Wetting and Penetrating Agent EH-6, 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0054] Preparation method: Weigh out fluchlorfenapyr, brofenoxam, wetting and dispersing agent, antifreeze, defoamer, and deionized water according to the specified proportions. After shearing and homogenizing, pour the mixture into a milling jar, add zirconia beads with a particle size of 0.2–0.6 mm, and mill until the particle size D… 50 After reaching a particle size of 0.1–0.6 μm, thickeners, preservatives, and wetting and penetrating agents are added, and the mixture is sheared and homogenized to obtain 30% fluchlorfenapyr·bromnifenac nano-suspension.

[0055] Preparation Example 2:

[0056] 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20)

[0057] 10% Fluchlorfenapyr, 20% Bromnifenac, 2% Block Copolymer Dispersant (D-800), 2% Phosphate Ester (7260-C), 2% Polycarboxylate (2700), 5% Wetting and Penetrating Agent EH-6, 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0058] Preparation method: Same as in preparation example 1.

[0059] Preparation Example 3:

[0060] 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20)

[0061] 10% Fluchlorfenapyr, 20% Bromnifenac, 1.5% Block Copolymer Dispersant (D-800), 4.5% Phosphate Ester (7260-C), 3% Polycarboxylate (2700), 5% Wetting and Penetrating Agent EH-6, 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0062] Preparation method: Same as in preparation example 1.

[0063] Preparation Example 4:

[0064] 30% Fluchlorfenapyr·Bromfenoxam nano-suspension (15:15)

[0065] 15% flufenoxuron, 15% bromonitrile, 1% block copolymer dispersant (D-800), 3% phosphate ester (7260-C), 2% polycarboxylate (2700), 5% wetting and penetrating agent EH-6, 0.15% xanthan gum, 0.5% magnesium aluminum silicate, 5% propylene glycol, 0.03% benzisothiazolinone, 0.5% silicone defoamer (0050), deionized water to make up the balance;

[0066] Preparation method: Same as in preparation example 1.

[0067] Preparation Example 5:

[0068] 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20)

[0069] 10% Fluchlorfenapyr, 20% Bromnifenac, 1% Block Copolymer Dispersant (D-800), 3% Phosphate Ester (7260-C), 2% Polycarboxylate (2700), 6% Wetting and Penetrating Agent EH-6, 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0070] Preparation method: Same as in preparation example 1.

[0071] Compare with Example 1:

[0072] 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20)

[0073] 10% Fluchlorfenapyr, 20% Bromnifenac, 1% Block Copolymer Dispersant (D-800), 3% Phosphate Ester (7260-C), 2% Polycarboxylate (2700), 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0074] Preparation method: Weigh out fluchlorfenapyr, bromfenac, wetting and dispersing agent, antifreeze, defoamer, and deionized water according to the proportion, and mix them by shearing and homogenization. Pour the mixture into a sand mill jar, add zirconia beads with a particle size of 0.2-0.6 mm, sand mill, add thickener and preservative, and shear and homogenize until uniform to obtain 30% fluchlorfenapyr·bromfenac suspension.

[0075] Compare with Example 2:

[0076] 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20)

[0077] 10% flufenoxuron, 20% bromonitrile, 1% block copolymer dispersant (D-800), 3% naphthalene sulfonate (2020), 2% polycarboxylate (2700), 5% wetting and penetrating agent EH-6, 0.15% xanthan gum, 0.5% magnesium aluminum silicate, 5% propylene glycol, 0.03% benzisothiazolinone, 0.5% silicone defoamer (0050), deionized water to make up the balance;

[0078] Preparation method: Weigh out fluchlorfenapyr, bromfenac, wetting and dispersing agent, antifreeze, defoamer, and deionized water according to the proportion, and mix them by shearing and homogenization. Pour the mixture into a sand mill jar, add zirconia beads with a particle size of 0.2-0.6 mm, and sand mill. Add thickener, preservative and wetting and penetrating agent, and shear and homogenize until uniform to obtain 30% fluchlorfenapyr·bromfenac suspension.

[0079] Compare with Example 3:

[0080] 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20)

[0081] 10% Fluchlorfonamide, 20% Bromnifenac, 1% Block Copolymer Dispersant (D-800), 3% Phosphate Ester (7260-C), 2% Polycarboxylate (2700), 0.5% Lignosulfonate WG4, 5% Wetting and Penetrating Agent EH-6, 0.15% Xanthan Gum, 0.5% Magnesium Aluminum Silicate, 5% Propylene Glycol, 0.03% Benzo[a]isothiazolinone, 0.5% Organosilicon Defoamer (0050), Deionized Water to make up the balance;

[0082] Preparation method: Same as control example 2.

[0083] Compare with Example 4:

[0084] 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20)

[0085] 10% flufenoxuron, 20% bromonitrile, 3% phosphate ester (7260-C), 3% polycarboxylate (2700), 0.15% xanthan gum, 0.5% magnesium aluminum silicate, 5% propylene glycol, 0.03% benzisothiazolinone, 0.5% silicone defoamer (0050), deionized water to make up the balance;

[0086] Preparation method: Same as control example 1.

[0087] Compare with Example 5:

[0088] 15% Fluchlorfenapyr·Bromfenoxam suspension concentrate (7.5:7.5)

[0089] 7.5% flufenoxuron, 7.5% bromonitrile, 4% alkylphenol polyoxyethylene ether, 4% phenethylphenol polyoxyethylene ether phosphate, 2% sodium lignosulfonate, 1% sodium polycarboxylate, 0.3% xanthan gum, 1% magnesium aluminum silicate, 5% ethylene glycol, 1% sodium sorbate, 0.5% silicone oil, deionized water to make up the balance.

[0090] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, water is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling and finally homogenization filtration to obtain 15% fluchlorfenapyr·bromnifenac suspension.

[0091] Quality testing

[0092] 1) Appearance test:

[0093] The test was conducted according to NY / T 1860.3-2016 "Guidelines for the Determination of Physicochemical Properties of Pesticides Part 3: Appearance".

[0094] Color determination: Take a certain amount of the test sample into a 100mL beaker, place it on a white background, and compare it with the standard colorimetric card to evaluate the color of the test sample.

[0095] Physical state determination: Take a certain amount of the test sample into a 100mL beaker and evaluate the physical state of the test sample.

[0096] Odor determination: Take a certain amount of the test sample into a 100mL beaker, place it in front of your nose, gently fan the mouth of the beaker with your right hand, and evaluate the odor of the test sample.

[0097] 2) Suspension rate determination:

[0098] The test was conducted according to GB / T14825-2006 "Determination of Pesticide Suspension Rate".

[0099] Accurately weigh 1.0 g (0.0002 g precise) of the test sample and place it in a graduated cylinder containing 100 mL of standard hard water at 30±2℃. Dilute to the mark with standard hard water at 30±2℃, stopper the cylinder, and invert the cylinder 30 times within 1 minute, using the center of the cylinder as the axis. Open the stopper and place the cylinder vertically in a constant temperature water bath without vibration, avoiding direct sunlight, for 30 minutes. Use a pipette to remove 9 / 10 (225 mL) of the suspension within 10-15 seconds, without shaking or lifting the sediment in the graduated cylinder, ensuring that the tip of the pipette is always a few millimeters below the liquid surface. Transfer the remaining 1 / 10 (25 mL) of suspension and precipitate to a clean 100 mL volumetric flask, dissolve and dilute to the mark with methanol, shake well, and filter.

[0100] 3) Thermal storage stability test:

[0101] According to GB / T 19136-2003 "Test Method for Thermal Storage Stability of Pesticides", the ampoules were placed in a biochemical incubator at (54±2)℃ for 14 days. After being taken out, the outside of the ampoules was wiped clean and weighed. For test samples whose mass did not change, the content of active ingredients was tested within 24 hours. The decomposition rate of active ingredients ≤5% was considered qualified.

[0102] 4) Particle size determination:

[0103] The particle size of the samples was determined using a Malvern Zetasizer Nano ZS90 nanoparticle size analyzer. A small amount of liquid sample was taken, diluted 1000 times with distilled water, and sonicated for 10 min to avoid multiple light scattering effects. The sample was then injected into a 1 cm × 1 cm × 4.8 cm standard sample cell to make the sample volume approximately 1 mL. Three measurements were performed, and the particle size data were recorded.

[0104] 5) Surface tension measurement:

[0105] The surface tension of microcapsule suspensions was determined using the platinum plate method. The platinum plate, measuring 24 mm × 10 mm × 0.1 mm, was roughened by sandblasting. The test was conducted at 25°C. The platinum plate was gently brought into contact with the surface (or interface) of the sample. Due to the surface tension of the liquid, the liquid pulls the platinum plate downwards until the surface tension of the liquid and other relevant forces reach equilibrium with the opposing force measured by the instrument, at which point the test value stabilizes. Test values ​​were recorded every 90 seconds, and the average of three tests was recorded. The instrument must be calibrated before measurement to ensure that the surface tension measured for water is within the range of 70 ± 0.5 mN / m. The platinum plate must be rinsed with distilled water and heated red-hot with an alcohol lamp. An automated surface tensiometer was used to design experiments to study the surface tension of different formulations.

[0106] Experimental Results and Analysis:

[0107] Table 1. Results of appearance tests for different formulations

[0108] Serial Number name Test results Preparation Example 1 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20) It is a white suspension. Preparation Example 2 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20) It is a white suspension. Preparation Example 3 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20) It is a white suspension. Preparation Example 4 30% Fluchlorfenapyr·Bromfenoxam nano-suspension (15:15) It is a white suspension. Preparation Example 5 30% Fluroxypyr·Bromoxynil Nanoparticle Suspension (10:20) It is a white suspension. Compare with Example 1 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20) It is a white suspension. Compare with Example 2 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20) It is a white suspension. Compare with Example 3 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20) It is a white suspension. Compare with Example 4 30% Fluroxypyr·Bromoxynil Suspension Concentrate (10:20) It is a white suspension. Compare with Example 5 15% Fluchlorfenapyr·Bromfenoxam suspension concentrate (7.5:7.5) It is a white suspension.

[0109] Table 2 shows that the suspension rates of preparation examples 1 to 5 were all greater than 90%, and the decomposition rate of the active ingredient content after heat storage was significantly lower than that of the control drug, indicating good stability after heat storage.

[0110] Table 2 Results of suspension rate and stability determination of different formulations

[0111]

[0112] The wetting properties of pesticide formulations on plant leaves depend on their surface tension. When the surface tension of the pesticide diluent is low, its residence time on plant leaves increases, thereby improving wettability. Preparation Examples 1-5 have lower surface tension than the control example, enabling them to better wet and adhere to the plant leaf surface, reducing the risk of slippage.

[0113] Table 3. Results of surface tension and particle size determination for different formulations.

[0114]

[0115]

[0116] Field efficacy trials

[0117] Field trials for the control of cabbage beet armyworm

[0118] Test subject: Beet armyworm;

[0119] Target crop: Cabbage (round cabbage, green variety)

[0120] Experimental location: The experimental field in Xiwanggezhuang Village, Renzhao Town, Pingdu City, Qingdao City, Shandong Province had moderate fertility and consistent cultivation conditions.

[0121] Experimental design: The experiment consisted of 5 treatments, 5 control treatments, and 1 water control, with 4 replicates, randomized arrangement, and plot area of ​​20m². 2 .

[0122] Experimental timing: The pesticide was applied once at the early stage of beet armyworm infestation, using 675 kg / hm² of water. 2 .

[0123] Application equipment: WS-16D Guardian electric sprayer, with a single fan-shaped mist nozzle and a working pressure of 0.15-0.4 MPa;

[0124] Application method: When preparing the pesticide, first add one-third of the actual water volume to the sprayer. Add a small amount of water to a small measuring cup and stir the pesticide thoroughly, then pour this mixture into the sprayer. Finally, add the remaining water and mix well. When applying the pesticide, first spray the control group using the constant flow spraying method, spraying evenly and at the calculated pace. When changing to a different pesticide, first clean the sprayer three times and then spray out all the water from the spray bar.

[0125] Weather during the experiment: The weather was good, and it was sunny on the day of application, with an average daily temperature of 24℃.

[0126] Investigation methods: Before applying the pesticide, the initial insect population was investigated. Five points were surveyed in each plot, with two cabbage plants surveyed at each point. The number of live insects was investigated 5 days and 15 days after the pesticide application.

[0127] Methods for calculating drug efficacy:

[0128]

[0129] Safety: During the experiment, the cabbage in each treatment plot grew well, and no phytotoxicity was observed in any treatment.

[0130] Efficacy test results: As shown in Table 4, the suspension concentrate of fluchlorfenapyr and bromonitrile can effectively control beet armyworm, and the control effect of nano-suspension concentrate is better than that of suspension concentrate.

[0131] The nano-suspension formulations prepared in Examples 1 to 5 are more easily absorbed by cabbage leaves, have a longer residual effect, and can effectively reduce the amount of pesticides used. Five days after application, the control efficacy of all formulations in Examples 1 to 5 was above 85%, demonstrating good rapid-acting properties; 15 days after application, with increasing time, the control efficacy of the nano-suspension formulations in Examples 1 to 5 was all above 95%.

[0132] The above experimental results show that the nano-suspension formulations of flufenoxuron and chlorantraniliprole have good rapid and sustained effects against the beet armyworm. Furthermore, they have no adverse effects on the target crop within the tested application range.

[0133] Table 4. Results of field trials on different treatments for controlling beet armyworm.

[0134]

[0135] The data in the table are the average of four studies. The letters indicate significance (lowercase 0.05, DMRT).

[0136] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A nano-suspension agent containing chlorantraniliprole and bromfenac, characterized in that, The composition, by weight percentage, includes: 1%–30% flufenoxuron, 1%–30% chlorantraniliprole, and the remainder being 1%–20% agriculturally acceptable wetting and dispersing agents, 0.1%–2% thickeners, 1%–10% antifreeze agents, 0.01%–0.3% preservatives, 0.1%–5% defoamers, 0.5%–10% wetting and penetrating agents, and deionized water to bring the total to 100%.

2. The nano-suspending agent according to claim 1, characterized in that, The weight percentage of fluchlorfenapyr and brofenoxam in the nano-suspension is 10% to 40%. Preferably, the weight percentage is 10%, 15%, 20%, 30%, 35%, or 40%.

3. The nano-suspension agent containing chlorantraniliprole and bromfenac according to claim 1, characterized in that, The mass ratio of the wetting and dispersing agent is 4% to 15%; Preferably, the mass ratio of the wetting and dispersing agent is 6% to 9%.

4. The nano-suspension agent containing chlorantraniliprole and bromfenac according to claim 1, characterized in that, The wetting and dispersing agent is a mixture of block copolymer dispersant D-800, phosphate ester 7260-C, and polycarboxylate 2700, with a mass ratio of 1:3:2, 1:2:3, 1:1:1, 2:3:1, 2:1:3, 3:2:1, 3:1:2, and 4:1:

1.

5. The nano-suspending agent according to claim 1, characterized in that, The thickener is a mixture of xanthan gum and magnesium aluminum silicate.

6. The nano-suspending agent according to claim 1, characterized in that, The antifreeze is propylene glycol; the preservative is benzisothiazolinone; and the defoamer is an organosilicone defoamer.

7. The nano-suspending agent according to claim 1, characterized in that, The wetting and penetrating agent is EH-6.

8. The method for preparing the nano-suspension agent according to any one of claims 1 to 7, characterized in that, Includes the following steps: Weigh out the following proportions: flufenoxuron, brofenac, wetting and dispersing agent, antifreeze, defoamer, and deionized water. Shear and homogenize the mixture, then pour it into a milling jar. Add zirconia beads with a particle size of 0.2–0.3 mm and mill until the particle size D… 50 After reaching a thickness of 0.1–0.6 μm, thickener, preservative, and wetting and penetrating agent are added, and the mixture is sheared and homogenized.

9. The use of the nano-suspending agent according to any one of claims 1 to 7, characterized in that, The described use is for the nano-suspension composition to control lepidopteran pests.

10. The use according to claim 9, characterized in that, The lepidopteran pest mentioned is the beet armyworm, and the effective ingredient dosage is 10–50 g.ai / hm. 2 The active ingredients are fluchlorfenapyr and brofenoxam.

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