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CN103704260B - A kind of Pesticidal combination containing bromine worm benzamide - Google Patents

A kind of Pesticidal combination containing bromine worm benzamide Download PDF

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CN103704260B
CN103704260B CN201310746485.4A CN201310746485A CN103704260B CN 103704260 B CN103704260 B CN 103704260B CN 201310746485 A CN201310746485 A CN 201310746485A CN 103704260 B CN103704260 B CN 103704260B
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pesticidal combination
imicyafos
bromotraniliprole
bromine worm
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CN103704260A (en
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林冰冰
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Haian Kehao Textile Co Ltd
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Abstract

The present invention relates to a kind of Pesticidal combination containing bromine worm benzamide, its active ingredient is Imicyafos and bromine worm benzamide two yuan of mixtures, and the ratio of weight and number of two kinds of active ingredients is 1 ~ 50: 1 ~ 55, and preferred weight portion rate is 5 ~ 25: 3 ~ 30; The parts by weight content that in Pesticidal combination, active ingredient is total is 1% ~ 80%; preferred weight number content is 5% ~ 40%; all the other are allow in agricultural chemicals to use and acceptable auxiliary element, and can be prepared into wetting powder, suspending agent, microemulsion, aqueous emulsion and water dispersible granules by known method, it is wide that the present composition has effect field; insecticide efficiency is high; and consumption is few, preventive effect is high, residual few; lasting period is long, is conducive to environmental protection.

Description

一种含有溴虫苯甲酰胺的杀虫组合物A kind of insecticidal composition containing bromotraniliprole

技术领域technical field

本发明涉及农药复配技术领域,具体涉及一种含有溴虫苯甲酰胺的杀虫组合物。The invention relates to the technical field of pesticide compounding, in particular to an insecticidal composition containing bromotraniliprole.

背景技术Background technique

Imicyafos(AKD-3088)是一种氰胺杂环类有机物,它由不对称有机磷与烟碱类杀虫剂的氰基亚咪唑烷组合而成,可用于萝卜、胡萝卜、草莓、茄子、番茄、黄瓜、甜瓜、西瓜、番薯以及土豆等作物,其化学结构式为:Imicyafos (AKD-3088) is a cyanamide heterocyclic organic compound, which is composed of asymmetric organophosphorus and cyanoimidazolidine of nicotinic insecticides, and can be used for radish, carrot, strawberry, eggplant, tomato , cucumber, melon, watermelon, sweet potato and potato and other crops, its chemical structure is:

溴虫苯甲酰胺主要是激活兰尼碱受体,释放平滑肌和横纹肌细胞内贮存的钙离子,引起肌肉调节衰弱,麻痹,直至最后害虫死亡。该有效成分表现出对哺乳动物和害虫兰尼碱受体极显著的选择性差异,大大提高了对哺乳动物和其他脊椎动物的安全性。邻甲酰氨基苯甲酰胺类杀虫剂对鳞翅目的夜蛾科、螟蛾科、蛀果蛾科、卷叶蛾科、粉蛾科、菜蛾科、细蛾科等均有很好的控制效果,还能控制鞘翅目象甲科、叶甲科、双翅目潜蝇科、烟粉虱等多种非鳞翅目害虫。对幼虫有非常突出的防效,缺点是对成虫防治效果有限,没有杀卵作用,内吸传导作用不强。Bromotiliprole mainly activates ryanodine receptors, releases calcium ions stored in smooth muscle and striated muscle cells, causes muscle regulation weakness, paralysis, and finally the death of pests. The active ingredient shows a very significant selectivity difference between mammals and pest ryanodine receptors, greatly improving the safety to mammals and other vertebrates. O-formamidobenzamide insecticides have a good control effect on Lepidoptera Noctuidae, Mothidae, Fruit Mothidae, Leaf Rolleridae, Melydidae, Plutella Plutella, and Thymothidae , It can also control various non-lepidopteran pests such as Coleoptera Weevilidae, Chrysophyte, Diptera Liminidae, and Bemisia tabaci. It has a very outstanding control effect on larvae. The disadvantage is that it has limited control effect on adults, no ovicidal effect, and weak systemic conduction.

溴虫苯甲酰胺经过长期使用后,害虫对其的抗性逐年加大,使农药用量不断增加,导致高毒、用量大、残留多、药效差等不良后果。且使用单一组分的杀虫剂,容易导致害虫产生抗药性是目前农药使用过程中面临的一个亟待解决的问题,而创制新型高效杀虫化合物投入大、周期长、科研实力要求较高,不符合目前我国农药企业的现状。而农药之间之间的复配既能解决农药单剂毒性大、效果差的问题,又投入少、研发周期短适合国内农药企业现状,并且不同农药之间的交互使用能够延缓作用物抗药性的产生,具有较为理想的使用效果,因此不同作用机理之间农药的复配是目前农药领域的研究热点。After long-term use of bromotraniliprole, the resistance of pests to it has increased year by year, which has led to an increase in the amount of pesticides used, resulting in adverse consequences such as high toxicity, large dosage, large residues, and poor efficacy. Moreover, the use of single-component insecticides is likely to lead to resistance of pests, which is an urgent problem to be solved in the process of using pesticides. However, the creation of new high-efficiency insecticide compounds requires a large investment, a long cycle, and high scientific research capabilities. In line with the current status of my country's pesticide enterprises. The compounding of pesticides can not only solve the problem of high toxicity and poor effect of a single pesticide, but also requires less investment and a short research and development cycle, which is suitable for the current situation of domestic pesticide companies, and the interactive use of different pesticides can delay the drug resistance of agents Therefore, the combination of pesticides with different mechanisms of action is a research hotspot in the field of pesticides.

发明内容Contents of the invention

根据现有技术的不足,本发明提出了一种含有溴虫苯甲酰胺的杀虫组合物,该组合物含有A、B两种有效活性组分,组分A选自imicyafos,B选自溴虫苯甲酰胺,本发明组合物具有作用领域广,杀虫效率高,且用量少,防效高,残留少,持效期长,有利于环境保护。According to the deficiencies in the prior art, the present invention proposes an insecticidal composition containing bromantraniliprole, the composition contains two effective active components A and B, component A is selected from imicyafos, and B is selected from bromine Tetrabenzamide, the composition of the present invention has a wide range of action, high insecticidal efficiency, less dosage, high control effect, less residue, long duration, and is beneficial to environmental protection.

本发明为一种以新型剂imicyafos与溴虫苯甲酰胺为有效成分进行两元混配的杀虫组合物制剂,其中本发明的杀虫组合物中有效成分新型杀虫剂imicyafos与溴虫苯甲酰胺的重量份数比为1~50∶1~55,在针对性的试验配方筛选的基础上,可将有效成分新型剂imicyafos与溴虫苯甲酰胺的重量份数比优选为5~25∶3~30。The present invention is a dual-mix insecticidal composition preparation with the novel agent imicyafos and bromotraniliprole as active ingredients, wherein the active ingredients in the insecticidal composition of the present invention are the novel insecticide imicyafos and bromotraniliprole The ratio of parts by weight of formamide is 1-50: 1-55. On the basis of targeted test formula screening, the ratio of parts by weight of the active ingredient imicyafos to bromotraniliprole is preferably 5-25 : 3-30.

本发明的农药杀虫组合物用农药制剂领域的制备方法可制备成的农药剂型为可湿性粉剂、悬浮剂、微乳剂、水乳剂和水分散粒剂,制剂中有效成分总重量占制剂中总重量的份数比为1%~80%,在针对性的试验配方筛选的基础上,制剂中有效成分总重量占制剂中总重量的份数比优选为5%~40%,其余为农药中常用助剂。The pesticide formulations that can be prepared by the preparation method in the field of pesticide formulations for the pesticide insecticidal composition of the present invention are wettable powders, suspension concentrates, microemulsions, water emulsions and water dispersible granules, and the total weight of active ingredients in the formulation accounts for the total weight of the formulation. The ratio of parts by weight is 1% to 80%. On the basis of targeted test formula screening, the ratio of the total weight of active ingredients in the preparation to the total weight of the preparation is preferably 5% to 40%, and the rest are pesticides. Common additives.

以上所述的杀虫组合物为微乳剂时,制剂中各组分的重量份数比为:When the above-mentioned insecticidal composition is a microemulsion, the weight and number ratio of each component in the preparation is:

该微乳剂的具体生产步骤为:将原药imicyafos、溴虫苯甲酰胺用助溶剂完全溶解,再加入乳化剂、防冻剂稳定剂等其他成分,均匀混合,最后加入水,充分搅拌后即可配成微乳剂。The specific production steps of the microemulsion are: completely dissolve the original drug imicyafos and bromotraniliprole with a cosolvent, then add emulsifier, antifreeze stabilizer and other ingredients, mix evenly, finally add water, and stir well Dubbed microemulsion.

以上所述的杀虫组合物为可湿性粉剂时,制剂中各组分的重量份数比为:When the above-mentioned insecticidal composition is a wettable powder, the ratio of parts by weight of each component in the preparation is:

该杀虫组合物可湿性粉剂具体加工步骤为:按上述配方将有效组分A和有效组分B以及分散剂、润湿剂和填料混合,在搅拌釜中均匀搅拌,经气流粉碎机后在混合均匀,即可制成本发明组合物的可湿性粉剂。The specific processing steps of the wettable powder of the pesticidal composition are as follows: mix the active component A, the effective component B, the dispersant, the wetting agent and the filler according to the above formula, stir evenly in the stirring tank, pass through the jet mill Mix evenly, then the wettable powder of the composition of the present invention can be prepared.

以上所述的杀虫组合物为悬浮剂时,制剂中各组分的重量份数比为:When the above-mentioned insecticidal composition is a suspension, the weight and number ratio of each component in the preparation is:

该悬浮剂的具体生产步骤为先将其他助剂混合,经高速剪切混合均匀,加入有效组分A和有效组分B,在磨球机中磨球2~3小时,使粒直径均在5mm以下,制得本发明所述的杀虫组合物的悬浮剂制剂。The specific production steps of the suspending agent are as follows: firstly mix other additives, mix evenly through high-speed shearing, add active component A and effective component B, and grind the balls in a ball mill for 2 to 3 hours, so that the particle diameter is uniform Below 5mm, the suspension formulation of the pesticidal composition of the present invention is prepared.

以上所述的杀虫组合物为水乳剂时,制剂中各组分的重量份数比为:When the insecticidal composition described above is an emulsion in water, the ratio of parts by weight of each component in the preparation is:

该水乳剂的具体生产步骤为:首先将原药有效组分A和有效组分B、溶剂和乳化剂、助溶剂加在一起,使溶解成均匀的油相;将部分水,抗冻剂,抗微生物剂等其他的农药助剂混合在一起成均匀的水相;在反应釜中高速搅拌的同时将油相加入水相,缓缓加水直至达到转相点,开启剪切机进行高速剪切,并加入剩余的水,剪切约半小时,形成水包油型的水乳剂。即制得本发明杀虫组合物的水乳剂。The specific production steps of the emulsion in water are as follows: first, the active component A of the original drug and the effective component B, solvent, emulsifier, and co-solvent are added together to dissolve into a uniform oil phase; part of the water, antifreeze, Mix other pesticide additives such as antimicrobial agents together to form a uniform water phase; add the oil phase to the water phase while stirring at high speed in the reactor, add water slowly until the phase inversion point is reached, and turn on the shearing machine for high-speed shearing , and add the remaining water, cut for about half an hour to form an oil-in-water emulsion. That is, the aqueous emulsion of the insecticidal composition of the present invention is prepared.

以上所述的杀虫组合物为水分散粒剂时,制剂中各组分的重量份数比为:When the insecticidal composition described above is a water-dispersible granule, the ratio of parts by weight of each component in the preparation is:

该杀虫组合物水分散粒剂具体加工步骤为:按上述配方将有效组分A、有效组分B和分散剂、润湿剂、崩解剂以及填料混合均匀,用超微气流粉碎机粉碎,经捏合,然后加入流化床造粒干燥机中进行造粒、干燥、筛分后经取样分析,即制得本发明所述的杀虫组合物的水分散粒剂。The specific processing steps of the insecticidal composition water-dispersible granules are as follows: mix the active component A, the effective component B, the dispersant, the wetting agent, the disintegrating agent and the filler uniformly according to the above formula, and pulverize it with an ultra-fine jet mill , kneaded, and then added to a fluidized bed granulation dryer for granulation, drying, sieving, and after sampling and analysis, the water-dispersible granules of the insecticidal composition of the present invention are obtained.

所述的乳化剂选自十二烷基苯磺酸钙与脂肪酸聚氧乙烯醚、烷基酚聚氧乙烯醚磺基琥珀酸酯、苯乙烯基苯酚聚氧乙烯醚、壬基酚聚氧乙烯醚、蓖麻油聚氧乙烯醚、脂肪酸聚氧乙烯基酯、聚氧乙烯脂肪醇醚中的至少一种。The emulsifier is selected from calcium dodecylbenzenesulfonate and polyoxyethylene fatty acid ether, alkylphenol polyoxyethylene ether sulfosuccinate, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene At least one of ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, polyoxyethylene fatty alcohol ether.

所述溶剂为二甲苯或生物柴油、甲苯、柴油、甲醇、乙醇、正丁醇、异丙醇、松节油、溶剂油、二甲基甲酰胺、二甲基亚砜、水等溶剂中的至少一种。The solvent is at least one of xylene or biodiesel, toluene, diesel oil, methanol, ethanol, n-butanol, isopropanol, turpentine, solvent naphtha, dimethylformamide, dimethyl sulfoxide, water and other solvents kind.

所述的分散剂选自聚羧酸盐、木质素磺酸盐、烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、烷基苯磺酸钙盐、萘磺酸甲醛缩合物钠盐、烷基酚聚氧乙烯醚、脂肪胺聚氧乙烯醚、脂肪酸聚氧乙烯酯、甘油脂肪酸酯聚氧乙烯醚中的至少一种。The dispersant is selected from polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylbenzenesulfonate calcium salt, naphthalenesulfonic acid formaldehyde condensate sodium salt, alkyl At least one of phenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester, glycerin fatty acid ester polyoxyethylene ether.

所述的湿润剂选自十二烷基硫酸钠、十二烷基苯磺酸钙、拉开粉松脂酸铜X.、润湿渗透剂F、烷基萘磺酸盐、聚氧乙烯三苯乙烯苯基磷酸盐、皂角粉、蚕沙、无患子粉中的至少一种。The wetting agent is selected from sodium lauryl sulfate, calcium dodecylbenzenesulfonate, copper rosinate X., wetting and penetrating agent F, alkylnaphthalenesulfonate, polyoxyethylene triphenyl At least one of ethylene phenyl phosphate, saponin powder, silkworm excrement, and sapindus powder.

所述的崩解剂选自膨润土、尿素、硫酸铵、氯化铝、柠檬酸、丁二酸、碳酸氢钠中的至少一种。The disintegrant is at least one selected from bentonite, urea, ammonium sulfate, aluminum chloride, citric acid, succinic acid, and sodium bicarbonate.

所述的增稠剂选自黄原胶、羟甲基纤维素、羟乙基纤维素、甲基纤维素、硅酸铝镁、聚乙烯醇中的至少一种。The thickener is selected from at least one of xanthan gum, hydroxymethyl cellulose, hydroxyethyl cellulose, methyl cellulose, magnesium aluminum silicate, and polyvinyl alcohol.

所述的稳定剂选自柠檬酸钠、间苯二酚中的至少一种。The stabilizer is at least one selected from sodium citrate and resorcinol.

所述的防冻剂选自乙二醇、丙二醇、丙三醇中的至少一种。The antifreezing agent is selected from at least one of ethylene glycol, propylene glycol, and glycerol.

所述的消泡剂选自硅油、硅酮类化合物、C10—20饱和脂肪酸类化合物、C8—10脂肪醇类化合物中的至少一种。The defoamer is at least one selected from silicone oil, silicone compounds, C10-20 saturated fatty acid compounds, and C8-10 fatty alcohol compounds.

所述的填料选自高岭土、硅藻土、膨润土、凹凸棒土、白炭黑、淀粉、轻质碳酸钙中的至少一种。The filler is at least one selected from kaolin, diatomaceous earth, bentonite, attapulgite, white carbon black, starch and light calcium carbonate.

本发明的杀虫组合物可以防治线虫类、等足类、鞘翅目类害虫、鳞翅目类害虫、腹足类、直翅目害虫、植物寄生性螨虫类、缨翅目害虫、双翅目害虫、膜翅目害虫、隐翅目害虫、虱目害虫、等翅目害虫、半翅目害虫、潮虫类、百足虫类、千足虫类等各种害虫。尤其对在土壤中破坏农园艺作物以及树木等的害虫、破坏农园艺作物以及树木的种子的害虫,例如线虫类、等足类、鞘翅目类害虫、鳞翅目类害虫、腹足类、直翅目害虫、植物寄生性螨虫类、半翅目害虫防效显著。The insecticidal composition of the present invention can control nematodes, isopods, Coleoptera pests, Lepidoptera pests, gastropods, Orthoptera pests, plant parasitic mites, Thysanoptera pests, Diptera pests, Pests, hymenoptera pests, paedoptera pests, lice pests, isoptera pests, hemiptera pests, woodworms, centipedes, millipedes and other pests. Especially for pests that destroy agricultural and horticultural crops and trees in the soil, and pests that damage the seeds of agricultural and horticultural crops and trees, such as nematodes, isopods, coleopteran pests, lepidopteran pests, gastropods, straight It has remarkable control effect on Pteroptera pests, plant parasitic mites and Hemiptera pests.

以上所述线虫类害虫包括根腐线虫、伪短体线虫、卢斯短体线虫、伤残短体线虫等根腐线虫类,大豆胞囊线虫、马铃薯金线虫等胞囊线虫类,花生根结线虫、南方根结线虫等根结线虫类,水稻干尖线虫、叶芽线虫等滑刃总科类,矮化线虫类,环线虫类,针线虫类,长囊线虫类,毛刺线虫类,草莓上线虫,松材线虫。另外对蚜虫、叶蝉、飞虱、叶甲、金针虫、地老虎、小菜蛾、菜粉蝶、稻蓟马等害虫均有较好防效。The above-mentioned nematode pests include root rot nematodes such as root rot nematodes, pseudo brevis nematodes, brevis brevis nematodes, and disabled brevis body nematodes, cyst nematodes such as soybean cyst nematodes and potato golden nematodes, and peanut root knot nematodes. Nematodes, root-knot nematodes such as root-knot nematodes, rice stem-point nematodes, leaf bud nematodes and other root-knot nematodes, dwarf nematodes, circular nematodes, needle nematodes, long cyst nematodes, burr nematodes, strawberry Nematode, pine xylophilus. In addition, it has good control effect on aphids, leafhoppers, planthoppers, leaf beetles, dayworms, cutworms, diamondback moths, cabbage butterfly, rice thrips and other pests.

本发明的农药杀虫组合物尤其对防治蚜虫科、粉虱科、叶蝉科及飞虱科害虫,尤其是各种虫类、梨木虱、菜青虫、小菜蛾、甜菜夜蛾、金纹细蛾、潜叶蛾、潜叶蝇、美洲斑潜蝇和蔬菜白粉虱等多种害虫具有高效作用。The pesticide and insecticidal composition of the present invention is especially effective for controlling pests of Aphididae, Whiteflyceae, Leafhoppers and Planthoppers, especially various insects, pear psyllids, cabbage caterpillars, diamondback moths, beet armyworms, and aureus. It is highly effective against various pests such as moth, leafminer, leafminer, liriomyza sativae and vegetable whitefly.

本发明的杀虫组合物相比同类药剂有很多其他优点,第一,将溴虫苯甲酰胺与新型杀虫剂imicyafos复配,提高了溴虫苯甲酰胺的杀虫效率,延缓了害虫对新型杀虫剂imicyafos的抗性,相比各自单剂作用范围更广,提高了杀虫功效;第二,延缓了害虫抗药性的产生,减少了农药反复使用次数,降低了农药使用量,降低农用成本;第三,该杀虫组合物的残留量更低,对环境更加友好,对农业产品的安全食用具有重大意义。Compared with similar medicaments, the insecticidal composition of the present invention has many other advantages. First, bromotraniliprole is compounded with the novel insecticide imicyafos, which improves the insecticidal efficiency of bromotraniliprole and delays the pests’ attack on the insecticide. The resistance of the new insecticide imicyafos has a wider range of action than the respective single agents, which improves the insecticidal efficacy; second, it delays the emergence of pest resistance, reduces the number of repeated use of pesticides, reduces the amount of pesticides used, and reduces Agricultural cost; thirdly, the insecticidal composition has lower residues, is more friendly to the environment, and is of great significance to the safe consumption of agricultural products.

具体实施方式:Detailed ways:

为了使本发明的目的、技术方案及优点更加清楚明白,本发明用以下具体实施例进行说明,但本发明绝非仅限于这些例子。本发明采用室内生物测定和田间试验相结合的方法,如无特别说明,以下提及的比例(包括百分比)都是重量份数比。In order to make the object, technical solution and advantages of the present invention clearer, the present invention is described with the following specific examples, but the present invention is by no means limited to these examples. The present invention adopts the method that indoor bioassay and field test are combined, and unless otherwise specified, the ratios mentioned below (including percentages) are all ratios in parts by weight.

实施例1:将imicyafos20份、溴虫苯甲酰胺5份、木质素磺酸盐8份、十二烷基硫酸钠12份和硅藻土55份混合,在搅拌釜中均匀搅拌,经气流粉碎机后在混合均匀,即制得本发明杀虫组合物的可湿性粉剂。Example 1: Mix 20 parts of imicyafos, 5 parts of bromotraniliprole, 8 parts of lignosulfonate, 12 parts of sodium lauryl sulfate and 55 parts of diatomaceous earth, stir evenly in a stirring tank, and pulverize by airflow Mix evenly after machine, promptly make the wettable powder of insecticidal composition of the present invention.

实施例2:将imicyafos8份、溴虫苯甲酰胺25份、烷基酚聚氧乙烯醚10份、氧乙烯三苯乙烯苯基磷酸盐10份和膨润土47份混合,在搅拌釜中均匀搅拌,经气流粉碎机后在混合均匀,即制得本发明杀虫组合物的可湿性粉剂。Example 2: Mix 8 parts of imicyafos, 25 parts of bromotraniliprole, 10 parts of alkylphenol polyoxyethylene ether, 10 parts of oxyethylene tristyrene phenyl phosphate and 47 parts of bentonite, and stir evenly in a stirring tank. After passing through the jet mill and mixing uniformly, the wettable powder of the insecticidal composition of the present invention can be obtained.

实施例3:将imicyafos3份、溴虫苯甲酰胺28份、分散剂11份、润湿剂12份和填料46份混合,在搅拌釜中均匀搅拌,经气流粉碎机后在混合均匀,即制得本发明杀虫组合物的可湿性粉剂。Example 3: Mix 3 parts of imicyafos, 28 parts of bromotraniliprole, 11 parts of dispersant, 12 parts of wetting agent and 46 parts of filler, stir evenly in a stirring tank, and mix evenly after passing through a jet mill, and then prepare Obtain the wettable powder of the insecticidal composition of the present invention.

实施例4:将烷基酚聚氧乙烯醚10份、丙三醇2份、羟甲基纤维素4份、硅油1份、水58份混合,经高速剪切混合均匀,依次加入imicyafos18份、溴虫苯甲酰胺7份,在磨球机中磨球2~3小时,使粒直径均在5mm以下,制得本发明所述的杀虫组合物的悬浮剂制剂。Example 4: Mix 10 parts of alkylphenol polyoxyethylene ether, 2 parts of glycerin, 4 parts of hydroxymethyl cellulose, 1 part of silicone oil, and 58 parts of water, mix evenly through high-speed shearing, and add 18 parts of imicyafos, 7 parts of bromotraniliprole were ground in a ball mill for 2 to 3 hours, so that the particle diameters were all below 5 mm, and the suspension preparation of the insecticidal composition of the present invention was prepared.

实施例5:将分散剂10份、防冻剂2份、增稠剂5份、消泡剂1份、水50份混合,经高速剪切混合均匀,依次加入imicyafos12份、溴虫苯甲酰胺20份,在磨球机中磨球2~3小时,使粒直径均在5mm以下,制得本发明所述的杀虫组合物的悬浮剂制剂。Example 5: Mix 10 parts of dispersant, 2 parts of antifreeze, 5 parts of thickener, 1 part of defoamer, and 50 parts of water, mix evenly through high-speed shearing, and then add 12 parts of imicyafos and 20 parts of bromotraniliprole Grind the balls in a ball mill for 2 to 3 hours so that the particle diameters are all below 5 mm to prepare the suspension formulation of the pesticidal composition of the present invention.

实施例6:将分散剂8份、防冻剂1份、增稠剂4份、消泡剂2份、水67份混合,经高速剪切混合均匀,依次加入imicyafos22份、溴虫苯甲酰胺6份,在磨球机中磨球2~3小时,使粒直径均在5mm以下,制得本发明所述的杀虫组合物的悬浮剂制剂。Example 6: Mix 8 parts of dispersant, 1 part of antifreeze, 4 parts of thickener, 2 parts of defoamer, and 67 parts of water, mix evenly through high-speed shearing, and then add 22 parts of imicyafos and 6 parts of bromotraniliprole Grind the balls in a ball mill for 2 to 3 hours so that the particle diameters are all below 5 mm to prepare the suspension formulation of the pesticidal composition of the present invention.

实施例7:将imicyafos22份、溴虫苯甲酰胺3份、松节油10份、蓖麻油聚氧乙烯醚7份、间苯二酚9份混合在一起,溶解成均匀的油相;将部分水、丙二醇2份、硅酮类化合物1份混合在一起成均匀的水相;在反应釜中高速搅拌的同时将油相加入水相,加入聚乙烯醇4份,缓缓加水直至达到转相点,开启剪切机进行高速剪切,并加入剩余的水补足100份,剪切约半小时,形成水包油型的水乳剂。即制得本发明杀虫组合物的水乳剂。Example 7: 22 parts of imicyafos, 3 parts of bromotraniliprole, 10 parts of turpentine, 7 parts of castor oil polyoxyethylene ether, and 9 parts of resorcinol are mixed together and dissolved into a uniform oil phase; part of the water, Mix 2 parts of propylene glycol and 1 part of silicone compound together to form a uniform water phase; while stirring at high speed in the reactor, add the oil phase to the water phase, add 4 parts of polyvinyl alcohol, and slowly add water until the phase inversion point is reached. Open the shearing machine and carry out high-speed shearing, and add the remaining water to make up 100 parts, and shear for about half an hour to form an oil-in-water emulsion. That is, the aqueous emulsion of the insecticidal composition of the present invention is prepared.

实施例8:将imicyafos6份、溴虫苯甲酰胺14份、溶剂18份、乳化剂8份、稳定剂7份混合在一起,溶解成均匀的油相;将部分水、防冻剂1份、消泡剂2份混合在一起成均匀的水相;在反应釜中高速搅拌的同时将油相加入水相,加入增稠剂3份,缓缓加水直至达到转相点,开启剪切机进行高速剪切,并加入剩余的水补足100份,剪切约半小时,形成水包油型的水乳剂。即制得本发明杀虫组合物的水乳剂。Example 8: Mix 6 parts of imicyafos, 14 parts of bromotraniliprole, 18 parts of solvent, 8 parts of emulsifier, and 7 parts of stabilizer to dissolve into a uniform oil phase; part of water, 1 part of antifreeze, disinfectant Mix 2 parts of the foaming agent together to form a uniform water phase; while stirring at high speed in the reactor, add the oil phase to the water phase, add 3 parts of the thickener, slowly add water until the phase inversion point is reached, and turn on the shearing machine for high-speed Cut, and add the remaining water to make up 100 parts, cut for about half an hour, and form an oil-in-water emulsion. That is, the aqueous emulsion of the insecticidal composition of the present invention is prepared.

实施例9:将imicyafos5份、溴虫苯甲酰胺20份、溶剂20份、乳化剂8份、稳定剂8份混合在一起,溶解成均匀的油相;将部分水、防冻剂1份、消泡剂2份混合在一起成均匀的水相;在反应釜中高速搅拌的同时将油相加入水相,加入增稠剂3份,缓缓加水直至达到转相点,开启剪切机进行高速剪切,并加入剩余的水补足100份,剪切约半小时,形成水包油型的水乳剂。即制得本发明杀虫组合物的水乳剂。Example 9: Mix 5 parts of imicyafos, 20 parts of bromotraniliprole, 20 parts of solvent, 8 parts of emulsifier, and 8 parts of stabilizer to dissolve into a uniform oil phase; part of water, 1 part of antifreeze, disinfectant Mix 2 parts of the foaming agent together to form a uniform water phase; while stirring at high speed in the reactor, add the oil phase to the water phase, add 3 parts of the thickener, slowly add water until the phase inversion point is reached, and turn on the shearing machine for high-speed Cut, and add the remaining water to make up 100 parts, cut for about half an hour, and form an oil-in-water emulsion. That is, the aqueous emulsion of the insecticidal composition of the present invention is prepared.

实施例10:将imicyafos21份、溴虫苯甲酰胺6份、脂肪胺聚氧乙烯醚11份、烷基萘磺酸盐11份、氯化铝4份以及膨润土47份混合均匀,用超微气流粉碎机粉碎,经捏合,然后加入流化床造粒干燥机中进行造粒、干燥、筛分后经取样分析,即制得本发明所述的杀虫组合物的水分散粒剂。Example 10: Mix 21 parts of imicyafos, 6 parts of bromotraniliprole, 11 parts of fatty amine polyoxyethylene ether, 11 parts of alkylnaphthalene sulfonate, 4 parts of aluminum chloride and 47 parts of bentonite, and use ultra-micro airflow Pulverized by a pulverizer, kneaded, then added to a fluidized bed granulation dryer for granulation, drying, sieving, and sampling analysis to obtain the water-dispersible granules of the insecticidal composition of the present invention.

实施例11:将imicyafos10份、溴虫苯甲酰胺18份、分散剂8份、润湿剂10份、崩解剂4份以及填料50份混合均匀,用超微气流粉碎机粉碎,经捏合,然后加入流化床造粒干燥机中进行造粒、干燥、筛分后经取样分析,即制得本发明所述的杀虫组合物的水分散粒剂。Example 11: Mix 10 parts of imicyafos, 18 parts of bromotraniliprole, 8 parts of dispersant, 10 parts of wetting agent, 4 parts of disintegrating agent and 50 parts of filler, pulverize with ultrafine jet mill, knead, Then put it into a fluidized bed granulation dryer for granulation, drying, sieving, and after sampling and analysis, the water-dispersible granules of the insecticidal composition of the present invention are obtained.

实施例12:将imicyafos5份、溴虫苯甲酰胺15份、分散剂10份、润湿剂14份、崩解剂3份以及填料53份混合均匀,用超微气流粉碎机粉碎,经捏合,然后加入流化床造粒干燥机中进行造粒、干燥、筛分后经取样分析,即制得本发明所述的杀虫组合物的水分散粒剂。Example 12: Mix 5 parts of imicyafos, 15 parts of bromotraniliprole, 10 parts of dispersant, 14 parts of wetting agent, 3 parts of disintegrating agent and 53 parts of filler, pulverize with ultrafine jet mill, knead, Then put it into a fluidized bed granulation dryer for granulation, drying, sieving, and after sampling and analysis, the water-dispersible granules of the insecticidal composition of the present invention are obtained.

实施例13:将原药imicyafos18份、溴虫苯甲酰胺7份用助溶剂完全溶解,再加入脂肪酸聚氧乙烯基酯10份、乙二醇2份、柠檬酸钠3份、间苯二酚4份等其他成分,均匀混合,最后加入水,充分搅拌后即可配成微乳剂。Example 13: Dissolve 18 parts of the original drug imicyafos and 7 parts of bromotraniliprole with a cosolvent, then add 10 parts of polyoxyethylene fatty acid ester, 2 parts of ethylene glycol, 3 parts of sodium citrate, and resorcinol 4 parts and other ingredients, mix evenly, and finally add water, stir well to form a microemulsion.

实施例14:将原药imicyafos10份、溴虫苯甲酰胺8份用助溶剂完全溶解,再加入乳化剂8份、防冻剂2份、稳定剂9份等其他成分,均匀混合,最后加入水,充分搅拌后即可配成微乳剂。Example 14: Dissolve 10 parts of the original drug imicyafos and 8 parts of bromotraniliprole with a cosolvent, then add 8 parts of emulsifier, 2 parts of antifreeze, 9 parts of stabilizer and other ingredients, mix evenly, and finally add water, After fully stirring, it can be formulated into microemulsion.

实施例15:将原药imicyafos5份、溴虫苯甲酰胺20份用助溶剂完全溶解,再加入乳化剂10份、防冻剂2份、稳定剂8份等其他成分,均匀混合,最后加入水,充分搅拌后即可配成微乳剂。Example 15: Completely dissolve 5 parts of the original drug imicyafos and 20 parts of bromotraniliprole with a cosolvent, then add 10 parts of emulsifier, 2 parts of antifreeze, 8 parts of stabilizer and other ingredients, mix evenly, and finally add water, After fully stirring, it can be formulated into microemulsion.

室内生测筛选与大田试验:Indoor bioassay screening and field test:

本发明采用室内生物测定和田间试验相结合的方法。如无特别说明,以下提及的比例(包括百分比)都是质量比。The present invention adopts the method of combining indoor bioassay and field test. Unless otherwise specified, the ratios (including percentages) mentioned below are all mass ratios.

活性测定实例:Examples of activity assays:

(1)供试药剂(1) Drugs to be tested

95%imicyafos原药,93%溴虫苯甲酰胺原药。95% imicyafos original drug, 93% bromotraniliprole original drug.

(2)供试虫源(2) Source of tested insects

室内累代饲养的小菜蛾幼虫,室内条件:温度(26±2)℃,相对湿度68%±5%,光照周期16/8h(L/D)。Plutella xylostella larvae raised for generations indoors, indoor conditions: temperature (26±2)°C, relative humidity 68%±5%, photoperiod 16/8h (L/D).

(3)单剂测定方法(3) Single-dose determination method

采用浸虫法分别将两组原药都用少量丙酮溶解,再用0.1%的吐温水溶液稀释成成等差的5个浓的溶液,稀释在烧杯里以备用,并以清水作为对照。The two groups of original drugs were dissolved in a small amount of acetone by worm soaking method, and then diluted with 0.1% Tween aqueous solution to form 5 concentrated solutions with equal difference, which were diluted in beakers for later use, and clear water was used as a control.

将大小一致的小菜蛾幼虫在浸虫笼的药液中浸渍5S,吸去多余药液后将其置于直径为9cm的培养皿中,皿中放有新鲜菜叶加盖。每浓度处理10头,重复4次,设空白对照。于(27±1)℃光照培养箱中保持24h后检查死亡率,用拨针轻触虫体无反应者为死亡。死亡率用Abbott公式校正,再根据浓度对数——死亡率机率值分析(Bliss)法,求出毒力回归方程和置死中量LC50的值。Plutella xylostella larvae of the same size were immersed in the medicinal solution of the insect cage for 5 seconds, and after absorbing the excess medicinal solution, they were placed in a petri dish with a diameter of 9 cm, and the dish was covered with fresh vegetable leaves. 10 heads were treated at each concentration, repeated 4 times, and a blank control was set. After keeping in the light incubator at (27±1)°C for 24 hours, the mortality was checked, and those who did not respond to the worm body with a needle were considered dead. Mortality was corrected by Abbott's formula, and then according to concentration logarithm-mortality probability value analysis (Bliss) method, the regression equation of toxicity and the value of LC 50 were calculated.

(4)不同配比的联合毒力测定方法(4) Combined toxicity assay method with different ratios

根据单剂的毒力测定结果,按有效成分18%重量份数比imicyafos:溴虫苯甲酰胺分别为5:13、7:11、9:9、11:7、13:5。According to the toxicity test results of a single agent, the ratios of imicyafos to bromotraniliprole were 5:13, 7:11, 9:9, 11:7, and 13:5 according to 18% by weight of active ingredients.

采用上述1.3方法进行毒力测定,计算LC50,并按孙云沛方法计算共毒系数(CTC),共毒系数CTC,计算公式如下:(以imicyafos为标准药剂,其毒力指数为100):The above-mentioned 1.3 method was used to measure the toxicity, and the LC50 was calculated, and the co-toxicity coefficient (CTC) was calculated according to Sun Yunpei's method.

溴虫苯甲酰胺的毒力指数(TI)=imicyafos的LC50/溴虫苯甲酰胺的LC50×100Bromotraniliprole Toxicity Index (TI) = LC 50 of imicyafos / LC 50 of Bromotraniliprole × 100

M的实际毒力指数(ATI)=imicyafos的LC50/M的LC50×100Actual Toxicity Index (ATI) of M = LC 50 of imicyafos / LC 50 of M × 100

M的理论毒力指数(TTI)=imicyafos的TI×P imicyafos+溴虫苯甲酰胺的TI×P溴虫苯甲酰胺M's Theoretical Toxicity Index (TTI) = TI of imicyafos × P imicyafos + TI of bromotraniliprole × P bromotraniliprole

M的共毒系数(CTC)=M的ATI/M的TTI×100M's co-toxicity coefficient (CTC)=M's ATI/M's TTI×100

式中:In the formula:

M为溴虫苯甲酰胺与imicyafos不同配比的混合物M is a mixture of different ratios of bromantraniliprole and imicyafos

P溴虫苯甲酰胺为溴虫苯甲酰胺在混剂中所占的比例P bromotraniliprole is the proportion of bromotraniliprole in the mixture

P imicyafos为imicyafos在混剂中所占的比例P imicyafos is the proportion of imicyafos in the mixture

(5)毒力测定结果及分析(5) Toxicity test results and analysis

表1imicyafos、溴虫苯甲酰胺对小菜蛾的室内测定结果Table 1 imicyafos, bromotraniliprole to Plutella xylostella indoor assay results

从表中可以看出,在不同比例的混配中,其共毒系数均大于120,表现出一定的增效作用,其中imicyafos:溴虫苯甲酰胺为11∶7的增效作用最明显,共毒系数为192.80。试验结果表明,在室内条件下溴虫苯甲酰胺、imicyafos两种药剂对小菜蛾均有较高的活性,不同比例配比的试验结果表明,按有效成分imicyafos∶溴虫苯甲酰胺为5:13、7:11、9:9、11:7、13:5时,均表现出较强的增效作用,其中以imicyafos∶溴虫苯甲酰胺为11∶7时,增效效果最好。建议对适宜配比11:7左右范围的混配制剂进行进一步的田间药效试验,以评价其田间实际应用效果。As can be seen from the table, in the mixing of different proportions, its co-toxicity coefficient is greater than 120, showing a certain synergistic effect, wherein imicyafos: bromotraniliprole is the most obvious synergistic effect of 11:7, The co-toxicity coefficient was 192.80. The test results show that under indoor conditions, bromotraniliprole and imicyafos have higher activity against diamondback moth. The test results of different ratios show that according to the active ingredient imicyafos: bromotraniliprole is 5: 13, 7:11, 9:9, 11:7, 13:5, all showed a strong synergistic effect, and the synergistic effect was the best when the ratio of imicyafos:bromotraniliprole was 11:7. It is recommended to conduct further field efficacy tests on the mixed preparations with a suitable ratio of about 11:7 to evaluate their actual application effects in the field.

大田实验:田间试验防治水稻病虫害Field experiment: Field experiment to control rice diseases and insect pests

(1)试验方法(1) Test method

试验在湖北省荆州市监利县程集镇罗湾村的双季稻田进行,试验地土壤为壤土,肥力中等,排灌方便,四周均种植双季稻。供试水稻用药前水稻长势良好。小区间筑小泥埂以防串灌,施药时田间有3~4cm浅水层,药后保水7d,试验在四(2)代稻飞虱低龄若虫发生高峰期(9月4日)下午用药1次,对水50kg/hm2,用工农16型背负式手动喷雾器均匀粗喷雾,时水稻处于灌浆中期,田间主要为白背飞虱,其次为灰飞虱,且1~3龄若虫占90%。施药当天为晴天,平均气温29.5℃;药后7d均无雨,天气对本试验基本无影响。The experiment was carried out in the double-cropping rice field of Luowan Village, Chengji Town, Jianli County, Jingzhou City, Hubei Province. The soil of the experimental site was loamy, with medium fertility and convenient drainage and irrigation. Double-cropping rice was planted all around. The rice under test was growing well before the treatment. Small mud ridges were built between plots to prevent string irrigation. There was a shallow water layer of 3 to 4 cm in the field when the pesticide was applied, and the water was kept for 7 days after the pesticide was applied. The test was applied in the afternoon when the fourth (2) generation rice planthopper young nymphs occurred at the peak (September 4). Once, spray 50kg/hm 2 of water evenly and coarsely with Gongnong 16 knapsack manual sprayer. When the rice is in the middle stage of grain filling, the field is mainly white-backed planthopper, followed by SBPH, and the 1st to 3rd instar nymphs account for 90%. %. The day of spraying was sunny, with an average temperature of 29.5°C; there was no rain for 7 days after spraying, and the weather basically had no effect on this experiment.

(2)调查方法(2) Survey method

共调查5次,药前(9月4日)调查虫口基数,药后2d(9月6日),药后7d(9月11日),药后14d(9月18日)分别调查1次。采取每小区平行跳跃式随机取样15点,每点2丛,共30丛稻,用盆拍法分别记录白背飞虱、灰飞虱的活虫数,然后计算其校正防效(以下简称防效)。A total of 5 surveys were carried out. The insect population base was investigated before the drug treatment (September 4), 2 days after the drug treatment (September 6), 7 days after the drug treatment (September 11), and 14 days after the drug treatment (September 18). . Take random sampling of 15 points in each plot, 2 clumps in each point, 30 clumps of rice in total, record the number of live insects of white-backed planthopper and SBPH, respectively, and then calculate the corrected control effect (hereinafter referred to as control effect) effect).

(3)药效计算方法(3) Calculation method of drug efficacy

虫口减退率(%)=(施药前活虫数一施药后活虫数)/施药前活虫数*l00;Insect population reduction rate (%) = (number of live insects before spraying - number of live insects after spraying) / number of live insects before spraying * l00;

(4)药害调查方法(4) Methods of drug hazard investigation

在药后2,7,14d观察水稻生长情况,目测药剂对水稻均无药害。The growth of the rice was observed at 2, 7, and 14 days after the application, and the pesticide had no phytotoxicity to the rice by visual inspection.

(5)田间药效试验试验结果(5) Field efficacy test results

表2处理药剂防治水稻稻飞虱田间药效试验结果Table 2 Field efficacy test results of treatment chemicals for controlling rice planthoppers

从表2可以看出,18%imicyafos·溴虫苯甲酰胺按11∶7的重量份混配组合防治水稻稻飞虱的效果明显优于22%溴虫苯甲酰胺SC、20%imicyafos SC对照单剂,18%imicyafos·溴虫苯甲酰胺在药后7天的杀虫效果分别为92.71%、93.38%和94.32%,杀虫效果随着用量的增加而递增。另外在试验剂量范围内,作物生长正常,各处理药剂均未出现对水稻的药害现象,说明其对水稻是安全的。It can be seen from Table 2 that the effect of 18% imicyafos·bromotraniliprole mixed according to the weight ratio of 11:7 to control rice planthoppers is significantly better than that of 22% bromotraniliprole SC and 20% imicyafos SC. The insecticidal effects of 18% imicyafos · bromantraniliprole were 92.71%, 93.38% and 94.32% respectively after 7 days of application, and the insecticidal effects increased with the increase of dosage. In addition, within the range of the test dosage, the crops grew normally, and there was no phytotoxicity phenomenon on the rice, which indicated that it was safe to the rice.

Claims (4)

1. the Pesticidal combination containing bromine worm benzamide, it is characterized in that: this Pesticidal combination is for the composite composite preparation of active ingredient two yuan with A novel agrochemical Imicyafos and B bromine worm benzamide, all the other components are usual auxiliaries in agricultural chemicals, and the structural formula of A novel agrochemical Imicyafos is:
,
In this Pesticidal combination, the ratio of weight and number of effective constituents A and B is 5 :13,7 :11,9 :9,11 :7,13 :5.
2. a kind of Pesticidal combination containing bromine worm benzamide according to claim 1, is characterized in that: in this Pesticidal combination, effective constituents A and B gross weight account for the percentage composition of total formulation weight amount is 1% ~ 80%.
3. a kind of Pesticidal combination containing bromine worm benzamide according to claim 1, is characterized in that: in this Pesticidal combination, effective constituents A and B gross weight account for the percentage composition of total formulation weight amount is 5% ~ 40%.
4. a kind of Pesticidal combination containing bromine worm benzamide according to claim 1, is characterized in that: the preparation formulation that Pesticidal combination of the present invention can be mixed with is wetting powder, suspending agent, microemulsion, aqueous emulsion and water dispersible granules.
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