CN103814940B - The ultra low volume liquids of containing novaluron and chrysanthemum ester insecticide - Google Patents
The ultra low volume liquids of containing novaluron and chrysanthemum ester insecticide Download PDFInfo
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Abstract
含氟酰脲与菊酯类杀虫剂的超低容量液剂，由氟酰脲与活性成分Ⅱ复配为活性成分，其余用助剂和溶剂补足至100%；活性成分Ⅱ为氟氯氰菊酯、氰戊菊酯、溴氰菊酯、醚菊酯中的任意一种。本发明所述的超低容量液剂加工方便、持效期长、工效高、靶标不易产生抗药性、环境污染低、省药省水，提高农药利用率，通过超低容量喷雾、低容量喷雾或超低容量静电喷雾能够防治水稻、小麦、玉米、蔬菜、烟草、茶树、果树和甘蔗的多种害虫。The ultra-low-capacity liquid formulation containing fluoride urea and pyrethroid insecticide, the active ingredient is compounded by fluoride urea and active ingredient II, and the rest is made up to 100% with auxiliaries and solvents; the active ingredient II is cyfluthrin, Any one of fenvalerate, deltamethrin, and etofenprox. The ultra-low-capacity liquid agent of the present invention is convenient to process, has a long duration of action, high work efficiency, is not easy to produce drug resistance in the target, has low environmental pollution, saves medicine and water, and improves the utilization rate of pesticides. Or ultra-low-capacity electrostatic spray can control a variety of pests in rice, wheat, corn, vegetables, tobacco, tea trees, fruit trees and sugarcane.
Description
技术领域technical field
本发明属于农药领域，尤其涉及一种含氟酰脲与菊酯类杀虫剂的超低容量液剂。The invention belongs to the field of pesticides, in particular to an ultra-low-capacity liquid formulation of fluorine-containing urea and pyrethroid pesticides.
背景技术Background technique
近几年，杀虫剂已成为农业生产的必需品，在防御病虫害方面起着极其重要的作用，随着人类生活水平的不断提高，食品和环境的健康问题日益受到人们的关注，因而世界各国均加大了对新农药和新剂型的开发力度，超低容量液剂是一种高效低毒，低残留的农药新制剂，该剂型能够降低药剂的使用量和使用频率，延缓害虫抗药性的产生，对环境友好，对人畜等非靶标安全，可节约施药用水量，提高防治工效，能够满足农业可持续发展的各种要求。In recent years, pesticides have become a necessity in agricultural production and play an extremely important role in the defense of diseases and insect pests. With the continuous improvement of human living standards, food and environmental health issues are increasingly concerned by people. Therefore, all countries in the world The development of new pesticides and new dosage forms has been intensified. The ultra-low volume liquid is a new pesticide preparation with high efficiency, low toxicity and low residue. This dosage form can reduce the amount and frequency of use of pesticides and delay the emergence of insecticide resistance. , friendly to the environment, safe for non-targets such as humans and animals, can save water consumption for pesticide application, improve control efficiency, and can meet various requirements for sustainable agricultural development.
氟酰脲的英文名称为：novaluron,分子式为：C17H9ClF8O4,化学名称为：±-1-[3-氯-4-（1,1,2-三氟-2-三氟甲氧基乙氧基）苯基]-3-（2,6-二氟苯基）脲，CAS号为：116714-46-6，结构式为：The English name of fluorourea is: novaluron, the molecular formula is: C 17 H 9 ClF 8 O 4 , and the chemical name is: ±-1-[3-chloro-4-(1,1,2-trifluoro-2-tri Fluoromethoxyethoxy)phenyl]-3-(2,6-difluorophenyl)urea, CAS number: 116714-46-6, structural formula:
氟酰脲是由以色列马克西姆化学品有限公司研发的新型含氟苯甲酰脲类昆虫生长调节剂，作用机理是阻止昆虫生长过程中几丁质合成，抑制蜕皮，对益虫安全，是优秀的高效低毒杀虫剂品种之一。在较低剂量时，显示出对鳞翅目、鞘翅目、半翅目以及双翅目昆虫的幼虫有明显的防除效果。可用于棉花、水稻、果树、蔬菜上的多种病虫害防治。Fluorourea is a new type of fluorine-containing benzoylurea insect growth regulator developed by Israel Maxim Chemicals Co., Ltd. The mechanism of action is to prevent the synthesis of chitin during the growth of insects and inhibit moulting. It is safe for beneficial insects and is excellent. One of the high-efficiency and low-toxic insecticide varieties. At lower doses, it shows obvious control effect on larvae of Lepidoptera, Coleoptera, Hemiptera and Diptera. It can be used to control various diseases and insect pests on cotton, rice, fruit trees and vegetables.
氟氯氰菊酯英文名称为Cyfluthrin，分子式为C22H18Cl2FNO3，化学名称为(1R,S)－顺,反式－2,2－二甲基－3－(2,2－二氯乙烯基)环丙烷羧酸－A－氰基－3－苯氧基－4－氟苄酯，化学结构式为The English name of cyfluthrin is Cyfluthrin, the molecular formula is C 22 H 18 Cl 2 FNO 3 , and the chemical name is (1R,S)-cis,trans-2,2-dimethyl-3-(2,2-dichloroethylene base) cyclopropanecarboxylic acid-A-cyano-3-phenoxy-4-fluorobenzyl ester, the chemical structure is
氟氯氰菊酯以触杀和胃毒作用为主，无内吸及熏蒸作用，杀虫谱广，作用迅速，持效期长，具用一些杀卵活性，并对某些成虫有拒避作用。对光稳定，对鳞翅目多种幼虫及蚜虫等害虫有良好的效果，适用于棉花、烟草、蔬菜、大豆、花生、玉米等作物。Cyfluthrin mainly has contact and stomach poisoning effects, no systemic and fumigation effects, wide insecticidal spectrum, rapid action, long-lasting effect, some ovicidal activity, and repellent effect on some adults. It is stable to light and has good effects on various lepidopteran larvae and aphids and other pests. It is suitable for cotton, tobacco, vegetables, soybeans, peanuts, corn and other crops.
氰戊菊酯英文名称为Phenvalerate，分子式为C25H22ClNO3，化学名称为(R,S)-Α-氰基-3-苯氧基苄基(R,S)- 2-(4-氯苯基)-3-甲基丁酸酯，化学结构式为The English name of fenvalerate is Phenvalerate, the molecular formula is C 25 H 22 ClNO 3 , and the chemical name is (R,S)-α-cyano-3-phenoxybenzyl(R,S)-2-(4- Chlorophenyl)-3-methylbutyrate, the chemical structure is
氰戊菊酯是广谱、高效、快速拟除虫菊酯。以触杀和胃毒作用为主，无内吸作用，对螨类无效，对鳞翅目幼虫、直翅目、半翅目、双翅目害虫有效，用于防治棉花蚜虫、叶蝉、蝽象、卷叶虫、菜青虫、大豆食心虫、小麦黏虫、红铃虫、棉铃虫、柑橘潜叶蛾幼虫，Fenvalerate is a broad-spectrum, highly effective, rapid pyrethroid. It is mainly used for contact killing and stomach poisoning, has no systemic effect, is ineffective against mites, is effective against Lepidoptera larvae, Orthoptera, Hemiptera, and Diptera pests, and is used to control cotton aphids, leafhoppers, and stinkbugs , leaf roller, cabbage caterpillar, soybean borer, wheat armyworm, red bollworm, cotton bollworm, citrus leaf miner larvae,
醚菊酯英文名称为Ethofenprox，分子式为C25H28O3，化学名称为2-(4-乙氧基苯基-2-甲基丙基-3-苯氧基苄基醚，化学结构式为The English name of Ethofenprox is Ethofenprox, the molecular formula is C 25 H 28 O 3 , the chemical name is 2-(4-ethoxyphenyl-2-methylpropyl-3-phenoxybenzyl ether, and the chemical structural formula is
醚菊酯具有杀虫谱广、杀虫活性高、击倒速度快、残效期长、对作物安全等特点。具有触杀、胃毒和内吸作用。用于防治鳞翅目、半翅目、鞘翅目、双翅目、直翅目和等翅目害虫，如褐色虱、白背飞虱、黑尾叶蝉、棉铃虫、红铃虫、桃蚜、瓜蚜、白粉虱、菜青虫、茶毛虫、茶尺蠖、茶刺蛾、桃和梨小食心虫、柑橘潜叶蛾、烟草夜蛾、小菜蛾、玉米螟、大螟、大豆食心虫等。Etoproxil has the characteristics of broad insecticidal spectrum, high insecticidal activity, fast knockdown speed, long residual effect period, and safety to crops. It has contact, stomach poisoning and systemic effects. Used to control Lepidoptera, Hemiptera, Coleoptera, Diptera, Orthoptera and Isoptera pests, such as brown lice, white-backed planthopper, black-tailed leafhopper, cotton bollworm, red bollworm, green peach aphid , melon aphid, whitefly, cabbage caterpillar, tea caterpillar, tea looper, tea thorn moth, peach and pear small borer, citrus leaf miner, tobacco armyworm, diamondback moth, corn borer, large borer, soybean borer, etc.
菊酯类杀虫剂是20 世纪70 年代研发成功的一类仿生杀虫剂，防治谱广，杀虫速效性好，但使用至今菊酯类杀虫剂已对大部分害虫已产生抗药性，防治效果不佳。氟酰脲单用防治作物害虫的防治谱窄，单用速效差，如长期单一使用，易产生抗性，防效降低。同时，如制备成乳油、可湿性粉剂、悬浮剂等常规剂型，这些常规剂型只能进行常规喷雾，如使用低容量喷雾，雾滴不均匀，达不到使用常喷雾的效果。随着农作物种植的规模化，使用上述常规剂进行常规喷雾存在着工效低，药剂用量大，防效低，药剂利用率低。Pyrethroid insecticides are a class of biomimetic insecticides successfully developed in the 1970s. They have a broad control spectrum and good quick-acting insecticidal effects. The control effect is not good. The single use of fluorourea to control crop pests has a narrow control spectrum, and the single use has poor quick effect. If it is used alone for a long time, it is easy to produce resistance and reduce the control effect. At the same time, if it is prepared into conventional dosage forms such as emulsifiable concentrates, wettable powders, and suspension concentrates, these conventional dosage forms can only be used for conventional spraying. If low-volume spraying is used, the droplets will be uneven, and the effect of regular spraying will not be achieved. With the scale of crop planting, conventional spraying with the above-mentioned conventional agents has low work efficiency, large dosage of agents, low control effect and low utilization rate of agents.
因此，如何对这两种药剂进行组合，以产生新的、更有效的防治效果，延缓这两种药剂的使用寿命，扩大防治虫谱，提高防效，特别是充分利用菊酯类等这种老农药成分的余力，减少新农药活性成分的开发成本是农药领域迫切需要解决的技术问题。Therefore, how to combine these two agents to produce new and more effective control effects, delay the service life of these two agents, expand the spectrum of insect control, and improve the control effect, especially by making full use of pyrethroids, etc. The remaining power of old pesticide ingredients and reducing the development cost of new pesticide active ingredients are technical problems that need to be solved urgently in the field of pesticides.
发明内容Contents of the invention
为解决以上技术问题，本发明提供一种含氟酰脲与氨基甲酸酯类杀虫剂的超低容量液剂制剂，并提供所述超低容量液剂的制备方法，该超低容量液剂进行低容量或超低容量喷雾，工效高，无需兑水，用量少，防效高，协调增效并扩大防治谱。In order to solve the above technical problems, the present invention provides an ultra-low volume liquid preparation containing fluorine urea and carbamate insecticide, and provides a preparation method of the ultra-low volume liquid, the ultra-low volume liquid Low-volume or ultra-low-volume spraying has high work efficiency, no need to add water, less dosage, high control efficiency, coordinated synergies and expanded control spectrum.
本发明制成的超低容量液剂剂型，它是以氟酰脲和活性组分II复配为活性成分，其余用表面活性剂和溶剂补足100%；活性组分II为三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、氰戊菊酯、高效氯氰菊酯、溴氰菊酯、醚菊酯的任意一种。The ultra-low-capacity liquid dosage form made by the present invention is made of fluoride and active component II as the active component, and the rest is supplemented by surfactant and solvent to make up 100%; the active component II is cyhalothrin, fluorine Any one of cypermethrin, bifenthrin, fenvalerate, beta-cypermethrin, deltamethrin, and etofenprox.
所述氟酰脲和活性组分II复配为活性成分，其总量的重量百分比含量为0.2%～40%，氟酰脲的重量百分比含量为0.1%～20%，活性组分II的重量百分比含量为0.1%～20%，表面活性剂的重量含量为1%～10%，溶剂补足至100%。The compound of the fluorourea and the active component II is the active ingredient, the total weight percentage content of which is 0.2% to 40%, the weight percentage content of the fluoride urea is 0.1% to 20%, and the weight percentage of the active component II is The percentage content is 0.1%-20%, the weight content of the surfactant is 1%-10%, and the solvent is supplemented to 100%.
本发明优选配方可为该超低容量液剂以氟酰脲和活性组分II复配为活性成分，其总量的重量含量为0.2%～40%， 5～20%；氟酰脲的重量含量为0.1%～20%， 1%～10%；活性组分II的重量含量为0.1%～20%， 4%～10%，助剂的重量含量为1%～10%， 3～10%；溶剂补足至100%。The preferred formula of the present invention can be that the ultra-low volume liquid is compounded with fluoride and active component II as the active ingredient, and its total weight content is 0.2% to 40%, 5 to 20%; the weight of fluoride The content is 0.1%～20%, 1%～10%; the weight content of active component II is 0.1%～20%, 4%～10%, the weight content of auxiliary agent is 1%～10%, 3～10% ; Make up to 100% solvent.
氟酰脲与三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、氰戊菊酯、高效氯氰菊酯、溴氰菊酯、醚菊酯中的任一杀虫剂活性成分复配成的超低容量液剂对靶标害虫具有极强的增效作用。Ultra-low-volume liquid formulation of fluorourea and any insecticide active ingredient in cyhalothrin, cyfluthrin, bifenthrin, fenvalerate, beta-cypermethrin, deltamethrin, and etofenprox It has a strong synergistic effect on target pests.
所述表面活性剂选自脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、烷基芳基聚氧丙烯聚氧乙烯醚、脂肪醇聚氧乙烯醚磷酸酯、烷基酚聚氧乙烯醚磷酸酯、苯乙基酚聚氧乙烯醚磷酸酯、烷基芳基聚氧丙烯聚氧乙烯醚磷酸酯、蓖麻油聚氧乙烯醚、十二烷基苯磺酸钙中的一种或一种以上的组合，优选脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、烷基芳基聚氧丙烯聚氧乙烯醚、蓖麻油聚氧乙烯醚、十二烷基苯磺酸钙。The surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, styrene ethylphenol polyoxyethylene ether, alkylaryl polyoxypropylene polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphoric acid Ester, Alkylphenol Polyoxyethylene Ether Phosphate, Styroylphenol Polyoxyethylene Ether Phosphate, Alkylaryl Polyoxypropylene Polyoxyethylene Ether Phosphate, Castor Oil Polyoxyethylene Ether, Dodecyl Benzene Sulfonate One or more combinations of calcium acid calcium, preferably fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, styrene ethylphenol polyoxyethylene ether, alkylaryl polyoxypropylene polyoxyethylene ether, Castor Oil Ethoxylates, Calcium Dodecyl Benzene Sulfonate.
所述的表面活性剂本身虽没有生物活性，但其的选择和加入可以提高药效、降低农药的用量，增加药剂在植物表面的润湿、展布、粘着、渗透、改善配伍作用，促进药剂的渗入并有利吸收。Although the surfactant itself has no biological activity, its selection and addition can improve the efficacy of the drug, reduce the amount of pesticides, increase the wetting, spreading, adhesion, penetration, and improve the compatibility of the agent on the plant surface, and promote the improvement of the chemical agent. Penetration and absorption.
所述溶剂为芳烃类溶剂、植物油类溶剂和极性溶剂中的一种或多种组合；芳烃类溶剂包括三甲苯、邻二氯苯、四甲苯、二乙苯、甲基丙基苯、丁苯、甲基萘、二线油；植物油类溶剂包括大豆油、棉籽油、玉米油、菜籽油、蓖麻油、松节油、油酸甲酯、油酸乙酯；极性溶剂包括苯乙酮、苯甲醇、二甲亚砜、N-甲基吡咯烷酮、N，N-二甲基甲酰胺、N，N-二甲基乙酰胺、正己醇、正辛醇、松油醇。The solvent is one or more combinations of aromatic solvents, vegetable oil solvents and polar solvents; aromatic solvents include trimethylbenzene, o-dichlorobenzene, tetramethylbenzene, diethylbenzene, methylpropylbenzene, butyl Benzene, methylnaphthalene, second-line oil; vegetable oil solvents include soybean oil, cottonseed oil, corn oil, rapeseed oil, castor oil, turpentine, methyl oleate, ethyl oleate; polar solvents include acetophenone, benzene Methanol, dimethylsulfoxide, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, n-hexanol, n-octanol, terpineol.
因超低容量液剂的施用方法是超低容量喷雾、低容量喷雾或超低容量静电喷雾，所以对溶剂有严格的要求，且超低容量液剂以溶剂为主要载体，溶剂的用量通常占制剂总量的一半以上，有些产品甚至达到90%。因此，溶剂品种的选择是配制超低容量液剂的关键技术也是难点，溶剂品种选择的不合适影响超低容量液剂喷雾时的雾滴大小和雾滴大小的均匀度，从而影响防效。故超低容量液剂的溶剂选择并不象乳油、微乳剂等常规液体制剂只要求溶解完全农药原药。Because the application method of the ultra-low volume liquid is ultra-low volume spray, low-volume spray or ultra-low-volume electrostatic spray, there are strict requirements on the solvent, and the ultra-low volume liquid uses solvent as the main carrier, and the amount of solvent usually accounts for More than half of the total preparations, some products even reach 90%. Therefore, the choice of solvent type is the key technology and difficulty of preparing ultra-low volume liquid agent. The inappropriate selection of solvent type affects the droplet size and the uniformity of droplet size when the ultra-low volume liquid agent is sprayed, thereby affecting the control effect. Therefore, the solvent selection of ultra-low volume liquid preparations is not like conventional liquid preparations such as emulsifiable concentrates and microemulsions, which only require complete dissolution of the original pesticide.
本发明所述的超低容量液剂的制备方法为，在带搅拌的反应容器中，先用溶剂将活性成分搅拌溶解后，再加入助剂成分，充分搅拌混合均匀，即得含氟酰脲和氨基甲酸酯类杀虫剂的超低容量液剂；工艺参数为：搅拌速度控制为60～150转/分钟，搅拌时间为15～60分钟，温度为常温，压力为常压。The preparation method of the ultra-low-capacity liquid agent of the present invention is as follows: in a stirred reaction vessel, the active ingredient is stirred and dissolved with a solvent, and then the auxiliary ingredient is added, and the fluorine-containing urea is obtained by fully stirring and mixing evenly. It is an ultra-low volume liquid agent of carbamate insecticides; the process parameters are as follows: the stirring speed is controlled at 60-150 rpm, the stirring time is 15-60 minutes, the temperature is normal temperature, and the pressure is normal pressure.
适合的靶标作物是水稻、小麦等粮食作物，甘蔗、香蕉、橡胶、棉花、茶树、柑橘、苹果、山楂、桃树等经济作物，番茄、茄子、辣椒、莴苣、芹菜、甘蓝、菜豆、蚕豆、豇豆、豌豆等蔬菜作物，黄瓜、南瓜、西瓜等葫芦科作物。Suitable target crops are food crops such as rice and wheat, economic crops such as sugar cane, banana, rubber, cotton, tea tree, citrus, apple, hawthorn, peach tree, tomato, eggplant, pepper, lettuce, celery, cabbage, kidney bean, broad bean, Cowpea, pea and other vegetable crops, cucumber, pumpkin, watermelon and other cucurbit crops.
本发明的超低容量液剂适合防治稻飞虱、稻纵卷叶螟、褐飞虱、白背飞虱、灰飞虱、二化螟、稻蓟马、稻瘿蚊、稻叶蝉、黑尾叶蝉、稻蛛椽蝽、象星蝽象、稻绿蝽象、红须盲蝽、稻负混虫、稻筒水螟、稻蝗、 蚜虫类、粉虱类、蚧类、矢尖盾蚧、朱绿蝽、桃小食心虫、桔潜蛾、茶细蛾、黄条跳甲、豆潜蝇。 角腊蚧、小菜蛾、二黑条叶甲、茶黄蓟马、烟蓟马、黄蓟马、柑橘黄蓟马、大豆荚瘿蚊、番茄潜叶蝇。The ultra-low-capacity liquid agent of the present invention is suitable for controlling rice planthopper, rice leaf roller, brown planthopper, white-backed planthopper, brown planthopper, rice stem borer, rice thrips, rice gall midge, rice leafhopper, black-tailed leafhopper Cicadas, rice spider rafters, elephant star bugs, rice green stinkbugs, red bearded stinkbugs, rice gnats, rice tube borers, rice locusts, aphids, whiteflies, scales, scorpion scales, Vermilion stinkbug, peach borer, orange moth, tea moth, yellow striped flea beetle, bean liriod. Horned wax scale, diamondback moth, two-black-striped leaf beetle, tea yellow thrips, tobacco thrips, yellow thrips, citrus yellow thrips, soybean pod gall midge, tomato leafminer.
主要通过超低容量喷雾、低容量喷雾或超低容量静电喷雾实现对作物害虫的有效防治。施用本发明的超低容量液剂的优选方法是超低容量喷雾，其次是低容量喷雾和超低容量静电喷雾，根据防治对象发生情况确定适宜的用药量，通常施药量是75～150g a.i./hm2.Effective control of crop pests is mainly achieved through ultra-low volume spraying, low-volume spraying or ultra-low-volume electrostatic spraying. The preferred method of applying the ultra-low volume liquid agent of the present invention is ultra-low volume spraying, followed by low-volume spraying and ultra-low-volume electrostatic spraying. The appropriate dosage is determined according to the occurrence of the control object, usually the dosage is 75-150g ai /hm 2 .
超低容量液剂通过筛选挥发性低、闪点高、对原药溶解性好、对作物药害低、粘度低的溶剂，施药时不兑水，而是用超低容量喷雾器械、低容量喷雾器械或超低容量静电喷雾器械直接施用。超低容量喷雾由于雾滴中不含高挥发性成分，其大小与质量从离开喷雾器械到达靶标过程中没有明显变化，减少了挥发与飘逸。雾滴细小而均匀，符合“生物最佳粒剂”要求，显著提高了沉积量。由于无需兑水施用，超低容量液剂适合用于水源缺乏、病虫害暴发性大面积发生且须短时间内大范围施药的场合，同时超低容量喷雾极大的降低操作者的劳动强度。The ultra-low-capacity liquid agent screens out solvents with low volatility, high flash point, good solubility to the original drug, low phytotoxicity to crops, and low viscosity. When spraying, do not add water, but use ultra-low-capacity spray equipment, low Direct application with volumetric spray or ultra-low volume electrostatic spray. Since the ultra-low volume spray does not contain highly volatile components in the droplets, its size and mass do not change significantly when it leaves the spray device and reaches the target, which reduces volatilization and drift. The mist droplets are fine and uniform, which meet the requirements of "biologically optimal granules", and significantly increase the deposition amount. Since it does not need to be applied with water, the ultra-low-volume liquid is suitable for occasions where water is scarce, outbreaks of diseases and insect pests occur in a large area, and large-scale application is required in a short period of time. At the same time, ultra-low-volume spraying greatly reduces the labor intensity of the operator.
本发明所述的超低容量液剂工效高，人工超低容量喷雾每亩只花10分钟（人工常规喷雾每亩耗时0.5-1小时）协调增效作用，氟酰脲和菊酯类杀虫剂复配在本申请限定的数值范围内其共毒系数均大于120，表现出明显的增效作用；药效好，均达85%以上；持效长，持效期长达14天，且14天后的对害虫的防治效果达80%以上、、节省水；可以降低环境污染，提高农药利用率，降低农药施用量。The ultra-low-capacity liquid agent described in the present invention has high work efficiency, and the artificial ultra-low-capacity spraying only takes 10 minutes per mu (artificial conventional spraying takes 0.5-1 hour per mu). The insecticide compound has its co-toxicity coefficient greater than 120 within the numerical range limited by the application, showing obvious synergistic effect; the drug effect is good, all reaching more than 85%; the lasting effect is long, and the lasting effect period is as long as 14 days. And after 14 days, the control effect on pests reaches more than 80%, saves water; can reduce environmental pollution, improve the utilization rate of pesticides, and reduce the amount of pesticides used.
具体实施方式detailed description
下面结合实施例对本发明进一步说明，但不限制本发明的范围。The present invention is further described below in conjunction with embodiment, but does not limit the scope of the present invention.
实施例1 5%氟酰脲·氟氯氰菊酯超低容量液剂（4：1）Example 1 5% fluorourea·cyfluthrin ultra-low volume solution (4:1)
氟酰脲 4 kgFluoride 4 kg
氟氯氰菊酯 1kgCyfluthrin 1kg
N,N-二甲基甲酰胺 13.0 kgN,N-Dimethylformamide 13.0 kg
甲基萘 5.0 kgMethylnaphthalene 5.0 kg
邻二氯苯 3.0 kgo-dichlorobenzene 3.0 kg
十二烷基苯磺酸钙 0.2 kgCalcium dodecylbenzenesulfonate 0.2 kg
蓖麻油聚氧乙烯醚 0.8kgCastor oil polyoxyethylene ether 0.8kg
玉米油 补足至100 kgCorn oil make up to 100 kg
制备工艺：在带搅拌的反应容器中，先用溶剂将氟酰脲和氟氯氰菊酯搅拌溶解后，再加入助剂成分，充分搅拌混合均匀，即得5%氟酰脲·氟氯氰菊酯超低容量液剂；工艺参数为：搅拌速度控制为60～150转/分钟，搅拌时间为15～60分钟，温度为常温，压力为常压。Preparation process: In a stirred reaction vessel, first use a solvent to stir and dissolve fluorourea and cyfluthrin, then add auxiliary ingredients, stir and mix well to obtain 5% fluorourea-cyfluthrin ultra-low volume liquid agent; the process parameters are: the stirring speed is controlled at 60-150 rpm, the stirring time is 15-60 minutes, the temperature is normal temperature, and the pressure is normal pressure.
按照与实施例1相同的制备工艺步骤，可以制备以下实施例。According to the same preparation process steps as in Example 1, the following examples can be prepared.
实施例2 6.2%氟酰脲·氟氯氰菊酯超低容量液剂（30：1）Example 2 6.2% fluorourea·cyfluthrin ultra-low volume solution (30:1)
氟酰脲 6.0 kgFluoride 6.0 kg
氟氯氰菊酯 0.2kgCyfluthrin 0.2kg
N-甲基吡咯烷酮 7.5 kgN-Methylpyrrolidone 7.5 kg
四甲苯 8.0 kgTetramethylbenzene 8.0 kg
油酸乙酯 7.0 kgEthyl oleate 7.0 kg
十二烷基苯磺酸钙 1.0 kgCalcium dodecylbenzenesulfonate 1.0 kg
苯乙基酚聚氧乙烯醚磷酸酯 1.5 kgPhenylphenol ethoxylate phosphate 1.5 kg
烷基酚聚氧乙烯醚磷酸酯 2.0 kgAlkylphenol ethoxylate phosphate 2.0 kg
二线油 补足至100 kgSecond line oil make up to 100 kg
实施例3 14%氟酰脲·氟氯氰菊酯超低容量液剂（5：2）Example 3 14% fluorourea·cyfluthrin ultra-low volume solution (5:2)
氟酰脲 10.0 kgFluoride 10.0 kg
氟氯氰菊酯 4.0 kgCyfluthrin 4.0 kg
N-甲基吡咯烷酮 6.0 kgN-Methylpyrrolidone 6.0 kg
N，N-二甲基乙酰胺 5.0 kgN,N-Dimethylacetamide 5.0 kg
松油醇 5.5 kgTerpineol 5.5 kg
四甲苯 5.0 kgTetramethylbenzene 5.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
辛基酚聚氧乙烯醚 1.5 kgOctylphenol ethoxylate 1.5 kg
蓖麻油聚氧乙烯醚 2.0 kgCastor oil ethoxylates 2.0 kg
菜籽油 补足至100 kgRapeseed oil make up to 100 kg
实施例4 20%氟酰脲·氟氯氰菊酯超低容量液剂（1:1）Example 4 20% fluorourea·cyfluthrin ultra-low volume solution (1:1)
氟酰脲 10.0 kgFluoride 10.0 kg
氟氯氰菊酯 10.0 kgCyfluthrin 10.0 kg
N，N-二甲基乙酰胺 10.0 kgN,N-Dimethylacetamide 10.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
三甲苯 4.0 kgTrimethylbenzene 4.0 kg
甲基丙基苯 10.0 kgMethpropylbenzene 10.0 kg
烷基酚聚氧乙烯醚 4.5kgAlkylphenol polyoxyethylene ether 4.5kg
蓖麻油聚氧乙烯醚 2.5 kgCastor oil ethoxylates 2.5 kg
脂肪醇聚氧乙烯醚磷酸酯 3.0kgFatty alcohol polyoxyethylene ether phosphate 3.0kg
油酸甲酯 补足至100 kgMethyl oleate make up to 100 kg
实施例5 11%氟酰脲·氟氯氰菊酯超低容量液剂(1:10)Example 5 11% fluorourea·cyfluthrin ultra-low volume liquid (1:10)
氟酰脲 1.0 kgFluoride 1.0 kg
氟氯氰菊酯 10.0 kgCyfluthrin 10.0 kg
N,N-二甲基甲酰胺 5.0 kgN,N-Dimethylformamide 5.0 kg
N-甲基吡咯烷酮 8.0 kgN-Methylpyrrolidone 8.0 kg
四甲苯 8.0 kgTetramethylbenzene 8.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
脂肪醇聚氧乙烯醚 2.0 kgFatty alcohol polyoxyethylene ether 2.0 kg
松节油 补足至100 kgTurpentine make up to 100 kg
实施例6 10.5%氟酰脲·氟氯氰菊酯超低容量液剂（1：20）Example 6 10.5% fluorourea·cyfluthrin ultra-low volume solution (1:20)
氟酰脲 0.5 kgFluoride 0.5 kg
氟氯氰菊酯 10kgCyfluthrin 10kg
N,N-二甲基甲酰胺 5.0 kgN,N-Dimethylformamide 5.0 kg
苯乙酮 10.0 kgAcetophenone 10.0 kg
油酸甲酯 8.0 kgMethyl oleate 8.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
苯乙基酚聚氧乙烯醚磷酸酯 3.0kgPhenylphenol polyoxyethylene ether phosphate 3.0kg
脂肪醇聚氧乙烯醚 2.0 kgFatty alcohol polyoxyethylene ether 2.0 kg
大豆油 补足至100 kgSoybean oil make up to 100 kg
实施例7 8.2%氟酰脲·氰戊菊酯超低容量液剂（40：1）Example 7 8.2% fluorourea·fenvalerate ultra-low volume liquid (40:1)
氟酰脲 8.0 kgFluoride 8.0 kg
氰戊菊酯 0.2 kgFenvalerate 0.2 kg
N,N-二甲基甲酰胺 5.0 kgN,N-Dimethylformamide 5.0 kg
N-甲基吡咯烷酮 4.0 kgN-Methylpyrrolidone 4.0 kg
苯乙酮 10.0 kgAcetophenone 10.0 kg
油酸甲酯 8.0 kgMethyl oleate 8.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
苯乙基酚聚氧乙烯醚磷酸酯 3.0kgPhenylphenol polyoxyethylene ether phosphate 3.0kg
脂肪醇聚氧乙烯醚 2.0 kgFatty alcohol polyoxyethylene ether 2.0 kg
大豆油 补足至100 kgSoybean oil make up to 100 kg
实施例8 9.2%氟酰脲·氰戊菊酯超低容量液剂（1：45）Example 8 9.2% fluorourea·fenvalerate ultra-low volume liquid (1:45)
氟酰脲 0.2 kgFluoride 0.2 kg
氰戊菊酯 9.0 kgFenvalerate 9.0 kg
N，N-二甲基乙酰胺 10.0 kgN,N-Dimethylacetamide 10.0 kg
N-甲基吡咯烷酮 9.0 kgN-Methylpyrrolidone 9.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
松节油 4.0 kgTurpentine 4.0 kg
甲基丙基苯 10.0 kgMethpropylbenzene 10.0 kg
烷基酚聚氧乙烯醚 3.0kgAlkylphenol polyoxyethylene ether 3.0kg
烷基芳基聚氧丙烯聚氧乙烯醚磷酸酯 1.5 kgAlkylaryl polyoxypropylene polyoxyethylene ether phosphate 1.5 kg
烷基芳基聚氧丙烯聚氧乙烯醚 3.0kgAlkylaryl polyoxypropylene polyoxyethylene ether 3.0kg
棉籽油 补足至100 kgCottonseed oil make up to 100 kg
实施例9 18%氟酰脲·氰戊菊酯超低容量液剂（1：1）Example 9 18% fluorourea·fenvalerate ultra-low volume liquid (1:1)
氟酰脲 9.0 kgFluoride 9.0 kg
氰戊菊酯 9.0 kgFenvalerate 9.0 kg
N-甲基吡咯烷酮 7.5 kgN-Methylpyrrolidone 7.5 kg
N,N-二甲基乙酰胺 8.0 kgN,N-Dimethylacetamide 8.0 kg
四甲苯 8.0 kgTetramethylbenzene 8.0 kg
苯甲醇 2.0 kgBenzyl alcohol 2.0 kg
油酸乙酯 5.0 kgEthyl oleate 5.0 kg
十二烷基苯磺酸钙 4.0 kgCalcium dodecylbenzenesulfonate 4.0 kg
脂肪醇聚氧乙烯醚磷酸酯 2.5 kgFatty alcohol polyoxyethylene ether phosphate 2.5 kg
烷基酚聚氧乙烯醚磷酸酯 3.5 kgAlkylphenol ethoxylate phosphate 3.5 kg
玉米油 补足至100 kgCorn oil make up to 100 kg
实施例10 40.0%氟酰脲·氰戊菊酯超低容量液剂（1:1）Example 10 40.0% fluorourea·fenvalerate ultra-low volume liquid (1:1)
氟酰脲 20.0 kgFluoride 20.0 kg
氰戊菊酯 20.0 kgFenvalerate 20.0 kg
N-甲基吡咯烷酮 6.0 kgN-Methylpyrrolidone 6.0 kg
N,N-二甲基甲酰胺 5.0 kgN,N-Dimethylformamide 5.0 kg
正辛醇 5.5 kgn-octanol 5.5 kg
二乙苯 5.0 kgDiethylbenzene 5.0 kg
松油醇 3.0 kgTerpineol 3.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
辛基酚聚氧乙烯醚 1.5 kgOctylphenol ethoxylate 1.5 kg
蓖麻油聚氧乙烯醚 2.0 kgCastor oil ethoxylates 2.0 kg
菜籽油 补足至100 kgRapeseed oil make up to 100 kg
实施例11 9%氟酰脲·氰戊菊酯超低容量液剂（8：1）Example 11 9% fluorourea·fenvalerate ultra-low volume liquid (8:1)
氟酰脲 8 kgFluoride 8 kg
氰戊菊酯 1.0kgFenvalerate 1.0kg
N，N-二甲基乙酰胺 10.0 kgN,N-Dimethylacetamide 10.0 kg
N-甲基吡咯烷酮 9.0 kgN-Methylpyrrolidone 9.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
松节油 4.0 kgTurpentine 4.0 kg
甲基丙基苯 10.0 kgMethpropylbenzene 10.0 kg
烷基酚聚氧乙烯醚 4.0kgAlkylphenol polyoxyethylene ether 4.0kg
烷基芳基聚氧丙烯聚氧乙烯醚磷酸酯 2.5 kgAlkylarylpolyoxypropylene polyoxyethylene ether phosphate 2.5 kg
烷基芳基聚氧丙烯聚氧乙烯醚 3.5kgAlkylaryl polyoxypropylene polyoxyethylene ether 3.5kg
二线油 补足至100 kgSecond line oil make up to 100 kg
实施例12 5.2%氟酰脲·醚菊酯超低容量液剂（25：1）Example 12 5.2% fluorourea·etoproxil ultra-low volume solution (25:1)
氟酰脲 5.0 kgFluoride 5.0 kg
醚菊酯 0.2 kgEtoproxil 0.2 kg
N-甲基吡咯烷酮 5.0 kgN-Methylpyrrolidone 5.0 kg
二甲亚砜 6.0 kgDimethyl sulfoxide 6.0 kg
苯乙酮 10.0 kgAcetophenone 10.0 kg
环氧大豆油 5.0 kgEpoxidized soybean oil 5.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
油酸甲酯 8.0 kgMethyl oleate 8.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
脂肪醇聚氧乙烯醚 2.0 kgFatty alcohol polyoxyethylene ether 2.0 kg
大豆油 补足至100 kgSoybean oil make up to 100 kg
实施例13 9.3%氟酰脲·醚菊酯超低容量液剂（1：30）Example 13 9.3% fluorourea·etoproxil ultra-low volume solution (1:30)
氟酰脲 0.3kgFluoride 0.3kg
醚菊酯 9.0kgEtoproxil 9.0kg
N-甲基吡咯烷酮 10.0kgN-Methylpyrrolidone 10.0kg
N,N-二甲基甲酰胺 5.0kgN,N-Dimethylformamide 5.0kg
丁苯 4.0kgButadiene 4.0kg
正丁醇 2.0kgn-Butanol 2.0kg
十二烷基苯磺酸钙 2.5kgCalcium dodecylbenzenesulfonate 2.5kg
苯乙基酚聚氧乙烯醚磷酸酯 1.0kgPhenylphenol polyoxyethylene ether phosphate 1.0kg
苄基联苯酚聚氧乙烯醚 2.5kgBenzyl biphenol polyoxyethylene ether 2.5kg
棉籽油 补足至100kgCottonseed oil make up to 100kg
实施例14 35%氟酰脲·醚菊酯超低容量液剂（1：6）Example 14 35% fluorourea·etofenprox ultra-low volume solution (1:6)
氟酰脲 5.0kgFluoride 5.0kg
醚菊酯 30.0kgEtoproxil 30.0kg
N,N-二甲基甲酰胺 6.0 kgN,N-Dimethylformamide 6.0 kg
N-甲基吡咯烷酮 15.0 kgN-Methylpyrrolidone 15.0 kg
二甲亚砜 4.0 kgDimethyl sulfoxide 4.0 kg
油酸乙酯 4.0 kgEthyl oleate 4.0 kg
松油醇 2.0 kgTerpineol 2.0 kg
十二烷基苯磺酸钙 2.0 kgCalcium dodecylbenzenesulfonate 2.0 kg
苯乙基酚聚氧乙烯醚 3.0kgPhenylphenol polyoxyethylene ether 3.0kg
脂肪醇聚氧乙烯醚磷酸酯 5.0 kgFatty alcohol polyoxyethylene ether phosphate 5.0 kg
蓖麻油 补足至100 kgCastor oil to top up to 100 kg
实施例15 20%氟酰脲·醚菊酯超低容量液剂（1：1）Example 15 20% fluorourea·etofenprox ultra-low volume solution (1:1)
氟酰脲 10.0kgFluoride 10.0kg
醚菊酯 10.0kgEtoproxil 10.0kg
N，N-二甲基乙酰胺 10.0 kgN,N-Dimethylacetamide 10.0 kg
N-甲基吡咯烷酮 9.0 kgN-Methylpyrrolidone 9.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
松节油 4.0 kgTurpentine 4.0 kg
甲基丙基苯 10.0 kgMethpropylbenzene 10.0 kg
烷基酚聚氧乙烯醚 3.0kgAlkylphenol polyoxyethylene ether 3.0kg
烷基芳基聚氧丙烯聚氧乙烯醚磷酸酯 1.5 kgAlkylaryl polyoxypropylene polyoxyethylene ether phosphate 1.5 kg
烷基芳基聚氧丙烯聚氧乙烯醚 3.0kgAlkylaryl polyoxypropylene polyoxyethylene ether 3.0kg
棉籽油 补足至100 kgCottonseed oil make up to 100 kg
实施例16 12%氟酰脲·醚菊酯超低容量液剂（2：1）Example 16 12% fluorourea·etofenprox ultra-low volume solution (2:1)
氟酰脲 8 kgFluoride 8 kg
醚菊酯 4kgEtoproxil 4kg
N-甲基吡咯烷酮 7.5 kgN-Methylpyrrolidone 7.5 kg
三甲苯 8.0 kgTrimethylbenzene 8.0 kg
正辛醇 2.0 kgn-octanol 2.0 kg
油酸乙酯 5.0 kgEthyl oleate 5.0 kg
十二烷基苯磺酸钙 1.0 kgCalcium dodecylbenzenesulfonate 1.0 kg
脂肪醇聚氧乙烯醚磷酸酯 2.5 kgFatty alcohol polyoxyethylene ether phosphate 2.5 kg
蓖麻油聚氧乙烯醚 2.0 kgCastor oil ethoxylates 2.0 kg
玉米油 补足至100 kgCorn oil make up to 100 kg
实施例17 12%氟酰脲·醚菊酯超低容量液剂（11：1）Example 17 12% fluorourea·etofenprox ultra-low volume solution (11:1)
氟酰脲 11 kgFluoride 11 kg
醚菊酯 1 kgEtoproxil 1 kg
N-甲基吡咯烷酮 7.5 kgN-Methylpyrrolidone 7.5 kg
丁苯 8.0 kgButadiene 8.0 kg
油酸乙酯 7.0 kgEthyl oleate 7.0 kg
十二烷基苯磺酸钙 1.0 kgCalcium dodecylbenzenesulfonate 1.0 kg
辛基酚聚氧乙烯醚 2.5 kgOctylphenol ethoxylate 2.5 kg
烷基酚聚氧乙烯醚磷酸酯 2.0 kgAlkylphenol ethoxylate phosphate 2.0 kg
玉米油 补足至100 kgCorn oil make up to 100 kg
对照1 10%氟酰脲超低容量液剂Control 1 10% fluorourea ultra-low volume liquid
氟酰脲 10.0 kgFluoride 10.0 kg
N，N-二甲基乙酰胺 10.0 kgN,N-Dimethylacetamide 10.0 kg
正己醇 5.0 kgn-Hexanol 5.0 kg
三甲苯 4.0 kgTrimethylbenzene 4.0 kg
甲基丙基苯 10.0 kgMethpropylbenzene 10.0 kg
烷基酚聚氧乙烯醚 4.5kgAlkylphenol polyoxyethylene ether 4.5kg
蓖麻油聚氧乙烯醚 2.5 kgCastor oil ethoxylates 2.5 kg
脂肪醇聚氧乙烯醚磷酸酯 3.0kgFatty alcohol polyoxyethylene ether phosphate 3.0kg
油酸甲酯 补足至100 kgMethyl oleate make up to 100 kg
使用的溶剂和助剂均与实施例4相同。The solvent and auxiliary agent used are all the same as in Example 4.
所制备的含氟酰脲与菊酯类杀虫剂的超低容量液剂外观为均一油状液体；低温相容性好，在–5℃条件下，冷藏7d不析出结晶和悬浮物；挥发性低，滤纸悬挂发测定结果，挥发率低于30%；对植物安全，无药害；采用闭口法测定，闪点大于70℃；粘度小于30mPa·s；导电率在1×10－6～1×10－10s/cm范围内。The prepared ultra-low-volume liquid formulation of fluorine-containing urea and pyrethroid insecticides has a uniform oily liquid appearance; good low-temperature compatibility, and no crystals and suspended solids are precipitated when stored at –5°C for 7 days; volatility Low, the filter paper hangs to send out the test results, and the volatility rate is less than 30%; it is safe to plants and has no phytotoxicity; it is measured by the closed-mouth method, and the flash point is greater than 70°C; the viscosity is less than 30mPa·s; the conductivity is 1×10 -6 ～1 ×10 -10 s/cm range.
下面再结合应用本发明实施例进行的田间药效测定结果进一步来说明本发明的有益效果。The beneficial effects of the present invention will be further described below in conjunction with the results of field drug efficacy assays carried out using the embodiments of the present invention.
本发明的应用实施例是采用室内毒力测定和田间药效试验相结合的方法。先通过室内毒力测定，明确两种药剂按一定比例复配后的共毒系数（CTC）, CTC＜80为拮抗作用，80＜ CTC＜120为相加作用， CTC＞120为增效作用，在室内毒力测定的基础上确定共毒系数（CTC）大于80即两种药剂混配达到相加和增效作用后，再进行田间药效试验验证其相加或增效的效果。The application example of the present invention adopts the method of combining indoor toxicity test and field efficacy test. The co-toxicity coefficient (CTC) of the two agents after compounding in a certain proportion is clarified first through the indoor toxicity test. CTC<80 means antagonistic effect, 80<CTC<120 means additive effect, and CTC>120 means synergistic effect. On the basis of the indoor toxicity test, it is determined that the co-toxicity coefficient (CTC) is greater than 80, that is, after the two agents are mixed to achieve additive and synergistic effects, then field efficacy tests are conducted to verify their additive or synergistic effects.
试验1test 1
氟酰脲和氟氯氰菊酯室内联合毒力测定试验Indoor Joint Toxicity Test of Fluoride and Cyfluthrin
将氟酰脲和氟氯氰菊酯按有效成分重量比例1:4、60:1、5:2、1:1、1:10、1:20混合配成二元复配剂，试验方法参照《中华人民共和国农业行业标准NY/T 1154.11-2008》、《中华人民共和国农业行业标准NY/T 1154.7-2006》，采用浸叶法，以甘蔗螟虫3龄若虫为试虫，药后48小时检查死虫数，计算死亡率。空白对照点滴等量清水。一般每个处理设置5个浓度梯度。用SPSS统计分析软件进行统计分析，计算各药剂的LC50，依此来评价供试药剂对试虫的活性，依孙云沛计算共毒系数（CTC）。Mix fluoride and cyfluthrin according to the weight ratio of active ingredients 1:4, 60:1, 5:2, 1:1, 1:10, 1:20 to form a binary compound. The test method refers to "Chinese People's The Agricultural Industry Standard of the People's Republic of China NY/T 1154.11-2008 and the Agricultural Industry Standard of the People's Republic of China NY/T 1154.7-2006 use the leaf soaking method, using the 3rd instar nymphs of the sugarcane borer as test insects, and check the number of dead insects 48 hours after the application , to calculate the death rate. The blank control was dripped with the same amount of water. Generally, 5 concentration gradients are set for each treatment. Statistical analysis was carried out with SPSS statistical analysis software, and the LC 50 of each agent was calculated to evaluate the activity of the tested agent on the test insects, and the co-toxicity coefficient (CTC) was calculated according to Sun Yunpei.
表1 氟酰脲和氟氯氰菊酯室内联合毒力测定结果（48小时）Table 1 Indoor joint toxicity test results of fluorourea and cyfluthrin (48 hours)
测定结果见表1，测定结果表明：氟酰脲和氟氯氰菊酯按有效成分重量比例1:4、60:1、5:2、1:1、1:10、1:20混合配制成二元复配剂，对甘蔗螟虫3龄幼虫的共毒系数分别为143.0、128.6、138.1、130.5、126.4、124.1，表明氟酰脲和氟氯氰菊酯按上述比例复配后对甘蔗螟虫均有增效作用。The measurement results are shown in Table 1, and the measurement results show that: fluorourea and cyfluthrin are mixed according to the weight ratio of active ingredients 1:4, 60:1, 5:2, 1:1, 1:10, 1:20 to prepare a binary compound The co-toxicity coefficients to the 3rd instar larvae of the sugarcane borer were 143.0, 128.6, 138.1, 130.5, 126.4, 124.1 respectively, which indicated that the combination of fluoride and cyfluthrin had synergistic effects on the sugarcane borer in the above ratio.
试验2test 2
氟酰脲和氰戊菊酯室内联合毒力测定试验Indoor Joint Toxicity Test of Fluoride and Fenvalerate
将氟酰脲和氰戊菊酯按有效成分重量比例40:1、1:45、1:1、8:1等比例混合配成二元复配剂，试验方法参照《中华人民共和国农业行业标准NY/T 1154.1-2006》、《中华人民共和国农业行业标准NY/T 1154.7-2006》，采用点滴法，以菜青虫3龄若虫为试虫，药后48小时检查死虫数，计算死亡率。空白对照点滴等量清水。一般每个处理设置5个浓度梯度。用SPSS统计分析软件进行统计分析，计算各药剂的LC50，依此来评价供试药剂对试虫的活性，依孙云沛计算共毒系数（CTC）。Mix fluoride and esfenvalerate according to the weight ratio of active ingredients of 40:1, 1:45, 1:1, 8:1 to make a binary compound. The test method refers to the "People's Republic of China Agricultural Industry Standards NY/T 1154.1-2006", "The Agricultural Industry Standard of the People's Republic of China NY/T 1154.7-2006", using the drip method, using the 3rd instar nymph of Pieris rapae as the test insect, checking the number of dead insects 48 hours after the application, and calculating the mortality rate. The blank control was dripped with the same amount of water. Generally, 5 concentration gradients are set for each treatment. Statistical analysis was carried out with SPSS statistical analysis software, and the LC 50 of each agent was calculated to evaluate the activity of the tested agent on the test insects, and the co-toxicity coefficient (CTC) was calculated according to Sun Yunpei.
表2 氟酰脲和氰戊菊酯室内联合毒力测定结果（48小时）Table 2 Indoor joint toxicity test results of fluorourea and fenvalerate (48 hours)
测定结果见表2，测定结果表明：氟酰脲和氰戊菊酯按有效成分重量比例40:1、1:45、1:1、8:1、16：1、1：5、1：10混合配制成二元复配剂，对菜青虫3龄幼虫的共毒系数分别为129.1、131.3、143.2、128.2、126.8、130.6、124.9，表明氟酰脲和氰戊菊酯按上述比例复配后对菜青虫均有增效作用。The test results are shown in Table 2. The test results show that: the weight ratio of fluoride and fenvalerate is 40:1, 1:45, 1:1, 8:1, 16:1, 1:5, 1:10 Mixing and preparing a binary compound, the co-toxicity coefficients to the 3rd instar larvae of Pieris rapae were 129.1, 131.3, 143.2, 128.2, 126.8, 130.6, 124.9, indicating that after compounding fluoride and fenvalerate according to the above ratio It has synergistic effect on cabbage caterpillar.
试验3Test 3
氟酰脲和醚菊酯室内联合毒力测定试验Indoor joint toxicity test of fluorourea and etofenproxil
将氟酰脲和醚菊酯按有效成分重量比例25:1、1:30、1:6、1:1、2:1、11：1等比例混合配成二元复配剂，试验方法参照《中华人民共和国农业行业标准NY/T 1154.14-2008》、《中华人民共和国农业行业标准NY/T 1154.7-2006》，采用浸叶法，以棉花棉铃虫3龄若虫为试虫，药后48小时检查死虫数，计算死亡率。空白对照等量清水。一般每个处理设置5个浓度梯度。用SPSS统计分析软件进行统计分析，计算各药剂的LC50，依此来评价供试药剂对试虫的活性，依孙云沛计算共毒系数（CTC）。Mix fluorourea and etofenproxil according to the weight ratio of active ingredients 25:1, 1:30, 1:6, 1:1, 2:1, 11:1 to form a binary compound. The test method refers to "People's Republic of China Agricultural Industry Standard NY/T 1154.14-2008", "People's Republic of China Agricultural Industry Standard NY/T 1154.7-2006", using the method of soaking leaves, using the 3rd instar nymph of cotton bollworm as the test insect, 48 hours after treatment Check the number of dead insects and calculate the mortality rate. Blank control equal volume of water. Generally, 5 concentration gradients are set for each treatment. Statistical analysis was carried out with SPSS statistical analysis software, and the LC 50 of each agent was calculated to evaluate the activity of the tested agent on the test insects, and the co-toxicity coefficient (CTC) was calculated according to Sun Yunpei.
表3 氟酰脲和醚菊酯室内联合毒力测定结果（48小时）Table 3 Indoor joint toxicity test results of fluorourea and etofenproxil (48 hours)
测定结果见表3，测定结果表明：氟酰脲和醚菊酯按有效成分重量比例25:1、1:30、1:6、1:1、2:1、11：1等比例混合配制成二元复配剂，对棉铃虫3龄幼虫的共毒系数分别为126.5、124.6、134.5、130.4、137.4、140.8、131.4、124.4，表明氟酰脲和醚菊酯按上述比例复配后对棉铃虫均有增效作用。The test results are shown in Table 3. The test results show that: fluorourea and etofenproxil are prepared by mixing the active ingredient weight ratios of 25:1, 1:30, 1:6, 1:1, 2:1, and 11:1. The co-toxicity coefficients of the binary compound to the 3rd instar larvae of cotton bollworm were 126.5, 124.6, 134.5, 130.4, 137.4, 140.8, 131.4, 124.4 respectively, indicating that fluoride and etofenprox were compounded according to the above proportions to the cotton boll Insects have a synergistic effect.
试验4Test 4
试验方法：参照≤GB／T17980.5-2004 农药田间试验准则（二）杀虫剂防治甘蔗螟虫≥ ；防治对象：甘蔗螟虫；Test method: refer to ≤GB/T17980.5-2004 Pesticide field test guidelines (2) Insecticides control sugarcane borer ≥; control object: sugarcane borer;
试验地点：广西崇左市扶绥县某甘蔗田；实施例1～实施例6和对照实施例1的施药方法：超低容量喷雾；对照药剂：10%氟酰脲EC和5%氟氯氰菊酯EC，用水稀释至30L常规喷雾。Test location: a sugarcane field in Fusui County, Chongzuo City, Guangxi; the application method of Examples 1 to 6 and Comparative Example 1: ultra-low volume spray; control agent: 10% fluoride EC and 5% cyfluthrin EC, diluted with water to 30L for regular spraying.
表4：防治甘蔗螟虫药效试验结果Table 4: Results of efficacy tests for controlling sugarcane borer
从表4中可以看出：本发明的超低容量液剂采用超低容量喷雾方法防治甘蔗螟虫比对照药剂常规喷雾速效性强、防治效果好、持效期较长。It can be seen from Table 4 that the ultra-low volume liquid agent of the present invention adopts the ultra-low volume spraying method to prevent and control sugarcane borer than the conventional spraying method of the control agent, which has stronger quick-acting effect, better control effect and longer duration.
试验5Test 5
试验方法：参照≤GB／T17980.13-2000 农药田间试验准则（一）杀虫剂防治十字花科蔬菜的鳞翅目幼虫≥ ；防治对象：菜青虫；Test method: Refer to ≤ GB/T17980.13-2000 Pesticide Field Test Guidelines (1) Insecticides control Lepidoptera larvae in cruciferous vegetables ≥; control object: cabbage caterpillar;
试验地点：广东佛山市郊；实施例7～实施例11和对照实施例1的施药方法：超低容量喷雾；对照药剂：10%氟酰脲EC和20%氰戊菊酯EC，用水稀释至30L常规喷雾。Test site: the suburbs of Foshan, Guangdong; the application method of embodiment 7 to embodiment 11 and comparative example 1: ultra-low volume spray; contrast agent: 10% fluoride EC and 20% fenvalerate EC, diluted with water to 30L regular spray.
表5：防治菜青虫药效试验结果Table 5: Results of drug efficacy test for preventing and controlling cabbage caterpillar
从表5中可以看出：本发明的超低容量液剂采用超低容量喷雾方法防治菜青虫比对照药剂常规喷雾速效性强、防治效果好、持效期较长。As can be seen from Table 5: the ultra-low volume liquid agent of the present invention adopts the ultra-low volume spraying method to prevent and control cabbage caterpillars than the conventional spraying method of the reference agent, which has stronger quick-acting effect, better control effect and longer duration.
试验6Test 6
试验方法：参照≤GB／T17980.5-2000 农药田间试验准则（一）杀虫剂防治棉铃虫≥ ；防治对象：棉花棉铃虫；Test method: Refer to ≤ GB/T17980.5-2000 Pesticide Field Test Guidelines (1) Insecticides control cotton bollworm ≥; control object: cotton bollworm;
试验地点：南昌市永修县某棉花田；实施例12～实施例17和对照实施例1的施药方法：超低容量喷雾；对照药剂：10%氟酰脲EC和20%醚菊酯EC，用水稀释至30L常规喷雾。Test location: a cotton field in Yongxiu County, Nanchang City; the application method of Examples 12 to 17 and Comparative Example 1: ultra-low volume spraying; control agents: 10% fluoride EC and 20% etofenprox EC, Dilute with water to 30L for regular spraying.
表6 防治棉花棉铃虫药效试验结果Table 6 Results of the efficacy test for controlling cotton bollworm
从表6中可以看出：本发明的超低容量液剂采用超低容量喷雾方法防治棉花棉铃虫比对照药剂常规喷雾速效性强、防治效果好、持效期较长。As can be seen from Table 6: the ultra-low volume liquid agent of the present invention adopts the ultra-low volume spraying method to prevent and control cotton bollworm than the conventional spraying of the contrast agent, which has stronger quick-acting effect, better control effect and longer duration.
其应用在防治稻飞虱、稻纵卷叶螟、褐飞虱、白背飞虱、灰飞虱、二化螟、稻蓟马、稻瘿蚊、稻叶蝉、黑尾叶蝉、稻蛛椽蝽、象星蝽象、稻绿蝽象、红须盲蝽、稻负混虫、稻筒水螟、稻蝗、 蚜虫类、粉虱类、蚧类、矢尖盾蚧、朱绿蝽、桃小食心虫、桔潜蛾、茶细蛾、黄条跳甲、豆潜蝇。 角腊蚧、小菜蛾、二黑条叶甲、茶黄蓟马、烟蓟马、黄蓟马、柑橘黄蓟马、大豆荚瘿蚊、番茄潜叶蝇等病虫害方面。It is used in the control of rice planthoppers, rice leaf rollers, brown planthoppers, white-backed planthoppers, brown planthoppers, rice stem borers, rice thrips, rice gall midges, rice leafhoppers, black-tailed leafhoppers, and rice spider gnats . Boreworm, orange miner, tea fine moth, yellow striped flea beetle, bean miner. In terms of pests and diseases, such as horned wax scale, diamondback moth, two-black-striped leaf beetle, tea yellow thrips, tobacco thrips, yellow thrips, citrus yellow thrips, soybean pod gall midge, tomato leafminer, etc.
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