CN105076138B - An insecticidal composition of chlorfenapyr and pyriproxyfen, its preparation and application - Google Patents
An insecticidal composition of chlorfenapyr and pyriproxyfen, its preparation and application Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种虫螨腈和吡丙醚的杀虫组合物及其制剂与应用,属于农药技术领域。The invention relates to an insecticidal composition of chlorfenapyr and pyriproxyfen, its formulation and application, and belongs to the technical field of pesticides.
背景技术Background technique
虫螨腈(Chlorfenapyr),化学名称为4-溴-2-(4-氯苯基)-1-乙氧基甲基-5-三氟甲基吡咯-3-腈,是美国氰胺公司于20世纪80年代后期通过对天然抗生素的化学结构改造而得以成功研制开发的一种芳基吡咯类杀虫杀螨剂,是一种昆虫体内线粒体氧化磷酸化作用的阻断剂。Chlorfenapyr (Chlorfenapyr), the chemical name is 4-bromo-2-(4-chlorophenyl)-1-ethoxymethyl-5-trifluoromethylpyrrole-3-carbonitrile, which is produced by American cyanamide company In the late 1980s, an arylpyrrole insecticide and acaricide was successfully developed by modifying the chemical structure of natural antibiotics. It is an inhibitor of mitochondrial oxidative phosphorylation in insects.
吡丙醚(Pyriproxyfen),化学名称为4-苯氧苯基(RS)-2-(2-吡啶基氧)丙基醚,是苯醚类扰乱昆虫生长的昆虫生长调节剂,属保幼激素类似物的新型杀虫剂,具有低毒、持效期长的特点,对作物安全,对鱼类低毒,对生态环境影响小。Pyriproxyfen (Pyriproxyfen), the chemical name is 4-phenoxyphenyl (RS)-2-(2-pyridyloxy) propyl ether, is an insect growth regulator that disrupts the growth of insects with phenyl ethers, and belongs to juvenile hormone A new type of insecticide similar to it has the characteristics of low toxicity and long-lasting effect, which is safe to crops, low toxicity to fish, and has little impact on the ecological environment.
农药单剂在使用时往往受防治效果、使用范围和药害等因素制约,而且随着病虫害抗药性的增强,防治效果降低。农药复配可克服原有农药单剂的使用缺陷,对于杀虫剂来说,常用的复配方式有:有机磷类与有机磷类、有机磷与拟菊酯类、有机磷与氨基甲酸酯类、有机氮与氨基甲酸酯类以及有机氮与拟菊酯类等。The use of single-dose pesticides is often restricted by factors such as control effect, application range, and phytotoxicity, and with the increase of resistance to pests and diseases, the control effect decreases. Pesticide compounding can overcome the shortcomings of the original pesticide single agent. For insecticides, the commonly used compounding methods are: organophosphorus and organophosphorus, organophosphorus and pyrethroids, organophosphorus and carbamate Classes, organic nitrogen and carbamates, organic nitrogen and pyrethroids, etc.
韭菜迟眼蕈蚊(Bradysia odoriphaga Yang et Zhang),俗称韭蛆,属双翅目,长角亚目,眼蕈蚊科,迟眼蕈蚊属,是为害我国北方特色蔬菜韭菜、大蒜、圆葱和大葱的重要地下害虫,其中以韭菜受害最为严重,是造成目前韭菜减产和农药残留超标的主要原因之一。Bradysia odoriphaga Yang et Zhang, commonly known as chive maggots, belongs to Diptera, Longocera, Oculophagoidae, and Bradysia odoriphaga. It is a characteristic vegetable in northern my country that damages leeks, garlic, and onions. Among them, leeks are the most serious pests, which is one of the main reasons for the current production reduction of leeks and excessive pesticide residues.
近年来,由于设施韭菜种植面积的增大,造成韭蛆的危害连年加重。常规杀虫剂多年连续使用导致害虫抗药性增加,防治效果不理想,有些地方的菜农为了保产违规使用高毒杀虫剂,频频引发了食品安全问题。因此,筛选高效、低毒、安全、环境友好的药剂非常必要。In recent years, due to the increase in the planting area of leeks in facilities, the harm of leek maggots has increased year after year. The continuous use of conventional insecticides for many years has led to increased resistance of pests and unsatisfactory control effects. In some places, vegetable farmers have used highly toxic insecticides in violation of regulations in order to maintain production, frequently causing food safety problems. Therefore, it is very necessary to screen high-efficiency, low-toxicity, safe and environment-friendly agents.
发明内容Contents of the invention
本发明的目的是提供一种虫螨腈和吡丙醚的杀虫组合物及其制剂与应用。本发明通过将虫螨腈和吡丙醚进行复配,制得的杀虫组合物对韭菜迟眼蕈蚊具有明显的增效作用,是一种高效、低毒、低残留的农药组合物;将该杀虫组合物制成各种剂型的杀虫剂,对韭菜迟眼蕈蚊均具有好的防治效果。The object of the present invention is to provide an insecticidal composition of chlorfenapyr and pyriproxyfen, its preparation and application. In the present invention, by compounding chlorfenapyr and pyriproxyfen, the insecticidal composition prepared has obvious synergistic effect on tardy-eyed fungi, and is a high-efficiency, low-toxicity, low-residue pesticide composition; The insecticidal composition is made into various formulations of insecticides, all of which have good control effects on tardy-eyed fungus chives.
本发明提供的一种杀虫组合物,它由质量比为(0.1~10):1的虫螨腈和吡丙醚组成。The insecticidal composition provided by the invention is composed of chlorfenapyr and pyriproxyfen in a mass ratio of (0.1-10):1.
上述的杀虫组合物中,虫螨腈的防治对象主要有小菜蛾、菜青虫、甜菜夜蛾、斜纹夜蛾、菜螟、菜蚜、斑潜蝇和蓟马等蔬菜害虫。In the above-mentioned insecticidal composition, the control objects of chlorfenapyr mainly include vegetable pests such as diamondback moth, cabbage caterpillar, beet armyworm, litura litura, cabbage borer, cabbage aphid, liriomyza and thrips.
上述的杀虫组合物中,吡丙醚的防治对象主要有同翅目(烟粉虱、温室白粉虱、桃蚜、矢尖蚧、吹棉蚧和红蜡蚧等)、缨翅目(棕榈蓟马)、鳞翅目(小菜蛾)、啮虫目(嗜卷书虱)、蜚蠊目(德国小蠊)、蚤目(跳蚤)、鞘翅目(异色瓢虫)、脉翅目(中华通草蛉)等昆虫,对粉虱、介壳虫和蜚蠊具有特效。In the above-mentioned insecticidal composition, the control objects of pyriproxyfen mainly include Homoptera (bemisia tabaci, greenhouse whitefly, green peach aphid, scorpion, cotton scale and red wax scale, etc.), Thysanoptera (palm Thrips), Lepidoptera (Plutella xylostella), Cycloptera (book lice), Blattata (German cockroach), Pleasia (fleas), Coleoptera (Heterochromatia), Neuroptera ( Chinese lacewing) and other insects have special effects on whiteflies, scale insects and cockroaches.
本发明将虫螨腈和吡丙醚按照一定比例进行复配,通过大量的生物测定筛选,发现本发明杀虫组合物对韭菜迟眼蕈蚊表现出明显的增效作用。参照孙云沛(Sun YP)法评价本发明中两种不同活性组分混合后的相互作用,其中,共毒系数大于120为增效作用,共毒系数小于80为拮抗作用,共毒系数在两者之间为相加作用。通过计算虫螨腈和吡丙醚混用后的共毒系数,评价两者混用后效果,结果显示,上述杀虫组合物中,所述虫螨腈和吡丙醚的质量比可为(0.1~10):1,具体可为(0.1~5):1、(0.1~1):1、(0.1~0.2):1、(0.2~10):1、(0.2~5):1、(0.2~1):1、(1~10):1、(1~5):1、(5~10):1、0.1:1、0.2:1、1:1、5:1或10:1,在上述质量比的范围内,均表现出增效作用。In the present invention, chlorfenapyr and pyriproxyfen are compounded according to a certain ratio, and through a large number of bioassay screenings, it is found that the insecticidal composition of the present invention exhibits obvious synergistic effect on T. tardigrades. With reference to Sun Yunpei (Sun YP) method, evaluate the interaction between two different active components in the present invention after mixing, wherein, the co-toxicity coefficient is greater than 120 for synergism, and the co-toxicity coefficient is less than 80 for antagonism, and the co-toxicity coefficient is greater than 120 for antagonism, and the co-toxicity coefficient is greater than 120 for antagonism. There is an additive effect between them. By calculating the co-toxicity coefficient of chlorfenapyr and pyriproxyfen after mixed use, the effect after the evaluation of the two mixed, the results show that in the above insecticidal composition, the mass ratio of chlorfenapyr and pyriproxyfen can be (0.1~ 10): 1, specifically (0.1~5): 1, (0.1~1): 1, (0.1~0.2): 1, (0.2~10): 1, (0.2~5): 1, (0.2 ~1):1, (1~10):1, (1~5):1, (5~10):1, 0.1:1, 0.2:1, 1:1, 5:1 or 10:1, Within the range of the above-mentioned mass ratio, all exhibit synergistic effect.
上述的杀虫组合物中,所述虫螨腈和吡丙醚的质量比优选为(0.1~0.25):1或(4~10):1,但不为0.25:1和4:1;更优选为(0.2~0.25):1或(4~5):1,但不为0.25:1和4:1;进一步优选为0.2:1或5:1。In the above insecticidal composition, the mass ratio of chlorfenapyr and pyriproxyfen is preferably (0.1-0.25):1 or (4-10):1, but not 0.25:1 and 4:1; more Preferably (0.2-0.25):1 or (4-5):1, but not 0.25:1 and 4:1; more preferably 0.2:1 or 5:1.
由于上述虫螨腈和吡丙醚按照上述比例复配后的增效作用,本发明提供的上述任意质量比的虫螨腈和吡丙醚组成的杀虫组合物在防治韭菜迟眼蕈蚊中的应用,也在本发明的保护范围内。Due to the synergistic effect of the above-mentioned chlorfenapyr and pyriproxyfen after compounding according to the above-mentioned ratio, the insecticidal composition composed of the above-mentioned chlorfenapyr and pyriproxyfen in any mass ratio provided by the present invention is effective in the prevention and treatment of tardigrade maggots. The application is also within the protection scope of the present invention.
由于原药是无法直接使用的,本发明进一步提供了一种杀虫剂,它由上述的杀虫组合物和其农药制剂上可接受的辅料制成,其中,所述杀虫组合物的质量百分含量可为2%~60%,具体可为6%~24%、6%~20%、6%~12%、12%~24%、12%~20%、20%~24%、6%、12%、20%或24%。Since the original drug cannot be used directly, the present invention further provides a kind of insecticide, which is made from the above-mentioned insecticidal composition and its acceptable auxiliary materials for pesticide preparations, wherein the quality of the insecticidal composition The percentage content can be 2% to 60%, specifically 6% to 24%, 6% to 20%, 6% to 12%, 12% to 24%, 12% to 20%, 20% to 24%, 6%, 12%, 20% or 24%.
上述的杀虫剂中,所述杀虫组合物的质量百分含量优选为10%~60%,更优选为12%~24%,进一步优选为12%~20%或20%~24%。Among the above-mentioned insecticides, the mass percentage of the insecticidal composition is preferably 10%-60%, more preferably 12%-24%, even more preferably 12%-20% or 20%-24%.
在本发明实施过程中,由于原药中有效成分的含量不可能是100%,如95%虫螨腈原药是指虫螨腈原药中虫螨腈的质量百分含量为95%,本发明杀虫组合物和杀虫剂在计算过程中,均已将其折算成有效成分的用量,即杀虫组合物和杀虫剂中原药的含量均是指其有效成分的含量。During the implementation of the present invention, since the content of active ingredients in the original drug cannot be 100%, such as 95% chlorfenapyr original drug means that the mass percentage of chlorfenapyr in the original drug is 95%. In the calculation process of the inventive insecticidal composition and insecticide, it has been converted into the amount of active ingredients, that is, the content of the original drug in the insecticidal composition and insecticide refers to the content of the active ingredients.
上述杀虫剂中,所述杀虫剂可采用目前任意已知的方法加工制成合适剂型的制剂,合适的剂型包括但不限于:悬浮剂、悬浮种衣剂、悬乳剂、乳油、水乳剂、微乳剂、水分散粒剂、可湿性粉剂、颗粒剂、浇泼剂、滴剂、微囊悬浮剂、微囊悬浮-悬浮剂等,优选悬浮剂剂型;常用助剂是润湿剂、分散剂、溶剂、隔离剂、稳定剂、防冻剂、防腐剂、填料、粘合剂等中的一种或几种,均为已知物质,是农药助剂中的常用助剂,可以根据剂型情况有所变化。Among the above-mentioned insecticides, the insecticides can be processed into preparations in suitable dosage forms by any currently known method, and suitable dosage forms include but are not limited to: suspensions, suspension seed coatings, suspoemulsions, emulsifiable concentrates, emulsions in water , microemulsion, water dispersible granule, wettable powder, granule, pouring agent, drop, microcapsule suspension, microcapsule suspension-suspension agent, etc., preferably suspension formulation; commonly used additives are wetting agent, dispersing One or several of the agents, solvents, release agents, stabilizers, antifreeze agents, preservatives, fillers, adhesives, etc., are known substances, and are commonly used auxiliaries in pesticide adjuvants. Something has changed.
上述杀虫剂在防治韭菜迟眼蕈蚊中的应用,也在本发明的保护范围内,施药结果表明,在施药后21天和35天,与单剂相比,本发明杀虫剂对韭菜迟眼蕈蚊具有明显的防治效果;所述杀虫剂中的总有效成分(杀虫组合物)的施用量为200~600g/hm2,具体可为200~400g/hm2、400~600g/hm2、200g/hm2、400g/hm2或600g/hm2,优选为400~600g/hm2,更优选为600g/hm2。The application of the above-mentioned insecticides in the prevention and treatment of the tardigrade leek is also within the protection scope of the present invention, and the application results show that after 21 days and 35 days of application, compared with a single dose, the insecticides of the present invention It has obvious control effect on tardigrades of chives; the application rate of the total active ingredients (insecticidal composition) in the insecticide is 200-600 g/hm 2 , specifically 200-400 g/hm 2 , 400 g/hm 2 ~600 g/hm 2 , 200 g/hm 2 , 400 g/hm 2 or 600 g/hm 2 , preferably 400 to 600 g/hm 2 , more preferably 600 g/hm 2 .
本发明具有如下有益效果:The present invention has following beneficial effect:
(1)本发明将虫螨腈和吡丙醚按照一定比例混配后,对韭菜迟眼蕈蚊具有明显的增效作用。(1) In the present invention, after mixing chlorfenapyr and pyriproxyfen according to a certain ratio, it has obvious synergistic effect on T. tardigrades.
(2)由于虫螨腈和吡丙醚两种药剂作用机理互不相同,组合物的应用有助于延缓害虫抗药性的发展,延长药剂的使用寿命。(2) Since the action mechanisms of chlorfenapyr and pyriproxyfen are different from each other, the application of the composition helps to delay the development of pest resistance and prolong the service life of the agents.
(3)将虫螨腈和吡丙醚混配后的杀虫组合物制成的农药制剂,对韭菜迟眼蕈蚊均具有较好的防治效果。(3) The pesticide preparation made from the insecticidal composition mixed with chlorfenapyr and pyriproxyfen has good control effect on tardy-eyed fungus.
具体实施方式detailed description
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。The experimental methods used in the following examples are conventional methods unless otherwise specified.
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。The materials and reagents used in the following examples can be obtained from commercial sources unless otherwise specified.
不同农药品种混配后,通常表现出三种作用类型,即相加作用、增效作用和拮抗作用,但具体为何种作用,只有通过大量试验才能知道。良好的复配增效配方,能明显提高实际防治效果,扩大药剂杀虫谱,并有助于延缓害虫抗药性的产生速度。After different pesticides are mixed, they usually show three types of effects, namely additive effect, synergistic effect and antagonistic effect, but the specific effect can only be known through a large number of experiments. A good compound and synergistic formula can significantly improve the actual control effect, expand the insecticidal spectrum of the pesticide, and help to delay the generation of pest resistance.
下述实施例1中,通过大量的筛选试验,按照不同配比对虫螨腈和吡丙醚进行复配,发现虫螨腈与吡丙醚复配对韭菜迟眼蕈蚊具有显著的协同增效作用。In the following example 1, through a large number of screening tests, chlorfenapyr and pyriproxyfen were compounded according to different ratios, and it was found that the compounding of chlorfenapyr and pyriproxyfen had a significant synergistic effect on the tardigrade leek. effect.
实施例1、杀虫组合物及其复配效果Embodiment 1, insecticidal composition and compound effect thereof
本实施例中,将虫螨腈和吡丙醚分别按照质量比为10:1、5:1、1:1、1:5或1:10的比例进行复配,并分别测试对韭菜迟眼蕈蚊二龄和四龄幼虫的联合毒力。In this example, chlorfenapyr and pyriproxyfen were compounded according to the mass ratio of 10:1, 5:1, 1:1, 1:5 or 1:10, respectively, and the effects on chives and tardigrade were tested respectively. Combined virulence of the second and fourth instar larvae of the fungus mosquito.
试验对象:韭菜迟眼蕈蚊二龄和四龄幼虫。Test object: the second and fourth instar larvae of T. chinensis.
试验药剂:95%虫螨腈原药和97%吡丙醚原药。将原药(折百后)按常规方法配制成需要的试验药剂。Test agents: 95% chlorfenapyr and 97% pyriproxyfen. The original drug (after 100% discount) is prepared into the required test drug according to the conventional method.
实验方法:采用胃毒触杀联合毒力法进行室内生物测定,分别选择室内饲养的韭菜迟眼蕈蚊二龄幼虫和四龄幼虫为目标害虫,每浓度处理25头幼虫,每处理重复4次,放置于25±1℃恒温培养箱内饲养观察,并将存活幼虫一直饲养至化蛹羽化,记录最终正常羽化成虫数。采用机率分析法和DPSv7.5软件处理数据,计算致死中浓度LC50,用LC50值按孙云沛法计算共毒系数,计算公式如式(1)所示。Experimental method: Indoor bioassay was carried out by stomach poison contact combined with toxicity method, and the second and fourth instar larvae of T. tardiformis were selected as the target pests respectively, and 25 larvae were treated at each concentration, and each treatment was repeated 4 times. Place them in a constant temperature incubator at 25±1°C for observation, and keep the surviving larvae until they pupate and emerge, and record the final number of adults that emerge normally. The probability analysis method and DPSv7.5 software were used to process the data, and the lethal intermediate concentration LC 50 was calculated, and the co-toxicity coefficient was calculated according to Sun Yunpei's method with the LC 50 value, and the calculation formula was shown in formula (1).
式(1) Formula 1)
设混合药剂为M,组成的各单剂为A、B、C…。LC50A为药剂A的致死中浓度;LC50B为药剂B的致死中浓度,LC 50混为药剂A+药剂B+药剂C+…的混剂的致死中浓度,混剂共毒系数为CTC,有效成分的百分含量为P。Let the mixed medicine be M, and the individual medicines be A, B, C.... LC 50A is the lethal intermediate concentration of agent A; LC 50B is the lethal intermediate concentration of agent B; LC 50 is the lethal intermediate concentration of the mixture of agent A+agent B+agent C+..., the co-toxicity coefficient of the mixture is CTC, the active ingredient The percentage content is P.
共毒系数(CTC)≥120表现为增效作用,CTC≤80表现为拮抗作用,80<CTC<120表现为相加作用。A co-toxicity coefficient (CTC) ≥ 120 represents a synergistic effect, a CTC ≤ 80 represents an antagonistic effect, and 80 < CTC < 120 represents an additive effect.
本发明杀虫组合物对韭菜迟眼蕈蚊二龄和四龄幼虫的联合毒力测试结果如表1所示。Table 1 shows the results of the joint toxicity test of the insecticidal composition of the present invention to the second and fourth instar larvae of T. chinensis.
表1、虫螨腈与吡丙醚混用对韭菜迟眼蕈蚊二龄和四龄幼虫的联合毒力Table 1. The combined toxicity of chlorfenapyr and pyriproxyfen to the second and fourth instar larvae of T.
由表1可以看出,本发明杀虫组合物中,虫螨腈与吡丙醚质量比为10:1、5:1、1:1、1:5和1:10时,均表现出增效作用,其中5:1、1:1和1:5的共毒系数较大,当比例为5:1时,共毒系数最高,即增效作用最明显。It can be seen from Table 1 that in the insecticidal composition of the present invention, when the mass ratio of chlorfenapyr to pyriproxyfen is 10:1, 5:1, 1:1, 1:5 and 1:10, all of them show an increase. In terms of efficacy, the co-toxicity coefficients of 5:1, 1:1 and 1:5 are relatively large. When the ratio is 5:1, the co-toxicity coefficient is the highest, that is, the synergistic effect is the most obvious.
下述实施例2-实施例7分别为将本发明杀虫组合物制成的各种制剂,可以用已知的方法制备成适合农业使用的任意一种剂型,比较好的剂型为悬浮剂、悬浮种衣剂、悬乳剂、乳油、水乳剂、微乳剂、水分散粒剂、可湿性粉剂、颗粒剂、浇泼剂、滴剂、微囊悬浮剂、微囊悬浮-悬浮剂。Following embodiment 2-embodiment 7 is the various preparations that insecticidal composition of the present invention is made respectively, can be prepared into any dosage form suitable for agricultural use by known method, and better dosage form is suspension concentrate, Suspension seed coating, suspoemulsion, emulsifiable concentrate, water emulsion, microemulsion, water dispersible granule, wettable powder, granule, pouring agent, drop, microcapsule suspension, microcapsule suspension-suspension concentrate.
为了更明确本发明的目的、技术方案及优点,本发明用以下具体实施例进行说明,但其活性成分及其配比、助剂等都不仅限于以下实施例。In order to clarify the purpose, technical solutions and advantages of the present invention, the present invention is illustrated with the following specific examples, but the active ingredients, their proportions, and auxiliary agents are not limited to the following examples.
实施例2、10%虫螨腈+2%吡丙醚悬浮剂Example 2, 10% chlorfenapyr + 2% pyriproxyfen suspending agent
一、配方1. Formula
以质量百分含量计,本实施例悬浮剂由下述组分组成:In terms of mass percentage, the suspending agent of this embodiment consists of the following components:
二、制备方法2. Preparation method
按照如下步骤制备悬浮剂:Prepare the suspension as follows:
将活性组分、分散剂、润湿剂和水等各组分按照配方的比例混合,经10000r/min高速剪切5分钟均匀,加入砂磨机研磨到所要求的粒径(平均粒径小于3微米),制成10%虫螨腈+2%吡丙醚悬浮剂。Mix active components, dispersant, wetting agent, water and other components according to the ratio of the formula, shear at 10000r/min for 5 minutes to be uniform, add sand mill to grind to the required particle size (average particle size is less than 3 microns), made into 10% chlorfenapyr + 2% pyriproxyfen suspension concentrate.
实施例3、10%虫螨腈+10%吡丙醚悬浮剂Example 3, 10% chlorfenapyr + 10% pyriproxyfen suspending agent
一、配方1. Formula
以质量百分含量计,本实施例悬浮剂由下述组分组成:In terms of mass percentage, the suspending agent of this embodiment consists of the following components:
二、制备方法2. Preparation method
按照如下步骤制备悬浮剂:Prepare the suspension as follows:
将活性组分、分散剂、润湿剂和水等各组分按照配方的比例混合,经10000r/min高速剪切5分钟均匀,加入砂磨机研磨到所要求的粒径(平均粒径小于3微米),制成10%虫螨腈+10%吡丙醚悬浮剂。Mix active components, dispersant, wetting agent, water and other components according to the ratio of the formula, shear at 10000r/min for 5 minutes to be uniform, add sand mill to grind to the required particle size (average particle size is less than 3 microns), made into 10% chlorfenapyr + 10% pyriproxyfen suspension concentrate.
实施例4、2%虫螨腈+10%吡丙醚悬浮剂Example 4, 2% chlorfenapyr + 10% pyriproxyfen suspending agent
一、配方1. Formula
以质量百分含量计,本实施例悬浮剂由下述组分组成:In terms of mass percentage, the suspending agent of this embodiment consists of the following components:
二、制备方法2. Preparation method
按照如下步骤制备悬浮剂:Prepare the suspension as follows:
将活性组分、分散剂、润湿剂和水等各组分按照配方的比例混合,经10000r/min高速剪切5分钟均匀,加入砂磨机研磨到所要求的粒径(平均粒径小于3微米),制成2%虫螨腈+10%吡丙醚悬浮剂。Mix active components, dispersant, wetting agent, water and other components according to the ratio of the formula, shear at 10000r/min for 5 minutes to be uniform, add sand mill to grind to the required particle size (average particle size is less than 3 microns), made into 2% chlorfenapyr + 10% pyriproxyfen suspension concentrate.
实施例5、5%虫螨腈+1%吡丙醚颗粒剂Example 5, 5% chlorfenapyr + 1% pyriproxyfen granules
一、配方1. Formula
以质量百分含量计,本实施例颗粒剂由下述组分组成:In terms of mass percentage, the granules of this embodiment consist of the following components:
二、制备方法2. Preparation method
按照如下步骤制备颗粒剂:Prepare granules as follows:
将上述组分混合均匀,制成软材,将制好的软材,经过挤压造粒机造粒,烘干,即制成5%虫螨腈+1%吡丙醚颗粒剂。Mix the above components evenly to make a soft material. The prepared soft material is granulated by an extrusion granulator and dried to make 5% chlorfenapyr + 1% pyriproxyfen granules.
实施例6、10%虫螨腈+2%吡丙醚可湿性粉剂Example 6, 10% chlorfenapyr + 2% pyriproxyfen wettable powder
一、配方1. Formula
以质量百分含量计,本实施例可湿性粉剂由下述组分组成:In terms of mass percentage, the wettable powder of this embodiment consists of the following components:
二、制备方法2. Preparation method
按照如下步骤制备可湿性粉剂:Prepare wettable powder according to the following steps:
将上述组分混合均匀,经过气流粉碎,再充分混匀,即制成10%虫螨腈+2%吡丙醚可湿性粉剂。The above-mentioned components are mixed uniformly, crushed by airflow, and then fully mixed to prepare 10% chlorfenapyr + 2% pyriproxyfen wettable powder.
实施例7、10%虫螨腈+2%吡丙醚微囊悬浮-悬浮剂Example 7, 10% chlorfenapyr + 2% pyriproxyfen microcapsule suspension-suspension agent
本实施例按照以下方法制备微囊悬浮悬浮剂,具体步骤如下:The present embodiment prepares the microcapsule suspension according to the following method, and the specific steps are as follows:
将4.12g 97%吡丙醚原药加入10g二甲苯中充分溶解,再加入3g异氰酸酯和1.5gPEG 600,充分搅匀,作为油相;0.2g三苯乙烯基酚聚氧乙烯醚、3g木质素磺酸钙和0.1g聚乙烯醇与53.54g水均匀混合作为水相;油相与水相混合,并用高速均质机剪切乳化,得到稳定的O/W乳状液;将O/W乳状液转移到烧瓶中,以200转/分钟的速度搅拌,升温到65℃,反应4小时,用柠檬酸调节pH值6-6.5;加入2g乙二醇,0.14g黄原胶搅拌均匀,水补足100g,即得到4%吡丙醚微胶囊悬浮剂。Add 4.12g of 97% pyriproxyfen technical substance into 10g of xylene to fully dissolve, then add 3g of isocyanate and 1.5g of PEG 600, stir well, and use it as the oil phase; 0.2g of tristyrylphenol polyoxyethylene ether, 3g of lignin Calcium sulfonate and 0.1g polyvinyl alcohol are uniformly mixed with 53.54g water as the water phase; the oil phase is mixed with the water phase, and sheared and emulsified with a high-speed homogenizer to obtain a stable O/W emulsion; the O/W emulsion Transfer to a flask, stir at a speed of 200 rpm, heat up to 65°C, react for 4 hours, adjust the pH value to 6-6.5 with citric acid; add 2g of ethylene glycol, 0.14g of xanthan gum, stir well, and make up 100g of water , to obtain 4% pyriproxyfen microcapsule suspension.
称取21.05g 95%虫螨腈原药,5g苯乙烯苯酚甲醛树脂聚氧乙烯聚氧丙烯醚,3g木质素磺酸钙,1.5g壬基酚聚氧乙烯醚,0.12g黄原胶,3g乙二醇,有机硅消泡剂0.5g,水补足100g。按照上述配方称取各组分并置于烧杯内,开启高速剪切机5分钟,然后砂磨机1500转/分钟研磨,检测样品粒径95%以上在1-5微米,平均粒径在3微米以下,得到20%虫螨腈悬浮剂。Weigh 21.05g 95% chlorfenapyr technical, 5g styrene phenol formaldehyde resin polyoxyethylene polyoxypropylene ether, 3g calcium lignosulfonate, 1.5g nonylphenol polyoxyethylene ether, 0.12g xanthan gum, 3g Ethylene glycol, 0.5g of silicone defoamer, and 100g of water. Weigh each component according to the above formula and place it in a beaker, turn on the high-speed shearing machine for 5 minutes, and then grind it with a sand mill at 1500 rpm. More than 95% of the sample particle size is 1-5 microns, and the average particle size is 3 Micron below, get 20% chlorfenapyr suspension concentrate.
将4%吡丙醚微囊悬浮剂与20%虫螨腈悬浮剂按照重量比1:1混合均匀即得到,2%吡丙醚+10%虫螨腈微囊悬浮-悬浮剂。Mix 4% pyriproxyfen microcapsule suspension concentrate and 20% chlorfenapyr suspension concentrate at a weight ratio of 1:1 to obtain 2% pyriproxyfen + 10% chlorfenapyr microcapsule suspension-suspension concentrate.
实施例8、田间药效试验Embodiment 8, field efficacy test
对实施例2-实施例7制得的各种剂型的制剂进行防治韭菜迟眼蕈蚊田间药效试验,考察其实际应用效果。The preparations of various dosage forms prepared in Examples 2-Example 7 were subjected to a field efficacy test for preventing and controlling T. tardigrades of Chinese chives, and their practical application effects were investigated.
1)施药方法1) Application method
采用灌根施药技术,将制剂初步稀释后随水均匀冲施。操作方法如下:在韭菜迟眼蕈蚊发生期将该组合物的悬浮剂、可湿性粉剂等剂型加水配成悬浮液随水冲施灌根,或喷淋在韭菜根部后浇水使用;该组合物的颗粒剂可加细沙混匀后撒施到韭菜根部后浇水使用。Using root irrigation application technology, the preparation is initially diluted and applied evenly with water. The operation method is as follows: add water to the suspending agent, wettable powder and other dosage forms of the composition during the occurrence period of the tardigrade leek, and make a suspension with water to rinse the roots, or spray it on the roots of the leek and then water it for use; the combination The granules can be mixed with fine sand, sprinkled on the roots of leeks, and then watered.
2)小区面积和重复(韭菜)2) Cell area and repetition (leek)
小区面积:30m2。Residential area: 30m 2 .
重复次数:重复4次。Number of repetitions: Repeat 4 times.
3)调查方法3) Survey method
受害株率调查:每小区“Z”字形五点取样,每点取1m行长的韭菜,统计受害株数。Survey on the rate of damaged plants: Sampling at five "Z"-shaped points in each plot, and taking leeks with a row length of 1m at each point, and counting the number of damaged plants.
4)调查时间和次数:4) Investigation time and frequency:
于施药21d和35d后调查防治效果,共调查2次。The control effect was investigated 21 days and 35 days after spraying, and the investigation was conducted twice.
5)计算方法:5) Calculation method:
计算各处理的虫口减退率和校正防效。计算公式如下:Calculate the population reduction rate and corrected control effect of each treatment. Calculated as follows:
虫口减退率(%)=(防治前虫口数-防治后虫口数)/防治前虫口数×100(2)Decrease rate of insect population (%)=(number of insect population before control-number of insect population after control)/number of insect population before control×100(2)
校正防效(%)=(药剂处理区虫口减退率-对照区虫口减退率)/(1-对照区虫口减退率)×100(3)Corrected control effect (%)=(the insect population reduction rate in the chemical treatment area-the insect population reduction rate in the control area)/(1-the insect population reduction rate in the control area)×100(3)
实验结果如表2所示。The experimental results are shown in Table 2.
表2虫螨腈与吡丙醚混配防治韭菜迟眼蕈蚊田间药效试验结果统计Table 2 Statistical results of the field efficacy test of the mixture of chlorfenapyr and pyriproxyfen in the control of tardigrade gnats
表2结果表明,当农药剂型都为悬浮剂时,实施例2(虫螨腈:吡丙醚=5:1)、实施例3(虫螨腈:吡丙醚=1:1)和实施例4(虫螨腈:吡丙醚=1:5)对韭菜迟眼蕈蚊的防效均高于两种药剂单独使用时的防效,其中,实施例2(虫螨腈:吡丙醚=5:1)的效果十分明显,与该比例下的杀虫组合物具有最优的增效作用的结果是一致的。当虫螨腈和吡丙醚的比例均为5:1,但剂型不同时,从结果可以看出:其中悬浮剂的防效最好,其次为微囊悬浮悬浮剂和可湿性粉剂,颗粒剂的防效较差。The results in Table 2 show that when the pesticide dosage forms are all suspension concentrates, Example 2 (chlorfenapyr: pyriproxyfen = 5: 1), Example 3 (chlorfenapyr: pyriproxyfen = 1: 1) and Example 4 (chlorfenapyr: pyriproxyfen = 1:5) has higher control effects on Chive tardigrades than the two agents alone, wherein, in Example 2 (chlorfenapyr: pyriproxyfen = The effect of 5:1) is very obvious, which is consistent with the result that the insecticidal composition under this ratio has the best synergistic effect. When the ratio of chlorfenapyr and pyriproxyfen is both 5:1, but the formulations are different, it can be seen from the results that the suspension agent has the best control effect, followed by microcapsule suspension concentrate, wettable powder, and granule The prevention effect is poor.
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