CN100352348C - 烯肟菌酯与霜脲氰的杀菌组合物 - Google Patents
烯肟菌酯与霜脲氰的杀菌组合物 Download PDFInfo
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- CN100352348C CN100352348C CNB031334210A CN03133421A CN100352348C CN 100352348 C CN100352348 C CN 100352348C CN B031334210 A CNB031334210 A CN B031334210A CN 03133421 A CN03133421 A CN 03133421A CN 100352348 C CN100352348 C CN 100352348C
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- enestroburin
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- urea cyanogen
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- missible oil
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Abstract
本发明公开了一种含有烯肟菌酯与霜脲氰的杀菌组合物，两组分基于活性组分的重量份数比为1∶100至100∶1。组合物中的活性组分重量百分含量为0.5-95%。组合物中含有至少两种载体，其中至少一种是表面活性剂。该组合物可以配制成乳油、悬浮剂、(水)乳剂、可湿性粉剂、(水分散)颗粒剂等剂型，用于防治由病原真菌引起的植物病害。
Description
技术领域
本发明属于农用杀菌剂领域。
背景技术
烯肟菌酯是防治谷物、水稻、水果、蔬菜及经济作物等多种植物病害的优秀杀菌剂，其杀菌谱广、活性高、具有预防及治疗作用、且与环境生物有良好的相容性，对由鞭毛菌、结合菌、子囊菌、担子菌及半知菌引起的多种植物病害有良好的防治效果。该化合物由中国沈阳化工研究院创制、在CN1191670A中首次公开。烯肟菌酯属甲氧基丙烯酸酯类的新型杀菌剂，这一类杀菌剂活性高、用量少，具有治疗和保护作用，被广泛用于防治农作物病害。但由于这一类杀菌剂的作用位点非常单一，病菌会对药剂产生适应性的变异，使药剂的防效降低甚至无效，产生抗药性。烯肟菌酯的抗性目前在田间尚未发现，但同类品种在欧洲已有产生抗性的相关报道。
发明内容
为了避免使用烯肟菌酯单剂可能带来的抗性发生、药效下降等问题，本发明公开了一种含有烯肟菌酯和霜脲氰的杀菌组合物、组合物的制备及应用。
烯肟菌酯化学名称：3-甲氧基-2-[2-((((1-甲基-3-(4-氯苯基)-2-丙烯基叉)氨基)氧)-甲基)苯基]丙烯酸甲酯，结构式如下：,
中文通用名：烯肟菌酯
分子式： C22H22CINO
分子量： 399.87
霜脲氰(英文通用名：cymoxanil，见化工部农药信息总站出版的《国外农药品种手册》)是一种高效、低毒杀菌剂，具有局部内吸作用，广泛应用于黄瓜、葡萄、蕃茄、荔枝、巨菜等十字花科蔬菜及烟草等上霜霉目真菌，如：疫霜属、霜霉属、单轴霜属。该化合物的化学名称：1-(2-氰基-2-甲氧基亚胺基)-3-乙基脲，结构如下：
中文通用名：霜脲氰
分子式：C7H10N4O3
分子量：198.2
现已发现，本发明提出的含有烯肟菌酯与霜脲氰的杀菌组合物，具有明显的增效作用，对农作物病害的防治效果有显著提高，并且能够扩大杀菌谱、延缓病原物抗药性的产生。烯肟菌酯与霜脲氰结构类型不同、作用机制各异，二者复配可以在一定程度上延缓病原物抗药性产生和发展，同时可以降低生产成本。
本发明的杀菌组合物，含有烯肟菌酯和霜脲氰两种活性组分，烯肟菌酯和霜脲氰基于活性组分的重量份数比为1∶100至100∶1。较适合的比例为1∶20至20∶1。
本发明的杀菌组合物中活性组分为总重量的0.5％至95％。本发明的杀菌剂组合物中含有活性组分的量取决于每种组分单独使用时的施用量，也取决于一种组分与另一种组分的比例以及增效作用的程度。
本发明的杀菌组合物中含有至少两种载体。载体可以是固体或液体，通常用于配制杀菌剂组合物的载体均可使用。
本发明组合物可以配制成乳油、悬浮剂、(水)乳剂、可湿性粉剂、(水分散)颗粒剂，也可以使用包含在聚合物胶囊中的溶液和粉末，如浸渍了活性物质的天然的或合成的材料或载体。这些制剂可由通用的方法制备，例如，将活性物质与液体溶剂和/或固体载体混合，同时加入表面活性剂如乳化剂、分散剂、稳定剂、湿润剂，还可以加入粘合剂、消泡剂、氧化剂、染料。农用组合物通常配制成各种制剂，由使用者在使用前稀释或直接使用。制剂中存在少量的表面活性剂载体有利于稀释。因此，本发明的组合物中至少一种载体是表面活性剂。
本发明还包括制备上述杀菌组合物的方法。如果水用作稀释剂，有机溶剂也能用作附助溶剂或稳定剂和防冻剂。适合的有机溶剂包括芳烃、氯代芳烃、氯代脂族烃、脂族烃，特别适用的是极性溶剂，例如异丙醇、丁醇、乙二醇、丙二醇、丙三醇、山梨醇、苯甲醇、糠醇和环己醇，以及丙酮、甲乙酮、甲基异丁基酮、环己酮、丁内酯，二甲基甲酰胺、吡咯烷酮、N-甲基吡咯烷酮同时，还有植物油和甲基溶纤维。
表面活性剂可以是乳化剂、分散剂或湿润剂；可以是非离子型的或离子型的。例如，十二烷基硫酸钠、仲烷基硫酸钠、十二烷基苯磺酸钠；聚氧乙烯脂肪酸脂、聚氧乙烯脂肪醇醚、聚氧乙烯脂肪氨，或直接使用市售的乳化剂：农乳0201B、农乳0203B等。用作分散剂和润湿剂的物质有：木质素磺酸钠、拉开粉、木质素磺酸钙，以及月桂醇硫酸钠、烷基醇聚氧乙烯基醚硫酸钠、辛基酚聚氧乙烯基醚硫酸盐、烷基酚聚氧乙烯基醚甲醛缩合物硫酸盐、烷基磺酸钠、十二烷基苯磺酸钠等。
粘合剂，可以是合成的例如羰甲基纤维素、聚乙烯醇或聚乙酸乙烯酯或天然的水溶性聚合物例如黄原胶、明胶、阿拉伯树胶、聚乙烯吡咯烷酮、硅酸镁铝、聚乙烯醇、聚乙二醇、酚醛树脂、虫胶、和海藻酸钠等，以粉末、颗粒或胶乳形式加入制剂中。
消泡剂为：泡敌、硅酮类、C8～10脂肪醇、磷酸酯类、C10～20饱和脂肪酸类(如癸酸)及酰胺等。
适合的固体载体包括天然的或合成的粘土和硅酸盐，适用于粉剂的固体载体包括天然形成的岩石粉末、白垩、石英、粘土、蒙脱土、二氧化硅、硅藻土、浮石、石膏、滑石、膨润土、高岭土、陶土、白碳黑及合成的磨碎的矿物质例如微分散的硅酸或氧化铝；适合的颗粒载体包括破碎的和分级的天然岩石例如方解石、大理石、浮石、海泡石和白云石及由有机物与无机物的粉末制成的合成颗粒。
根据组合物的制剂类型，固体制剂含有按重量计5％至85％的活性物质，较佳地为10-80％；液体制剂含有按重量计1-70％活性物质；悬浮液制剂含有按重量计10-60％的活性物质。以下所有百分含量均为重量百分数。
乳油通常含有10-50％活性组分，还含有溶剂(在需要时也含有共溶剂)、2-20％乳化剂和0-20％的其它添加剂，例如稳定剂、渗透剂和腐蚀抑制剂。可湿性粉剂通常含有10-85％的活性组分，除了固体惰性载体外，通常含有3-10％的分散剂，如果需要，含有0-10％的稳定剂和/或其它添加剂，例如渗透剂或粘着剂。(水分散性)颗粒剂通常制成10-100国际标准筛目(1.676-0.152mm)颗粒，可以通过团聚或浸透方法制备。通常颗粒剂含有0.5-75％的活性组分和0-10％的添加剂，例如稳定剂、表面活性剂、缓慢释放调节剂和粘合剂。悬浮剂通常需搅拌砂磨，以获得稳定的非沉积可流动性产物，它通常含有10-75％活性组分，0.5-15％分散剂，0.1-10％的触变剂，0-10％的其它添加剂例如消泡剂、腐蚀抑制剂、稳定剂、渗透剂和粘着剂，水或有机液体，其中活性组分基本上是不溶解的。某些有机固体或无机盐可以溶解在制剂中，以有助于防止沉积作用或作为防冻剂。含水的分散液和乳化液，例如用水稀释本发明的可湿性粉剂或浓缩物得到的组合物也在本发明的范围之内。上述乳液可以是油包水型或水包油型的，可具有浓稠的浆状稠度。
本发明描述的产物可以呈成品制剂形式提供，即组合物中各物质已经混合；但组合物的成分也可以以单独制剂提供，使用前在桶(罐)中直接混合。本发明的浓缩物通常与水混合得到所需活性物质的浓度。
本发明的组合物可用于防治由病原真菌引起多种植物的病害，如谷类、小麦、水稻、葡萄、草莓、黄瓜、西葫芦、辣椒、甜椒、茄子、番茄、菜豆、豇豆、韭菜、莴苣、白菜、向日葵、荔枝、烟草、橡胶和一些花卉、中药材、草坪等。本发明的杀菌剂组合物的施用场所为农田、果园或仓库等。
本发明的组合物也可以与其它具有除草、杀虫或杀菌性能的化合物特别是保护性杀菌剂混合使用，还可以与杀线虫剂、防护剂、生长调节剂、植物营养素或土壤调节剂混合使用。
本发明还包括一种现场杀灭真菌的方法，在作物和/或果实感病之前或之后，向作物和/或果实及其生长或储存的场所施用本发明的组合物。可以按普通的方法施用，如浇注、喷射、喷雾、撒粉、散布。本发明的施用量随天气条件或作物状态变化。保护作用的持续时间通常与组合物中单个化合物的含量有关，也与外界因素相关，例如气候，但通过使用适当的剂型可以减缓气候的影响。
本发明的组合物具有四个优点：一是组合物在一定配比范围内表现出极好的增效作用，组合物的杀菌效果较其单剂有了明显提高，从而降低了使用剂量，在减少农民用药成本的同时，降低了对环境影响程度。二是扩大了杀菌谱，药剂特性也得到极强的优势互补，一种药剂能同时防治多种作物病害，提供了一种极其方便有效的防治手段。对谷物、蔬菜、水果、草坪及热带作物等多种植物由病原真菌引起的植物病害例如：霜霉病、疫病、稻瘟病、赤霉病、猝倒病、绵疫病、白锈病、黑胫病等均有良好的防治效果。三是混配可以大幅降低生产成本。四是该组合物的应用，能延缓单剂的抗性产生与发展，品种间的结构相差较大，不存在交互抗性。从而扩大了烯肟菌酯的防治对象、延长其使用周期。
具体实施方式
本发明用以下具体实例进行详细说明，以使本发明的优点更明显，但本发明绝非限于这些例子。所有制剂的配比中百分比均为重量百分比；生物活性部分的处理剂量均为有效含量。
组合物的制备与生物活性实例
1.乳油的配制
按配方要求，分别加入溶剂、原药、乳化剂，混合均匀，必要时用热水浴加热溶解，即得到透明状乳油。如实例1～3配方。
实施例1(20％乳油)
霜脲氰10％，烯肟菌酯10％，农乳500#7.5％，农乳600-2#4.5％，10％N-甲基吡咯烷酮10％，二甲苯补足至100％。
实施例2(30％乳油)
霜脲氰20％，烯肟菌酯10％，农乳500#10％，农乳OX-6355％，甲基异丁基酮10％，N-甲基吡咯烷酮10％，二甲苯补足至100％。
实施例3(40.5％乳油)
霜脲氰36％，烯肟菌酯4.5％，农乳500#13％，农乳OX-6355.5％，甲基异丁基酮10％，N-甲基吡咯烷酮10％，二甲苯补足至100％。
2.可湿性粉剂的配制
按配方要求，将原药、各种助剂及填料等充分混合，经超细粉碎机粉碎后，即得到加工产品。如实例4～7配方
实施例4(25％可湿性粉剂)
霜脲氰12.5％，烯肟菌酯12.5％，十二烷基硫酸钠1.5％，白碳黑5％，木质素磺酸钠8％，轻质碳酸钙补足至100％。
实施例5(30％可湿性粉剂)
霜脲氰20％，烯肟菌酯10％，十二烷基硫酸钠1.5％，羧甲基纤维素1％，辛基酚聚氧乙烯基醚硫酸盐10％，白碳黑5％，轻质碳酸钙补足至100％。
实施例6(45％可湿性粉剂)
霜脲氰25％，烯肟菌酯20％，十二烷基苯磺酸钠2％，白碳黑10％，萘酚磺酸甲醛缩合物钠盐10％，轻质碳酸钙补足至100％。
实施例7(52.5％可湿性粉剂)
霜脲氰50％，烯肟菌酯2.5％，十二烷基苯磺酸钠2％，白碳黑10％，萘酚磺酸甲醛缩合物钠盐10％，轻质碳酸钙补足至100％。
3.水乳剂的配制
将原药、溶剂、乳化剂加在一起，使溶解成均匀油相。将水、抗冻剂等混合一起，成为均一水相。在高速搅拌下，将水相加入到油相或将油相加入到水相，形成分散性良好的水乳剂。如实例8～10配方。
实施例8(15％水乳剂)
霜脲氰10％，烯肟菌酯5％，聚乙烯醇1.5％，失水山梨醇脂肪酸酯聚氧乙烯基醚8％，烷基-二乙二醇醚-磺酸钠2.5％，农乳2201 2％，N-甲基吡咯烷酮8％，乙二醇8％，水补足至100％。
实施例9(20％水乳剂)
霜脲氰10％，烯肟菌酯10％，聚乙烯醇0.9％，烷基芳基聚氧乙烯聚氧丙烯醚8.5％，农乳2201 15％，二甲基甲酰胺12％，乙二醇10％，水补足至100％。
实施例10(28.5％水乳剂)
霜脲氰1.5％，烯肟菌酯27％，聚乙烯醇0.9％，烷基芳基聚氧乙烯聚氧丙烯醚8.5％，农乳2201 15％，二甲基甲酰胺12％，乙二醇10％，水补足至100％。
4.水分散性颗粒剂的配制
将原药和粉状载体、润湿展着剂及粘结剂等进行混合粉碎，再加水捏合后，加入装有一定规格筛网的造粒机中进行造粒。然后再经干燥、筛分(按筛网范围)即得颗粒状产品。
如实例11～13配方。
实施例11(40％水分散性颗粒剂)
霜脲氰5％，烯肟菌酯35％，甲基萘磺酸钠甲醛缩合物10％，十二烷基苯磺酸钠12％，可溶性淀粉15％，，凹凸棒土补足至100％。
实施例12(50％水分散性颗粒剂)
霜脲氰25％，烯肟菌酯25％，亚甲基萘磺酸钠10％，十二烷基苯磺酸钠15％，聚乙烯吡咯烷酮5％，凹凸棒土补足至100％。
实施例13(60％水分散性颗粒剂)
霜脲氰35％，烯肟菌酯25％，甲基萘磺酸钠甲醛缩合物12％，十二烷基苯磺酸钠15，可溶性淀粉15％，，凹凸棒土补足至100％。
5.悬浮剂的配制
按配方要求，以水为介质，将原药、分散剂、助悬剂和防冻剂等加入砂磨釜中，进行研细，制成悬浮剂。如实例14～15配方。
实施例14(25％悬浮剂)
霜脲氰10％，烯肟菌酯15％，甲基萘磺酸钠甲醛缩合物5.5％，0203B5％，白碳黑2％，硅酸镁铝0.3％，乙二醇8％，磷酸三丁酯少许，水补足至100％。
实施例15(35％悬浮剂)
霜脲氰22.5％，烯肟菌酯12.5％，木质素磺酸钙3％，白碳黑1％，0203B 5％，0201B 2％，乙二醇8％，磷酸三丁酯少许，水补足至100％。
6.生物活性
田间药效测试分级标准执行农业部药检所《农药田间试验准则》的分级标准分级记载，以病情指数计算防治效果。
实施例16抑菌活性(马铃薯晚疫病)
在室内采用含毒介质方法，测定制剂实施例4(25％可湿性粉剂)及单剂25％烯肟菌酯乳油、50％霜脲氰可湿粉对马铃薯晚疫病的抑菌效果。试验方法：在PDA培养基(全营养)中分别加入定量药剂(另设不加药空白对照)，冷却后接种马铃薯晚疫病菌(Phytophthora infestans)，在24℃无光照条件下培养，培养120小时后进行结果调查。
测试结果如下：
实施例17抑菌活性(辣椒疫病)
在室内采用含毒介质方法，测定制剂实施例1(20％乳油)及25％烯肟菌酯乳油、50％霜脲氰可湿粉对辣椒疫病的抑菌效果。试验方法：在PDA培养基(全营养)中分别加入定量药剂(设不加药空白对照)，冷却后接种辣椒疫病菌(Phytophthora capsici)菌种，接种后在24℃无光照条件下培养，培养120小时后进行结果调查。测试结果如下：
实施例18盆栽活性(黄瓜霜霉病)
试验采取盆栽幼苗法，测定实施例9(20％水乳剂)以及25％烯肟菌酯乳油、50％霜脲氰可湿粉对黄瓜霜霉病的防治效果。试验方法：将黄瓜幼苗培养至2叶平展期，按200、100、50、25ug/ml处理剂量(另设喷清水的空白对照)在作物喷雾机上进行喷雾处理，24小时后接种黄瓜霜霉病菌(Pseudoperaospora cubensis)，接种后在人工气候箱内保湿培养，7天后进行结果调查。测试结果如下：
实施例19盆栽活性(番茄晚疫病)
试验采取盆栽幼苗法，测定实施例12(50％水分散性颗粒剂)以及25％烯肟菌酯乳油、50％霜脲氰可湿粉对番茄晚疫病的防治效果。试验方法：将番茄幼苗培养至4叶期，按200、100、50、25ug/ml处理剂量(另设喷清水的空白对照)在作物喷雾机上进行喷雾处理，24小时后接种番茄晚疫病菌(P.infestans de Bary)，接种后在人工气候箱内保湿培养，8天后进行结果调查。测试结果如下：
实施例20盆栽活性(葡萄霜霉病)
试验采取盆栽幼苗法，测定实施例14(25％悬浮剂)以及25％烯肟菌酯乳油、50％霜脲氰可湿粉对葡萄霜霉病的防治效果。试验方法：将插扦葡萄幼苗培养至3叶期，按200、100、50、25ug/ml处理剂量(另设喷清水的空白对照)在作物喷雾机上进行喷雾处理，24小时后接种葡萄霜霉病病菌(Plasmopara viticola)，接种后在人工气候箱内保湿培养，10天后进行结果调查。测试结果如下：
实施例21 田间小区防治效果(马铃薯晚疫病)
在田间测定实施例7(52.5％可湿粉)及25％烯肟菌酯乳油、50％霜脲氰可湿粉马铃薯晚疫病的防治效果。马铃薯品种：川渝218；病原菌：马铃薯晚疫病菌(P.infestansdeBary)；方法：在连年发病较重的马铃薯产区，于马铃薯晚疫病发病初期进行药剂处理。实施例7(52.5％可湿粉)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药3次，间隔7天，第3次施药后14天调查防效。测试结果如下：
实施例21 田间小区防治效果(黄瓜霜霉病)
在保护地内测定实施例13(60％水分散颗粒剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉黄瓜霜霉病的防治效果。黄瓜品种：新泰密刺；病原菌：黄瓜霜霉病菌(Pseudoperaospora cubensis)；方法：在连年发病较重的蔬菜主产区，于黄瓜霜霉病发病初期进行药剂处理。实施例13(60％水分散颗粒剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药4次，间隔7天，第4次施药后8天调查防效。测试结果如下：
实施例22 田间小区防治效果(葡萄霜霉病)
在田间测定实施例2(30％乳油)及25％烯肟菌酯乳油、50％霜脲氰可湿粉葡萄霜霉病的防治效果。黄瓜品种：巨丰；病原菌：葡萄霜霉病菌(Plasmopara viticola)；方法：在葡萄霜霉病的发病初期进行药剂处理。实施例2(30％乳油)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药3次，间隔7天，第3次施药后10天调查防效。测试结果如下：
实施例23田间小区防治效果(番茄晚疫病)
在保护地内测定实施例5(30％可湿性粉剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉番茄晚疫病的防治效果。番茄品种：毛粉402；病原菌：番茄晚疫病(Phytophthorainfestans)；于春季3月下旬，在田间初见病斑时施药；实施例5(30％可湿性粉剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药3次，间隔7天，第3次施药后8天调查防效。测试结果如下：
实施例24田间小区防治效果(辣椒疫病)
在保护地内测定实施例11(40％水分散颗粒剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉辣椒疫病的防治效果。辣椒品种：牛耳王；病原菌：辣椒疫霉(P.capsici Leonian)；于春季3月下旬，在田间初见病株时施药；实施例11(40％水分散颗粒剂)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药4次，间隔7天，第4次施药后7天调查防效。测试结果如下：
实施例25田间小区防治效果(大白菜霜霉病)
在田间条件下测定实施例3(40.5％乳油)及25％烯肟菌酯乳油、50％霜脲氰可湿粉大白菜霜霉病的防治效果。大白菜品种：中白50号；病原菌：大白菜霜霉病(Peronosporaparasitica)；于秋季9月中旬，在田间初见病株时施药；实施例3(40.5％乳油)及25％烯肟菌酯乳油、50％霜脲氰可湿粉的施药量均为每公顷(有效成分)400、200、100、50克，施药4次，间隔7天，第4次施药后7天调查防效。分级标准及防治效果计算同实施例18。测试结果如下：
Claims (7)
1、一种杀菌组合物，含有烯肟菌酯和霜脲氰，烯肟菌酯和霜脲氰基于活性组分的重量份数比为1∶100至100∶1。
2、根据权利要求1所述的杀菌组合物，其特征在于：烯肟菌酯和霜脲氰基于活性组分的重量份数比为1∶20至20∶1。
3、根据权利要求1或2所述的杀菌组合物，其特征在于：组合物中的活性组分重量百分含量为0.5-95％。
4、根据权利要求1所述的杀菌组合物，其特征在于：组合物中含有至少两种载体，其中至少一种是表面活性剂。
5、根据权利要求1所述的杀菌组合物，其特征在于：该组合物配制成乳油、悬浮剂、水乳剂、可湿性粉剂或水分散颗粒剂。
6、权利要求1所述的杀菌组合物用于防治由病原真菌引起的植物病害的用途。
7、一种杀灭真菌的方法，其特征在于：在作物和/或果实感病之前或之后，向作物和/或果实及其生长或储存的场所施用权利要求1或5所述的杀菌组合物。
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| CN1312001A (zh) * | 1995-06-16 | 2001-09-12 | 诺瓦提斯公司 | 杀微生物的组合物 |
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| CN1191670A (zh) * | 1998-02-10 | 1998-09-02 | 化工部沈阳化工研究院 | 不饱和肟醚类杀虫、杀真菌剂 |
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