CN105794797A - 一种含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物 - Google Patents
一种含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物 Download PDFInfo
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- CN105794797A CN105794797A CN201610332952.2A CN201610332952A CN105794797A CN 105794797 A CN105794797 A CN 105794797A CN 201610332952 A CN201610332952 A CN 201610332952A CN 105794797 A CN105794797 A CN 105794797A
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- Prior art keywords
- flumorph
- prothioconazoles
- pyrrole metsulfovax
- bactericidal composition
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/84—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms six-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,4
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明的目的是一种杀菌组合物,它含有氟吗啉、丙硫菌唑和吡噻菌胺,其中氟吗啉、丙硫菌唑和吡噻菌胺的重量比为10‑50:1‑20:20‑60。本发明所涉及的三种化合物结构,经试验证明,相互混配不会产生抵触,可协同增效,减少用药量,降低成本。而且氟吗啉、丙硫菌唑和吡噻菌胺的复配尚未有报道。
Description
技术领域
本发明属于农药复配领域,涉及一种杀菌组合物,尤其是一种以氟吗啉、丙硫菌唑和吡噻菌胺为主要活性组分的杀菌组合物及其该杀菌组合物在农业生产中的应用。
背景技术
氟吗啉属吗啉类农用杀菌剂。对霜霉属、疫霉素病菌特别有效。对葡萄、马铃薯和番茄上的卵菌纲,尤其是霜霉科和疫霉属菌有杀菌效力,可与触杀性杀菌剂(二噻农、代森锰锌或铜化合物)混用。
丙硫菌唑是拜耳公司研制的一种新型广谱***硫酮类杀菌剂,主要用于防治谷类、麦类豆类作物等众多病害,丙硫菌唑毒性低,无致畸,致突变型,对胚胎无毒性,对人和环境安全。其作用机理是抑制真菌中甾醇的前体---羊毛甾醇或2,4-亚甲基二氢羊毛甾14位上的脱甲基化作用。丙硫菌唑的作用机理是抑制真菌中甾醇的前体一一羊毛甾醇或24-亚甲基二氢芈毛醉l4位上的脱甲基化作用,即脱甲基化抑制剂(DMIs)。不仅具有很好的内吸活性,优异的保护、治疗和铲除活性,且持效期长。通过大量的田间药效试验,结果表明丙硫菌唑对作物不仅具有良好的安全性,防病治病效果好,而且增产明显,同***类杀茵剂相比,丙硫菌唑具有更广谱的杀菌活住。
吡噻菌胺为日本三井化学公司研发的新颖酰胺类杀菌剂,其与现有的羧酰胺类杀菌剂有不同的杀菌谱。除了与现有羧酰胺类杀菌剂一样对担子菌有效外,其对子囊菌、不完全菌亦有效,现被推荐用于防治对其他杀菌剂具抗性的灰霉病和白粉病。
目前以上三种原药都有和其他化合物复配使用,但没有人或企业将以上三种化学物质混合使用。
发明内容
在试验过程中,研发人员惊喜的发现,氟吗啉、丙硫菌唑和吡噻菌胺按一定比例混配有很强的增效作用,又针对吡噻菌胺抗性增加等问题,故提出本发明,目的是提供一个适用范围广、成本低、效果好的含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物。本发明还有一个目的是提供该杀菌组合物的用途。
本发明的措施是通过下列措施来实现的。
一种杀菌组合物,它含有氟吗啉、丙硫菌唑和吡噻菌胺,其中氟吗啉、丙硫菌唑和吡噻菌胺的重量比为10-50:1-20:20-60。
所述的杀菌组合物,其中氟吗啉、丙硫菌唑和吡噻菌胺的较优重量比为20:5:50。
所述的杀菌组合物,其中氟吗啉、丙硫菌唑和吡噻菌胺的累积重量占制剂总量的百分比为15~50%。
氟吗啉、丙硫菌唑和吡噻菌胺组合物的制剂中含有1-5重量份的沉香香料。
氟吗啉、丙硫菌唑和吡噻菌胺组合物的制剂中含有1-3重量份的香附子提取物。
所述的杀菌组合物,氟吗啉、丙硫菌唑和吡噻菌胺与助剂、载体等加工成农药上允许的任意一种剂型。
所述的杀菌组合物,其特征在于可加工成的剂型是水乳剂、悬浮剂、微胶囊剂、可湿性粉剂、水分散粒剂。
所述的杀菌组合物在防治禾谷类和果树、瓜类、蔬菜等的多种病害方面的应用。
本发明的具体实施方案如下:
本发明的技术方案之一,所述的杀菌组合物为水乳剂,组分的重量份数为:
该水乳剂的具体生产步骤为:
首先将原药氟吗啉、丙硫菌唑和吡噻菌胺、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。即制得含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物的水乳剂。
本发明的技术方案之二,所述的杀菌组合物为悬浮剂,组分的重量份数为:
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,加入氟吗啉、丙硫菌唑和吡噻菌胺,在磨球机中磨球2~3小时,使粒直径均在5mm以下,制得本发明所述的含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物的悬浮剂制剂。
本发明的技术方案之三,所述的杀菌组合物为微胶囊剂,组分的重量百分比为:
在装有搅拌装置的三口烧瓶中加入尿素和甲醛(物质的量比约为l:1.5-2.0),用氢氧化钠溶液调节溶液的pH值到8-9左右,然后升温至70-80℃,反应得到稳定的脲醛树脂预聚体。取一定量的氟吗啉、丙硫菌唑与吡噻菌胺的原药溶于环己烷中,并在溶液中加入乳化分散剂,伴随剧烈搅拌,配成以含乳化分散剂的水溶液为水相的O/W型稳定乳液。将上述的脲醛树脂预聚体加入乳液中,调节pH值,在酸催化条件下发生聚合反应,使油相物质被包裹起来,形成微胶囊颗粒。缓慢升温,固化,温度控制在40-50℃,固化时间1h。选择加入适量的助剂,即可得稳定的微囊悬浮剂。
本发明的技术方案之四,所述的杀菌组合物为可湿性粉剂,组分的重量百分比为:
该杀菌组合物可湿性粉剂具体加工步骤为:按上述配方将氟吗啉、丙硫菌唑和吡噻菌胺以及分散剂、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。
本发明的技术方案之五,所述的杀菌组合物为水分散粒剂,组分的重量百分比为:
该杀菌组合物水分散粒剂具体加工步骤为:按上述配方将氟吗啉、丙硫菌唑、吡噻菌胺和分散剂、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,制得本发明所述的含有氟吗啉、丙硫菌唑和吡噻菌胺的杀菌组合物的水分散粒剂。
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任一种或一种以上以任意比例组成的混合物。
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、水等溶剂中的任一种或一种以上以任意比例组成的混合溶剂。
所述增效剂是指具有增强药剂渗透力,润湿扩展能力,击倒害虫速度,提高农药的耐雨水冲刷力,从而提高农药杀虫、杀菌效果的一类安全、环保、无毒、无残留的新型助剂,可选自有机硅农药增效剂ZC-650或有机硅农药渗透剂扩展剂Agrowet810c、农用有机硅农药增效剂Silwet408、氮酮中的任一种。
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一种或多种。
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BX.、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、无患子粉中的一种或多种。
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、碳酸氢钠中的一种或多种。
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、聚乙烯醇中的一种或多种。
所述的稳定剂选自:柠檬酸钠、间苯二酚中的一种。
所述的抗冻剂选自:乙二醇、丙二醇、丙三醇中的一种或多种。
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一种或多种。
所述的乳化分散剂包括:润湿剂、分散剂、稳定剂、增稠剂、消泡剂和防冻剂等。
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、轻质碳酸钙中的一种或多种。
本发明的有益效果是:
1、本发明所涉及的三种化合物结构,经试验证明,相互混配不会产生抵触,可协同增效,减少用药量,降低成本。而且氟吗啉、丙硫菌唑和吡噻菌胺的复配尚未有报道。
2、对已产生抗性的病原菌仍有很高的药效,可延缓抗药性的产生。
3、降低了农药使用量,增强了对环境的友好性。
4、降低了农药使用量,也降低了用药成本,增强了该配方的市场竞争力。
5、增加了助剂沉香香料,可以明显提高杀菌效果,而且关于沉香用于农作物提高杀菌效果方面从未有过任何报道。
具体实施方式
氟吗啉、丙硫菌唑与吡噻菌胺的复配
1材料与方法
1.1试验材料
1.1.1供试药剂
95%吡噻菌胺原药;96%氟吗啉;80%丙硫菌唑原药。
1.1.2供试病原菌
荔枝褐斑病菌,分离于东莞市大朗镇的病叶标本,采用组织分离法对病原菌分离纯化,并在室内用健康荔枝叶片回接确定病原物,在PDA斜面培养基上于4℃冰箱中培养保存。
1.2试验方法及增效作用测定
1.2.1单剂毒力测定
药液配制:
95%吡噻菌胺原药用二甲基甲酰胺(DMF)为溶剂溶解,96%氟吗啉、丙硫菌唑用丙酮,分别配成10000μg/ml母液,再用0.1%吐温水溶液的吐温水溶液将母液稀释成5-6个浓度梯度。
首先是菌种及菌柄的准备:无菌操作下,将荔枝褐斑病菌接种在PDA培养基上,在25℃,RH80%的恒温培养箱中培养5天后,用灭菌的直径为0.5cm的打孔器在菌落边缘打取菌饼数枚,备用。
其次是含毒培养基的制备:无菌操作下,用移液枪从低浓度到高浓度依次准确量取配置好的药液加入已融化并冷却至45℃左右的培养基里,混合均匀后倒入已灭菌的直径为9cm的培养皿内冷凝,每个处理重复三次,以不含药剂为对照,最终制成含不同浓度药液的含毒平板。
最后是药液处理:无菌操作下,将菌柄移至含毒平板中央,正面朝下,置于25℃培养箱中培养6d,当对照菌株菌落直径长到6.5cm以上时,采用“十字交叉法”测量。根据抑制率的机率值和药剂系列浓度的对数值之间的线性回归分析,求出两种单剂抑制菌丝生长的EC50值、相关系数以及毒力回归方程。
在预备试验的基础上,用以上方法分别对单剂吡噻菌胺和氟吗啉、丙硫菌唑进行毒力测定,二者EC50值分别为0.98㎎/l和4.62㎎/l。
1.2.2混配组合设置
30%吡噻菌胺·氟吗啉、丙硫菌唑水分散粒剂质量比分别为5%+25%、7.5%+22.5%、15%+15%、22.5%+7.5%和25%+5%共5个混配组合。
1.2.3混剂毒力测定
用单剂毒力测定方法按照混配比例进行混剂的毒力测定。
按照孙云沛法将测定的各处理的EC50值换算成实际混用毒力指数(ATI);根据混剂的配比,获得理论混用毒力指数(TTI),按下列公式计算混剂的共毒系数(CTC)。
单剂毒力指数=(标准药剂EC50/供试药剂EC50)×100
ATI=(标准药剂EC50/供试药剂(混用)EC50)×100
TI I=A的毒力指数*A在混用中的含量(%)+B的毒力指数*B在混用中的含量(%)
CTC=(ATI/TTI)×100
若共毒系数大120,表明有增效作用;若明显低于100(80以下),表明为拮抗作用;100-120之间,表明为相加作用,数据见表1。
表1不同配比吡噻菌胺·氟吗啉、丙硫菌唑混剂对荔枝白星病菌的毒力
表2不同配比吡噻菌胺·氟吗啉、丙硫菌唑复配对荔枝白星病菌的联合毒力
2结果与分析
根据杀菌剂联合毒力测定结果,吡噻菌胺·氟吗啉、丙硫菌唑质量比为5:1:5时共毒系数为136.1,表现为增效作用,质量比为5:1:10时共毒系数为158.4,表现为明显增效作用,其余表现为相加作用,所以认为吡噻菌胺和氟吗啉、丙硫菌唑的最佳配比为5:1:10。3田间试验测定对荔枝白星病和荔枝褐斑病的防治效果
3.1田间试验测定对荔枝白星病的防治效果
3.1.1试验园基本情况
试验地设在广东省东莞市大朗镇一农户的荔枝园中进行,土壤为壤土.肥力中等,施肥与管理水平与当地栽培条件一致。荔枝供试品种为新红星,树龄11年,株距×行距=3m×5m,亩栽树55株,历年发病严重。
3.1.2试验设计
小区按随机区组排列,每小区2株树,重复4次。于荔枝开花后7—10d即开始施药,每10-15d施药一次,共施药3次;对照区喷等量清水。
配药时,先用少量水将药剂充分溶解后,再加入适量水进行全株喷雾处理,均匀喷雾。喷药时均采用机动喷雾器,工作压力为2.0-2.3kg/cm2,喷头孔径1.2mm。小区喷液量按675升/公顷施用,将药液均匀的喷施到作物叶正、反两面。以药液湿润叶片,不下滴为度。
3.1.3调查方法
每小区均调查两株,每株分东、西、南、北、中五个方向各固定2个新梢,定期调查其全部叶片,记录总叶数、各级病叶数,计算防治效果。
分级方法如下:
0级:无病斑;
1级:病斑面积占整个叶面积的10%以下;
3级:病斑面积占整个叶面积的11%~25%;
5级:病斑面积占整个叶面积的26%~40%;
7级:病斑面积占整个叶面积的41%-65%;
9级:病斑面积占整个叶面积的66%以上。
3.1.4调查时间和次数
本试验针对荔枝树春稍,共调查4次,即药前病情指数调查,第1次药后10天防效调查,第2次药后10天及第3次药后14天的防效调查。
3.1.5药效计算方法
病叶率(%)=病叶数/调查总叶数×100
病情指数=∑(各级病叶数×相对级数值)/(调查总叶数×9)×100
防治效果(%)=〔1-(空白对照区药前病情指数×处理区药后病情指数)/(空白对照区药后病情指数×处理区药前病情指数)〕×100
3.1.6对作物的直接影响
观察作物是否有药害产生,如有药害要记录药害程度和类型。此外,也应记录对作物的其他有益影响(如促进生长等)。
3.1.7试验结果及分析
表3各处理防治荔枝白星病的效果
结果分析:
由表3可以看出,30%吡噻菌胺·氟吗啉、丙硫菌唑5:1:10的混配组合防治荔枝白星病的效果十分显著。试验证明复配制剂在高浓度的用量下防治效果显著优于低浓度用量下的效果。在每亩10ml的用量下第3次药后14天的最高防效可达到85%左右。而吡噻菌胺和氟吗啉、丙硫菌唑单剂的防效分别在80%以下,,显著次于复配制剂。复配制剂的速效性和持效性都比较突出,为理想的防治荔枝白星病药剂。试验期间观察,其对荔枝安全,未产生不良影响。
综上所述,本发明含有吡噻菌胺和氟吗啉、丙硫菌唑的杀菌组合,对荔枝白星病和荔枝褐斑病都有很好的防治效果,且其对靶标作物安全。与单剂相比,本发明杀菌组合物具有持效期长,使用方便,对环境污染少,不易产生药害的优点。适用于防治卵菌、子囊菌、担子菌、半知菌等病原真菌引起的多种植物病害。通过复配,提高杀菌活性,扩大杀菌谱,拓宽使用范围,降低成本,对多种病害起到一药兼治的作用,减轻人力物力,提高生产效益。所以,本复配制剂的发明与推广对社会具有十分重要的意义。
以上所述并非对本发明的技术范围作任何限制,凡依据本发明技术实质对以上的实施例所作的任何修改、等同变化与修饰,均仍属于本发明的技术方案的范围内。
Claims (8)
1.一种杀菌组合物,其特征在于:含有氟吗啉、丙硫菌唑和吡噻菌胺两种活性组分,其中氟吗啉、丙硫菌唑和吡噻菌胺的重量比为10-50:1-20:20-60。
2.根据权利要求1所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑与吡噻菌胺的重量比为20-30:5-10:30-50。
3.根据权利要求1所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑与吡噻菌胺的重量比为25:5:50。
4.根据权利要求1所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑和吡噻菌胺累积所占制剂的重量百分比为15~50%。
5.根据权利要求1所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑和吡噻菌胺组合物的制剂中含有1-5重量份的沉香香料。
6.根据权利要求1所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑和吡噻菌胺组合物的制剂中含有1-3重量份的香附子提取物。
7.根据权利要求1 所述的杀菌组合物,其特征在于:氟吗啉、丙硫菌唑和吡噻菌胺与助剂和助溶剂复配成农药上允许的任意一种剂型。
8.根据权利要求1所述的杀菌组合物,其特征在于:可加工成的剂型是水乳、悬浮剂、微胶囊剂、可湿性粉剂和水分散粒剂等剂型。
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