CN105994338B - 一种含氟环唑与异菌脲的微乳剂 - Google Patents
一种含氟环唑与异菌脲的微乳剂 Download PDFInfo
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- CN105994338B CN105994338B CN201610626186.0A CN201610626186A CN105994338B CN 105994338 B CN105994338 B CN 105994338B CN 201610626186 A CN201610626186 A CN 201610626186A CN 105994338 B CN105994338 B CN 105994338B
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- microemulsion
- iprodione
- epoxiconazole
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- surfactant
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
本发明涉及一种含氟环唑与异菌脲的微乳剂,由如下组分及其重量百分含量组成:活性成分2‑40%,表面活性剂1‑30%,溶剂2‑20%,溶剂1‑20%,消泡剂0.5‑5%,防冻剂0.5‑5%,水补足100%;其中所述活性成分为氟环唑与异菌脲的混合物,二者重量比为20∶1至2∶1。本发明还涉及所述微乳剂的制备方法和用途。
Description
技术领域
本发明涉及农业领域,具体涉及一种含氟环唑与异菌脲的微乳剂以及其制备方法和用途。
背景技术
微乳剂(microemulsion,ME)是20世纪80年代国外出现的一种农药新剂型,是一种对环境友好的绿色农药制剂。它以水为基质,不用或仅用少量有机溶剂,含适量表面活性剂与其他助剂,为透明单相液体,属于热力学经时稳定的分散体系,不燃不爆、生产操作、贮运安全、环境污染少。微乳剂以水为主溶剂不但节省了大量有机溶剂,而且药剂施用后大为减轻了对环境的压力,对于维护农业生态环境具有重要意义,有利于农业的可持续发展。
氟环唑是一种内吸性***类杀菌剂,纯品为固体,作用机理为甾醇生物合成中C-14脱甲基化酶抑制剂,抑制病菌麦角甾醇的合成,阻碍病菌细胞壁的形成,兼具保护和治疗作用。氟环唑适用于小麦、大麦、水稻、甜菜、油菜、豆科作物、蔬菜、葡萄和苹果等多种作物,对作物安全、无药害,可防治立枯病、白粉病等多种病害。
异菌脲是一种二甲酰亚胺类高效广谱杀菌剂,纯品为白色结晶,难溶于水,易溶于丙酮、二甲基甲酰胺等有机溶剂。异菌脲作用机理为抑制蛋白激酶,控制许多细胞功能的细胞内信号,包括碳水化合物结合进入真菌细胞组分的干扰作用,进而抑制真菌孢子的萌发及产生,也可抑制菌丝生长。适用于瓜类、番茄、辣椒、茄子、园林花卉、草坪等多种作物、蔬菜及观赏植物等,主要防治灰霉病、早疫病、黑斑病、菌核病等多种植物病害。
CN101416640A公开了一种含异菌脲和氟环唑的杀菌剂组合物,公开了所述组合物可制备成可湿性粉剂、水分散粒剂、悬浮剂、水乳剂、乳油等。
现有技术公开的含氟环唑和异菌脲的上述剂型的配方还有进一步优化的空间,质量控制指标还有待提高。
现有技术未公开报道含氟环唑和异菌脲的微乳剂。
发明内容
本发明的目的为克服现有技术中氟环唑和异菌脲制剂的缺陷,研制氟环唑和异菌脲微乳剂,其各项质量指标优异,能够有效提高农药利用率。
为了解决上述问题,本发明采用以下的技术方案。
本发明一方面涉及一种含氟环唑与异菌脲的微乳剂,该微乳剂由如下组分及其重量百分含量组成:
活性成分2-40%
表面活性剂1-30%
溶剂2-20%
助溶剂1-20%
消泡剂0.5-5%
防冻剂0.5-5%
水补足100%;
优选地,各组分及其重量百分含量为:
活性成分8-20%
表面活性剂12-30%
溶剂6-15%
助溶剂5-10%
消泡剂0.5-3%
防冻剂1-5%
水补足100%;
更优选地,各组分及其重量百分含量为:
活性成分12-18%
表面活性剂12-16%
溶剂10-12%
助溶剂6-8%
消泡剂1-2%
防冻剂3-5%
水补足100%;
其中所述活性成分为氟环唑与异菌脲的混合物,二者重量比为2∶1至20∶1,优选为5∶1至10∶1,更优选为6∶1至9∶1,最优选8∶1。
在本发明所述的配方中,其中,
所述表面活性剂选自N,N′,N″-十二烷基二乙烯三胺五乙酸钠与三丁基酚聚氧乙烯醚中的一种或两种。更优选地,所述表面活性剂为N,N′,N″-十二烷基二乙烯三胺五乙酸钠与三丁基酚聚氧乙烯醚的混合物,二者的重量比为1∶5至5∶1,优选1∶2至2∶1。其中所述三丁基酚聚氧乙烯醚中聚氧乙烯的聚合度为6-30,优选8-16,更优选10-12。
所述溶剂选自丙酮、二甲基亚砜、二甲基甲酰胺、环己烷、环己酮、石油醚中的一种或多种。
所述助溶剂选自正丁醇、异丁醇、异丙醇、异戊醇中的一种或多种。
所述消泡剂选自磷酸丁酯、磷酸异丁酯、硅酮、正辛醇、聚二甲基硅氧烷中的一种或多种。
所述防冻剂选自丙二醇、乙二醇、丙三醇、聚乙二醇中的一种或多种。
不受任何理论束缚,本发明配方的选择,尤其表面活性剂的选择,所得到的微乳剂具有较好的稳定性,各项质量控制指标优异,杀菌效果优异。
本发明另一方面涉及所述微乳剂的制备方法,其主要包含如下步骤,
(1)将溶剂和助溶剂混合均匀,之后加入活性成分,并搅拌均匀,得到油相;其中搅拌速度可以为100-1000转/分,搅拌时间为30-60分钟;
(2)将表面活性剂、消泡剂、防冻剂加入水中,并搅拌均匀,得到水相;其中搅拌速度可以为100-1000转/分,搅拌时间为15-30分钟;
(3)边搅拌边将步骤(1)得到的油相加入步骤(2)得到的水相中,继续搅拌,搅拌速度可以为100-1000转/分,搅拌时间为15-40分钟,制成微乳剂。
本发明另一方面涉及所述微乳剂用于防治植物病害的用途。所述植物病害包括:
玉米病害:玉米大斑病(突脐蠕孢菌(Exserohilum turcicum))、玉米小斑病(玉蜀黍平脐蠕孢菌(Bipolaris maydis))、玉米锈病(高粱柄锈菌(Puccinia sorghi));
水稻病害:稻瘟病(稻瘟梨孢(Magnaporthe grisea))、长蠕孢叶斑病(宫部旋孢腔菌(Cochliobolus miyabeanus))、纹枯病(立枯丝核菌(Rhizoctonia solani))和恶苗病(藤仓赤霉(Gibberellafuj ikuroi))。
棉花病害:镰孢菌萎蔫病(尖孢镰刀菌(Fusarium oxysporum))、猝倒病(立枯丝核菌(立枯丝核菌(Rhizoctonia solani))、黄萎病(大丽花轮枝孢(Verticillium dahlia))。
黄瓜病害:灰霉病(灰葡萄孢(Botrytis cinerea))、黄瓜霜霉病(假霜霉属古巴假霜霉菌(Pseudoperonospora cubensis))、黄瓜白粉病(单丝壳白粉菌(Sphaerothecafuliginea))、黄瓜炭疽病(葫芦科刺盘孢菌(Colletotrichumorbiculare));
十字花科蔬菜病害:交链包属叶斑病(Alternaria japonica)、白斑病(芜青白斑病菌(Cercosporella brassicae))、根肿病(甘蓝根肿菌(Plasmodiophora brassicae))、和霜霉病(寄生霜霉(Peronospora parasitica))。
大麦、小麦、燕麦和黑麦病害:白粉病(禾白粉菌(Erysiphe graminis))、赤霉病(禾谷镰孢(Fusarium graminearum)、燕麦镰孢(F.avenacerum)、大刀镰孢(F.culmorum)、F.asiatricum、雪腐微托菌(Microdochium nivale))、锈病(条形柄锈菌(Pucciniastriiformis)、禾柄锈菌(P.graminis)、小麦叶锈病菌(P.recondite)、云纹病(小麦叶枯病菌(Septoria tritici))、颖枯病(颖枯球腔菌(Leptosphaeria nodorum))和网斑病(Pyrenophora teres Drechsler)。
葡萄病害:炭疽病(痂囊腔菌(Elsinoe ampelina))、晚腐病(Glomerellacingulata)、白粉病(Uncinula necator)、锈病(葡萄层锈菌(Phakopsoraampelopsidis))、黑腐病(Guignardia bidwellii)、霜霉病(葡萄生轴霜霉(Plasmoparaviticola))和灰霉病(灰霉病菌(Botrytis cinerea))。
番茄病害:早疫病(索兰氏链格孢(Alternaria solani))、叶霉病(黄枝孢霉(Cladosporium fulvum))、和晚疫病(致病疫霉(Phytophthora infestans))。
油菜病害:菌核病(核盘菌(Sclerotinia sclerotiorum))、黑斑病(甘蓝黑斑病链格孢(Alternaria brassicae))、白粉病(Erysiphe cichoracearum)、黑胫病(Leptosphaeria maculans)。
大豆病害:豆荚疫病和茎疫病(Diaporthe phaseolorum var.sojae)、锈病(Phakopsora pachyrhizi)、茎腐病(大豆疫霉(Phytophthora sojae))、灰霉病(灰葡萄孢霉(Botrytis cinerea)。
花生病害:叶斑病(球座尾孢菌(Cercospora personata))、褐叶斑病(花生尾孢菌(Cercospora arachidicola))和白绢病(齐整小核菌(Sclerotium rolfsii))。
马铃薯病害:早疫病(索兰氏链格孢(Alternaria solani))和晚疫病(致病疫霉(Phytophthora infestans))、粉红腐烂病(Phytophthora erythroseptica)、粉状疮痂病(Spongospora subterranean f.sp.subterranea)和丝核菌病(Rhizoctonia solani)。
甜菜病害:尾孢菌叶斑病(甜菜尾孢(Cercospora beticola))、叶枯病(Thanatephorus cucumeris)、根腐病(Aphanomyces cochlioides)。
优选地,本发明所述微乳剂用于防治玉米小斑病(玉蜀黍平脐蠕孢菌(Bipolarismaydis))和水稻纹枯病(立枯丝核菌(Rhizoctonia solani))。
有益效果
本发明配方的选择,尤其表面活性剂的选择,所得到的微乳剂具有较好的稳定性,各项质量控制指标优异,杀菌效果优异。
具体实施方式
为了理解本发明,下面以实施例进一步说明本发明,但不限制本发明。
下述实施例中,除另有说明外,所述百分比均为重量百分比。
(一)制剂实施例
实施例1 18%微乳剂
氟环唑16%,异菌脲2%,N,N′,N″-十二烷基二乙烯三胺五乙酸钠5%,三丁基酚聚氧乙烯(10)醚10%,二甲基亚砜12%,异丁醇8%,磷酸丁酯1%,丙三醇5%,水余量。
将溶剂和助溶剂混合均匀,之后加入活性成分,以100转/分的转速搅拌30分钟,得到油相。将表面活性剂、消泡剂、防冻剂加入水中,以200转/分的转速搅拌25分钟,得到水相。边搅拌边将油相加入水相中,以200转/分的转速继续搅拌30分钟,制成微乳剂。
实施例2 12%微乳剂
氟环唑10.5%,异菌脲1.5%,N,N′,N″-十二烷基二乙烯三胺五乙酸钠8%,三丁基酚聚氧乙烯(12)醚4%,二甲基甲酰胺10%,异丁醇6%,硅酮1%,丙二醇4%,水余量。
制备方法同实施例1。
实施例3 20%微乳剂
氟环唑18%,异菌脲2%,N,N′,N″-十二烷基二乙烯三胺五乙酸钠9%,三丁基酚聚氧乙烯(10)醚9%,环己酮15%,异丙醇10%,正辛醇0.5%,乙二醇5%,水余量。
制备方法同实施例1。
实施例4 14%微乳剂
氟环唑12%,异菌脲2%,N,N′,N″-十二烷基二乙烯三胺五乙酸钠16%,丙酮8%,异戊醇8%,磷酸异丁酯0.5%,丙二醇5%,水余量。
制备方法同实施例1。
实施例5 8%微乳剂
氟环唑7%,异菌脲1%,三丁基酚聚氧乙烯(12)醚10%,二甲基甲酰胺6%,异丙醇4%,磷酸丁酯0.5%,丙三醇4%,水余量。
制备方法同实施例1。
对比例1 18%微乳剂
氟环唑16%,异菌脲2%,十二烷基苯磺酸钙5%,甘油脂肪酸酯聚氧乙烯醚10%,二甲基亚砜12%,异丁醇8%,磷酸丁酯1%,丙三醇5%,水余量。
制备方法同实施例1。
对比例2 20%微乳剂
氟环唑18%,异菌脲2%,木质素磺酸钠15%,甲苯15%,异丙醇10%,正辛醇0.5%,乙二醇5%,水余量。
制备方法同实施例1。
对比例3 20%水乳剂
异菌脲15%,氟环唑5%,环己酮10%,二甲苯20%,司盘808%,OP-10磷酸酯6%,乙二醇4%,有机硅0.1%,余量为水。
按照已知方法制备成水乳剂。
(二)质量指标测定
1、低温稳定性测定
根据GB-T 19137-2003对本发明制剂的低温稳定性进行测定。具体为将试样在0℃贮存14天后,观察其外观变化。结果见下表。
表1 低温稳定性测定
样品 | 结果 |
实施例1 | 无变化 |
实施例2 | 无变化 |
实施例3 | 无变化 |
实施例4 | 基本无变化 |
实施例5 | 基本无变化 |
对比例1 | 乳液浑浊,有分层现象 |
对比例2 | 乳液浑浊,有分层现象 |
对比例3 | 乳液浑浊,严重分层 |
结果显示,本发明样品经冷贮之后,外观基本无变化。而对照样品则乳液浑浊,有分层现象。
2、热贮稳定性测定
根据GB-T 19136-2003对本发明制剂的热贮稳定性进行测定。具体为将样品置于安培瓶中,54℃贮存14天后,观察外观并测定活性成分含量,计算分解率。结果见下表。
表2 热贮稳定性测定
样品 | 外观 | 分解率 |
实施例1 | 无变化 | 0.5% |
实施例2 | 无变化 | 0.8% |
实施例3 | 无变化 | 0.8% |
实施例4 | 基本无变化 | 1.3% |
实施例5 | 基本无变化 | 1.5% |
对比例1 | 分层 | 6.6% |
对比例2 | 分层 | 5.8% |
对比例3 | 严重分层 | 9.2% |
结果显示,经过热贮之后,本发明样品外观基本无变化,且分解率较低。相比之下,对照样品出现分层,且活性成分分解率较高。
3、乳液稳定性测定
根据GB/T 1603-2001对本发明制剂的乳液稳定性进行测定。具体为,在250ml烧杯中,加入100ml 30℃的标准硬水,用移液管吸取1ml微乳剂样品,搅拌均匀后移入量筒中,并将量筒置于30℃恒温水浴中,静置1小时,观察乳液分离情况。结果如下。
表3 乳液稳定性测定
结果显示,本发明样品在1小时之后乳液上无浮油,下无沉淀,澄清透明。而对照样品则在乳液表面产生浮油,乳液浑浊。
(三)室内毒力测定
采用生长速率法测定本发明的组合物对水稻纹枯病菌(立枯丝核菌(Rhizoctoniasolani)的抑菌效果。
将供试药剂分别配成1000mg/L的母液,然后取适量按照预定比例混合并用2%的吐温80水溶液配制5个浓度梯度,然后加至约45℃的培养基中,混合均匀并倒入灭菌的培养皿内,冷却后形成带毒的培养基平面,清水为空白对照,各浓度重复5次。之后,接入直径为5mm的菌饼,将培养皿置于25℃,湿度80%的培养箱中培养。96小时后,取出培养皿,测量菌落直径,并通过下式计算各药剂处理对病菌的抑制生长率,并求出各处理对病原菌的EC50。
然后,按照孙云沛法计算各处理的共毒系数。若共毒系数大于120,表明有增效作用;共毒系数小于80,表明为拮抗作用;共毒系数在80-120之间,表明为相加作用。结果见下表。
表4 水稻纹枯病菌测定结果
其中,A为氟环唑;B为异菌脲。
结果显示,本发明药剂在所限定的比例范围内对水稻纹枯病菌具有协同增效作用,但在所限定的比例之外,则不表现出增效作用。
(四)田间药效试验
测定本发明组合物对玉米小斑病的田间防效。
试验药剂为本发明制剂实施例1-5所述制剂。
对照药剂为对比例1-3制剂,以及15%氟环唑微乳剂、12%异菌脲悬浮剂。
试验药剂、对照药剂和清水对照的小区处理采用随机区组排列,小区面积50平方米,4次重复。施药处理7天后采用随机五点取样法进行调查,并采用病情指数法计算各处理的防效。结果见下表。
病害分级标准如下:
0级:无病斑;
1级:病斑面积占整叶面积的5%以下;
3级:病斑面积占整叶面积的6%~15%;
5级:病斑面积占整叶面积的16%~25%;
7级:病斑面积占整叶面积的26%~50%;
9级:病斑面积占整叶面积的50%以上。
防效计算方法为:
表5 玉米小斑病田间药效试验结果
田间试验结果显示,本发明药剂对玉米小斑病的防效明显高于对照药剂。
上述实例仅仅是对本发明的进一步解释,并不是对本发明的限定,通过将上述方案进行简单的调整进而得到的方案,同样在本申请的保护范围之内。
Claims (9)
1.一种含氟环唑与异菌脲的微乳剂,由如下组分及其重量百分含量组成:
活性成分2-40%
表面活性剂1-30%
溶剂2-20%
助溶剂1-20%
消泡剂0.5-5%
防冻剂0.5-5%
水补足100%;
其中所述活性成分为氟环唑与异菌脲的混合物,二者重量比为2:1至20:1;
所述表面活性剂选自N,N',N''-十二烷基二乙烯三胺五乙酸钠与三丁基酚聚氧乙烯醚的混合物,二者的重量比为1:5至5:1。
2.根据权利要求1所述的微乳剂,其特征在于,各组分及其重量百分含量为:
活性成分8-20%
表面活性剂9-18%
溶剂6-15%
助溶剂5-10%
消泡剂0.5-3%
防冻剂1-5%
水补足100%;
其中所述活性成分为氟环唑与异菌脲的混合物,二者重量比为5:1至10:1。
3.根据权利要求1或2所述的微乳剂,其特征在于,
N,N',N''-十二烷基二乙烯三胺五乙酸钠与三丁基酚聚氧乙烯醚的重量比为1:2至2:1。
4.根据权利要求1或2所述的微乳剂,其特征在于,所述溶剂选自丙酮、二甲基亚砜、二甲基甲酰胺、环己烷、环己酮、石油醚中的一种或多种。
5.根据权利要求1或2所述的微乳剂,其特征在于,所述助溶剂选自正丁醇、异丁醇、异丙醇、异戊醇中的一种或多种。
6.根据权利要求1或2所述的微乳剂,其特征在于,所述消泡剂选自磷酸丁酯、磷酸异丁酯、硅酮、正辛醇、聚二甲基硅氧烷中的一种或多种。
7.根据权利要求1或2所述的微乳剂,其特征在于,所述防冻剂选自丙二醇、乙二醇、丙三醇、聚乙二醇中的一种或多种。
8.一种权利要求1或2所述微乳剂的制备方法,其特征在于,包含如下步骤,
(1)将溶剂和助溶剂混合均匀,之后加入活性成分,并搅拌均匀,得到油相;
(2)将表面活性剂、消泡剂、防冻剂加入水中,并搅拌均匀,得到水相;
(3)边搅拌边将步骤(1)得到的油相加入步骤(2)得到的水相中,继续搅拌,制成微乳剂。
9.权利要求1或2所述的微乳剂用于防治植物病害的用途。
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