CN104247712B - 一种含吡唑醚菌酯和代森锰锌的可分散油悬浮剂 - Google Patents
一种含吡唑醚菌酯和代森锰锌的可分散油悬浮剂 Download PDFInfo
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Abstract
本发明公开了一种含有吡唑醚菌酯和代森锰锌可分散油悬浮剂,其中,吡唑醚菌酯3‑40%,代森锰锌5‑60%,乳化剂2‑25%,分散剂2‑15%,润湿剂1‑8%,增稠剂1‑7%,防冻剂1‑5%,稳定剂1‑6%,分散介质余量。本发明组分合理,剂型环保,与现有的单一制剂相比,除具有很好的杀菌效果外,而且有显著的增效作用,对作物安全性好。本发明对黄瓜霜霉病和苹果炭疽病有优异的防治效果。
Description
技术领域
本发明涉及一种农用杀菌剂,具体的说是由第一活性成分吡唑醚菌酯和第二活性成分代森锰锌组成的可分散油悬浮剂,属于农药复配技术领域。
背景技术
吡唑醚菌酯,又名唑菌胺酯,英文通用名:Pyraclostrobin,化学名称: 甲基(N)-[[[1-(4-氯苯)吡唑-3基)-氧]-0-甲氧基]-N-甲氧氨基甲酸酯。熔点63.7~65.2℃。吡唑醚菌酯属甲氧基丙烯酸酯类杀菌剂,主要作用于真菌的线粒体呼吸链中的细胞色素 bel复合物,阻止电子传递从而抑制真菌生长。能防除所有类型的真菌病原体,杀菌谱广,对多种作物,包括麦类、葡萄 、果树、蔬菜的多种病害有效,主要用于防治葡萄白粉病、霜霉病;小麦白粉病、锈病;大麦叶锈病;香蕉黑叶条斑病;番茄早、晚疫病等。
代森锰锌,其他中文名大生,英文通用名Mancozeb,化学名称:乙撑双二硫代氨基甲酸锰和锌络盐。代森锰锌纯品为白色粉末,工业品为灰白色或淡黄色粉末,有臭鸡蛋味,难溶于水,不溶于大多数有机溶剂,但能溶于吡啶中,对光、热、潮湿不稳定,易分解出二硫化碳,遇碱性物质或铜、汞等物质均易分解放出二硫化碳而减效,挥发性小。代森锰锌是杀菌谱较广的保护性杀菌剂,主要是抑制菌体内丙酮酸的氧化,对果树、蔬菜上的炭疽病、早疫病等多种病害有效,同时它常与内吸性杀菌剂混配,用于延缓抗性的产生。由于它的这一特性,目前代森锰锌及其复配制剂的登记以可湿性粉剂为主,但可湿性粉剂药效较差。
可分散油悬浮剂是指以油为分散介质,将农药原药和各种助剂(乳化剂、功能性助剂、惰性填料等)经湿法超微粉碎得到的高分散、稳定的农药制剂。油类包括植物油或矿物油、甲酯油。可分散油悬浮剂用水稀释喷雾在植物上易形成一层药膜,因为植物表面有蜡质层,根据相似相亲相容原理,渗透传导性强,黏着性好,耐雨水冲刷,药效发挥更好,有效成分利用率高,而且剂型环保。
目前在农业部登记的可分散油悬浮剂农药产品多为玉米、小麦田除草剂,现有技术没有解决的主要问题是:1、吡唑醚菌酯原药的熔点较低(63.7~65.2℃),做可分散油悬浮剂生产时砂磨温度过高,原药溶解形成黏糊状物质,导致无法砂磨和生产,并且有效成分易分解失效;2、可分散油悬浮剂是一种热力学不稳定体系,随着时间推移,代森锰锌易出现结底、分层等变化;3、吡唑醚菌酯和代森锰锌复配制成可分散油悬浮剂,上述两方面的问题同时存在,难度更大。
发明内容
本发明的目的在于提供一种组分合理,杀菌效果好,对作物安全的含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂。
本发明的另一目的在于提供制备上述可分散油悬浮剂的方法。
为了克服现有技术的缺陷,本发明的技术方案是这样解决的:
一种含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂,由以下重量百分比的组分组成:吡唑醚菌酯 3-40%,代森锰锌 5-60%,乳化剂 2-25%,分散剂 2-15%,润湿剂1-8%,增稠剂1-7%,防冻剂1-5%,稳定剂1-6%,分散介质余量。
所述的乳化剂选自BY(蓖麻油聚氧乙烯醚)系列乳化剂(BY-110、BY-125、BY-140)、十二烷基苯磺酸钙、脂肪醇聚氧乙烯醚、农乳700#(通用名:烷基酚甲醛树脂聚氧乙烯醚)、农乳2201、斯盘-60#(通用名:山梨醇酐单硬脂酸酯)、吐温-60#(通用名:失水山梨醇单硬脂酸酯聚氧乙烯醚)、农乳1601#(通用名:苯乙基苯酚聚氧乙烯聚氧丙烯醚)、TERSPERSE 4894(美国亨斯迈公司出品);
所述的分散剂选自聚羧酸盐、木质素磺酸盐、EO-PO嵌段共聚物、磷酸酯及其盐类、磺酸盐类、烷基萘磺酸盐(扩散剂NNO)、TERSPERSE 2020(美国亨斯迈公司出品,烷基萘磺酸盐类);
所述润湿剂选自烷基酚聚氧乙烯基醚甲醛缩合物硫酸盐、烷基酚聚氧乙烯醚磷酸酯、苯乙基酚聚氧乙烯基醚磷酸酯、烷基硫酸盐、烷基磺酸盐、萘磺酸盐、TERSPERSE 2500(美国亨斯迈公司出品);
所述增稠剂选自如白炭黑、聚乙烯醇、膨润土、凹凸棒土、硅酸镁铝;
所述防冻剂选自乙二醇、丙二醇、甘油、尿素、无机盐类如氯化钠;
所述稳定剂选自有机酸、有机碱、酯类、醇类、抗氧剂、环氧氯丙烷、妥尔油;
所述分散介质选自大豆油、菜籽油、玉米油、油酸甲酯及其甲酯化油类、柴油、机油、矿物油及酯类溶剂。
上述可分散油悬浮剂的配制方法为:先将分散介质、乳化剂、分散剂、润湿剂、稳定剂加入反应釜,混合、分散均匀;高速剪切状态下加入吡唑醚菌酯和代森锰锌原药、增稠剂和防冻剂,在锆珠研磨介质下进行砂磨,研磨至粒径5um以下,即可制得含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂。
本发明由于加入不同的助剂,使该可分散油悬剂分散性好,热贮稳定性好,悬浮率高,两种成分的组合,延缓的病害抗性的发生。本发明解决了吡唑醚菌酯和代森锰锌配制成可分散油悬浮剂的难题,该剂型和其常见剂型可湿性粉剂相比,具有环保、提高药效,对作物安全性高,耐雨水冲刷,持效期长的特点,对蔬菜果树白粉病、炭疽病、霜霉病,黑星病、轮纹病、斑点落叶病、叶斑病等农作物病害有很好的防效。
具体实施方式
为了防治农业生产上的蔬菜、果树霜霉病,发明人以吡唑醚菌酯与代森锰锌进行了相互复配的增效研究,具体方法为:
试验采用黄瓜霜霉病菌(Pseudoperonospora cubensis)为测试对象。将原药配制成需要的试验药剂(剂型为可分散油悬浮剂),试验方法参考《中华人民共和国农业行业标准NY/T1156.3—2006》。首先将单剂及各混配药剂设置5个不同浓度梯度(在预备试验结果的基础上,抑菌率在5%~90%的范围内按等比级数设定)。试验靶标菌为采自田间自上向下4叶~6叶位的黄瓜霜霉病菌叶片,用4℃蒸馏水洗下叶片背面的霜霉病菌孢子囊,配成悬浮液(浓度控制在每毫升1×105 个~1×107个孢子囊),4℃下存放备用;将药液均匀喷施于健康叶片背面,待药液自然风干后,将各处理叶片叶背向上,按处理标记后排放在保湿盒中。试验设不含药剂的处理作空白对照。用准备好的新鲜孢子囊悬浮液点滴10μL接种于叶片背面。每叶片接种4滴,每处理不少于5片叶。在药剂处理后24h接种。接种后盖上皿盖,置于人工气候箱或有光照的保湿箱,在每天连续光照/黑暗12h交替,温度为17℃~22℃,相对湿度90%以上的条件下培养。视处理及空白对照发病情况测量并记录病斑直径,单位为毫米(mm),计算防治效果。通过防治效果的机率值和系列浓度的对数值之间的线性回归分析,求出各药剂的EC50 值,用孙云沛法计算混剂的共毒系数(CTC),以此来评价供试药剂对病菌的活性。
复配制剂的共毒系数(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。
室内毒力测定结果表明:吡唑醚菌酯与代森锰锌以重量比为1:20~2:1混用对黄瓜霜霉病菌有较好的毒力,均有显著的增效作用。
下面结合实施例对本发明内容作进一步说明,配方中的百分比均为重量百分比。
制剂实施例1
称取吡唑醚菌酯5%,代森锰锌50%,脂肪醇聚氧乙烯醚3%,聚氧乙烯聚氧丙烯嵌段共聚物5%,十二烷基苯磺酸钙7%,蓖麻油聚氧乙烯醚3%,白炭黑1%,有机膨润土1%,BHT 2%,油酸甲酯补足100%。上述原料经混合,用砂磨机砂磨至粒径小于5 um即制得55%吡唑醚菌酯·代森锰锌可分散油悬浮剂。
制剂实施例2
称取吡唑醚菌酯10%,代森锰锌40%,脂肪醇聚氧乙烯醚3%,TERSPERSE 2020 5%,十二烷基苯磺酸钙5%,BY-110# 2%,吐温-60#3%,白炭黑1%,硅酸镁铝1%,大豆油补足100%。上述原料经混合,用砂磨机砂磨至粒径小于5um即制得50%吡唑醚菌酯·代森锰锌可分散油悬浮剂。
制剂实施例3
称取吡唑醚菌酯7%,代森锰锌35%,烷基酚聚氧乙烯醚磷酸酯3%,聚氧乙烯聚氧丙烯嵌段共聚物5%,十二烷基苯磺酸钙4%,农乳700# 3%,蓖麻油聚氧乙烯醚2%,白炭黑1%,有机膨润土1%,BHT 2%,玉米油补足100%。上述原料经混合,用砂磨机砂磨至粒径小于5um即制得42%吡唑醚菌酯·代森锰锌可分散油悬浮剂。
制剂实施例4
称取吡唑醚菌酯3%,代森锰锌5%,脂肪醇聚氧乙烯醚3%,扩散剂NNO 3%,斯盘-60#6%,农乳2201# 3%,聚乙烯醇3%,BHT2%,环氧氯丙烷2%,油酸甲酯补足100%。上述原料经混合,用砂磨机砂磨至粒径小于5um即制得8%吡唑醚菌酯·代森锰锌可分散油悬浮剂。
上述制剂配方,加速热贮性试验,有效成分不分解,代森锰锌悬浮率≧95%,吡唑醚菌酯悬浮率≧93%。
生物实施例:防治苹果炭疽病田间试验
2013年在陕西省咸阳市进行了制剂实施例1(55%吡唑醚菌酯·代森锰锌可分散油悬浮剂)防治苹果炭疽病田间试验,验证了该药剂对苹果炭疽病的防治效果、有效剂量及对苹果的安全性。试验作物为苹果树,防治对象为苹果炭疽病[Glomerella cingulata(Stonem.) Schr.etSpanld.]。试验设在咸阳兴平市店张镇, 土壤为黏土, 地势平坦, 地力均匀, pH值7.1,肥力较好, 试验地栽培条件均匀一致,苹果品种为红富士,树龄为15年,行株距为5m×6m,该园炭疽病历年发生较重。试验药剂及稀释倍数详见表2。另设空白对照,每小区3棵树,共72个小区,随机区组排列。喷药防治试验从发病初期开始进行,分别于6月25日、7月25日、8月25日共喷药3次,全树均匀喷雾施药,以叶片正反面、果面均匀着药,稍有药滴下淌为度。
调查与统计方法:
于采收前调查药效, 每小区调查2株树, 每株树从东、南、西、北、中不同方位,分上、中、下部位, 每方位随机最少抽查20个果, 记录各果实的发病级别,以此计算病情指数和药剂的防效。每次喷药后第1天及药后若干天, 观察药剂各处理对果实和叶片的影响。
病果分级标准:
0级:无病斑;
1级:每果1—2个病疤;
3级:每果3—4个病疤;
5级:每果5—6个病疤;
7级:每果7—10个病疤;
9级:每果10个以上病疤。
田间试验结果表明:55%吡唑醚菌酯·代森锰锌可分散油悬浮剂800倍、1000倍、1200倍对苹果炭疽病有很好的防效,防效分别为92.02%、89.05%、87.16%,优于55%吡唑醚菌酯·代森锰锌可湿性粉剂相同剂量下的防效,也明显优于25%吡唑醚菌酯乳油1000倍、70%代森锰锌可湿性粉剂600倍对苹果炭疽病的防效,防效差异达到极显著水平,表现出显著的增效作用。
对苹果树的安全性调查,每次喷药后第1天及药后若干天观察, 各试验处理对果实、叶片无药害现象发生,但两种可湿性粉剂药剂对苹果果实表面产生了粉状物,对商品价值有一定影响。
试验结果表明吡唑醚菌酯与代森锰锌复配制成可分散油悬浮剂,明显提高了对苹果炭疽病的防治效果,降低了用药量及用药成本,对苹果生长安全,是防治苹果炭疽病的理想药剂。
Claims (7)
1.一种含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂,其特征在于所述的可分散油悬浮剂由以下重量百分比的组分组成:吡唑醚菌酯 3-40%,代森锰锌 5-60%,乳化剂 2-25%,分散剂 2-15%,润湿剂1-8%,增稠剂1-7%,防冻剂1-5%,稳定剂1-6%,分散介质余量;
所述的乳化剂选自BY系列乳化剂、十二烷基苯磺酸钙、脂肪醇聚氧乙烯醚、农乳700#、农乳2201、斯盘-60#、吐温-60#、农乳1601#、TERSPERSE 4894;
所述的分散剂选自聚羧酸盐、EO-PO嵌段共聚物、磷酸酯及其盐类、磺酸盐类、TERSPERSE 2020;
所述润湿剂选自烷基酚聚氧乙烯基醚甲醛缩合物硫酸盐、烷基酚聚氧乙烯醚磷酸酯、苯乙基酚聚氧乙烯基醚磷酸酯、烷基硫酸盐、烷基磺酸盐、萘磺酸盐、TERSPERSE 2500;
所述增稠剂选自白炭黑、聚乙烯醇、膨润土、凹凸棒土、硅酸镁铝。
2.根据权利要求1所述含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂,其特征在于:所述防冻剂选自乙二醇、丙二醇、甘油、尿素、氯化钠。
3.根据权利要求1所述含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂,其特征在于:所述稳定剂选自有机酸、有机碱、酯类、醇类、抗氧剂、环氧氯丙烷、妥尔油。
4.根据权利要求1所述含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂,其特征在于:所述分散介质选自大豆油、菜籽油、玉米油、柴油、机油、矿物油及酯类溶剂。
5.权利要求1所述含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂的配制方法,其特征在于:先将分散介质、乳化剂、分散剂、润湿剂、稳定剂加入反应釜,混合、分散均匀;高速剪切状态下加入吡唑醚菌酯和代森锰锌原药、增稠剂和防冻剂,在锆珠研磨介质下进行砂磨,研磨至粒径5um以下,即可制得含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂。
6.权利要求1所述含有吡唑醚菌酯和代森锰锌的可分散油悬浮剂在防治蔬菜果树白粉病、炭疽病、霜霉病,黑星病、轮纹病、斑点落叶病、叶斑病中的应用。
7.根据权利要求6所述应用,农作物病害为黄瓜霜霉病或苹果炭疽病。
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