CN111138379A - 广谱杀菌无公害促生长噻唑锰锌化合物及其组合物 - Google Patents
广谱杀菌无公害促生长噻唑锰锌化合物及其组合物 Download PDFInfo
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- CN111138379A CN111138379A CN201811305284.XA CN201811305284A CN111138379A CN 111138379 A CN111138379 A CN 111138379A CN 201811305284 A CN201811305284 A CN 201811305284A CN 111138379 A CN111138379 A CN 111138379A
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- Prior art keywords
- manganese
- zinc
- compound
- thiazole
- water content
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- -1 thiazole manganese zinc Chemical compound 0.000 title claims abstract description 341
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 166
- 239000011572 manganese Substances 0.000 claims description 120
- 239000011701 zinc Substances 0.000 claims description 113
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- 239000003899 bactericide agent Substances 0.000 claims description 46
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 41
- 229910052748 manganese Inorganic materials 0.000 claims description 41
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
- C07D285/01—Five-membered rings
- C07D285/02—Thiadiazoles; Hydrogenated thiadiazoles
- C07D285/04—Thiadiazoles; Hydrogenated thiadiazoles not condensed with other rings
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Abstract
本发明的广谱杀菌无公害促生长的噻唑锰锌化合物,相比单一制剂,对农作物施用时既杀菌又同时补充锰锌,相对比复配,制剂含量准确,减少繁琐制剂过程,方便施用,且易于制备,能耗更低,更绿色环保,还有更好的存储稳定性或防治效果等,适用于制备含有该化合物的组合物及防治农作物上各种细菌性和真菌性病害和或促进作物健康或生长发育的农药,或用于保护工业材料不受病菌侵害等领域的药剂中的应用。
Description
技术领域
本发明涉及农药技术领域,具体地说是提供广谱杀菌噻唑锰锌的稳定性更好的新化合物以及其农用组合物及其制备方法和用途。
背景技术
噻唑锌,化学名称为双(2-氨基-5-巯基-1,3,4-噻二唑)锌,CAS:1202750-31-9,分子式,C4H4N6S4Zn,分子量329.77,可用于精细化工领域包括感光或材料学等方面,也是由浙江新农化工股份有限公司研制的有机锌广谱杀菌剂。该药兼具内吸、传导、预防、保护、治疗等多重作用,且其治疗作用的效果大于保护作用,是防治农作物细菌性病害的新一代高效、低毒、广谱杀菌剂,对各种细菌性和真菌性病害均有较好的防治效果。20%噻唑锌悬浮剂(商品名:碧生),被科技部等四部委认定为“国家萤点推广新产品”。网上报道具有六大特点:一是杀菌谱广。对细菌性病害特效,对真菌性病害高效,是功能齐全的杀菌剂。二是效果突出。“强力保护+快速内吸治疗”,持效期长达半个月,低毒、无公害。三是剂型环保。超微制剂,对果实无污染,是无公害农产品生产的首选药剂。四是适用于几乎所有作物,无药害,对作物花、幼果安全。五是高效补锌。能促进花芽分化、花粉管的伸长、授粉和促花保果,也能消除果树缺锌的小叶病、莲花叶、鸡腿枝。六是混用增效好,除强酸强碱农药外都可混配,可以在推荐剂量下和市面上推广的防治真菌性杀菌剂进行科学混用,综合防效远远高于单用一种真菌性药剂,同时延缓抗性,确保安全无药害,七是安全性好,不会刺激螨类、锈壁虱的繁殖,农民的好评度高,已经成为推动无公害农产品保健栽培的优秀主流杀菌剂(文献:冷鹏,杀菌剂噻唑锌的应用效果[J].浙江农业科学,2010(06):1355.;魏方林,戴金贵,朱国念,朱洪斌,创制杀菌剂——噻唑锌[J].世界农药,2008(02):47-48)。
噻唑锌的作用机理:噻唑锌的结构由二个基团组成杀菌。一是噻唑基团,在植物体外对细菌无抑制力,但在植物体内却是高效的治疗剂,药剂在植株的孔纹导管中,细菌受到严重损害,其细胞壁变薄继而瓦解,导致细菌的死亡。二是锌离子,具有既杀真菌又杀细菌的作用。药剂中的锌离子与病原菌细胞膜表面上的阳离子(H+,K+等)交换,导致病菌细胞膜上的蛋白质凝固杀死病菌;部分锌离子渗透进入病原菌细胞内,与某些酶结合,影响其活性,导致机能失调,病菌因而衰竭死亡。
噻唑锰,化学名称为双(2-氨基-5-巯基-1,3,4-噻二唑)锰,分子式C4H4N6S4Mn,分子量319.31,目前并未用于防治农作物细菌性病害。
许多资料表明,叶绿体含锰量高。锰是维持叶绿体结构所必需的微量元素。在叶绿体中,锰与蛋白质结合形成酶蛋白,是光合作用中不可缺少的参与者。缺锰时,膜结构遭破坏而导致叶绿体解体,叶绿素含量下降。如甜菜缺锰时,其栅栏组织和海绵组织细胞中叶绿体的数目、体积和叶绿素含量都明显减少。
锰能促进种子萌发和幼苗早期生长,对生长素促进胚芽鞘伸长的效应有刺激作用,能加快种子内淀粉和蛋白质的水解过程,促使单糖和氨基酸能及时供幼苗利用。供锰充足还能提高结实率,对幼龄果树提早结果有良好的作用。此外,锰对维生素C的形成以及加强茎的机械组织等都有良好的作用。
锰对根系的生长也有影响。缺锰时植物侧根几乎完全停止生长,根中无液泡的小细胞数量增多。这也表明缺锰对细胞伸长的影响大于对分裂作用的影响,而全球不少土壤缺锰,对作物生长带来不利影响。
目前,公开的文献有限的报道了噻唑锰和噻唑锌的制备和用途[专利文献、噻二唑类金属络合物及其制备方法和用途CN1152869]的制备方法]。
到目前为止,国内外尚无公开文献报道的国内外尚无公开文献报道的噻唑锰和噻唑锌的复配,更无文献报道制备新型噻唑锰锌化合物或含水量在一定范围的噻唑锰锌化合物,而农林生产中需要杀菌的时候同时补充锰锌的杀菌剂。
化学药物的多晶型在药物研究中具有重要地位,且适用于更佳的药学需要。热分析方法在材料科学、化学或药物分析等中具有重要的价值和地位,能单独用来检测化合物的多晶型或过程中晶型的变化(李增余,《热分析》,清华大学出版社,1987年8月第一版)。差热分析法(DTA)是较为常用的分析方法,它既可用于物质的定性鉴别,也可用于定量分析或表征化合物结构,早在1968年的第二届国际热分析会议上,就被Barta等用来鉴定未知化合物。
发明内容
本发明所涉及的是噻唑锰锌新化合物,既杀菌又补充微量元素锰和锌,即噻唑锰锌或其含水的化合物或其水合物,双(2-氨基-5-巯基-1,3,4-噻二唑)锰锌,分子式为(C4H4N6S4)(Mn2+)V(Zn2+)K,含水量在0.00-13%,或分子式为C4H4N6S4(Mn2+)V(Zn2+)K·wH2O,含水量在0.00-13%,噻唑锰锌分子中锰和锌的摩尔数或其比例在0.0001~0.9999∶0.9999~0.0001之间,噻唑锰锌分子中锰和锌的摩尔数均在0.0001~0.9999之间,并且,噻唑锰锌分子中锰和锌的摩尔数之和等于1,即V+K=1,以及其农药组合物及其制备方法和用途。
本发明的噻唑锰锌化合物或复合物包括但不仅限于:
[C4H4N6S4(Mn)0.95(Zn)0.05·,含水量可在0.0-13%],[C4H4N6S4(Mn)0.5(Zn)0.5,含水量可在0.0-13%],[C4H4N6S4(Mn)0.9(Zn)0.1,含水量可在0.0-13%],
[C4H4N6S4(Mn)0.8(Zn)0.2,含水量可在0.0-13%],[C4H4N6S4(Mn)0.7(Zn)0.3,含水可在0.0-13%],[C4H4N6S4(Mn)0.65(Zn)0.35,含水可在0.0-13%],[C4H4N6S4(Mn)0.6(Zn)0.4,含水量可在0.0-13%],[C4H4N6S4(Mn)0.4(Zn)0.6,含水量在0.0-13%],
[C4H4N6S4(Mn)0.35(Zn)0.65,含水量可在0.0-13%],[C4H4N6S4(Mn)0.3(Zn)0.7,含水量在0.0-13%],[C4H4N6S4(Mn)0.2(Zn)0.8,含水量在0.0-13%],[C4H4N6S4(Mn)0.1(Zn)0.9,含水量在0.0-13%],[C4H4N6S4(Mn)0.05(Zn)0.95,含水可在0.0-13%];
或[C4H4N6S4(Mn)0.95(Zn)0.05·wH2O,含水量可在0.0-13%],
[C4H4N6S4(Mn)0.5(Zn)0.5·wH2O,含水量可在0.0-13%],[C4H4N6S4(Mn)0.9(Zn)0.1·wH2O,含水量可在0.0-13%],[C4H4N6S4(Mn)0.8(Zn)0.2·wH2O,含水量可在0.0-13%],
[C4H4N6S4(Mn)0.7(Zn)0.3·wH2O,含水可在0.0-13%],[C4H4N6S4(Mn)0.65(Zn)0.35·wH2O,含水可在0.0-13%],[C4H4N6S4(Mn)0.6(Zn)0.4·wH2O,含水量可在0.0-13%],
[C4H4N6S4(Mn)0.4(Zn)0.6·wH2O,含水量在0.0-13%],[C4H4N6S4(Mn)0.35(Zn)0.65·wH2O,含水量可在0.0-13%],[C4H4N6S4(Mn)0.3(Zn)0.7·wH2O,含水量在0.0-13%],
[C4H4N6S4(Mn)0.2(Zn)0.8·wH2O,含水量在0.0-13%],[C4H4N6S4(Mn)0.1(Zn)0.9·wH2O,含水量在0.0-13%],[C4H4N6S4(Mn)0.05(Zn)0.95·wH2O,含水可在0.0-13%];
噻唑锰锌化合物可含有一定数量的水,含水量可在0.00-13%;
噻唑锰锌无水物可含有一定b量的水,含水量可在0.00-3%。
尽管目前使用噻唑锌,但有的土壤却需要杀菌或同时缺乏锰和锌,却不能得到有效补充,目前并无噻唑锌和噻唑锰相关复配,若使用复配存在配制的上不方便或配制剂量的准确上的问题,由此影响作物生长和杀菌,也可能影响环境与生态安全,甚至造成作物药害,有可能导致多方面的不良影响,本发明的噻唑锰锌在溶液状态下反应制备所得,形成均匀和含量稳定的产物,这不是两种固体物质物理混合能媲美的。若进行物理混合,需要分别先制备噻唑锌和噻唑锰,显然比制备单一噻森锰锌化合物繁琐得多,而且物理混合易导致两种物料的含量不准确。此外,本研究还发现稳定性更好的噻唑锰锌水合物具有更好的易获得性,可形成药物学或农药上的较佳选择,这却长期以来为行业内人士所忽视。
不仅如此,本发明还发现本发明的新化合物水合物在生产制造过程或环保处置过程的优点,文献1(CN1152869)制备现有技术的噻唑锰或噻唑锌反应需要温度高达70-80℃,且实施例的干燥温度须100℃,势必消耗更多的能量,不利于构建能源节约型生产,使得总杂质增加,不利于原料的储存稳定性。这反映稳定性不同程度更好的噻唑锰锌水合物在生产中有更好的可获得性,同时也说明本发明的物质更具有生产的便利性。
本发明获得的噻唑锰锌化合物新型分子中含结晶水的噻唑锰锌引湿性低于不含结晶水的噻唑锰锌,更利于制剂制造,便于储存和运输,降低制造费用和成本。本发明的不同的新分子式和新分子结构的噻唑锰锌复合物及其水合物在稳定性和施用上等方面有不同的优势。进一步说,本发明噻唑锰锌复合物具有更好的工业化价值或农药价值。
令人惊奇的是,特征性的,本发明的水合物的热分析(TG-DSC或者TG-DTA)图谱的失重平台下(约在45-162℃之前的失重曲线下)具有对应的吸热峰,热分析图谱显示出新型结构的噻唑锰锌水合物,在药物学上具有现实或未来的意义或价值。
噻唑锰锌或其水合物的制备包括但不仅限于如下方法:
在反应容器中加2-氨基-5-巯基-1,3,4-噻二唑,加水和/或有机溶剂C1-C6的低分子醇(选自但不仅限于甲醇、乙醇、异丙醇、正丁醇等)、C2-C8的低分子醚(选自但不仅限于乙醚、四氢呋喃、异丙醚等)、C2-C6的低分子腈中的一种或几种,搅拌溶解,加碳酸钠、碳酸氢钠、氢氧化钠、碳酸钾、碳酸氢钾、氢氧化钾中的一种或几种或其水溶液,搅拌,加锰盐或其溶剂化合物或其溶液和锌盐或其溶剂化合物或其溶液,锰盐或其溶剂化合物选自但不仅限于硫酸锰、一水硫酸锰、氯化锰、氯化锰4水合物、醋酸锰、醋酸锰4水合物、硝酸锰、硝酸锰4水合物或其水溶液中的一种或几种,水溶性的锌盐选自但不仅限于硫酸锌、七水硫酸锌、氯化锌、醋酸锌、硝酸锌或其水溶液中的一种或几种,搅拌,待固体充分析出,过滤,用水、C1-C6的低分子醇、C2-C8的低分子醚、C3-C8的低分子酮、C2-C6的低分子腈、C1-C6的低分子卤代烃中的一种或几种洗一次到数次,过滤,所得固体用水、Cl-C6的低分子醇、C2-C8的低级醚、C3-C8的低分子酮、C1-C6的低级卤代烃中的一种或几种洗涤,过滤,干燥得噻唑锰锌或噻唑锰锌结晶水合物;
其中,反应中所使用的2-氨基-5-巯基-1,3,4-噻二唑:碱(选自但不仅限于碳酸钠、氢氧化钠、氢氧化钾、异辛酸钠等中的一种)中的一种的当量比约为1∶1~1.2;第一步反应中所使用的2-氨基-5-巯基-1,3,4-噻二唑(重量g)与水、或C1-C6的低分子醇、或C2-C8的低级醚(选自但不仅限于乙醚、四氢呋喃、异丙醚等)、或C2-C6的低级腈(选自但不仅限于乙腈、丙腈等)等有机溶剂中的一种或几种重量体积比为一般为:1(g)∶3.5~60(ml),较优选的比为:1(g)∶5~40(ml);2-氨基-5-巯基-1,3,4-噻二唑与锰盐和锌盐的总当量比约为1∶0.98~1.1。
噻唑锰锌或其水合物的合成溶剂选自但不仅限于水、乙腈、四氢呋喃、甲醇、乙醇、异丙醇、乙酸乙酯、醋酸丁酯、甲酸乙酯、乙醚、四氢呋喃、异丙醚、二氯甲烷、氯仿等中的一种或几种。
本发明中的有机溶剂低级醇或低分子醇的碳原子数定义为C1-C6(即:1-6个碳原子的醇),如甲醇、乙醇、异丙醇等;低级醚或低分子醚的碳原子数定义为C2-C8,如乙醚、丁醚、四氢呋喃等;低级卤代烃的碳原子数定义为C1-C6,包括二氯甲烷、二氯乙烷、氯仿等;低级酯的碳原子数定义为C2-C8,除非特别指明为甲酸低级酯的外,否则为包括醋酸丁酯、乙酸乙酯、甲酸乙酯等;C3-C8的低分子酮定义为3-8个碳原子的酮,包括丙酮,丁酮、异己酮等;关于任何一类描述为“低级或低分子”化合物碳原子数量的标记方法只要在文本中出现一次,其它任何未进行标记的描述为“低级或低分子”的同类化合物的碳原子数与本文中已经标明的数量是一致的。
本发明的产物的干燥方式可以为在不同温度(譬如20-70℃之间干燥)、干燥时间、或附有其它干燥剂(包括硅胶,五氧化二磷、无水氯化钙、无水硫酸钠等)的环境条件下、或使用常压或减压的方式对最后的产物进行干燥。其干燥温度较优选在35-60℃。
无水物的制备可在不同温度(如90-110℃)、干燥时间(可以到数日)、或附有其它干燥剂(包括硅胶,分子筛、五氧化二磷、氢氧化钠、碱石灰、无水碳酸钠、无水氯化钙、无水硫酸钠、无水硫酸镁等)的环境条件下、或并使用常压或减压的方式对最后的产物进行干燥,也可先由无水苯混合放置数日处理或蒸馏带水的方法,并结合本文中描述的其它干燥方法干燥后获得。
本发明中的噻唑锰锌新化合物等的水分测定参照2010版中国药典附录VIII M第一法A,采用卡尔费休法测定,并用特定的卡尔费休水分测定仪测定相关物的水分。
本发明在一方面,提供噻唑锰锌化合物及其结晶水合物或无定型水合物化合物。
本发明在另一方面,提供噻唑锰锌新化合物以及它们的制备方法。
本发明提供一种药用组合物,其中包括任何一种或多种由本发明的方法制备的噻唑锰锌新化合物,和一种或多种药学可接受的赋形剂。
本发明进一步提供制备药物制剂的方法,其中包括任何一种或多种由本发明的方法制备的噻唑锰锌新化合物制剂或和至少一种或药学可接受的赋形剂的合并。
本发明进一步提供噻唑锰锌新化合物,在制备用于杀菌等农药组合物中的用途。
本发明提供噻唑锰锌新化合物与单一噻唑锰或噻唑锌相比,不仅一次性形成稳定的化合物,能同时提供锰和锌微量元素,为促进作物生长提供条件,提供多靶点的杀菌手段,为保护作物生长提供手段。
本发明提供噻唑锰锌新化合物与单一噻唑锰或噻唑锌或噻唑锰或噻唑锌的复配物相比,减少分次生产的繁琐,利于降低能耗,降低该药物运营成本。
本发明噻唑锰锌新化合物制备成本比单一噻唑锰或噻唑锌的复配物降低数倍。
本发明的噻唑锰锌新化合物比噻唑锰或噻唑锌无水物更易于制备,本发明产物的制备温度大幅低于对比文献1(对比文献1、噻二唑类金属络合物及其制备方法和用途,CN1152869)的实施例1和2的噻唑锰或噻唑锌无水物制备,利于节省时间和能耗。
不仅如此,本发明还发现本发明的新化合物在生产制造过程或环保处置过程的优点,本发明发现,现有技术的文献(文献1、CN 1152869;)的实施例1和2中,制备噻唑锰或噻唑锌无水物的干燥温度达约100℃,这势必消耗更多的能量,升温和降温过程也较长,不利于能源节约型生产;而本发明的噻唑锰锌新化合物水合物制备过程中干燥仅需约40-65℃,能耗更低,产物稳定性或药效学研究发现完全能满足药物学上的要求。这反映稳定性更好的噻唑锰锌新化合物特别是其水合物在生产中具有更好的可获得性,且具有更低的能耗优势,同时也说明本发明的物质更具有生产的便利性和更好的工业化价值。
1、制剂质量可控性比较实验
农药制剂的原药含量的准确对农作物病害的防治具有重要性作用,由于制剂制备过程中装量等误差的存在,导致每袋制剂的含量不会具有绝对等同性,因此,在制剂质量控制设置一个质量范围(譬如主药的标示量经常设置为90-110%)来控制制剂的含量指标等。若原药吸潮导致称样不准,而制剂成品的含量必须控制在主药无水物的法定标示量计算为90-110%之间,这会导致成品不合格率大幅提升。在RH62±5%、25±2℃条件下将不同来源的含量已确定的噻唑锰锌新化合物原料和含量已确定的符合实施例1-1A、1-3A、1-5A分子结构比例的噻唑锰和噻唑锌无水物原料分别分散摊开成约5毫米厚暴露在空气中24小时,然后分别按照分摊前明确的含量分别称取样品,并按照本说明书实施例8法的方法制备主药无水物标示量为90-110%之间的制剂(含量规格为噻唑锰锌20g/袋,锰和锌的标示量以其理论含量计),当原料药以主药无水物的标示量的100%,即按绝对无水物计算精密称取同等重量噻唑锰锌2000克投料用于制备100袋单位制剂时,其余辅料及配比等均相同。在最终制剂成品中随机取袋重差异合格的40袋测定每袋噻唑锰锌制剂中锰和锌的含量(样品中锰锌的含量测定方法参考如下文献方法:阿力甫·阿布都,阿不力孜·艾力,王旭.火焰原子吸收光谱法测定小茴香中的铜、铁、锰和锌[J].光谱实验室,2012,29(04):2357-2359.;张平,胡国俊,火焰原子吸收光谱法测定莼菜中的锌、铜、锰[J].武汉化工学院学报,1997(03):15-17.;样品用硝酸与盐酸组成的王水溶解进行预处理),以每袋噻唑锰锌制剂中锰或锌的含量超过其标示量(含量规格为噻唑锰锌20g/袋,锰或锌的标示量以其理论含量计)的90-110%范围为不合格,实验结果如下表。
表1.制剂可控性比较实验研究结果
由上述两个实验结果可见,实施例法原料药制备的样品未出现不合格情况,本发明的噻唑锰锌新化合物在制备固体制剂时的成品率远远高于噻唑锰锌无水物原料的,当制剂主药的含量减少时,导致其杀菌能力下降,对农作物的病菌防治不利,说明本发明的噻唑锰锌新化合物利于提升制剂制造时的质量可控性,利于制剂成品合格率大幅度提升,有利于农作物病菌的防治和作物生长。
本发明不仅制备更稳定的噻唑锰锌新化合物,而且提供该新化合物的组合物,该杀菌活性化合物组合物中含有噻唑锰锌新化合物A和另外任意一种已知杀菌活性或抗病毒药化合物B,它应用于防治植物真菌、细菌、病毒引起的病害。该杀菌活性化合物组合物具有协同杀菌或抗病毒药活性、改善与植物的相容性,从而满足农业生产的需要。
本发明的新型噻唑锰锌化合物用于制备含有有效剂量的噻唑锰锌新化合物与有效剂量的杀菌药物或和抗菌药物或抗病毒药和或植物生长调节剂或有效剂量的农药上可接受的杀虫剂组成的药物组合物或农药组合物,及其他药学上可接受的辅料制备药学上可接受的农药制剂;即,有效剂量的活性成分A——噻唑锰锌新化合物和有效剂量的活性成分B制备新的药物组合物或农药组合物;其中,活性成分A与活性成分B重量比可选自为180∶1~1∶100(可以其无水物或含水物计算重量);其中,活性成分A与活性成分B重量比可较优选自为100∶1~1∶100(可以其无水物或含水物计算重量);其中,活性成分A与活性成分B重量比也可较优选自为80∶1~1∶80(可以其无水物或含水物计算重量);所述的活性成分B选自但不仅限于其中的任意一种或几种选自B.1)-B.13)的化合物及其药学上可接受盐或其溶剂化合物(活性成分B选自不仅限于如下参考文献中的农药化合物,参考文献A:刘长令,柴宝山主编,《新农药创制与合成》,化学工业出版社,2013年,北京;文献B:孙家隆,齐军山,《现代农药应用技术丛书:杀菌剂卷》,化学工业出版社,2017年,北京;C:郑桂玲,孙家隆,《现代农药应用技术丛书:杀虫剂卷》,化学工业出版社,2017年,北京;D:孙家隆,《现代农药合成技术》,化学工业出版社出版,2011年,北京;E:现代农药手册,刘长令,杨吉春,化学工业出版社,2018年,北京;文献F:刘长令主编,《世界农药大全:杀菌剂卷,》,化学工业出版社,北京,出版时间:2006;文献G:刘长令编《世界农药大全:杀虫剂卷》,化学工业出版社,北京,2012;);
B.1)甲氧基丙烯酸酯类杀菌剂或抗病毒药,选自但不仅限于嘧菌酯、醚菌酯、肟菌酯、吡唑醚菌酯、烯肟菌酯、唑菌酯、氟嘧菌酯、啶氧菌酯、苯醚菌酯、烯肟菌胺或苯氧菌胺、氰烯菌酯、Picarbutrazox、肟醚菌胺、唑菌胺酯、丁香菌酯、氯啶菌酯、苯噻菌酯、UBF307、KZ165、烯丙苯噻唑、双氯氰菌胺等中的一种或几种;
B.2)三唑类杀菌剂,选自但不仅限于苯醚甲环唑、烯唑醇、氟环唑、腈苯唑、氟硅唑、粉唑醇、戊唑醇、己唑醇、腈菌唑、戊菌唑、丙环唑、四氟醚唑、三唑醇、联苯三唑醇、三唑酮、叶菌唑、种菌唑、丙硫菌唑、亚胺菌唑、灭菌唑、环丙唑醇、氯氟醚菌唑(mefentrifluconazole)、异丙芬三氟康唑ipfentrifluconazole、糠菌唑、腈苯唑、氟喹唑、呋醚唑、戊环唑、乙环唑、三氟苯唑、高效烯唑醇、三唑酮等中的一种或几种;
B.3)酰胺类杀菌剂,选自但不仅限于甲霜灵、精甲霜灵、氟酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌酰胺、萎锈灵、联苯吡菌胺、氟唑菌苯胺、氟唑环菌胺、氟唑菌酰胺、吡噻菌胺、噻呋酰胺、氟啶酰菌胺和吡唑萘菌胺、氟苯醚酰胺、氟醚菌酰胺、环己磺菌胺、甲噻诱胺、高效苯霜灵、噻氟菌胺、噻酰菌胺、噻唑菌胺、硅噻菌胺、呋吡菌胺、环氟菌胺、氟吡菌胺、苯酰菌胺、环酰菌胺、环丙酰菌胺、磺菌胺、甲磺菌胺、引唑磺菌胺、稻温酰胺、Bixafen、Fluxapyroxad、Sedaxane等中的一种或几种;
B.4)咪唑类杀菌剂中的一种,选自但不仅限于氰霜唑、氟菌唑、高效抑霉唑、咪唑菌酮、噁咪唑、稻温酯、丙硫咪唑、苯硫咪唑、噻菌灵、抑霉唑、麦穗宁等中的一种或几种;
B.5)二羧酰亚胺类杀菌剂,选自但不仅限于腐霉利、异菌脲、乙烯菌核利、克菌丹、菌核净、甲基立枯磷等中的一种或几种;
B.6)氨基甲酸酯类杀菌剂,选自但不仅限于霜霉威盐酸盐、乙霉威、苯菌灵、多菌灵、甲基硫菌灵、缬霉威、苯噻菌胺、缬菌胺Valifenalate等中的一种或几种;
B.7)抗菌素类杀菌剂或抗病毒药,选自但不仅限于井冈霉素、硫酸链霉素、春雷霉素、梧宁霉素、申嗪霉素、多抗霉素、宁南霉素、硫酸链霉素、中生菌素、农抗120、金核霉素、长川霉素、四霉素等中的一种或几种;
B.8)噁唑类杀菌剂,选自但不仅限于恶霜灵、恶霉灵、噁唑菌酮、啶菌噁唑、氟噻唑吡乙酮、苄氟噁唑砜、二氯噁菌唑和甲磺酰菌唑等中的一种或几种;
B.9)吗啉类杀菌剂或抗病毒药,选自但不仅限于十三吗啉、烯酰吗啉、氟吗啉、盐酸吗啉胍等中的一种或几种;
B.10)嘧啶类杀菌剂,选自但不仅限于嘧菌环胺、嘧霉胺、乙嘧酚、嘧菌胺、氟嘧菌胺、双苯菌胺、SYP-3773、SYP-3810等中的一种或几种;
B.11)喹啉类杀菌剂,选自但不仅限于二氰蒽醌、丙氧喹啉、苯氧喹啉、喹诺氟美林(Quinofumelin)等中的一种或几种;
B.12)二硫代氨基甲酸盐类杀菌剂或抗病毒药,选自但不仅限于代森联、福美双、福美锌、代森铵、代森锌、代森锰、代森锰锌、丙森锌等中的一种或几种;
B.13)其他杀菌剂或抗病毒药或植物生长调节剂,选自但不仅限于敌瘟磷、三乙膦酸铝、百菌清、稻瘟灵、咯菌腈或者氢氧化铜、松脂酸铜、去氢松脂酸铜、拌种咯、氟咯菌氰、异长乙烯酮肟内酰胺、蛇床子素、毒氟磷、酚菌酮、甲噻诱胺、聚六亚甲基双胍盐酸盐、溴菌腈、吲唑磺菌胺、王铜、壬菌铜、喹啉铜、盐酸吗啉胍、琥胶肥酸铜、辛菌胺醋酸盐、氨基寡糖素、香菇多糖、噻霉酮、乙蒜素、烯丙苯噻唑、双氯氰菌胺、大黄素甲醚、大黄酚、氟唑活化酯、S-诱抗素、氨基寡糖素、吡啶硫酸锌、小檗碱及药学可接受的盐(譬如盐酸小檗碱、硫酸氢小檗碱、硫酸小檗碱等)、丁子香酚、硫磺、硫酸铜、五水硫酸铜、王铜、氧化铜、碱式硫酸铜、叶枯唑、异长叶烯酮肟内酰胺、大蒜素、愈创木酚、Quinolactacide、脱氢乙酸、氯溴异氰尿酸、香芹酚、塞唑锌及其水合物、辛唑嘧菌胺、Pyribencarb、Flutianil(OK-5203)、Meptyldinocap、Pyriofenone、Fenpyrazamine、Tolprocarb、Isofetamid、Isopyrazam、Penflufen、Benzovindiflupyr(SYN545192)、Tebufloquin、Oxathiapiprolin、螺环菌胺、螺嘧环胺、乙膦铝、异稻瘟净、苦参碱、苦参素、噻菌铜或其水合物、噻森铜或其水合物、苯菌酮、氟唑菌酰羟胺(pydiflumetofen)、咪鲜胺、咪鲜胺锰络合物、咪鲜胺铜络合物、茉莉酸甲酯等中的一种;或植物生长调节剂选自但不仅限于胺鲜酯、氯吡苯脲、复硝酚钠、芸苔素、赤霉素、6-苄基氨基嘌呤、三十烷醇、萘乙酸或其药用盐、多效唑、乙烯利、萘乙酸甲酯、氟节酸、抗倒酯、烯效唑、吲哚丁酸、吡啶醇、抗倒胺、矮健素、矮壮素、芸苔素内脂、增产灵、增甘磷等中的一种或几种;
杀虫剂选自但不仅限于定虫隆、伏虫隆、杀虫隆、氟虫脲、氟铃脲、氟螨脲、氟幼脲、氟啶脲、灭幼脲、除虫脲、丁醚脲、抑食肼、噻嗪酮、双氧威、或虫酰肼、杀螟磷、敌百虫、甲基对硫磷、氯唑磷、哒嗪硫磷、喹硫磷、三唑磷、噻唑硫磷、二嗪磷、辛硫磷、杀螟硫磷、甲基嘧啶磷、倍硫磷、杀螟腈、丙溴磷、毒死蜱、甲基毒死蜱、丙硫磷、甲丙硫磷、乐果、马拉硫磷、杀扑磷、丁硫克百威、丙硫克百威、戊氰威、仲丁威、异丙威、唑蚜威、抗蚜威、速灭威、混灭威、甲萘威、灭虫威、灭多威、或硫双灭多威、三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、甲氰菊酯、氰戊菊酯、氯氰菊酯、高效氯氰菊酯、溴氰菊酯、四溴菊酯、醚菊酯、或戊菊酯、阿维菌素、甲氨基阿维菌素、伊维菌素或其药学上可接受的盐等中的任意一种或几种(活性成分B选自但不仅限于文献A、C、D、E、G中杀虫剂或杀螨剂等,文献A:刘长令,柴宝山主编,《新农药创制与合成》,化学工业出版社,2013年,北京;文献C:郑桂玲,孙家隆,《现代农药应用技术丛书∶杀虫剂卷》,化学工业出版社,2017年,北京;D:孙家隆,《现代农药合成技术》,化学工业出版社出版,2011年,北京;E:现代农药手册,刘长令,杨吉春,化学工业出版社,2018年,北京;文献G:刘长令编《世界农药大全:杀虫剂卷》,化学工业出版社,北京,2012;)。
所述的噻唑锰锌新化合物的组合物,其含有活性成分A和任意一种活性成分活性成分B选自但不仅限于嘧菌酯、醚菌酯、吡唑醚菌酯、烯肟菌酯、肟菌酯、唑菌酯、氟嘧菌酯、苯醚菌酯、烯肟菌胺或苯氧菌胺、氰烯菌酯、Picarbutrazox、肟醚菌胺、唑菌胺酯、丁香菌酯、氯啶菌酯、UBF307、KZ165、苯醚甲环唑、烯唑醇、氟环唑、腈苯唑、氟硅唑、粉唑醇、戊唑醇、腈菌唑、环丙唑醇、戊菌唑、丙环唑、四氟醚唑、三唑醇、联苯三唑醇、三唑酮、叶菌唑、种菌唑、丙硫菌唑、亚胺菌唑、灭菌唑、环丙唑醇、甲霜灵、氟酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌酰胺、氟醚菌酰胺、氰霜唑、氟菌唑、高效抑霉唑、咪唑菌酮、噁咪唑、稻温酯、腐霉利、异菌脲、乙烯菌核利、克菌丹、菌核净、霜霉威盐酸盐、苯菌灵、多菌灵、甲基硫菌灵、缬霉威、苯噻菌胺、井冈霉素、硫酸链霉素、春雷霉素、申嗪霉素、恶霜灵、恶霉灵、噁唑菌酮、啶菌噁唑、十三吗啉、烯酰吗啉、氟吗啉、嘧菌环胺、嘧霉胺、乙嘧酚、嘧菌胺、氟嘧菌胺、二氰蒽醌、丙氧喹啉、苯氧喹啉、代森联、福美双、福美锌、代森铵、代森锌、代森锰、代森锰锌、丙森锌、敌瘟磷、三乙膦酸铝、百菌清、稻瘟灵、咯菌腈或者氢氧化铜、松脂酸铜、去氢松脂酸铜、拌种咯、氟咯菌氰、咪鲜胺、咪鲜胺锰络合物、咪鲜胺铜络合物、蛇床子素、双苯菌胺、井冈霉素、硫酸链霉素、春雷霉素、梧宁霉素、申嗪霉素、多抗霉素、宁南霉素、硫酸链霉素、中生霉素、农抗120、金核霉素、长川霉素、春日霉素、毒氟磷、酚菌酮、丙硫咪唑、苯硫咪唑、氯氟醚菌唑(甲芬三氟康唑,mefentrifluconazole)、异丙芬三氟康唑(ipfentrifluconazole)、氟噻唑吡乙酮、烯丙苯噻唑、大黄素甲醚、大黄酚、氟噻唑吡乙酮、烯丙苯噻唑、双氯氰菌胺、香豆素、大黄素甲醚、大黄酚、氟唑活化酯、二氯噁菌唑和甲磺酰菌唑、S-诱抗素、氨基寡糖素、吡啶硫酸锌、小檗碱、盐酸小檗碱、硫酸氢小檗碱、硫酸小檗碱、灭菌丹、异长叶烯酮肟内酰胺、大蒜素、愈创木酚、Quinolactacide、脱氢乙酸、氯溴异氰尿酸、香芹酚、噻氟菌胺、噻酰菌胺、噻唑菌胺、硅噻菌胺、呋吡菌胺、环氟菌胺、氟吡菌胺、苯酰菌胺、环酰菌胺、环丙酰菌胺、磺菌胺、甲磺菌胺、引唑磺菌胺、稻温酰胺、Bixafen、Fluxapyroxad、Sedaxane、辛唑嘧菌胺、Pyribencarb、Flutianil、Meptyldinocap、Pyriofenone、Fenpyrazamine、缬菌胺Valifenalate、Tolprocarb、Isofetamid、Isopyrazam、Penflufen、苯并烯氟菌唑(Benzovindiflupyr)、Tebufloquin、Oxathiapiprolin、糠菌唑、腈苯唑、氟喹唑、螺环菌胺、螺嘧环胺、乙膦铝、甲基立枯磷、异稻瘟净、精甲霜灵、高效苯霜灵、苦参碱、苦参素、噻菌铜或其水合物、噻森铜或其水合物、塞唑锌、塞唑锌水合物、噻菌铜、噻菌铜水合物、苯菌酮、氟唑菌酰羟胺、茉莉酸甲酯、呋醚唑、戊环唑、乙环唑、三氟苯唑、高效烯唑醇、三唑酮、噻菌灵、抑霉唑、麦穗宁或植物生长调节剂等或其药学上可接受的盐或溶剂化合物、定虫隆、伏虫隆、杀虫隆、氟虫脲、氟铃脲、氟螨脲、氟幼脲、氟啶脲、灭幼脲、除虫脲、丁醚脲、抑食肼、噻嗪酮、双氧威、或虫酰肼、杀螟磷、敌百虫、甲基对硫磷、氯唑磷、哒嗪硫磷、喹硫磷、三唑磷、噻唑硫磷、二嗪磷、辛硫磷、杀螟硫磷、甲基嘧啶磷、倍硫磷、杀螟腈、丙溴磷、毒死蜱、甲基毒死蜱、丙硫磷、甲丙硫磷、乐果、马拉硫磷、杀扑磷、丁硫克百威、丙硫克百威、戊氰威、仲丁威、异丙威、唑蚜威、抗蚜威、速灭威、混灭威、甲萘威、灭虫威、灭多威、或硫双灭多威、三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、甲氰菊酯、氰戊菊酯、氯氰菊酯、高效氯氰菊酯、溴氰菊酯、四溴菊酯、醚菊酯、或戊菊酯、阿维菌素、甲氨基阿维菌素、伊维菌素或其药学上可接受的盐等中的任意一种或几种中的任意一种或几种,活性成分A与活性成分B重量比较优选为1∶80~80∶1,更较优选重量为1∶60~60∶1。
所述的噻唑锰锌新化合物,用于制备含有噻唑锰锌新化合物的药物组合物,该新化合物或其组合物与药学上可接受的载体制成药学上可接受的制剂选自但不仅限于干悬浮剂、干混悬剂、可湿性粉剂、粉剂、颗粒剂、分散粒剂、片剂、泡腾片、微囊剂、水分散粒剂、悬浮剂、悬乳剂、水乳剂、微乳剂、乳油、控释或缓释制剂(缓释或控释片、或缓释或控释胶囊、或缓释或控释微丸、或缓释或控释颗粒)、微胶囊制剂、油悬浮剂、可分散液剂(DC)、种子处理干粉剂、种子处理可分散粉剂、颗粒剂、分散粒剂、微囊悬浮剂、种子处理悬浮剂、种子处理微囊悬浮剂或者悬浮种衣剂等。
所述的组合物制剂中,药学上可接受的载体选自但不仅限于湿润剂、粘合剂、分散剂、增稠剂、防冻剂、防腐剂、崩解剂、稳定剂、成膜剂、消泡剂、着色剂、润滑剂或助流剂、填料和/或水等中的一种或几种。
所述的噻唑锰锌新化合物或其药物组合物的用途,为用于制备防治农作物上病害和促进作物生长发育的药物中的应用。
所述的病害选自但不仅限于:溃疡病、条斑病、锈病、颖枯病、网斑病、白粉病、霜霉病、疫病、叶斑病、全蚀病、雪霉病、黑穗病、叶枯病、褐斑病或稻瘟病、或缺锌或缺锰引起的病害中等的一种或几种。白菜:软腐细菌性病害,黑斑病、炭疽病、锈病、白粉病、缺锌老化叶;花生:花生青枯病、死棵烂根病、花生叶斑病;水稻:僵苗、黄秧烂秧、细菌性条斑病、白叶枯病、纹枯病、稻瘟病、缺锌火烧苗;黄瓜:细菌性角斑病、溃疡病、霜霉病、靶标病、黄点病、缺锌黄化叶;可钝化病毒;番茄:细菌性溃疡病、晚疫病、褐斑病、炭疽病、小叶病,钝化病毒;缺锌或缺锰的作物;发病初期,稀释100-800倍液喷雾。发病严重加大(减小)稀释倍数。间隔5-12天左右连续防治2-3次。
噻唑锰锌新化合物的作用机理独特,噻唑锰锌杀菌机理中,既有噻唑基团对细菌的独特防效(噻唑基团在植物体内是高效的治疗剂),又有锌离子对真菌、细菌的优良防治作用,同时内吸性能好,具有良好治疗和保护的双重作用。经药效持久力测定,20%噻唑锰锌新化合物的混悬剂在通常用量下,持效期可达10~14天。
本发明杀菌组合物协同增效效应非常显著。根据噻唑锰锌新化合物组分A与组分B杀菌组合物杀菌作用大于噻唑锰锌新化合物组分A与组分B杀菌作用总和之事实,所述本发明杀菌组合物协同增效作用是明显的。
组分B为式B.1)丙烯酸酯类杀菌剂或抗病毒药时,I∶B质量比选自但不仅限于5∶50~80∶1,优选质量比为20∶30~40∶5。
组分B为式B.2)三唑类杀菌剂时,A∶B质量比选自但不仅限于5∶50~80∶1,优选质量比为20∶20~40∶5。
组分B为式B.3)酰胺类杀菌剂时,A∶B质量比选自但不仅限于5∶40~80∶1,优选质量比为20∶20~40∶5。
组分B为式B.4)咪唑类杀菌剂时,A∶B质量比选自但不仅限于5∶60~80∶1,优选质量比为20∶30~40∶10。
组分B为式B.5)二羧酰亚胺类杀菌剂时,A∶B质量比选自但不仅限于5∶60~80∶1,优选质量比为20∶50~40∶10。
组分B为式B.6)氨基甲酸酯类杀菌剂时,A∶B质量比选自但不仅限于5∶80~80∶5,优选质量比为20∶60~40∶10。
组分B为式B.7)抗菌素类杀菌剂或抗病毒药时,A∶B质量比选自但不仅限于5∶80~80∶1,优选质量比为20∶70~40∶2。
组分B为式B.8)噁唑类杀菌剂时,A∶B质量比选自但不仅限于5∶60~80∶5,优选质量比为20∶50~40∶10。
组分B为式B.9)吗啉类杀菌剂或抗病毒药时,A∶B质量比选自但不仅限于5∶80~80∶5,优选质量比为20∶50~40∶10。
组分B为式B.10)嘧啶类杀菌剂时,A∶B质量比选自但不仅限于5∶60~80∶10,优选质量比为20∶50~40∶10。
组分B为式B.11)喹(唑)啉(酮)类杀菌剂时,A∶B质量比选自但不仅限于5∶60~80∶10,优选质量比为20∶50~40∶10。
组分B为式B.12)二硫代氨基甲酸盐类杀菌剂或抗病毒药时,A∶B质量比选自但不仅限于5∶80~80∶10,优选质量比为20∶50~40∶10。
组分B为式B.13)其他类杀菌剂或抗病毒药或植物生长调节剂时,A∶B质量比选自但不仅限于5∶80~80∶1,优选质量比为20∶50~50∶10。
本发明的新化合物或其杀菌组合物有较好的杀菌活性或抗病毒活性,对病原细菌和真菌有效,例如选自但不仅限于用于防治下列病菌:病原细菌中的黄单胞菌属(Xanthomonas)、假单胞菌属(Pseudomonas)、欧氏杆菌属(Erwinia);病原真菌中的子囊菌纲(Ascomycetes):黑星菌属(Venturia)、白粉菌属(Erysiphe)、核盘菌属(Sclerotinia);病原真菌中的担子菌纲(Basidiomycetes):黑粉菌属(Ustilago)、赤霉属(Gibberella);病原真菌中的卵菌纲(Oomycota):疫霉属(Phytophthora)、单轴霉属(Plasmopara);病原真菌中的半知菌类(Deuteromyces):丝核菌属(Rhizoctonia)、葡萄孢属(Botrytis)、梨孢属(Pyricularia)、尾孢属(Cercospora)、离蠕孢属(Bipolaris)、炭疽菌属(Colletotrichum)等。
本发明的新化合物或其杀菌组合物选自但不仅限于用于防治植物或农作物青枯病、细菌性角斑病、软腐病、溃疡病、炭疽病、霜霉病、疫病、稻瘟病、稻曲病、纹枯病、恶苗病、白粉病、锈病、叶枯病、灰霉病、叶斑病、斑点落叶病、黑痘病、黑穗病、枯萎病、黑斑病、黑星病、轮纹病、褐斑病、根腐病、菌核病、枯萎病或疮痂病。
在本发明范围内,这里公开所指的植物或农作物优选或选自但不仅限于以下种类:禾谷类小麦、大麦、水稻、玉米、高梁、甘薯等;果树类苹果、梨、桃、山核桃、核桃、柑橘、葡萄、荔枝、香蕉、桂圆、芒果、枇杷;蔬菜类黄瓜、西瓜、吊瓜、丝瓜、甜瓜、菠菜、芹菜、番茄、辣椒、茄子、姜、葱、蒜、韭菜、甘蓝、大白菜、草莓、莴笋、菜豆、豇豆、蚕豆、萝卜、胡萝卜、马铃薯、山药、芋、莲藕、荸荠、茭白等;糖料植物类甜菜、甘蔗等;油料作物类大豆、花生、油菜、芝麻、向日葵等;或诸如烟草、茶、可可豆、棉花等、或缺锌或缺锰的作物。这种列举并不表示具有任何限制。
本发明的新化合物或其组合物还可用于保护工业材料不受病菌侵害的领域的药物,这些工业领域包括或选自但不仅限于木材、纸张、皮革、建筑物等,本发明组合物可以防止诸如腐烂、变色或发霉之类不良作用。
本发明的新化合物或其组合物对下列植物病害有效,选自但不仅限于下列病害:
假单胞菌属(Pseudomonas)菌种引起的黄瓜细菌性角斑病、烟草野火病、茄科青枯病等;黄单胞菌属(Xanthomonas)菌种引起的黄瓜细菌性叶枯病、甘蓝黑腐病、柑橘溃疡病等;欧氏杆菌属(Erwinia)菌种引起的大白菜软腐病、梨火疫病等;
疫霉属(Pyhtophthora)菌种引起的马铃薯、番茄的疫病等;单轴霉属(Plasmopara)菌种引起的葡萄霜霉病等;白粉菌属(Erysiphe)菌种引起的烟草、芝麻、向日葵及瓜类等白粉病等;赤霉属(Gibberella)菌种引起的大、小麦及玉米等多种禾本科植物赤霉病、水稻恶苗病;黑星菌属(Venturia)菌种引起的苹果的黑星病等;核盘菌属(Sclerotinia)菌种引起的多种植物菌核病等;黑粉菌属(Ustil-ago)菌种引起的小麦散黑粉病等;葡萄孢属(Botrytis)菌种引起的多种植物的灰霉病等;梨孢属(Pyricularia)菌种引起的稻瘟病等;尾孢属(Cercospora)菌种引起的甜菜褐斑病、花生褐斑病等;离蠕孢属(Bipolaris)菌种引起的玉米小斑病、水稻胡麻叶斑等病;丝核菌属(Rhi-zoctonia)菌种引起的棉花立枯病和水稻纹枯病等;炭疽菌属(Colletotrichum)菌种引起的苹果、梨、棉花、葡萄、冬瓜、黄瓜、辣椒、茄子等多种果树和蔬菜的炭疽病等;霜霉菌引起的葡萄霜霉病等;劳尔氏杆菌属菌种引起的番茄或花生青枯病等;棒形杆菌属菌种引起的番茄溃疡病等。
另外令人特别感兴趣的是,对植物或种子处于不利的生长环境或受到伤害时,施用本发明化合物或其组合物对植物或种子抵抗逆境能力有非常显著的改善,例如恢复生长、叶片嫩绿、促进根系生长等,植物在防治植物病害所需要的浓度时对活性化合物组合物具有良好的耐受性的事实,允许处理植物的地上部分的花和果以及种子。术语“逆境”包括不适合的湿度、冰雹、干旱、低温、多雨等。
本发明的杀菌组合物使用的方法包括对要处理的植物或其生长场所、或种子、或材料,以混合施用总有效活性杀菌量的式A和式B活性化合物。可在真菌侵染材料、植物或种子之前或之后施用。
所述式A为本发明的噻唑锰锌新化合物,式B为选自前述B.1)-B.13)中任意一种或几种的杀菌或抗病毒药或植物生长调节剂活性化合物。
本文所用术语“生长场所”包括生长处理植物、或播种栽培植物种子的田地,或种子埋置于土壤中的场所。术语“种子”包括植物繁殖材料如扦条、幼苗、种子、发芽或浸泡的种子。
本发明的新化合物或其组合物可以制备成农业或农药上可以接受的固体状或液体状制剂。新化合物或组合物可通过混合活性成分A和B与药学上可接受的或农药学可接受的辅料或辅助成分用已知的方法制备。其制剂选自但不仅限于干悬浮剂、可湿性粉剂、粉剂、颗粒剂、分散粒剂、片剂、泡腾片、微囊剂、水分散粒剂、悬浮剂、悬乳剂、水乳剂、控释或缓释制剂、微胶囊制剂、油悬浮剂、可分散液剂(DC)、种子处理干粉剂、种子处理可分散粉剂、颗粒剂、分散粒剂、微囊悬浮剂、种子处理悬浮剂、种子处理微囊悬浮剂或者悬浮种衣剂等。
本发明的新化合物或其组合物所述药学上可接受的或农药学可接受的辅料或辅助成分选自但不仅限于湿润剂、粘合剂、分散剂、增稠剂、防冻剂、防腐剂、崩解剂、稳定剂、增效剂、成膜剂、消泡剂、着色剂、润滑剂或助流剂、乳化剂、pH值调节剂、填料和/或水等及其它有益于有效成分在制剂中稳定或活性化合物发挥的已知物质,都是制备中常用或农业上农药学上可接受的各种成分,并无特别限定,具体成分和用量根据需要通过试验确定。
所述的湿润剂选自但不仅限于EO/PO嵌段聚醚、脂肪醇聚氧乙烯醚、脂肪醇乙氧基化合物、牛油脂乙氧基铵盐、烷基萘磺酸盐、烷基萘磺酸钠、烷基萘磺酸钙、脂肪醇聚氧乙烯醚硫酸盐、酰基谷胺酸盐等药学上可接受的中的一种或几种。
所述分散剂选自但不仅限于萘磺酸缩合物钠盐、苯酚磺酸缩合物钠盐、甲基萘磺酸钠甲醛缩合物、木质素磺酸钠、亚甲基二萘磺酸钠、丙烯酸均聚物钠盐、聚羧酸盐分散剂、二辛基磺基琥珀酸钠盐、EO/PO嵌段聚醚、马来酸-丙烯酸共聚物钠盐、达润D06、达润DCM-82等药学上可接受的中的一种或几种;
其中,聚羧酸盐分散剂选自但不仅限于:国外公司产品:1)Solvay(索尔维)公司(原罗地亚公司)的Geropon T/36和GeroponT/72(聚羧酸盐);2)Huntsman(亨斯曼)公司的Tersperse2700(聚丙烯酸接枝共聚物)、Tersperse2735(聚丙烯酸接枝共聚物,液体)和Tersperse2100;3)日本Takemoto(竹本油脂会社)的YUS-WG5(聚羧酸酯)、CH7000(白色液体)、YUS-WG5、YUS-WP1。4)Croda(禾大)公司的Atlox 4913(甲基丙烯酸/甲基丙烯酸酯甲酯与聚氧乙烯的共聚物)和Atlox Metasperse 550S(改性的丙烯酸-苯乙烯共聚物)。5)BASF(巴斯夫)公司的Sokalan PA15/20(丙烯酸均聚物钠盐)、Sokalan CP 5(丙烯酸-马来酸共聚物钠盐)、Sokalan HP 25(改性聚羧酸盐)和Sokalan PA80S(聚丙烯酸)。6)Clariant(科莱恩)公司的DispersogenPSL 100(聚丙烯酸酯接枝共聚物)。7)AkzoNobel(阿克苏诺贝尔)公司的Agrilan700(改性聚丙烯酸酯共聚物)。8)Lamberti(宁柏迪)公司的EmulsonAG TP1(聚羧酸盐类,白色乳状液体)、Emulson AG TRN 14105(聚羧酸盐类梳型结构)。9)Tanatex(拓纳)化学公司的D1001(聚羧酸盐)。10)陶氏公司的DURAMAXM D-205(液体)、D-305(液体)、D-518(聚羧酸盐)。国内公司产品:1)北京广源公司:GY-D(D03-D08)系列产品(苯乙烯磺酸盐聚合物的聚羧酸盐)。2)北京汉莫克化学技术公司:D1001、D1002、D1003(聚羧酸盐)。3)北京理工大学LG-3(聚羧酸盐)。4)上海是大高分子材料有限公司:SD-816、SD-817、SD-818、SD-819(聚羧酸盐)。5)江苏擎宇化工科技公司:SP-2728、SP-2750、SP-2836(聚羧酸盐)。6)北京格林泰姆(Gree-times)助剂公司:Greesperse BD55、BD58、BE13(液体)(聚羧酸盐)等药学上可接受的中的一种或几种。
所述的乳化剂选自但不仅限于十二烷基苯磺酸钠、十二烷基苯磺酸钙、脂肪醇磷酸酯钾酯、烷基酚聚氧乙烯醚磷酸盐、脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、聚氧乙烯醚失水山梨醇脂肪酸酯、丙二醇聚氧乙烯聚氧丙烯醚嵌段共聚物、司盘或斯盘系列(譬如斯盘-40、斯盘-60、斯盘-80等)、吐温系列(譬如吐温-40、吐温-60、吐温-80等)、农乳700#、农乳2201#、TX-10、农乳1601(通用名:苯乙基苯酚聚氧乙烯聚氧丙烯醚)、农乳600#、农乳400#等药学上可接受的中的一种或几种;
所述增稠剂选自但不仅限于果胶、阿拉伯胶、西黄蓍胶、黄原胶、海藻酸钠、硅酸铝镁、羧甲基纤维素钠、羧甲基纤维素钠钙、淀粉磷酸酯钠、辛烯基琥珀酸淀粉钠、聚乙烯醇、交联羧甲基纤维素、交联聚乙烯吡咯烷酮、聚乙烯吡咯烷酮、低取代羟丙基纤维素、聚乙二醇800-20000、甲基纤维素、乙基纤维素、羟丙基纤维素、PEG-80甘油基牛油酯、PEC-8PPG(聚丙二醇)-3二异硬脂酸酯、PEG-200氢化甘油基棕榈酸酯、PEG-n(n=6、8、12)蜂蜡、PEG-4异硬脂酸酯、PEG-n(n=3、4、8、150)二硬脂酸酯、PEG-18甘油基油酸酯/椰油酸酯、PEG-8二油酸酯、PEG-200甘油基硬脂酸酯、PEG-n(n=28、200)甘油基牛油酯、PEG-7氢化蓖麻油、PEG-40霍霍巴油、PEG-2月桂酸酯、PEG-120甲基葡萄糖二油酸酯、PEG-150季戊四硬脂酸酯、PEG-55丙二醇油酸酯、PEG-160山梨聚糖三异硬脂酸酯、PEG-n(n=8、75、100)硬脂酸酯、PEG-150/癸基/SMDI共聚物(聚乙二醇-150/癸基/甲基丙烯酸酯共聚物)、PEG-150/硬脂基/SMDI共聚物、PEG-90。异硬脂酸酯、PEG-8PPG-3二月桂酸酯、鲸蜡豆蔻酯、鲸蜡棕榈酯、C18-36酸乙二醇酯、季戊四硬脂酸酯、季戊四山嵛酸酯、丙二醇硬脂酸酯、山嵛酯、鲸蜡酯、三山嵛酸甘油酯、三羟基硬脂酸甘油酯等药学上可接受的中的一种或几种。
所述溶剂选自但不仅限于甲苯、二甲苯、三甲苯、环己酮、N-甲基吡咯烷酮、溶剂油(牌号S-150、S-180、S-200)、生物柴油、甲酯化植物油、油酸甲酯、脂肪酸甲酯、大豆油、松脂基植物油、甲醇、乙醇、异丙醇、正丁醇、醋酸仲丁酯、乙二醇单乙醚、水等中的一种或几种;水为去离子水或蒸馏水或纯水等。
所述防冻剂选自乙二醇、丙二醇、丙三醇、聚乙二醇100-2000、异丙醇、尿素、无机盐类如氯化钠等药学上可接受的中的一种或几种。
所述成膜剂选自但不仅限于聚乙烯醇、聚醋酸乙烯酯、聚乙烯乙二醇聚甲基丙烯酸乙二醇酯、羧甲基纤维素、阿拉伯树胶、黄原胶、淀粉、聚乙二醇2000-20000等具有粘结性和成膜性的高分子聚合物等药学上可接受的中的一种或几种。
所述崩解剂选自但不仅限于尿素、蔗糖、葡萄糖、氯化钠、硫酸铵、硫酸钠、可溶性淀粉、淀粉、变性淀粉、微晶纤维素、交联羧甲基纤维素、羧甲基淀粉钠、交联聚乙烯吡咯烷酮、低取代羟丙基纤维素、表面活性剂(十二烷基硫酸钠等)等药学上可接受的中的一种或几种。
所述防腐剂选自但不仅限于甲醛、水杨酸苯酯、对羟基苯甲酸丁酯、尼泊金甲酯、尼泊金乙酯、尼泊金丙酯、山梨酸钾、苯甲酸、苯甲酸钠等药学上可接受的中的一种或几种。
所述稳定剂选自但不仅限于甘油、环氧大豆油、环氧氯丙烷、亚磷酸三苯酯、缩水甘油醚或季戊四醇、木糖醇、2,6-二叔丁基-4-甲基苯酚、聚乙二醇400-20000、EDTA二钠、EDTA二钠2水合物、EDTA钙钠4水合物、山梨醇、羧甲基纤维素钠、离子型表面活性剂或非离子型表面活性剂、羟乙基或丙基纤维素、聚乙烯醇、司盘系列、吐温系列、海藻酸盐系列等药学上可接受的中的一种或几种。
所述消泡剂选自但不仅限于有机硅类消泡剂(包括但不仅限于AFE-316、TanafoamSLX、Tanaform S、Tanaform AF等)、聚醚消泡剂、聚醚改性有机硅消泡剂(包括但不仅限于DF-825、DF-281、DT-650、DM-115M、DM-193、DM198、DM-M1040、DM-1090、DM-DA1952、LM-110、JH-935)、N型消泡剂、蔗糖脂肪酸酯类消泡剂、脂肪醇类消泡剂、复合型消泡剂等药学上可接受中的一种或多种。
药学上可接受的pH调节剂可以是药学上可接受的无机酸或有机酸、无机碱或有机碱,也可以是广义的路易斯酸或碱,可以含有一种或者几种,选自但不仅限于盐酸、磷酸、丙酸、醋酸及醋酸盐、乳酸以及乳酸药用盐、枸橼酸药用盐、碳酸钠、碳酸氢钠、碳酸氢钾、氢氧化钠、氢氧化钾、磷酸盐、酒石酸及其药用盐、硼砂、硼酸、多羟基羧酸及药用盐,如葡萄糖醛酸、葡萄糖酸、乳糖酸、苹果酸、苏糖酸、葡庚糖酸、氨水、三乙醇胺、三乙胺和二乙烯三胺等中的一种或者几种。
所述着色剂选自但不仅限于氧化铁、氧化钛、偶氮染料等药学上可接受的中的一种或几种。
所述填料选自但不仅限于硫酸钠、硫酸铵、尿素、蔗糖、葡萄糖、硅藻土、滑石粉、膨润土、凹凸棒土、高岭土、轻质碳酸钙、白炭黑、淀粉、变性淀粉、微晶纤维素、环糊精、山梨醇、甘露醇、磷酸钙等药学上可接受的中的一种或几种;
所述药学上可接受的润湿剂和粘合剂,选自但不仅限于淀粉、胶化淀粉、甲基纤维素、羧甲基纤维素钠、乙基纤维素、低取代羟丙基纤维素、聚乙烯吡咯烷酮、PVP K-30、西黄蓍胶、海藻酸及其盐等中的一种或几种;
所述药学上可接受的润滑剂和助流剂,选自但不仅限于硬脂酸、硬脂酸镁、聚乙二醇4000-20000、滑石粉、微粉硅胶、十二烷基硫酸镁等药学上可接受的中的一种或几种;
对可湿性粉剂,可使用的助剂选自但不仅限于:分散剂、润湿剂、填料同本发明前所描述等药学上可接受的中一种或多种。
对于水分散粒剂来说,选自但不仅限于,分散剂、润湿剂、崩解剂、粘结剂、稳定剂、填料等选自但不仅限于同本发明前所描述中的一种或多种。
对悬浮剂,可使用的助剂选自但不仅限于:分散剂、乳化剂、润湿剂、增稠剂、防腐剂、消泡剂、稳定剂、防冻剂等同本发明前所描述中的一种或多种。
对悬浮种衣剂,可使用的助剂选自但不仅限于:粘结剂如选自但不仅限于多糖类高分子化合物(可溶性淀粉、聚丙烯接枝共聚物、黄原酸胶、微生物粘质物)、纤维素衍生物(羟丙基甲基纤维素、羧甲基纤维素钠、乙基纤维素)、海藻类如海藻酸钠、琼脂,松香、石蜡、明胶、果胶,聚乙烯醇、聚乙二醇、聚醋酸乙烯酯、聚丙烯酰胺、聚乙烯吡咯烷酮及多元醇聚合物水溶性合成品,无机粘结剂(硅酸镁铝、粘土、水玻璃、石膏)中一种或多种;分散剂、乳化剂、润湿剂、增稠剂、防腐剂、消泡剂、稳定剂、防冻剂等同本发明前所描述。
本发明所描述的活性化合物组合物的制剂或药剂可以用通用方法制备。
本发明组合物用于防治植物病害的制剂一般包括1~90质量百分比的活性化合物,优选20~60质量百分比。
本发明的杀菌组合物可以以其本身浓缩物形式或以一般的常规制剂形式使用,根据靶标病害的性质不同采用浇灌、喷雾、弥雾、拌种、撒施或涂刷方法,其施用总有效活性杀菌量随天气条件、作物状态或施用方法而变化。
本发明杀菌活性化合物组合物有非常突出的优点:
1.本发明杀菌组合物协同增效明显,可充分发挥噻唑锰锌新化合物对细菌性病害高效,对真菌性病害普遍有效的特点及其良好的保护性能;
2.本发明杀菌组合物可由不同作用机制的有效成分组成,可有效减缓病害的抗性产生,降低噻唑锰锌新化合物或其它任意已知活性化合物单独使用带来的抗性风险;3.本发明杀菌组合物不仅可提高抗菌或抑菌的效果,也扩大防病谱,能同时对作物发生的细菌性病害和部分真菌性病害起到很好的预防或治疗效果,减少用药次数,减轻环境压力,从而起到预防为主、综合防治的效果;
4.本发明杀菌组合物通过复配减少了药剂的使用量,减轻农药对环境的压力,同时降低了成本;
5.本发明杀菌组合物可显著改善作物的耐受性,使药剂对作物的安全性更高;
6.本发明杀菌组合物可通补充微量元素,促进植物生长、提高抗逆性和抗病性。
附图说明
图1为噻唑锰锌[C4H4N6S4(Mn)0.5(Zn)0.5]水合物热分析图谱(实施例1-2A)
图2为噻唑锰锌[C4H4N6S4(Mn)0.5(Zn)0.5]水合物红外光谱图(实施例1-2A)
图3为噻唑锰锌[C4H4N6S4(Mn)0.8(Zn)0.2]水合物热分析图谱(实施例1-4A)
图4为噻唑锰锌[C4H4N6S4(Mn)0.8(Zn)0.2]水合物红外光谱图(实施例1-4A)
图5为噻唑锰锌[C4H4N6S4(Mn)0.2(Zn)0.8]水合物热分析图谱(实施例1-6A)
图6为噻唑锰锌[C4H4N6S4(Mn)0.2(Zn)0.8]水合物红外光谱图(实施例1-6A)
图7为噻唑锰锌[C4H4N6S4(Mn)0.2(Zn)0.8]水合物X粉末衍射图(实施例1-6A)
具体实施方式
除了在实施例中以及另有指示时,说明书和权利要求书中所用的所有的数值应被理解为在所有的实例中以术语“约”进行修饰,因此,除非有相反的指示,本说明书和所附的权利要求书中所给出的数值参数是近似值,其可以根据通过本公开内容所寻求的所需要性质而改变,最起码地,并且不是意欲限制等同原则权利要求范围的应用,每个数值参数应考虑有效数字的数和常规四舍五入方法来解释。
虽然设定公开内容的宽范围的数值范围和参数是近似值。但是在具体实施例中所给出的数值被尽可能精确地报道,任意数值本质上包含某些由在它们各自的测试中发现的标准偏差所必然产生的误差。
需要指出的是,除非文中明确地另外说明,在本说明书和附加的权利要求中使用的单数形式“一个”、“一种”以及“该”包括指代物的复数形式,所以,例如。如果提及含有“一种化合物”的组合物时包括两种或多种化合物的混合物,另外需要注意的是,除非本文明确地另外说明,术语“或”通常包括“和/或”。
如本文所用,术语“得到”,或“获得”是指有价值的含量或纯度水平分离得到的化合物,所述的含量和纯度水平包括但不限于大于90%、95%、96%、97%、98%和99%的含量和纯度水平。所述的含量或纯度水平可通过关于的高效液相色谱、LC-MS、火焰原子吸收光谱法等方法测定。采用傅立叶变换红外光谱仪测定样品红外光谱数据,所用仪器包括Nexus智能型傅立叶变换红外光谱仪(Thermo Nicolet)等。
本“溶剂合物”在此处是指还包括渗入到晶体结构中的溶剂分子的分子、原子和/或离子的晶型,溶剂合物的溶剂分子可处于规则排列和/或无序排列,本发明的溶剂合物是溶剂水合物。多晶型在此处是指具有相同的化学组成但形成晶体的分子、原子和/或离子的空间排列不同的晶体。
药物组合物或农药组合物:本文所用“药物组合物或农药组合物”是指药物的组合物或农药的组合物,所述的组合物可以含有至少一种药学上可接受的载体。
本文所用“药学上可接受的赋形剂或载体”是指适用于本文所提供的化合物给药的药用载体或溶媒,其包括本领域技术人员公知的适用于特定给药方式的任何此类载体。
在本发明中,除非有其他说明,其药学上可接受的盐或溶剂合物或其包合物中的“其”代表其中之一或它们的或它们中的任一。
本文所公开的“范围”以下限和上限的形式。可以分别为一个或多个下限,和一个或多个上限。给定范围是通过选定一个下限和一个上限进行限定的。选定的下限和上限限定了特别范围的边界。所有可以这种方式进行限定的范围是包含和可组合的,即任何下限可以与任何上限组合形成一个范围。例如,针对特定参数列出了50-100和80-120的范围,理解为50-100和80-120的范围也是预料到的。此外,如果列出的最小范围值1和2,和如果列出了最大范围值3,4和或5,则下面的范围可全部预料到:1-3、1-4、1-5、2-3、2-4、和或2-5。
在本发明中,除非有其他说明,“适量”代表完成本发明所需要的较佳或最佳的量或质量或重量或体积等。
在本发明中,除非有其他说明,“该组合或其组合”表示所述各元件的多组分混合物,例如两种、三种、四种以及直到最大可能的多组分混合物。
在本发明中,除非有其他说明,所有“份”和百分数(%)可以是指重量份数或重量百分数或重量体积百分数。
在本发明中,除非有其他说明,数值范围“a-b”表示a到b之间的任意实数组合的缩略表示,其中a和b都是实数。例如数值范围“0-10”表示本文中已经全部列出了“0-10”之间的全部实数,“0-10”只是这些数值组合的缩略表示。
在本发明中,除非有其他说明,整数数值范围“a-b”表示a到b之间的任意整数组合的缩略表示,其中a和b都是整数。例如整数数值范围“1-N”表示1、2......N,其中N是整数。
如果没有特别指出,本说明书所用的术语“一种”指“至少一种”。
如果没有特别指出,本发明所述的百分数(包括重量百分数)的基准都是所述组合物的总重量。在本发明中,除非有其他说明,所有组合物中各组分的百分数之和为100%。
为了进一步了解本发明,下面结合实施例对本发明优选实施方案进行描述,但是应当理解,这些描述只是为进一步说明本发明的特征和优点,而不是对本发明权利要求的限制。
水分测定:采用V310S-KHF锂电池材料及电极膜片专用卡氏水分测定仪(四川禾业科技有限公司)测定水分。方法为:将气源连接至加热炉,将干燥样品瓶装入加热槽,温度设置约为178℃,升温速度:30℃/min,干燥氮气流量调整为50ml/min,吹扫样品瓶和管路内可能存在水分,等待再次平衡。取干燥的样品瓶装入约0.1-0.3g的样品,其余按照该仪器说明书规定操作。
红外光谱:溴化钾压片,测定样品红外光谱数据,所使用的仪器包括美国热电公司NICOLET 5700FTIR Spectrometer,Nexus智能型傅立叶变换红外光谱仪(Thermo Nicolet)等。红外光谱仪仪器公司名称:美国热电公司NICOLET 5700FTIR Spectrometer,使用功能:中红外4000-400cm-1,分辨率4cm-1。最高可达0.09cm-1。
热分析方法
测试条件:Setaram公司Setsys 16,样品量3-10mg左右,升温速度:10K/min,N2流速:50ml/min,温度:一般为室温~400℃左右。
令人意外的是,特征性的,本发明的水合物的热分析(TG-DTA或者TG-DSC)图谱的失重平台下具有对应的吸热峰,热分析图谱显示出噻唑锰锌的结晶水合物。
粉末X衍射法
利用D/MX-IIIA X射线衍射仪,电压:约30-60ky,电流:约30-100mA,扫描速度:10°/min,铜靶,波长wavelength(A):1.54,衍射角2θ,扫描范围3-60°,测定了样品的粉末X射线衍射图,全部峰位置在±0.2°2θ内;或利用德国Bruker公司的D8Advance X射线衍射仪,波长:1.54,衍射角2θ,扫描范围3-60°,其它(电压、电流等指标)大约同前,对样品进行测量。本说明书中的各附图与数据互为佐证。在铜靶下有的化合物呈现无定型,有的呈现多晶型。利用粉末X射线衍射法测量,在衍射角2θ(3-60°)测量范围内,本发明的噻唑锰锌水合物(实施例1-6A)可在包括如下2θ±0.2值的位置具有相应的特征值:
具体实施例
实施例1-1A 化合物噻唑锰锌[C4H4N6S4(Mn)0.5(Zn)0.5]的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌溶解,然后加一水硫酸锰(0.015mol)2.535g和七水硫酸锌(0.015mol)4.314g溶于适量水的混合溶液,大量沉淀析出,在30-40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在100℃左右真空干燥5h左右,得棕灰色固体7.1g;熔点大于290℃;红外光谱(νKBr maxcm-1)3372.4,3272.1,3174.6,2938.3,2848.2,2722.8,1612.2,1507.0,1434.2,1345.1,1129.2,1079.7,1056.8,1024.2778.4,756.2,706.1,629.5;含量分析(原子吸收光谱法):Mn8.31%(理论值8.46%),Zn9.87%(理论值10.07%)。
实施例1-2A 化合物噻唑锰锌[C4H4N6S4(Mn)0.5(Zn)0.5]水合物的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌溶解,然后加加一水硫酸锰(0.015mol)2.535g和七水硫酸锌(0.015mol)4.314g溶于适量水的溶液,在30℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.5g;卡氏法测定水分为6.62%;热分析:失重约6.82%(见附图1),在失重下具有对应的吸热峰(DTA)(见附图1);红外光谱(νKBr maxcm-1)(见附图2):3295.8,1609.6,1523.0,1046.1,1365.5,1244.6,1125.0,1045.7,753.1,619.8,534.7;X粉末衍射:以衍射角2θ,在3-60°范围内测定有多个明显的特征峰(粉末X射线衍射,见附图3)约:含量分析(原子吸收光谱法):Mn 7.83%,Zn 9.35%。
实施例1-3A 噻唑锰锌[C4H4N6S4(Mn)0.8(Zn)0.2]化合物的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌溶解,然后加一水硫酸锰(0.024mol)4.056g和七水硫酸锌(0.006mol)1.726g溶于适量水的溶液,在40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.2g;熔点大于280℃;元素分析:理论值:C14.95%,H 1.25%,N 26.15%,S 39.91%;实测值:C 14.82%,H 1.33%,N 26.03%,S39.78%,含量分析(原子吸收光谱法):Mn13.71%(理论值13.67%),Zn4.06%(理论值4.07%)。
实施例1-4A 化合物噻唑锰锌[C4H4N6S4(Mn)0.8(Zn)0.2]水合物的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌溶解,然后加一水硫酸锰(0.024mol)4.056g和七水硫酸锌(0.006mol)1.726g溶于适量水的溶液,在40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.9g;熔点大于280℃;卡氏法测定水分为7.16%,热分析:失重约7.39%(见附图3),在失重下具有对应的吸热峰(DTA);红外光谱(νKBr maxcm-1)(见附图4):3292.7,3172.4,1607,1517.4,1396.5,1349.9,1128.2,1047.7,764.2,704.5,636.9;含量分析(原子吸收光谱法):Mn12.65%,Zn3.76%。
实施例1-5A 噻唑锰锌化合物[C4H4N6S4(Mn)0.2(Zn)0.8]的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钾3.4g溶于适量水的溶液,搅拌溶解,然后加一水硫酸锰(0.006mol)1.014g和七水硫酸锌0.024mol)6.902g溶于适量水的溶液,在40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.2g;熔点大于290℃;元素分析:理论值:C14.66%,H 1.23%,N25.65%,S 39.14%;实测值:C 14.51%,H 1.34%,N 25.52%,S39.01%,含量分析(原子吸收光谱法):Mn3.31%(理论值3.35%),Zn15.88%(理论值15.96%)。
实施例1-6A 噻唑锰锌[C4H4N6S4(Mn)0.2(Zn)0.8]水合物的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌溶解,然后加一水硫酸锰(0.006mol)1.014g和七水硫酸锌(0.024mol)6.902g溶于适量水的溶液,在40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.7g;熔点大于290℃;卡氏法测定水分为1.34%,热分析:失重约1.42%(见附图5),失重下具有对应的吸热峰(DTA)(见附图5);红外光谱(vKBr maxcm-1)(见附图6):3373.5,3277.1,3175.1,3110.2,2938.8,2848.6,2723.6,1612.6,1507.4,1434.3,1345.6,1129.9,1078.2,1055.6,1024.4,998,777.6,756.5,706.7,628.7,503.4;含量分析(原子吸收光谱法):Mn3.28%,Zn15.67%;X粉末衍射:以衍射角2θ,在3-60°范围内测定有多个明显的特征峰(粉末X射线衍射,见附图7)约:11.22,13.32,15.53,17.79,19.17,20.76,21.48,22.59,22.97,24.30,24.98,26.29,26.85,28.04,28.82,30.83,31.33,32.36,33.51,34.04,35.78,36.24,37.68,39.84,43.96,46.24,46.89,47.55,49.19,50.97,51.23,52.68,53.57,55.42。
实施例1-7A 噻唑锰锌化合物[C4H4N6S4(Mn)0.1(Zn)0.9]的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌,然后加氯化锰4水合物(0.003mol)0.594g和七水硫酸锌(0.027mol)7.765g溶于适量水的溶液,在室温搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在100℃左右鼓风干燥4h左右,得棕灰色固体6.8g,熔点大于290℃;元素分析:理论值:C 14.62%,H1.23%,N 25.57%,S 39.02%;实测值:C 14.52%,H 1.32%,N 25.48%,S 39.11%,含量分析(原子吸收光谱法):Mn1.65%(理论值1.67%),Zn17.83%(理论值17.90%)。
实施例2 噻唑锰锌化合物[C4H4N6S4(Mn)0.9(Zn)0.1]的水合物的制备
在室温下,于250ml烧瓶中加2-氨基-5-巯基-1,3,4-噻二唑(0.06mol)7.991g,加水30ml,搅拌,加氢氧化钠2.45g溶于适量水的溶液,搅拌,然后加一水硫酸锰(0.027mol)5.293g和七水硫酸锌(0.003mol)0.863g溶于适量水的溶液,在40℃左右搅拌半个小时,取出放置冷却,抽滤,少量水洗固体至滤液无硫酸根离子,抽滤,所得固体摊薄在50℃左右鼓风干燥4h左右,得棕灰色固体7.3g,熔点大于280℃;卡氏法测定水分为11.12%,热分析:失重约11.47%,失重下具有对应的吸热峰。
实施例3 噻唑锰锌化合物[C4H4N6S4(Mn)0.7(Zn)0.3]、[C4H4N6S4(Mn)0.65(Zn)0.35]、[C4H4N6S4(Mn)0.6(Zn)0.4]、[C4H4N6S4(Mn)0.4(Zn)0.6]、[C4H4N6S4(Mn)0.3(Zn)0.7]等噻唑锰锌化合物或其水合物的制备均可参照实施例1-1A~实施例1-7A或实施例2的中相应的方法合成,其熔点均大于280℃;噻唑锰锌化合物[C4H4N6S4(Mn)0.7(Zn)0.3]、[C4H4N6S4(Mn)0.65(Zn)0.35]、[C4H4N6S4(Mn)0.6(Zn)0.4]、[C4H4N6S4(Mn)0.4(Zn)0.6]、[C4H4N6S4(Mn)0.3(Zn)0.7]水合物的含水量大约2.0~9.0%之间。
实施例4:可湿性粉剂的制备
将50%噻唑锰锌新化合物、萘磺酸缩合物钠盐3.0%、高分子聚羧酸盐5.0%、滑石粉2.0%、轻质碳酸钙5.0%、高岭土至总量为100%充分混合,再通过超细粉碎至800目,得可湿性粉剂。可湿性粉剂中含50%噻唑锰锌新化合物。
实施例5:水分散颗粒剂的制备
将噻唑锰锌新化合物(按无水物重量计)60%、十二烷基苯磺酸钠3%、聚羧酸盐分散剂(SD-819)4%、氯化铵5%、羧甲基淀粉钠5%、甲基纤维素2%、黄原胶0.15%、硫酸钠4%、聚乙烯吡咯烷酮(PVP K-30)4%、聚醚改性有机硅消泡剂(DM-1090)0.1%、微粉硅胶补足100%;纯水适量;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-1090]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-1090用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例6:噻唑锰锌悬浮剂的制备
将噻唑锰锌新化合物(按无水物重量计)20%、牛油脂乙氧基胺盐4.0%、萘磺酸缩合物钠盐1.0%、丙烯酸均聚物钠盐1.0%、黄原胶0.2%、淀粉磷酸酯钠2.5%、丙二醇5.0%、山梨酸钾0.5%、聚醚消泡剂0.5%、蒸馏水补至100%,投入到砂磨机中砂磨120分钟,过滤,即得悬浮剂。
实施例7:噻唑锰锌悬浮剂的制备
将噻唑锰锌新化合物30%(按无水物重量计)、苯乙基酚聚氧乙烯醚磷酸酯三乙醇胺盐(601PT)2.0%、壬基酚聚氧乙烯醚(NP-10)2%、尿素3%、黄原胶0.15%、硅酸镁铝1%、聚醚改性有机硅消泡剂(DM198)0.1%、聚乙二醇4003%、山梨酸钾0.5%、纯水补足至100%,投入到砂磨机中砂磨120分钟,60目筛过滤,即得20%的悬浮剂。得到的悬浮剂经测定技术指标:外观为易流动液体,粒径D90(1~5μm)>90%,悬浮率>95%,入水分散性优,冷和热稳定性及稀释稳定性均合格。噻唑锰锌悬浮剂用水稀释300-500倍液可对植物或作物喷雾。
实施例8:噻唑锰锌新化合物水可分散性粒剂的制备(20%的噻唑锰锌)
称取20克噻唑锰锌新化合物(按无水物重量计)、农药用分散剂(2700)3克、烷基萘磺酸缩聚物钠盐5克、农药用润湿剂(1004)2克、硫酸铵4克、可溶性淀粉10克、轻质碳酸钙补足至100克。将上述物料混合均匀,在气流粉碎机中粉碎至325目以上,加入适量的75%乙醇水溶液后拌合,放入挤压造粒机中造粒,60℃烘干后筛分制得水可分散性粒剂。
实施例9 噻唑锰锌干悬浮剂的制备
配方为:40%噻唑锰锌新化合物(按无水物重量计)、尿素4%、十二烷基硫酸钠2%、木质素磺酸钠盐5%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、聚醚改性有机硅消泡剂(DF-825)0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.3%、高岭土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料重量110%的水进行混合搅拌,得到浆液。将混合均匀后的浆液经砂磨机砂磨直至95%的粒径在0.2~5微米之间后,然后将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例10:噻唑锰锌嘧菌酯复配悬浮剂的制备
将30%噻唑锰锌新化合物(按无水物重量计)和20%嘧菌酯、脂肪醇聚氧乙烯醚2%、烷基萘磺酸钠3%、亚甲基二萘磺酸钠1%、马来酸-丙烯酸均聚物钠盐3%、黄原胶0.05%、硅酸铝镁0.6%、辛烯基琥珀酸淀粉钠2.3%、丙三醇2%、水扬酸苯酯0.4%、有机硅消泡剂(Tanaform AF)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切20分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例11:噻唑锰锌肟菌酯复配干悬浮剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和20%肟菌酯、尿素4%、十二烷基硫酸钠2%、木质素磺酸盐5%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、聚醚改性有机硅消泡剂(DF-825)0.1%、聚乙二醇-2000 1%、高岭土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料重量110%的纯水进行混合搅拌,得到浆液。将混合均匀后的浆液经砂磨机砂磨直至95%的粒径在0.2~5微米之间后,然后将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例12:复配悬浮剂的制备
将45%活性化合物[40%噻唑锰锌新化合物(按无水物重量计)和5%苯醚甲环唑]、烷基萘磺酸盐2.0%、酰基谷胺酸盐1.2%、脂肪醇聚氧乙烯醚硫酸盐1.3%、苯酚磺酸缩合物钠盐2.0%、甲基萘磺酸钠甲醛缩合物3.0%、辛烯基琥珀酸淀粉钠1.0%、甲基纤维素0.3%、丙三醇2.0%、对羟基苯甲酸丁酯0.2%、有机硅消泡剂(Tanaform AF)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,过滤后即得复配悬浮剂。
实施例13:噻唑锰锌氟噻唑吡乙酮复配干悬浮剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和10%氟噻唑吡乙酮、尿素4%、十二烷基硫酸钠2%、木质素磺酸盐5%、聚羧酸盐分散剂(SD-819)4%、PVP K-304%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、聚醚改性有机硅消泡剂(DF-825)0.1%、聚乙二醇-1000 1%、高岭土补足100%;制备过程:将配方量的原药和辅料及上述原辅料重量110%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至95%的粒径在0.2~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例14:噻唑锰锌吡唑醚菌酯复配水分散颗粒剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和20%吡唑醚菌酯、尿素4%、羧甲基淀粉钠5%、木质素磺酸盐5%、聚羧酸盐分散剂(SD-819)4%、黄原胶0.1%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、十二烷基硫酸钠2%、聚乙烯吡咯烷酮(PVP K-30)4%、聚醚改性有机硅消泡剂(DM-1090)0.1%、高岭土补足100%;纯水适量;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-1090]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-1090用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例15:复配农药悬浮剂的制备
将32%活性化合物[30%噻唑锰锌新化合物(按无水物重量计)和2%烯唑醇]、牛油脂乙氧基铵盐2.0%、黄原胶0.1%、酰基谷胺酸盐1%、苯酚磺酸缩合物钠盐2.0%、甲基萘磺酸钠甲醛缩合物2.0%、辛烯基琥珀酸淀粉钠2.0%、丙三醇2.0%、对羟基苯甲酸丁酯0.2%、有机硅消泡剂(Tanaform S)0.2%、去离子水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得32%活性化合物。
实施例16:噻唑锰锌氟环唑水分散颗粒剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和5%氟环唑、尿素4%、羧甲基淀粉钠5%、木质素磺酸盐2%、聚羧酸盐分散剂(SD-819)4%、黄原胶0.2%、辛烯基琥珀酸淀粉钠0.6%、甲基纤维素2%、PVP K-304%、十二烷基硫酸钠2%、DM-10900.1%、高岭土补足100%;纯水适量;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-1090]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-1090用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液粘合进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例17:复配悬浮剂的制备
将10%噻唑锰锌新化合物(按无水物重量计)和40%氟硅唑、脂肪醇聚氧乙烯醚2.0%、黄原胶0.1%、牛油脂乙氧基胺盐1.0%、高分子聚羧酸盐(Geropon T/36)3.0%、苯乙基酚聚氧乙烯醚磷酸酯三乙醇胺盐(601PT)1%、二辛基磺基琥珀酸钠盐1.0%、尿素3.0%、DM1930.1%、去离子水补加至100%,投入到高剪切均质乳化机中高速剪切20min,再用高压均质机均质后即得复配悬浮剂。
实施例18:复配悬浮剂的制备
将30%噻唑锰锌新化合物和20%粉唑醇、脂肪醇乙基氧化物2.0%、甲基纤维素0.3%、EO/PO嵌段聚醚1.0%、烷基萘磺酸盐1.0%、聚羧酸盐(SPED-300)2%、丙烯酸均聚物钠盐1.5%、异丙醇2.0%、聚醚消泡剂0.05%、有机硅消泡剂(Tanaform AF)0.05%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例19:噻唑锰锌戊唑醇复配悬浮剂的制备
将30%噻唑锰锌新化合物(按无水物重量计)和10%戊唑醇、羟丙基纤维素0.3%、脂肪醇聚氧乙烯醚3.0%、甲基萘磺酸钠甲醛缩合物2.0%、聚羧酸盐(SPED-300)2%、环氧氯丙烷2.0%、丙三醇2.0%、黄原胶0.2%、DM-10900.1%、纯水补足充分混合,再投入到高剪切均质乳化机中高速剪切粗磨和均质,再泵至砂磨机中砂磨,砂磨至D90粒径为0.2-5微米,60目筛过滤,即得悬浮剂。
实施例20:复配悬浮剂的制备
将35%活性化合物[30%噻唑锰锌新化合物(按无水物重量计)和5%已唑醇组合物]、聚羧酸盐(SPED-300)2%、酰基谷胺酸盐2.0%、脂肪醇聚氧乙烯醚硫酸盐1%、苯酚磺酸缩合物钠盐1.0%、甲基萘磺酸钠甲醛缩合物2.0%、辛烯基琥珀酸淀粉钠2.0%、黄原胶0.1%、环氧大豆油5.0%、丙三醇2.0%、有机硅消泡剂(Tanaform AF)0.15%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得复配悬浮剂。
实施例21:噻唑锰锌腈菌唑复配水分散颗粒剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和12%腈菌唑、尿素4%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、羧甲基淀粉钠5%、聚乙烯吡咯烷酮(PVP K-30)4%、十二烷基硫酸钠2%、黄原胶0.2%、辛烯基琥珀酸淀粉钠0.5%、甲基纤维素2%、聚醚改性有机硅消泡剂(DF-825)0.1%、高岭土补足100%;水适量;制备工艺同实施例16。
实施例22:复配组合物悬浮剂的制备
将30%噻唑锰锌新化合物(实施例1法制备,按无水物重量计)和10%戊菌唑、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、黄原胶0.1%、高分子聚羧酸盐4.0%、硅酸铝镁0.5%、异丙醇2.0%、有机硅消泡剂(Tanaform AF)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例23:复配悬浮剂的制备
将35%噻唑锰锌新化合物(按无水物重量计)和5%春雷霉素、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、亚甲基二萘磺酸钠2.0%、高分子聚羧酸盐(Geropon T/36)3.0%、黄原胶0.3%、尿素2.0%、有机硅消泡剂(Tanaform AF)0.1%、EDTA钙钠4水合物0.9%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例24:复配悬浮剂的制备
将30%噻唑锰锌新化合物和5%三唑醇组合物、烷基萘磺酸盐1.3%、酰基谷胺酸盐2.0%、脂肪醇聚氧乙烯醚硫酸盐1%、苯酚磺酸缩合物钠盐1.0%、甲基萘磺酸钠甲醛缩合物2.0%、辛烯基琥珀酸淀粉钠2.0%、丙三醇2.0%、Tanaform AF 0.1%、EDTA钙钠0.5%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得复配悬浮剂。
实施例25:复配悬浮剂的制备
将30%噻唑锰锌新化合物和10%联苯三唑醇、聚羧酸盐(SPED-300)2%、酰基谷胺酸盐2%、脂肪醇聚氧乙烯醚1.0%、苯酚磺酸缩合物钠盐1.0%、甲基萘磺酸钠甲醛缩合物2%、辛烯基琥珀酸淀粉钠1%、乙基纤维素0.3%、尿素2.0%、DM1980.1%、EDTA钙钠0.5%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得复配悬浮剂。
实施例26:复配悬浮剂的制备
将20%噻唑锰锌新化合物(按无水物重量计)和20%噻菌铜、聚羧酸盐(SPED-300)2%、酰基谷胺酸盐2.0%、脂肪醇聚氧乙烯醚硫酸盐1.0%、苯酚磺酸缩合物钠盐1.0%、甲基萘磺酸钠甲醛缩合物2.0%、羧甲基纤维素钠1.0%、丙三醇2.0%、DM198 0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得复配悬浮剂。
实施例27:复配悬浮剂的制备
将25%噻唑锰锌新化合物和25%甲霜灵、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、萘磺酸缩合物钠盐2.0%、高分子聚羧酸盐(Geropon T/36)4.0%、聚乙烯醇0.5%、尿素2.0%、聚醚改性有机硅消泡剂(DM-198)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例28:复配悬浮剂的制备
将20.0%噻唑锰锌新化合物和20.0%氟酰胺、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、丙烯酸均聚物钠盐1.0%、高分子聚羧酸盐(Geropon T/36)4.0%、聚乙烯醇0.5%、环氧大豆油5.0%、尿素2.0%、聚醚改性有机硅消泡剂(DM198)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例29:复配水分散颗粒剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和21.2%氟唑菌酰胺、硫酸钠4%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、羧甲基淀粉钠5%、聚乙烯吡咯烷酮(PVP K-30)4%、十二烷基硫酸钠2%、黄原胶0.1%、辛烯基琥珀酸淀粉钠0.5%、乙基纤维素2%、DM-198 0.1%、EDTA钙钠4水合物0.5%、硅藻土补足100%;纯水适量;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-198]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-198用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液粘合进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例30:复配悬浮剂的制备
将20%噻唑锰锌新化合物和40%噻菌灵、脂肪醇乙氧基化合物3.0%、烷基萘磺酸盐1.0%、脂肪醇聚氧乙烯醚硫酸盐4.0%、苯酚磺酸缩合物钠盐3.0%、亚甲基二萘磺酸钠1.5%、甲基萘磺酸钠甲醛缩合物0.5%、聚乙二醇-800 1%、聚醚改性有机硅消泡剂(DM198)0.15%、EDTA钙钠0.5%、蒸馏水补加至100%,投入到高剪切均质乳化机中高速剪切30min,再用高压均质机均质后即得复配悬浮剂。
实施例31:噻唑锰锌甲霜灵复配水分散颗粒剂的制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和15%甲霜灵、尿素4%、低取代羟丙基纤维素4%、木质素磺酸盐2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、十二烷基硫酸钠2%、黄原胶0.2%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、聚醚改性有机硅消泡剂(DM-198)0.1%、EDTA钙钠0.5%、高岭土补足100%;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-198]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-198用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液粘合进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例32:复配悬浮剂的制备
将60%噻唑锰锌新化合物和5%梧宁霉素、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、萘磺酸缩合物钠盐2.0%、高分子聚羧酸盐(Geropon T/36)4.0%、聚乙烯醇0.5%、尿素2.0%、DM1930.15%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例33:春雷噻唑锰锌中生复配悬浮剂的制备
将35%噻唑锰锌新化合物(按无水物重量计)、2%春雷霉素、3%中生菌素、脂肪醇乙基氧化物2.0%、EO/PO嵌段聚醚1.0%、木质素磺酯钠1.0%、高分子聚羧酸盐(GeroponT/36)3.0%、聚乙烯醇0.5%、环氧大豆油5%、尿素2.0%、DM198 0.1%、EDTA钙钠0.5%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例34:组合物悬浮剂的制备
将45%活性化合物[10.0%噻唑锰锌新化合物(按无水物重量计)和35.0%霜霉威盐酸盐]、脂肪醇聚氧乙烯醚3.0%、EO/PO嵌段聚醚1.0%、高分子聚羧酸盐(Geropon T/36)4.0%、淀粉磷酸酯钠0.5%、季戊四醇1.0%、尿素2.0%、聚醚改性有机硅消泡剂(DM198)0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例35:组合物悬浮剂的制备
将50%噻唑锰锌新化合物和10%井冈霉素、脂肪醇乙基氧化物4.0%、EO/PO嵌段聚醚1.0%、低取代羟丙基纤维素1.0%、甲基萘磺酸钠甲醛缩合物2.0%、高分子聚羧酸盐(Geropon T/36)4.0%、聚乙烯醇0.5%、尿素2.0%、聚醚改性有机硅消泡剂(DM-198)0.1%、EDTA钙钠4水合物0.5%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例36:春雷噻唑锰锌中生组合物干悬浮剂的制备
配方为:35%噻唑锰锌新化合物(按无水物重量计)、2%春雷霉素、3%中生菌素、尿素4%、十二烷基硫酸钠2%、达润DCM-822%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)2%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、聚醚改性有机硅消泡剂(DM198)0.1%、聚乙二醇-800 1%、高岭土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料总重量130%的纯水进行混合搅拌,得到浆液。将混合均匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,然后将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在2.0-7.0Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例37:组合物悬浮剂的制备
将20%噻唑锰锌新化合物和20%稻温酯、烷基萘磺酸盐2.3%、酰基谷胺酸盐2.0%、脂肪醇聚氧乙烯醚硫酸盐1.0%、苯酚磺酸缩合物钠盐1.0%、甲基萘磺酸钠甲醛缩合物2.0%、辛烯基琥珀酸淀粉钠2.0%、季戊四醇1%、丙三醇2.0%、DM-115M 0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切25分钟,再泵至砂磨机中砂磨90分钟,60目筛过滤,即得复配悬浮剂。
实施例38:组合物悬浮剂的制备
将25.0%噻唑锰锌新化合物和25.0%恶霉灵、烷基萘磺酸盐4.0%、EO/PO嵌段聚醚1.0%、亚甲基二萘磺酸钠1.0%、高分子聚羧酸盐(Geropon T/36)3.5%、聚乙烯醇0.5%、环氧大豆油5.0%、尿素2.0%、尼泊金乙酯0.1%、EDTA钙钠4水合物0.1%、DM-115M0.1%、纯水补至100%,投入到高剪切均质乳化机中高速剪切30分钟,再输至砂磨机中,循环砂磨3次即得复配悬浮剂。
实施例39:组合物的干悬浮剂制备
配方为:20%噻唑锰锌新化合物(按无水物重量计)和15%烯酰吗啉、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM198 0.1%、聚乙二醇-800 1%、硅藻土补足100%;制备过程:将配方量的原药和辅料及上述原辅料总重量130%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在2.0-7.0Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例40:复配组合物的干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和30%百菌清、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM198 0.1%、聚乙二醇-800 1%、硅藻土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料总重量130%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例41 噻唑锰锌丁香菌酯组合物的干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和10%丁香菌酯、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM198 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.8%、硅藻土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料总重量130%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例42 噻唑锰锌和肟醚菌胺复配干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和10%肟醚菌胺、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM-DA1952 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、硅藻土补足100%;制备工艺同实施例41。
实施例43:噻唑锰锌和丙硫菌唑干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和17.4%丙硫菌唑、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM-198 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、硅藻土补足100%;制备工艺同实施例41。
实施例44:噻唑锰锌新化合物和唑胺菌酯干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和20%唑胺菌酯、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇10%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM-DA1952 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、高岭土补足100%;制备工艺同实施例41。
实施例45:噻唑锰锌氟嘧菌酯复配的干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和20%氟嘧菌酯、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、山梨醇8%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM198 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、高岭土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料总重量120%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例46:噻唑锰锌和咯菌腈可湿性粉剂
称取20克噻唑锰锌新化合物(按无水物重量计)、25克咯菌腈、烷基萘磺酸缩聚物钠盐3克、十二烷基硫酸钠2克、白炭黑3克、高岭土补足至100克。将上述物料混合均匀,在气流粉碎机中粉碎至325目以上,制得可湿性粉剂。
实施例47:噻唑锰锌新化合物和异长乙烯酮肟内酰胺可湿性粉剂的制备
称取噻唑锰锌新化合物(实施例3法制备)20克、异长乙烯酮肟内酰胺20克、SD-819(聚羧酸盐)3克、达润D063克、十二烷基硫酸钠2克、白炭黑3克、高岭土补足至100克。将上述物料混合均匀,在气流粉碎机中粉碎至325目以上,制得可湿性粉剂。
实施例48-76复配可湿性粉剂的制备
表2各复配农药的可湿性粉剂的制备(按照实施例47的方法制备)
注:表3中复配实施例单号的组分噻唑锰锌新化合物(A)为实施例1-2A法制备,双号为实施例1-4A法制备。
实施例77:40%噻唑锰锌新化合物和环丙唑醇水分散颗粒剂的制备
称取20克噻唑锰锌新化合物(实施例3法制备,按无水物重量计)、环丙唑醇20克、尿素4%、低取代羟丙基纤维素4%、木质素磺酸盐2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、十二烷基硫酸钠2%、黄原胶0.2%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、聚醚改性有机硅消泡剂(DM-198)0.1%、EDTA钙钠0.5%、高岭土补足100%;
制备过程:将配方量的原药和辅料[除下述辅料外:十二烷基硫酸钠、PVP K-30、DM-198]经粉碎到过300目筛粉末,将辅料:十二烷基硫酸钠、PVP K-30、DM-198用适量的纯水溶解混合,再将粉末置于GHL系列高效湿法混合制粒机中,加入上述水溶液粘合进行湿法制粒,过40目筛制备颗粒,经50-60℃干燥约3小时,然后将固体颗粒过40目筛整粒,再将其经分装机分装于袋中,得水分散颗粒剂。
实施例78-284复配水分散颗粒剂的制备
表3各复配的水分散颗粒剂的制备(参照实施例77工艺制备)
注:表中复配组分噻唑锰锌新化合物(A)(本表中实施例尾致1-7号分别用实施例1-1A至1-7A法制备原料药,其余为实施例2法或实施例3法制备任一原料药);表中实施例78-284的主药噻唑锰锌新化合物(A)的重量均可以无水物或以水合物直接计算重量。
实施例285:农药组合物分散粒剂的制备
将10%噻唑锰锌新化合物(实施例1法制备)、3%戊唑醇、6.2%甲霜灵、15.4%丙硫菌唑、EO/PO嵌段聚醚4%、萘磺酸盐3%、可溶性淀粉5%、黄原胶1%、硅藻土加到100%,充分混合,再投入到高剪切均质乳化机中高速剪切粗磨和均质,再泵至砂磨机中砂磨至D90粒径为0.2-5微米,再常规工艺造粒成型得水分散粒剂。
实施例286:四种活性成分的种衣剂的制备
将5%噻唑锰锌新化合物(实施例3法制备)、2.75%甲霜灵、6.88%丙硫菌唑、1.0%咯菌腈、烷基萘磺酸盐1.0%、脂肪醇聚氧乙烯醚3.0%、丙烯酸均聚物钠盐1.0%、羧甲基纤维素1.0%、丙三醇3.0%、黄原胶0.2%、DM198 0.1%、偶氮染料0.2%、聚乙二醇-800 1%、EDTA钙钠4水合物0.3%、纯水加到100%,充分混合,再投入到高剪切均质乳化机中高速剪切粗磨和均质,再泵至砂磨机中砂磨,砂磨至D90粒径为0.2-5微米,60目筛过滤,即得悬浮型种衣剂。
实施例287:悬浮种衣剂的制备
将3%噻唑锰锌新化合物、3.59%氟唑菌苯胺、5.74%甲霜灵、7.18%丙硫菌唑、烷基萘磺酸盐2.0%、脂肪醇聚氧乙烯醚3.0%、甲基萘磺酸钠甲醛缩合物2.0%、阿拉伯树胶2.0%、丙三醇3.0%、黄原胶0.2%、氧化铁0.2%、DM198 0.1%、纯水加到100%,充分混合,再投入到高剪切均质乳化机中高速剪切粗磨和均质,再泵至砂磨机中砂磨,砂磨至D90粒径为0.2-5微米,60目筛过滤,即得悬浮型种衣剂。
实施例288:四种活性成分的悬浮种衣剂的配制
将1%噻唑锰锌新化合物、1.47%丙硫菌唑、0.29%戊唑醇、8.59%吡虫啉、萘磺酸钠盐2.0%、高分子聚羧酸盐(Geropon T/36)3.0%、甲基萘磺酸钠甲醛缩合物2.0%、聚醋酸乙烯酯2.0%、乙二醇3.0%、羧甲基纤维素钠0.2%、EDTA钙钠4水合物0.1%、DM1980.1%、氧化钛0.2%、纯水加到100%,充分混合,再投入到高剪切均质乳化机中高速剪切粗磨和均质,再泵至砂磨机中砂磨,砂磨至D90粒径为0.2-5微米,60目筛过滤,即得悬浮型种衣剂。
实施例289:种子处理干粉剂的制备
将6%噻唑锰锌新化合物(实施例1法制备)和4%多菌灵、萘磺酸缩合物钠盐3%、滑石粉2.0%、轻质碳酸钙5.0%、硅藻土加到100%,充分混合,再通过超细粉碎至一定粒径,得干粉剂。
实施例290-445复配干悬浮剂的制备
表4.表中各复配的干悬浮剂的制备(辅料配比如实施例45,按照实施例45方法制备)
注:表中仅列出实施例290-445的主药或活性组分或原药的配比量以百分比%计(均以无水物或噻唑锰锌新化合物计算重量或重量比),A为噻唑锰锌新化合物(本表中实施例尾数1-7号分别用实施例1-1A至1-7A法制备的原药,其余为实施例2法或实施例3法制备的任一原药),其余组分或辅料量均分别按实施例45的配比取用,各实施例制备分别按照实施例45的制备工艺进行。
实施例446:噻唑锰锌三十烷醇芸苔素复配的干悬浮剂制备
配方为:20%噻唑锰锌新化合物(按无水物重量计)和1%三十烷醇、0.7%芸苔素、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、辛烯基琥珀酸淀粉钠1%、山梨醇8%、甲基纤维素2%、DM198 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、高岭土补足100%;
制备过程:将配方量的原药和辅料及上述原辅料总重量120%的纯水进行混合搅拌,得到浆液。将混匀后的浆液经砂磨机砂磨直至90%的粒径在0.1~5微米之间后,将悬乳浆液泵入压力式喷雾干燥器进行干燥造粒,喷雾压力控制在3.0-6.5Mpa,干燥气体进气温度为110-140℃,出气温度为55-70℃,造粒后物料经筛分得到80~150目的干悬浮剂。
实施例447:噻唑锰锌苄基氨基嘌呤复硝酚钠复配的干悬浮剂制备
配方为:30%噻唑锰锌新化合物(按无水物重量计)和0.2%的6-苄基氨基嘌呤、0.3%复硝酚钠、尿素4%、十二烷基硫酸钠2%、聚羧酸盐(SPED-300)2%、聚羧酸盐分散剂(SD-819)4%、聚乙烯吡咯烷酮(PVP K-30)4%、黄原胶0.2%、辛烯基琥珀酸淀粉钠0.5%、山梨醇8%、甲基纤维素2%、辛烯基琥珀酸淀粉钠1.0%、DM198 0.1%、聚乙二醇-800 1%、EDTA钙钠4水合物0.5%、高岭土补足100%;制备过程同实施例446。
实施例448本发明实施例可通过室内毒力测定,明确A和B两种药剂按一定比例复配后的增效比值(SR),评价联合作用;SR<0.5为拮抗作用,0.5≤SR≤1.5为相加作用,SR>1.5为增效作用。
试验方法:经预试确定各药剂有效抑制浓度范围后,药剂按有效成分含量分别设多个剂量处理,设纯水对照。试验参考《农药生物测定技术》(陈年春主编,北京农业大学出版社出版,1998年)和《农药室内生物测定试验准则杀菌剂》进行,采用菌丝生长速率法测定药剂对不同作物病菌的毒力。在洁净区中于培养箱中在26±1℃将病菌在马铃薯琼脂培养基(PDA)中培养72h后,在无菌操作台用十字交叉法测量菌落直径,计算各处理净生长量、菌丝生长抑制率。
净生长量(mm)=测量菌落直径-5
菌丝生长抑制率(%)=[(对照组净生长量-处理组净生长量)/对照组净生长量]×100
将菌丝生长抑制率换算成机率值(y),药液浓度(μg/mL)转换成对数值(x),以最小二乘法求得毒力回归方程(y=a+bx),并由此计算出每种药剂的EC50值。同时根据Wadley法计算两药剂不同配比联合增效比值(SR),SR<0.5为拮抗作用,0.5≤SR≤1.5为相加作用,SR>1.5为增效作用。计算公式如下:
理论(组合)EC50=(a+b)/[(a/A的实测EC50值)+(b/B的实测EC50值)]
上式中,a为活性成分A在组合物中的比例,b为活性成分B在组合物中的比例。
增效比率(SR)=理论EC50值/观测EC50值
测定噻唑锰锌新化合物(实施例1-2A法)和氟噻唑吡乙酮按比例混配在离体实验中对马铃薯晚疫病菌的毒力,试验对象为马铃薯晚疫病菌,结果如表5所示。
表5噻唑锰锌新化合物(A)与氟噻唑吡乙酮(B)复配对马铃薯晚疫病菌离体实验的毒力测定
试验结果表明:噻唑锰锌新化合物能有效杀菌,同时与氟噻唑吡乙酮(B)混配配比在20∶1~1∶20之间均有相加作用或增效作用,同时施用可节省工时费用,在10∶1~1∶10之间有增效作用,噻唑锰锌新化合物复配有效延缓抗性的产生。
实施例449参考实施例448的方法研究噻唑锰锌新化合物(实施例1-2A法)与嘧菌酯复配组分对水稻条斑病病菌的离体杀菌作用,试验对象为水稻条斑病病菌,结果见表6。
表6、噻唑锰锌新化合物(A)与嘧菌酯(B)复配对水稻条斑病病菌离体实验的毒力测定
供试药 | 配比 | 观测EC50(mg/L) | 理论EC50(mg/L) | 增效比率(SR) |
A | 1∶0 | 12.13 | ||
B | 0∶1 | 4.47 | ||
A∶B | 40∶1 | 10.02 | 11.64 | 1.16 |
A∶B | 20∶1 | 8.35 | 11.21 | 1.34 |
A∶B | 10∶1 | 6.59 | 10.50 | 1.59 |
A∶B | 1∶1 | 3.76 | 6.53 | 1.74 |
A∶B | 1∶5 | 3.18 | 5.00 | 1.57 |
A∶B | 1∶10 | 3.14 | 4.74 | 1.51 |
A∶B | 1∶20 | 4.27 | 4.61 | 1.08 |
试验结果表明:噻唑锰锌新化合物能有效杀菌,同时与嘧菌酯(B)混配配比在40∶1~1∶20之间均有相加作用或增效作用,同时施用可大幅节省工时费用,当配比在10∶1~1∶10之间时,增效显著,该复配有效延缓抗性产生。
实施例449参考实施例448的方法研究噻唑锰锌新化合物(实施例1-6A法)与春雷霉素复配对黄瓜角斑病菌的离体杀菌作用,试验对象为黄瓜角斑病病菌,结果见表7。
表7、噻唑锰锌新化合物(A)和春雷霉素(B)混配对复配对黄瓜角斑病菌的毒力测定结果
试验结果表明:噻唑锰锌新化合物能有效杀菌,同时与春雷霉素(B)混配配比在40∶1~1∶20之间均有相加作用或增效作用,同时施用可大幅减少工时费用,当配比在10∶1~1∶10之间时增效显著,该复配能有效延缓对黄瓜角斑病菌抗药性产生。
实施例450参考实施例448的方法研究噻唑锰锌新化合物(实施例1-7A法)与甲磺酰菌唑复配组分对柑桔溃疡病的离体杀菌作用,试验对象为柑桔溃疡病病菌,结果见表8。
表8、噻唑锰锌新化合物(A)与甲磺酰菌唑(B)复配对柑桔溃疡病病菌离体实验的毒力测定
上表实验结果表明:噻唑锰锌新化合物能有效杀菌,同时与甲磺酰菌唑(B)混配配比在40∶1~1∶20之间均有相加作用或增效作用,同时施用可减少工时费用,当配比在10∶1~1∶10之间时,增效显著,上述复配有效延缓抗性产生。
工业实用性等及其说明等:
以上通过具体实施方式和实施例对本发明进行了详细说明,不过应理解,这些说明并不对本发明的范围构成任何限制,相关技术人员明显能在在不偏离本发明的精神和保护范围的情况下,可以对本发明的技术方案及其实施方式进行多种修饰、改进和替换与组合,来实现本发明技术,这些均因落入本发明的保护范围内。特别需要指出的是,可以理解,很多细节的变化是可能的,所有相类似的替换和改动对本领域技术人员来说是显而易见的,它们都被视为包括在本发明的精神、范围和内容中,本发明并不限于上述实施例。
Claims (10)
1.噻唑锰锌新化合物,其特征在于:噻唑锰锌新化合物的分子式为:(C4H4N6S4)(Mn2+)V(Zn2+)K,含水量在0.00-13%,或C4H4N6S4(Mn)V(Zn)K·wH2O,含水量在0.00-13%,噻唑锰锌新化合物分子中锰和锌的摩尔数或其比例在0.0001~0.9999:0.9999~0.0001之间,噻唑锰锌分子中锰和锌的摩尔数均在0.0001~0.9999之间,噻唑锰锌新化合物分子中锰和锌的摩尔数之和等于1,即V+K=1。
2.根据权利要求1所述的噻唑锰锌新化合物,其特征在于:噻唑锰锌新化合物的分子式包括[C4H4N6S4(Mn)0.95(Zn)0.05,含水量在0.0-13%],[C4H4N6S4(Mn)0.5(Zn)0.5,含水量在0.0-13%],[C4H4N6S4(Mn)0.9(Zn)0.1,含水量可在0.0-13%],[C4H4N6S4(Mn)0.8(Zn)0.2,含水量在0.0-13%],[C4H4N6S4(Mn)0.7(Zn)0.3,含水在0.0-13%],[C4H4N6S4(Mn)0.65(Zn)0.35,含水在0.0-13%],[C4H4N6S4(Mn)0.6(Zn)0.4,含水量在0.0-13%],[C4H4N6S4(Mn)0.4(Zn)0.6,含水量在0.0-13%],[C4H4N6S4(Mn)0.35(Zn)0.65,含水量在0.0-13%],[C4H4N6S4(Mn)0.3(Zn)0.7,含水量在0.0-13%],[C4H4N6S4(Mn)0.2(Zn)0.8,含水量在0.0-13%],[C4H4N6S4(Mn)0.1(Zn)0.9,含水量在0.0-13%],[C4H4N6S4(Mn)0.05(Zn)0.95,含水在0.0-13%];
或[C4H4N6S4(Mn)0.95(Zn)0.05·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.5(Zn)0.5·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.9(Zn)0.1·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.8(Zn)0.2·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.7(Zn)0.3·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.65(Zn)0.35·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.6(Zn)0.4·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.4(Zn)0.6·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.35(Zn)0.65·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.3(Zn)0.7·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.2(Zn)0.8·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.1(Zn)0.9·wH2O,含水量在0.00-13%],
[C4H4N6S4(Mn)0.05(Zn)0.95·wH2O,含水量在0.00-13%]。
3.根据权利要求1所述的噻唑锰锌新化合物,其特征在于:利用粉末X射线衍射法测量,在衍射角2θ,3-60°的测量范围内,在如下2θ值的位置具有相应的特征值:11.22,13.32,15.53,17.79,19.17,20.76,21.48,22.59,22.97,24.30,24.98,26.29,26.85,28.04,28.82,30.83,31.33,32.36,33.51,34.04,35.78,36.24,37.68,39.84,43.96,46.24,46.89,47.55,49.19,50.97,51.23,52.68,53.57,55.42。
4.根据权利要求1所述的噻唑锰锌新化合物,其特征在于:其含水化合物的热分析图谱,在TG-DSC或者TG-DTA曲线约在45-162℃之间的失重曲线下具有对应的吸热峰。
5.根据权利要求1-4中任一所述的噻唑锰锌新化合物的制备方法,其特征在于:其制备方法为:在反应容器中加2-氨基-5-巯基-1,3,4-噻二唑,加水,搅拌,加碳酸钠、碳酸氢钠、氢氧化钠、碳酸钾、碳酸氢钾、氢氧化钾中的一种或几种或其水溶液,搅拌,加锰盐或其溶剂化合物或其溶液和锌盐或其溶剂化合物或其溶液,锰盐或其溶剂化合物选自但不仅限于硫酸锰、一水硫酸锰、氯化锰、氯化锰4水合物、醋酸锰、醋酸锰4水合物、硝酸锰、硝酸锰4水合物或其水溶液中的一种或几种,水溶性的锌盐选自但不仅限于硫酸锌、七水硫酸锌、氯化锌、醋酸锌、硝酸锌或其水溶液中的一种或几种,搅拌,待固体充分析出,过滤,用水、有机溶剂C1-C6的低分子醇、C2-C8的低分子醚、C3-C8的低分子酮、C2-C6的低分子腈、C1-C6的低分子卤代烃、C2-C8的低分子酯中的一种或几种洗一次到数次,过滤,所得固体干燥得新型噻唑锰锌新化合物;
其中,反应中所使用的2-氨基-5-巯基-1,3,4-噻二唑与碱的当量比约为1:1~1.2;第一步反应中所使用的2-氨基-5-巯基-1,3,4-噻二唑与水、或C1-C6的低分子醇、或C2-C8的低级醚、或C2-C6的低分子腈有机溶剂中的一种或几种重量体积比为一般为:1(g):3.5~60(ml),较优选的比为:1(g):5~40(ml);2-氨基-5-巯基-1,3,4-噻二唑与锰盐和锌盐的总当量比较优选约为1:0.98~1.05;
其中,有机溶剂C1-C6的低分子醇,选自但不仅限于甲醇、乙醇、异丙醇、丁醇;C2-C6的低分子腈选自但不仅限于乙腈;C2-C8的低分子醚或低分子醚选自但不仅限于乙醚、异丙醚、四氢呋喃、甲基四氢呋喃;C1-C6低级卤代烃选自但不仅限于二氯甲烷、氯仿;C2-C8低分子酯选自但不仅限于醋酸丁酯、乙酸乙酯、甲酸乙酯;C3-C8的低分子酮选自但不仅限于丙酮,丁酮、异己酮。
6.根据权利要求1-4中任一所述的噻唑锰锌新化合物,其特征在于:有效剂量的噻唑锰锌新化合物与有效剂量的杀菌药物或和抗菌药物或抗病毒药和或植物生长调节剂或有效剂量的农药上可接受的杀虫剂组成的药物组合物或农药组合物,及其他药学上可接受的辅料制备药学上可接受的农药制剂;即,有效剂量的活性成分A——噻唑锰锌新化合物和有效剂量的活性成分B制备新的药物组合物或农药组合物;其中,活性成分A与活性成分B重量比可选自为180∶1~1∶100,可以其无水物或含水物计算重量;其中,活性成分A与活性成分B重量比可较优选自为100∶1~1∶100,可以其无水物或含水物计算重量;其中,活性成分A与活性成分B重量比也可较优选自为80∶1~1∶80,可以其无水物或含水物计算重量;所述的活性成分B选自但不仅限于其中的任意一种或几种选自B.1)-B.13)或杀虫剂的化合物及其药学上可接受盐或其溶剂化合物;活性成分B选自不仅限于如下参考文献中的农药化合物,参考文献A:刘长令,柴宝山主编,新农药创制与合成,化学工业出版社,2013年,北京;文献B:孙家隆,齐军山,现代农药应用技术丛书:杀菌剂卷,化学工业出版社,2017年,北京;文献C:郑桂玲,孙家隆,现代农药应用技术丛书:杀虫剂卷,化学工业出版社,2017年,北京;文献D:孙家隆,现代农药合成技术,化学工业出版社出版,2011年,北京;文献E:现代农药手册,刘长令,杨吉春,化学工业出版社,2018年,北京;
B.1)甲氧基丙烯酸酯类杀菌剂或抗病毒药,选自但不仅限于嘧菌酯、醚菌酯、肟菌酯、吡唑醚菌酯、烯肟菌酯、唑菌酯、氟嘧菌酯、啶氧菌酯、苯醚菌酯、烯肟菌胺或苯氧菌胺、氰烯菌酯、Picarbutrazox、肟醚菌胺、唑菌胺酯、丁香菌酯、氯啶菌酯、苯噻菌酯、UBF307、KZ165、烯丙苯噻唑、双氯氰菌胺中的一种或几种;
B.2)三唑类杀菌剂,选自但不仅限于苯醚甲环唑、烯唑醇、氟环唑、腈苯唑、氟硅唑、粉唑醇、戊唑醇、己唑醇、腈菌唑、戊菌唑、丙环唑、四氟醚唑、三唑醇、联苯三唑醇、三唑酮、叶菌唑、种菌唑、丙硫菌唑、亚胺菌唑、灭菌唑、环丙唑醇、氯氟醚菌唑、异丙芬三氟康唑、糠菌唑、腈苯唑、氟喹唑、呋醚唑、戊环唑、乙环唑、三氟苯唑、高效烯唑醇、三唑酮中的一种或几种;
B.3)酰胺类杀菌剂,选自但不仅限于甲霜灵、精甲霜灵、氟酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌酰胺、萎锈灵、联苯吡菌胺、氟唑菌苯胺、氟唑环菌胺、氟唑菌酰胺、吡噻菌胺、噻呋酰胺、氟啶酰菌胺和吡唑萘菌胺、氟苯醚酰胺、氟醚菌酰胺、环己磺菌胺、甲噻诱胺、高效苯霜灵、噻氟菌胺、噻酰菌胺、噻唑菌胺、硅噻菌胺、呋吡菌胺、环氟菌胺、氟吡菌胺、苯酰菌胺、环酰菌胺、环丙酰菌胺、磺菌胺、甲磺菌胺、引唑磺菌胺、稻温酰胺、Bixafen、Fluxapyroxad、Sedaxane中的一种或几种;
B.4)咪唑类杀菌剂中的一种,选自但不仅限于氰霜唑、氟菌唑、高效抑霉唑、咪唑菌酮、噁咪唑、稻温酯、丙硫咪唑、苯硫咪唑、噻菌灵、抑霉唑、麦穗宁、咪鲜胺、咪鲜胺锰络合物、咪鲜胺铜络合物中的一种或几种;
B.5)二羧酰亚胺类杀菌剂,选自但不仅限于腐霉利、异菌脲、乙烯菌核利、克菌丹、菌核净、甲基立枯磷中的一种或几种;
B.6)氨基甲酸酯类杀菌剂,选自但不仅限于霜霉威盐酸盐、乙霉威、苯菌灵、多菌灵、甲基硫菌灵、缬霉威、苯噻菌胺、缬菌胺Valifenalate中的一种或几种;
B.7)抗菌素类杀菌剂或抗病毒药,选自但不仅限于井冈霉素、硫酸链霉素、春雷霉素、梧宁霉素、申嗪霉素、多抗霉素、宁南霉素、硫酸链霉素、中生菌素、农抗120、金核霉素、长川霉素、四霉素中的一种或几种;
B.8)噁唑类杀菌剂,选自但不仅限于恶霜灵、恶霉灵、噁唑菌酮、啶菌噁唑、氟噻唑吡乙酮、苄氟噁唑砜、二氯噁菌唑和甲磺酰菌唑中的一种或几种;
B.9)吗啉类杀菌剂或抗病毒药,选自但不仅限于十三吗啉、烯酰吗啉、氟吗啉、盐酸吗啉胍中的一种或几种;
B.10)嘧啶类杀菌剂,选自但不仅限于嘧菌环胺、嘧霉胺、乙嘧酚、嘧菌胺、氟嘧菌胺、双苯菌胺、SYP-3773、SYP-3810中的一种或几种;
B.11)喹啉类杀菌剂,选自但不仅限于二氰蒽醌、丙氧喹啉、苯氧喹啉、喹诺氟美林中的一种或几种;
B.12)二硫代氨基甲酸盐类杀菌剂或抗病毒药,选自但不仅限于代森联、福美双、福美锌、代森铵、代森锌、代森锰、代森锰锌、丙森锌中的一种或几种;
B.13)其他杀菌剂或抗病毒药或植物生长调节剂,选自但不仅限于敌瘟磷、三乙膦酸铝、百菌清、稻瘟灵、咯菌腈或者氢氧化铜、松脂酸铜、去氢松脂酸铜、拌种咯、氟咯菌氰、异长乙烯酮肟内酰胺、蛇床子素、毒氟磷、酚菌酮、甲噻诱胺、聚六亚甲基双胍盐酸盐、溴菌腈、吲唑磺菌胺、王铜、壬菌铜、喹啉铜、盐酸吗啉胍、琥胶肥酸铜、辛菌胺醋酸盐、氨基寡糖素、香菇多糖、噻霉酮、乙蒜素、烯丙苯噻唑、双氯氰菌胺、香豆素、大黄素甲醚、大黄酚、氟唑活化酯、S-诱抗素、氨基寡糖素、吡啶硫酸锌、小檗碱及药学可接受的盐、盐酸小檗碱、硫酸氢小檗碱、硫酸小檗碱、丁子香酚、硫磺、硫酸铜、五水硫酸铜、王铜、氧化铜、碱式硫酸铜、叶枯唑、异长叶烯酮肟内酰胺、大蒜素、愈创木酚、Quinolactacide、脱氢乙酸、氯溴异氰尿酸、香芹酚、塞唑锌及水合物、辛唑嘧菌胺、Pyribencarb、Flutianil、Meptyldinocap、Pyriofenone、Fenpyrazamine、Tolprocarb、Isofetamid、Isopyrazam、Penflufen、Benzovindiflupyr、Tebufloquin、Oxathiapiprolin、螺环菌胺、螺嘧环胺、乙膦铝、异稻瘟净、苦参碱、苦参素、噻菌铜或其水合物、噻森铜或其水合物、苯菌酮、氟唑菌酰羟胺、ydiflumetofen、茉莉酸甲酯中的一种;或植物生长调节剂选自但不仅限于胺鲜酯、氯吡苯脲、复硝酚钠、芸苔素、赤霉素、6-苄基氨基嘌呤、三十烷醇、萘乙酸或其药用盐、多效唑、乙烯利、萘乙酸甲酯、氟节酸、抗倒酯、烯效唑、吲哚丁酸、吡啶醇、抗倒胺、矮健素、矮壮素、芸苔素内脂、增产灵、增甘磷中的一种或几种;
杀虫剂选自但不仅限于定虫隆、伏虫隆、杀虫隆、氟虫脲、氟铃脲、氟螨脲、氟幼脲、氟啶脲、灭幼脲、除虫脲、丁醚脲、抑食肼、噻嗪酮、双氧威、或虫酰肼、杀螟磷、敌百虫、甲基对硫磷、氯唑磷、哒嗪硫磷、喹硫磷、三唑磷、噻唑硫磷、二嗪磷、辛硫磷、杀螟硫磷、甲基嘧啶磷、倍硫磷、杀螟腈、丙溴磷、毒死蜱、甲基毒死蜱、丙硫磷、甲丙硫磷、乐果、马拉硫磷、杀扑磷、丁硫克百威、丙硫克百威、戊氰威、仲丁威、异丙威、唑蚜威、抗蚜威、速灭威、混灭威、甲萘威、灭虫威、灭多威、或硫双灭多威、三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、甲氰菊酯、氰戊菊酯、氯氰菊酯、高效氯氰菊酯、溴氰菊酯、四溴菊酯、醚菊酯、或戊菊酯、阿维菌素、甲氨基阿维菌素、伊维菌素或其药学上可接受的盐中的任意一种或几种,活性成分B选自但不仅限于文献A、C、D、E中杀虫剂或杀螨剂,文献A:刘长令,柴宝山主编,新农药创制与合成,化学工业出版社,2013年,北京;文献C:郑桂玲,孙家隆,现代农药应用技术丛书:杀虫剂卷,化学工业出版社,2017年,北京;文献E:现代农药手册,刘长令,杨吉春,化学工业出版社,2018年,北京。
所述的噻唑锰锌新化合物的组合物,较优选:其含有活性成分A和任意一种活性成分B选自但不仅限于嘧菌酯、醚菌酯、吡唑醚菌酯、烯肟菌酯、肟菌酯、唑菌酯、氟嘧菌酯、苯醚菌酯、烯肟菌胺或苯氧菌胺、氰烯菌酯、Picarbutrazox、肟醚菌胺、唑菌胺酯、丁香菌酯、氯啶菌酯、UBF307、KZ165、苯醚甲环唑、烯唑醇、氟环唑、腈苯唑、氟硅唑、粉唑醇、戊唑醇、腈菌唑、环丙唑醇、戊菌唑、丙环唑、四氟醚唑、三唑醇、联苯三唑醇、三唑酮、叶菌唑、种菌唑、丙硫菌唑、亚胺菌唑、灭菌唑、环丙唑醇、甲霜灵、氟酰胺、双炔酰菌胺、啶酰菌胺、氟吡菌酰胺、氟醚菌酰胺、氰霜唑、氟菌唑、高效抑霉唑、咪唑菌酮、噁咪唑、稻温酯、腐霉利、异菌脲、乙烯菌核利、克菌丹、菌核净、霜霉威盐酸盐、苯菌灵、多菌灵、甲基硫菌灵、缬霉威、苯噻菌胺、井冈霉素、硫酸链霉素、春雷霉素、申嗪霉素、恶霜灵、恶霉灵、噁唑菌酮、啶菌噁唑、十三吗啉、烯酰吗啉、氟吗啉、嘧菌环胺、嘧霉胺、乙嘧酚、嘧菌胺、氟嘧菌胺、二氰蒽醌、丙氧喹啉、苯氧喹啉、代森联、福美双、福美锌、代森铵、代森锌、代森锰、代森锰锌、丙森锌、敌瘟磷、三乙膦酸铝、百菌清、稻瘟灵、咯菌腈或者氢氧化铜、松脂酸铜、去氢松脂酸铜、拌种咯、氟咯菌氰、咪鲜胺、咪鲜胺锰络合物、咪鲜胺铜络合物、蛇床子素、双苯菌胺、井冈霉素、硫酸链霉素、春雷霉素、梧宁霉素、申嗪霉素、多抗霉素、宁南霉素、硫酸链霉素、中生霉素、农抗120、金核霉素、长川霉素、春日霉素、毒氟磷、酚菌酮、丙硫咪唑、苯硫咪唑、氯氟醚菌唑、异丙芬三氟康唑、氟噻唑吡乙酮、烯丙苯噻唑、大黄素甲醚、大黄酚、氟噻唑吡乙酮、烯丙苯噻唑、双氯氰菌胺、大黄素甲醚、大黄酚、氟唑活化酯、二氯噁菌唑和甲磺酰菌唑、S-诱抗素、氨基寡糖素、吡啶硫酸锌、小檗碱、盐酸小檗碱、硫酸氢小檗碱、硫酸小檗碱、灭菌丹、异长叶烯酮肟内酰胺、大蒜素、愈创木酚、Quinolactacide、脱氢乙酸、氯溴异氰尿酸、香芹酚、噻氟菌胺、噻酰菌胺、噻唑菌胺、硅噻菌胺、呋吡菌胺、环氟菌胺、氟吡菌胺、苯酰菌胺、环酰菌胺、环丙酰菌胺、磺菌胺、甲磺菌胺、引唑磺菌胺、稻温酰胺、Bixafen、Fluxapyroxad、Sedaxane、辛唑嘧菌胺、Pyribencarb、Flutianil、Meptyldinocap、Pyriofenone、Fenpyrazamine、缬菌胺、Valifenalate、Tolprocarb、Isofetamid、Isopyrazam、Penflufen、Benzovindiflupyr、Tebufloquin、Oxathiapiprolin、糠菌唑、腈苯唑、氟喹唑、螺环菌胺、螺嘧环胺、乙膦铝、甲基立枯磷、异稻瘟净、精甲霜灵、高效苯霜灵、苦参碱、苦参素、噻菌铜或其水合物、噻森铜或其水合物、塞唑锌、塞唑锌水合物、苯菌酮、氟唑菌酰羟胺、茉莉酸甲酯、呋醚唑、戊环唑、乙环唑、三氟苯唑、高效烯唑醇、三唑酮、噻菌灵、抑霉唑、麦穗宁或植物生长调节剂或其药学上可接受的盐或溶剂化合物、定虫隆、伏虫隆、杀虫隆、氟虫脲、氟铃脲、氟螨脲、氟幼脲、氟啶脲、灭幼脲、除虫脲、丁醚脲、抑食肼、噻嗪酮、双氧威、或虫酰肼、杀螟磷、敌百虫、甲基对硫磷、氯唑磷、哒嗪硫磷、喹硫磷、三唑磷、噻唑硫磷、二嗪磷、辛硫磷、杀螟硫磷、甲基嘧啶磷、倍硫磷、杀螟腈、丙溴磷、毒死蜱、甲基毒死蜱、丙硫磷、甲丙硫磷、乐果、马拉硫磷、杀扑磷、丁硫克百威、丙硫克百威、戊氰威、仲丁威、异丙威、唑蚜威、抗蚜威、速灭威、混灭威、甲萘威、灭虫威、灭多威、或硫双灭多威、三氟氯氰菊酯、氟氯氰菊酯、联苯菊酯、甲氰菊酯、氰戊菊酯、氯氰菊酯、高效氯氰菊酯、溴氰菊酯、四溴菊酯、醚菊酯、或戊菊酯、阿维菌素、甲氨基阿维菌素、伊维菌素或其药学上可接受的盐中的任意一种或几种中的任意一种或几种,活性成分A与活性成分B重量比较优选为1︰80~80︰1,更较优选重量为1︰60~60︰1。
7.根据权利要求1-6中任一所述的噻唑锰锌新化合物,其特征在于:用于制备含有噻唑锰锌新化合物的药物组合物,该新化合物或其组合物与药学上可接受的载体制成药学上可接受的制剂,选自但不仅限于可湿性粉剂、水分散粒剂、悬浮剂、悬乳剂、水乳剂、颗粒剂、种子处理干粉剂、种子处理可分散粉剂、微囊悬浮剂、种子处理悬浮剂、种子处理微囊悬浮剂或者悬浮种衣剂。
8.根据权利要求6所述的广谱杀菌无公害促生长新锰化合物及其组合物,其特征在于:药学上可接受的载体选自但不仅限于湿润剂、粘合剂、分散剂、增稠剂、防冻剂、防腐剂、崩解剂、稳定剂、成膜剂、消泡剂、着色剂、润滑剂或助流剂、乳化剂、填料和/或水。
9.根据权利要求1-8中任一所述的噻唑锰锌新化合物或其组合物的用途,其特征在于:用于制备防治农作物上病害和或促进作物健康或生长发育的药物或用于保护工业材料不受病菌侵害的领域的药物中的应用。
10.根据权利要求1-9任一项所述的噻唑锰锌新化合物或其药物组合物的用途,农作物优选或选自但不仅限于以下种类:禾谷类小麦、大麦、水稻、玉米、高粱、甘薯;果树类苹果、梨、桃、山核桃、柑橘、葡萄、荔枝、香蕉、桂圆、芒果、枇杷;蔬菜类黄瓜、西瓜、吊瓜、丝瓜、甜瓜、菠菜、芹菜、番茄、辣椒、茄子、姜、葱、蒜、韭菜、甘蓝、大白菜、草莓、莴笋、菜豆、豇豆、蚕豆、萝卜、胡萝卜、马铃薯、山药、芋、莲藕、荸荠、茭白;糖料植物类甜菜、甘蔗;油料作物类大豆、花生、油菜、芝麻、向日葵;或诸如烟草、茶、可可豆、棉花、或缺锌或缺锰的作物;所述的病害选自但不仅限于:溃疡病、条斑病、锈病、颖枯病、网斑病、白粉病、霜霉病、疫病、叶斑病、全蚀病、雪霉病、黑穗病、叶枯病、褐斑病或稻瘟病、或缺锌或缺锰引起的病害中的一种或几种。
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