CN110856486A - 一种含二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂 - Google Patents
一种含二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂 Download PDFInfo
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- CN110856486A CN110856486A CN201810958264.6A CN201810958264A CN110856486A CN 110856486 A CN110856486 A CN 110856486A CN 201810958264 A CN201810958264 A CN 201810958264A CN 110856486 A CN110856486 A CN 110856486A
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Abstract
本发明涉及一种含二甲戊灵和丙炔氟草胺的微囊悬浮‑悬浮剂，其中二甲戊灵为微胶囊状态，丙炔氟草胺为悬浮状态，二甲戊灵和丙炔氟草胺的重量比为400:1‑1:5。本发明的微囊悬浮‑悬浮剂用于防治棉花、大蒜、小麦、玉米、水稻、大豆、花生、柑橘、葡萄、甘蔗、马铃薯、芹菜、草莓、大麦、向日葵、高粱田中的禾本科杂草及阔叶杂草，增效作用显著。
Description
技术领域
本发明涉及农药剂型领域，具体的涉及一种含二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂。
背景技术
微囊悬浮-悬浮剂是一种成分微囊化，另一种成分为悬浮剂，二者混合到一起后形成的一种稳定的剂型。是以高分子材料作为囊壁或囊膜，通过界面聚合、乳化交联聚合等各种化学、物理的方法，将囊芯的农药活性成分制备成微胶囊，然后，稳定的悬浮在水中，再和另外一种活性成分混合组成的一种具有微胶囊和悬浮剂共同优点的微囊悬浮-悬浮剂。例如可以在满足延长药效释放的同时具有速效性的特点，使农药活性成分不受光、微生物影响的同时提高药效、耐雨水冲刷等，是未来农药制剂技术发展的一类重要方向。
二甲戊灵(Pendimethalin)，又称二甲戊乐灵，苯胺类除草剂，可有效防除一年生禾本科和某些一年生阔叶杂草，广泛应用于玉米、大豆、花生、棉花、直播旱稻、马铃薯、烟草、蔬菜等多种作物，防治田间的稗草、马唐、狗尾草、早熟禾、藜、苋等杂草。
丙炔氟草胺(Flumioxazin)，是日本住友化学工业株式会社创制并开发的N-苯基邻氨甲酞亚胺类除草剂，可抑制原卟啉原氧化酶，导致光敏作用和细胞膜脂质的过氧化，对细胞膜共嫩和机构造成不可逆的破坏，大田中，茎叶处理后敏感杂草的茎叶坏死，日光照射后死亡，土壤处理后敏感的杂草芽坏死，在短暂的日光照射后死亡。
现有技术中，并没有二甲戊灵和丙炔氟草胺的组合物及其微囊悬浮-悬浮剂的相关报道。本发明要解决的一个技术问题就是制备一种组分合理，方便使用的二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂，以便达到减少施药次数，提高经济效益的目的。
发明内容
为了解决上述技术问题，本发明是通过以下技术方案实现的：
一种含二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂，其特征在于以二甲戊灵和丙炔氟草胺为活性成分，其中二甲戊灵为微胶囊状态，丙炔氟草胺为悬浮状态，二甲戊灵和丙炔氟草胺的重量比为400:1-1:5；优选地，二甲戊灵和丙炔氟草胺的重量比为400:1-1:2；二甲戊灵的重量含量为1％～60％，丙炔氟草胺的重量含量为1％～60％，囊壁材料的重量含量为1％～20％，引发剂的重量含量为0.1％～5％，助剂(表面活性剂、增稠剂、防冻剂、pH调节剂、消泡剂等)的重量含量为1％～25％，保护胶体0.1-5％，助溶剂的重量含量为1％～20％，溶剂补足至100％；
所述的囊壁材料由树脂形成，包括聚氨酯树脂、聚脲树脂、脲-甲醛树脂、三聚氰胺-甲醛树脂和苯酚-甲醛树脂，优选为多异氰酸酯、脲醛树脂；
所述的表面活性剂：阴离子型表面活性剂(包括烷基苯磺酸盐、烷磺酸盐、烯磺酸盐，单烷基硫酸酯盐、聚氧乙烯烷基醚硫酸酯盐、聚氧乙烯烷基苯基醚硫酸酯盐等)和两性表面活性剂(烷基甜菜碱、烷基酰胺甜菜碱、羰基甜菜碱、羟磺基甜菜碱等)的组合；
所述的引发剂为醋酸、盐酸、乙二胺、三乙胺、或三乙醇胺的一种或任意几种组合；
保护胶体包括：阿拉伯树胶、海藻酸、海藻酸盐。
防冻剂选自乙二醇、丙二醇、尿素、二甘醇、甘油等的一种或几种；
增稠剂选自黄原胶、聚乙烯醇、有机膨润土、羟甲基纤维素、硅酸镁铝等的一种或几种；
所述的助溶剂为甲醇、乙醇、丙酮、环己酮、二甲基亚砜、四氢呋喃等的一种或几种；
溶剂为水、N-甲基吡咯烷酮、环己醇、环氧大豆油、植物大豆油中的一种或几种，溶剂优选为水。
本发明的微囊悬浮-悬浮剂的制备方法为：在带保温和搅拌的反应容器中，将二甲戊灵溶于助溶剂中，然后加入阴离子型表面活性剂(烷基苯磺酸盐、烷磺酸盐、烯磺酸盐，单烷基硫酸酯盐、聚氧乙烯烷基醚硫酸酯盐、聚氧乙烯烷基苯基醚硫酸酯盐等)、溶剂和囊壁材料进行高速搅拌，搅拌速度为800～1600转/分钟，搅拌均匀后，加入引发剂，按40～150转/分钟的搅拌速度进行低速搅拌，且逐步升温至40-75℃，然后在40-75℃保温条件下按40～150转/分钟的搅拌速度搅拌3-6个小时，得二甲戊灵的微囊悬浮剂；再将丙炔氟草胺、两性表面活性剂(烷基甜菜碱、烷基酰胺甜菜碱、羰基甜菜碱、羟磺基甜菜碱等)、增稠剂、防冻剂、pH调节剂、消泡剂等经过高速剪切混合均匀，在球磨机中球磨1-4小时，使微粒粒径全部在5μm以下后加入到微胶囊悬浮剂的水相溶液中，按40～150转/分钟的搅拌速度搅拌0.5-3个小时，去离子水补足余量，制成本发明的微囊悬浮-悬浮剂。
本发明的微囊悬浮-悬浮剂可以用于防治禾棉花、大蒜、小麦、玉米、水稻、大豆、花生、柑橘、葡萄、甘蔗、马铃薯、芹菜、草莓、大麦、向日葵、高粱天的本科作物中的杂草。例如马唐、狗尾草、看麦娘、鲤肠、稗草、菵草等。
本发明的有益效果是：
1、增效作用明显，与各单剂相比，本发明的组合物具有明显的协同增效作用；
2、微囊悬浮-悬浮剂中创造性的加入保护胶体，可以在满足延长药效释放的同时具有速效性的特点，使农药活性成分不受光、微生物影响的同时提高药效、耐雨水冲刷等；
3、对哺乳动物安全，降低农药活性成分对作物的毒性，对目标作物安全。
附图说明
图1二甲戊灵·丙炔氟草胺微囊悬浮-悬浮剂在水中的释放曲线
具体实施方式
下面结合实施例对本发明进一步的说明，实施例中的百分比均为重量比，但本发明并不局限于此。
1、室内活性测定
为进一步了解本申请的混配对杂草的联合作用，发明人对二甲戊灵和丙炔氟草胺的混配进行了室内活性测定：
供试靶标：稗草
试验方法：采用温室盆栽法：将供试靶标杂草种子播种在塑料钵内盖上细土后放在温室内培养，待杂草长至2～4叶期进行茎叶喷雾处理，每钵喷药液1mL，每处理重复4次，并设不含药剂的处理为对照。处理后置于温室内培养，定期观察靶标杂草的生长情况，15天后计算防效，然后用最小二乘法计算ED50(95％置信区间)，并按孙云沛法计算共毒系数(CTC)。测试结果见表1。
表1不同配比二甲戊灵和丙炔氟草胺对稗草的联合作用测定结果
由表1可以看出，二甲戊灵和丙炔氟草胺的组合物在400:1-1:5的比例范围内对稗草具有明显的增效作用。
2、制备微囊悬浮-悬浮剂
1.1、乳化剂组合的选择
将常用的阴离子表面活性剂、非离子表面活性剂、两性表面活性剂和阳离子表面活性剂，用常用的正交实验法筛选优秀的乳化剂组合，结果见表2。
表2不同乳化剂的交叉乳化效果
注：+++表示乳化非常好，++表示乳化较好，+表示乳化一般，-表示不乳化。
上述结果表明，将不同的表面活性剂(阴离子型和两性)混合后，乳化效果最好，而单独使用一种乳化剂，乳化效果一般，当共同使用阳离子和阴离子表面活性剂时甚至出现不乳化的现象。因此，在选择表面活性剂的时候，选择将阴离子表面活性剂作为助剂1，将两性表面活性剂作为助剂2使用，以提高乳化效果。
1.2、制剂实施例
实施例1：40.1％二甲戊灵·丙炔氟草胺微囊悬浮-悬浮剂
配方：二甲戊灵40％，丙炔氟草胺0.1％，二甲基亚砜6％，乙二胺1％，十二烷基苯磺酸钠6％，海藻酸盐1％，烷基甜菜碱7％，多异氰酸酯7％，乙二醇0.1％，黄原胶0.5％，水补足至100％。
制备工艺：在带保温和搅拌的反应容器中，将二甲戊灵溶于二甲基亚砜中，然后加入十二烷基苯硫酸钠、海藻酸盐、溶剂和多异氰酸酯高速搅拌(1000转/分钟)，搅拌均匀后，加入乙二胺，低速搅拌(45转/分钟)，且逐步升温至70℃，然后70℃保温条件下低速搅拌(50转/分钟)5个小时，得含二甲戊灵的微囊悬浮剂；再将丙炔氟草胺、烷基甜菜碱、乙二醇、黄原胶经过高速剪切混合均匀，在球磨机中球磨2.5小时，使微粒粒径全部在5μm以下后加入到微胶囊悬浮剂的水相溶液中，低速搅拌(50转/分钟)1.5个小时，去离子水补足余量，制成微囊悬浮-悬浮剂。
按照与实施例1相同的制备工艺，制备实施例2。
实施例2：60％二甲戊灵·丙炔氟草胺微囊悬浮-悬浮剂
二甲戊灵20％，丙炔氟草胺40％，二甲基亚砜5％，乙二胺2％，十二烷基苯硫酸钠2％，海藻酸盐1％，烷基甜菜碱8％，多异氰酸酯8％，乙二醇0.1％，黄原胶0.5％，水补足至100％。
对比例1：按实施例1的制备方法制备对比例1，不同仅在于未加入海藻酸盐。
本发明实施例1和对比例1制备得到微囊悬浮-悬浮剂的基本指标见表3。
表3本发明的微囊悬浮-悬浮剂基本指标
上述测试说明本发明的微囊悬浮-悬浮剂的性能优异，分散、悬浮性好，具有微胶囊和悬浮剂的双重优点；与对比例1比较，悬浮率有了一定的提高。
1.3、二甲戊灵微胶囊在水中的释放速度测定
向每份微胶囊中加入10mL水，浸泡1天后离心分离液体和微胶囊，取出液体测定二甲戊灵的量，再向微胶囊中加入10mL水，这样重复6天，得到6天中每天的微胶囊释放的二甲戊灵。以释放时间为横坐标，释放率为纵坐标，做出释放率与释放时间关系的曲线，得到二甲戊灵微胶囊在水中的释放曲线，测试结果见图1。可见本发明的微胶囊在加入保护性胶体后，缓释性能优异，有效成分均匀释放，释放周期长。
3、田间药效试验
供试药剂：实施例1-2及对比例1的复配除草剂。
对照药剂：33％二甲戊灵乳油(对照药剂1)，50％丙炔氟草胺可湿性粉剂(对照药剂2)。
防治作物：棉花。
防除对象：狗尾草、苘麻、稗草、反枝苋
试验方法：试验于棉花田内进行，每个组别处理3次重复，处理面积约为20m2，按照试验小区的面积，准确称量好各种药剂，苗前喷雾处理。统计给药后30d杂草死亡情况，比较各种药剂的除草活性，此外，还要在药后40d内观察作物的生长情况，以考察药剂对作物是否有药害。结果见表4。
表4二甲戊灵·丙炔氟草胺微囊悬浮-悬浮剂药后30d除草效果
大田试验结果表明，二甲戊灵·丙炔氟草胺微囊悬浮-悬浮剂对棉花幼苗无药害。后续的调查中，所有供试的药剂中，本发明的微囊悬浮-悬浮剂持效期明显长于各单剂的持效期，说明本发明中所述成分做成微囊悬浮-悬浮剂之后显著延长了药剂的持效期。
Claims (8)
1.一种含二甲戊灵和丙炔氟草胺的微囊悬浮-悬浮剂，其特征在于以二甲戊灵和丙炔氟草胺为活性成分，其中二甲戊灵为微胶囊状态，丙炔氟草胺为悬浮状态，二甲戊灵和丙炔氟草胺的重量比为400:1-1:5。
2.根据权利要求1的微囊悬浮-悬浮剂，其特征在于二甲戊灵的重量含量为1％～60％，丙炔氟草胺的重量含量为1％～60％，囊壁材料的重量含量为1％～20％，引发剂的重量含量为0.1％～5％，助剂的重量含量为1％～25％，保护胶体0.1-5％，助溶剂的重量含量为1％～20％，溶剂补足至100％。
3.根据权利要求1-2任一所述的微囊悬浮-悬浮剂，其特征在于所述助剂为表面活性剂、增稠剂、防冻剂、pH调节剂、消泡剂中的一种或几种，所述的囊壁材料由树脂形成，包括聚氨酯树脂、聚脲树脂、脲-甲醛树脂、三聚氰胺-甲醛树脂和苯酚-甲醛树脂。
4.根据权利要求3所述的微囊悬浮-悬浮剂，其特征在于所述的囊壁材料为多异氰酸酯、脲醛树脂。
5.根据权利要求3所述的微囊悬浮-悬浮剂，其特征在于所述的表面活性剂为阴离子型表面活性剂和两性表面活性剂；所述阴离子型表面活性剂为烷基苯磺酸盐、烷磺酸盐、烯磺酸盐、单烷基硫酸酯盐、聚氧乙烯烷基醚硫酸酯盐、聚氧乙烯烷基苯基醚硫酸酯盐；所述两性表面活性剂为烷基甜菜碱、烷基酰胺甜菜碱、羰基甜菜碱、羟磺基甜菜碱；保护胶体包括：阿拉伯树胶、海藻酸、海藻酸盐。
6.根据权利要求2-5任一所述的微囊悬浮-悬浮剂，其特征在于：所述的引发剂为醋酸、盐酸、乙二胺、三乙胺、或三乙醇胺的一种或任意几种组合；所述防冻剂选自乙二醇、丙二醇、尿素、二甘醇、甘油的一种或几种；所述增稠剂选自黄原胶、聚乙烯醇、有机膨润土、羟甲基纤维素、硅酸镁铝的一种或几种；所述的助溶剂为甲醇、乙醇、丙酮、二甲基亚砜、四氢呋喃、环己酮的一种或几种；所述溶剂为：水、N-甲基吡咯烷酮、环己醇、环氧大豆油、植物大豆油中的一种或几种。
7.权利要求1-6任一所述的微囊悬浮-悬浮剂的制备方法：其特征在于：在带保温和搅拌的反应容器中，将二甲戊灵溶于助溶剂中，然后加入阴离子表面活性剂、溶剂和囊壁材料进行高速搅拌，搅拌速度为800～1600转/分钟，搅拌均匀后，加入引发剂，按40～150转/分钟的搅拌速度进行低速搅拌，且逐步升温至40-75℃，然后在40-75℃保温条件下按40～150转/分钟的搅拌速度搅拌3-6个小时，得二甲戊灵的微囊悬浮剂；再将丙炔氟草胺、两性表面活性剂、增稠剂、防冻剂、pH调节剂、消泡剂，经过高速剪切混合均匀，在球磨机中球磨1～4小时，使微粒粒径全部在5μm以下后加入到微胶囊悬浮剂的水相溶液中，按40～150转/分钟的搅拌速度搅拌0.5-3个小时，去离子水补足余量，制成微囊悬浮-悬浮剂。
8.权利要求1-6任一所述的微囊悬浮-悬浮剂用于防治棉花、大蒜、小麦、玉米、水稻、大豆、花生、柑橘、葡萄、甘蔗、马铃薯、芹菜、草莓、大麦、向日葵、高粱田禾本科杂草及阔叶杂草的应用。
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