CN102245019B - 含农药树脂组合物的制造方法 - Google Patents
含农药树脂组合物的制造方法 Download PDFInfo
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- CN102245019B CN102245019B CN200980149273.XA CN200980149273A CN102245019B CN 102245019 B CN102245019 B CN 102245019B CN 200980149273 A CN200980149273 A CN 200980149273A CN 102245019 B CN102245019 B CN 102245019B
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- maleic anhydride
- white carbon
- anhydride copolymer
- styrene maleic
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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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
-
- 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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
- A01N43/08—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings with oxygen as the ring hetero atom
-
- 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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
-
- 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
- A01N43/74—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 five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/78—1,3-Thiazoles; Hydrogenated 1,3-thiazoles
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- A—HUMAN NECESSITIES
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Abstract
依照本发明,提供能够容易地设计具有期望的溶出率历程的含农药的树脂组合物并且能够制造该含农药树脂组合物的方法。本发明涉及含农药树脂组合物的制造方法,该方法包括:按照以啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的组合物中的啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA满足0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%的方式,分别选择啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA;混合啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑使其达到以上选择的含有率AcSA和含有率CaSA。
Description
技术领域
本发明涉及控制了农药活性成分的溶出的含农药树脂组合物的制造方法。
本申请以2008年12月12日在日本申请的特愿2008-317194号为基础要求优先权,将其内容援引于此。
背景技术
含有农药活性成分的固体状农药制剂,例如散布在水田等的水中来使用。农药活性成分显示高水溶性的农药制剂的情况下,有时农药活性成分从该农药制剂中过快地溶出。如果农药活性成分的溶出速度过快,则有时存在发生药害、无法得到充分的残效性(residual effect)等问题。
为了解决这种问题,以往已提出并开发出控制了农药活性成分的溶出的农药制剂。例如在专利文献1中提出了一种含农药树脂组合物,其特征在于,将(a)至少一种水易溶性农药原药、(b)熔点或软化点为50℃以上且小于130℃的非水溶性物质或水难溶性物质、以及(c)白炭黑在(b)的熔点或软化点~130℃的温度下加热混合而得到。
另外,在专利文献2中,提出了一种含有含农药树脂组合物、进行了控制溶出的漂浮移动性良好的水面施用农药制剂和其制造方法,以及进行了控制溶出的农药组合物,该含农药树脂组合物的特征在于,由农药活性成分、聚乙烯和疏水性二氧化硅构成。
但是,即使是专利文献1和2所述的农药组合物或农药制剂,有时也并不能说农药活性成分的溶出控制充分,期望开发出更充分地控制了农药活性成分的溶出的农药组合物。
另外,在专利文献3中,提出了含有农药活性成分、苯乙烯马来酸酐共聚物和溶出控制剂(水溶性高分子、氧化硅或表面活性剂)的组合物形成相溶状态或基质的农药制剂。另外,在专利文献4中,提出了含有农药活性成分、苯乙烯马来酸酐共聚物和作为溶出控制剂的脂肪酸金属盐的组合物形成相溶状态或基质的农药制剂。在专利文献3和4中,作为比较例记载了一种组合物,其使用了50质量%的亲水性白炭黑。该组合物的初期突释(initial burst)(添加到水中后经过15分钟时的溶出率)大,而且在经过72小时时变为溶出率不再增加的所谓滞留(deadstock)状态。
现有技术文献
专利文献
专利文献1:日本特开平8-92007号公报
专利文献2:日本特开平11-315004号公报
专利文献3:WO2006/013972
专利文献4:WO2007/091494
发明内容
但是,即使是上述专利文献3中提出的含有农药活性成分、苯乙烯马来酸酐共聚物和溶出控制剂的组合物,也必须试验农药活性成分、苯乙烯马来酸酐共聚物和溶出控制剂的组成比,调整成最佳组成比以使初期突释为适度的大小并且即使在经过72小时时溶出率也还继续增加。因此,要设计出具有期望的溶出率历程的含农药树脂组合物就需要很长时间。
所以,本发明的目的在于提供能够容易地设计具有期望的溶出率历程的含农药树脂组合物并且能够制造该含农药树脂组合物的方法。
因而,本发明人等鉴于这种现有技术的实际情况进行了认真研究,结果发现,通过制备组成比不同的多种组合物,分别求出它们的溶出率历程,用线性最小二乘法解析溶出率和组成比的数据,导出用于由组成比推出溶出率的式子,按照该推定式设计组成比,从而能够容易地制造具有期望的溶出率历程的含农药树脂组合物。
另外,发现即使是专利文献3、4等中溶出率历程不适当的比较例中使用亲水性白炭黑的组合物,如果按照本发明的方法来选择组成比,也能够容易地设计并制造初期突释具有适度大小且即使在经过72小时时溶出率也还继续增加的组合物。本发明是以这些知识为基础完成的。
即,本发明包含以下方案。
[1]一种含农药树脂组合物的制造方法,其包括:
以任意组成比混合在25℃的水中的溶解度为100ppm以上的农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑,制备多种组合物,
将该组合物各自造粒成平均粒径为10~25μm,测定将其添加到25℃的蒸馏水中后经过t时间时的农药活性成分A的溶出率Y(t)[质量%],
用线性最小二乘法解析以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率Ac[质量%]和白炭黑的含有率Ca[质量%]、与上述测定的溶出率Y(t),求出式(I),
式(I):Yev(t)=a(t)×AcS+b(t)×CaS+c(t)
(其中,式(I)中的Yev(t)表示添加后经过t时间时的农药活性成分A的推定溶出率[质量%];a(t)、b(t)和c(t)表示用线性最小二乘法求得的经过时间t的系数;自变量t表示添加后的经过时间[小时];AcS和CaS表示以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率[质量%]和白炭黑的含有率[质量%]),
在所述式(I)中,添加到25℃的蒸馏水中后经过15分钟时的农药活性成分A的推定溶出率Yev(0.25)成为40质量%以下的、农药活性成分A的含有率AcS在5质量%~35质量%的范围选择、白炭黑的含有率CaS在0.1质量%以上的范围选择;
混合农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑使其达到以上选择的含有率AcS和含有率CaS。
[2]如上述[1]所述的含农药树脂组合物的制造方法,其中,所述农药活性成分A是新烟碱类化合物。
[3]如上述[1]所述的含农药树脂组合物的制造方法,其中,所述农药活性成分A是选自烯啶虫胺、吡虫啉、啶虫脒、噻虫嗪、噻虫胺、噻虫啉和呋虫胺中的至少一种化合物。
[4]一种含农药树脂组合物的制造方法,其包括:
从满足0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%的范围分别选择以啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA;
混合啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑使其达到上述选择的含有率AcSA和含有率CaSA。
[5]如上述[1]~[4]中任一项所述的含农药树脂组合物的制造方法,其中,白炭黑的疏水度为20%以下。
[6]如上述[1]~[5]中任一项所述的含农药树脂组合物的制造方法,其中,所述苯乙烯马来酸酐共聚物混合树脂是苯乙烯马来酸酐共聚物与具有来自松香或其衍生物、或者、水杨酸或其衍生物的重复单元的聚合物的混合物。
[7]一种含农药树脂组合物,由上述[1]~[6]中任一项所述的制造方法制得。
[8]一种含农药树脂组合物,其含有啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑,其中,以啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA满足0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%。
[9]一种原料用药物粉末(bulk powder),由上述[7]或[8]所述的合农药树脂组合物构成。
[10]一种农药制剂,含有上述[9]所述的原料用药物粉末。
[11]如上述[10]所述的农药制剂,其中,原料用药物粉末的平均粒径为200μm以下。
[12]一种农药制剂的制造方法,包括将上述[7]或[8]所述的含农药树脂组合物造粒。
[13]如上述[12]所述的农药制剂的制造方法,其中,用选自转动造粒法、搅拌造粒法、挤出造粒法、压延造粒法、破碎造粒法和流动造粒法中的至少一种方法进行造粒。
依照本发明的含农药树脂组合物的制造方法,能够容易地设计并制造将农药活性成分短期内大量溶出的现象、即初期突释抑制到适度的大小,并且抑制了本来应该溶出的农药活性成分没有全部溶出而残留的现象、即滞留的含农药树脂组合物和农药制剂。而且,本发明的含农药树脂组合物和农药制剂,既维持了残效性又没有因农药活性成分的作物残留量增加而发生药害的这种情况,进而能够防止在环境中的残留。另外,除上述效果以外,通过提高光稳定性、控制挥散性、提高耐雨性等而具有提高农药活性成分的残效性和减少向环境中的流失的效果以及减少总散布药量、减少散布次数、减轻对散布者的毒性等效果,尤其可用作种子处理剂和土壤处理剂。
具体实施方式
[含农药树脂组合物]
本发明的含农药树脂组合物的制造方法包括:
以任意组成比混合在25℃的水中的溶解度为100ppm以上的农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑,制备多种组合物,将该组合物各自造粒成平均粒径为10~25μm,测定将其添加到25℃的蒸馏水中后经过t时间时的农药活性成分A的溶出率Y(t)[质量%],
用线性最小二乘法解析以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率Ac[质量%]和白炭黑的含有率Ca[质量%]、与上述测定的溶出率Y(t),求出式(I):Yev(t)=a(t)×AcS+b(t)×CaS+c(t)(其中,式(I)中的Yev(t)表示添加后经过t时间时的农药活性成分A的推定溶出率[质量%];a(t)、b(t)和c(t)表示用线性最小二乘法求得的经过时间t的系数;自变量t表示添加后的经过时间[小时];AcS和CaS表示以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率[质量%]和白炭黑的含有率[质量%]),
在所述式(I)中,添加到25℃的蒸馏水中后经过15分钟时的农药活性成分A的推定溶出率Yev(0.25)成为40质量%以下的、农药活性成分A的含有率AcS从5质量%~35质量%的范围选择、白炭黑的含有率CaS从0.1质量%以上的范围选择;混合农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑使其达到上述选择的含有率AcS和含有率CaS。
(农药活性成分A)
本发明中所用的农药活性成分A在25℃的水中的溶解度为100ppm以上、优选为500ppm以上。作为该农药活性成分A,可使用杀菌剂、杀虫剂、杀螨剂、植物生长调节剂、除草剂、杀鼠剂、抗茵剂、抗霉剂、抗藻剂等一般作为农药使用的化合物。可以单独使用或混合2种以上使用这些化合物。
作为农药活性成分A,可例示烯啶虫胺(水溶解度:590000ppm(20℃))、啶虫脒(水溶解度:4250ppm(25℃))、吡虫啉(水溶解度:510ppm(20℃))、噻虫嗪(水溶解度:4100ppm(20℃))、噻虫胺(水溶解度:327ppm(20℃))、噻虫啉(水溶解度:185ppm(20℃))、呋虫胺(水溶解度:54300ppm(20℃))等新烟碱类化合物;乙酰甲胺磷(水溶解度:790000ppm(20℃))、N’-(4-氯邻甲基苯甲酰)-N,N-二甲基甲酰胺(水溶解度:250ppm(20℃))、DDVP(水溶解度:约18000ppm(25℃))等磷系化合物;恶虫威(水溶解度:280ppm(20℃))、杀螟丹(水溶解度:200000ppm(20℃))、乙硫苯威(水溶解度:1800ppm(20℃))等氨基甲酸酯类化合物;杀线威(水溶解度:280000ppm(25℃))、灭多威(水溶解度:58000ppm(20℃))、D-D(水溶解度:2000ppm(20℃))等其它杀虫性化合物等。在它们中,优选新烟碱类化合物,更优选烯啶虫胺、啶虫脒、吡虫啉、噻虫嗪、噻虫胺、噻虫啉或呋虫胺,特别优选啶虫脒。
(苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂)
本发明中所用的苯乙烯马来酸酐共聚物包括使苯乙烯与马来酸酐发生共聚反应而得到的树脂及其衍生物。作为该衍生物,可举出将苯乙烯与马来酸酐发生共聚反应而得到的树脂用醇进行酯化的产物、中和该酯化物的产物、用磺化剂磺化的产物、用胺进行酰亚胺化的产物等。作为该衍生物,优选用醇进行酯化的产物。苯乙烯马来酸酐共聚物的聚合方式,没有特别限定,既可以是单体单元的重复为无规或嵌段中的任一种的方式,也可以是分子链的形态为直链或支链状中的任一种的方式。作为支链状的分子链,例如可以通过接枝聚合得到。
苯乙烯马来酸酐共聚物混合树脂是所述苯乙烯马来酸酐共聚物与其它树脂的混合物。作为可供混合的其它树脂,可举出聚烯烃系树脂、聚(甲基)丙烯酸系树脂、聚苯乙烯系树脂、聚酯系树脂、聚氯乙烯系树脂、聚偏氯乙烯树脂、聚酰胺树脂、聚缩醛树脂、聚碳酸酯树脂、聚氨酯树脂等。
作为聚烯烃系树脂,可举出低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、聚乙烯蜡、乙烯·α-烯烃共聚物弹性体等聚乙烯树脂;乙烯·乙酸乙烯酯共聚物、乙烯·(甲基)丙烯酸共聚物、聚丙烯、丙烯·乙烯共聚物、乙烯·丙烯共聚物、聚丁烯、乙烯·丙烯·丁二烯共聚物等。
作为聚(甲基)丙烯酸系树脂,可举出甲基丙烯酸甲酯均聚物;使丙烯酸烷基酯或甲基丙烯酸烷基酯与乙烯、苯乙烯、α-甲基苯乙烯、丙烯腈等其它单体共聚而得到的(甲基)丙烯酸系共聚物;使(甲基)丙烯酸烷基酯、丁二烯、苯乙烯和丙烯腈共聚而得到的耐冲击性(甲基)丙烯酸树脂等。
作为聚苯乙烯系树脂,可举出苯乙烯的均聚物;高抗冲聚苯乙烯(HIPS)、甲基丙烯酸甲酯·丁二烯·苯乙烯共聚物、苯乙烯·(甲基)丙烯酸共聚物、苯乙烯·丙烯腈共聚物等。
作为聚酯系树脂,可例示聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯等芳香族聚酯;以及在涂料用树脂等中使用的通过二醇与二羧酸的缩合而得到的聚酯等,其中,优选由脂肪族系的二醇与二羧酸的缩聚而得到的脂肪族聚酯。
另外,可例示以3-羟基丁酸酯·3-羟基戊酸酯共聚物为代表的聚羟基链烷酸酯共聚物、以聚乳酸为代表的单一羟基链烷酸酯得到的均聚物、聚己内酯、聚乳酸与聚酯的共聚物等生物分解性树脂。
作为聚氯乙烯系树脂,可举出氯乙烯均聚物;氯乙烯与乙烯、丙烯、丙烯腈、偏氯乙烯、乙酸乙烯酯等其它单体的共聚物等。
在这些树脂中,从与农药活性成分的相性和农药活性成分的溶出控制性方面考虑,特别优选具有来自松香或其衍生物、或者、水杨酸或其衍生物的重复单元的聚合物。
松香是从松科植物得到的天然树脂。其主要成分是松香酸和其异构体等。已知因为松香酸的羧基的反应性高,所以可以通过与含有环氧基、硅烷醇基、烷氧基硅烷基、羟基、氨基、亚氨基、异氰酸酯基、嵌段化异氰酸酯基、环碳酸酯基、乙烯基醚基、乙烯基硫醚基、氨基羟甲基、烷基化氨基羟甲基、缩醛基、缩酮基等官能团的化合物反应得到各种松香衍生物。作为松香衍生物,可例示妥尔松香(tall rosin)、松香改性苯酚、松香改性马来酸等。
作为具有来自水杨酸或其衍生物的重复单元的聚合物,可举出水杨酸或其衍生物缩合而得到的聚合物、水杨酸或其衍生物与其它羟基羧酸缩合而得到的聚合物等。作为市售的具有来自水杨酸或其衍生物的重复单元的聚合物,可例示POVIRON公司制的线型聚水杨酸酯等。
苯乙烯马来酸酐共聚物混合树脂在苯乙烯马来酸酐共聚物与其它树脂的混合比例方面没有特别限定,例如在使用具有来自松香或其衍生物、或者、水杨酸或其衍生物的重复单元的聚合物作为其它树脂时,以混合树脂的重量为基准,苯乙烯马来酸酐共聚物的混合比例优选是30~99质量%、更优选是50~99质量%。
(白炭黑)
本发明中所用的白炭黑被称为合成无定形二氧化硅、含水硅酸、湿式二氧化硅或合成硅酸等。优选白炭黑的一次粒子的平均粒径是0.5~100nm。另外,白炭黑通常具有Si-O的网状结构,但本发明中优选不具有一定的晶体结构(即,无定形二氧化硅粉末)。白炭黑优选有亲水性。具体而言,优选白炭黑的疏水度在20%以下,更优选在5%以下,特别优选为0%。
应予说明,疏水度可通过以下程序测定。首先在200ml的烧杯中称取白炭黑0.2g,在其中加入蒸馏水50ml,用磁力搅拌器搅拌。在搅拌的溶液中用滴管慢慢滴加甲醇。将确认没有浮在溶液表面的粉体的点作为终点,由下式算出疏水度。
疏水度(%)=x/(50+x)×100
其中,x是甲醇的滴加量(ml)。
作为亲水性白炭黑的市售品,可例示DSL.JAPAN公司制的商品名“Carplex#80”、“Carplex#67”、“Carplex#1120”、和“Carplex XR”;TosohSilica公司制的商品名“Nipsil NS-T”、“Nipsil NS-K”、和“Nipsil NA”;日本AEROSIL公司制的商品名“AEROSIL200”;株式会社Tokuyama制的商品名“Fineseal”、和“TOKUSIL”。
在本发明的含农药树脂组合物的制造方法中,首先,以任意组成比混合前述的农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂(以下,有时记载为“水难溶性树脂”)和白炭黑,制备多种组合物。
该组合物的制备方法,只要是农药活性成分A、水难溶性树脂和白炭黑被均匀混合的方法,就没有特别限定,在本发明中,优选熔融法、溶剂法、和pH析出法。无论哪一种制备方法,都优选使农药活性成分A或啶虫脒溶解或分散在由水难溶性树脂形成的基质中。
熔融法是具有将农药活性成分A、水难溶性树脂和白炭黑加热熔融进行混炼的工序的制备方法。
作为熔融法,更具体而言,可例示下述方法:将水难溶性树脂加到混炼机等中使其加热熔融,在其中分别添加农药活性成分A和白炭黑进行熔融混炼的方法;将农药活性成分A、水难溶性树脂和白炭黑混合,用加热式连续混炼机等加热熔融该混合物进行混炼的方法。
熔融法中的熔融时的温度只要是农药活性成分A不分解且与水难溶性树脂充分地相溶或均匀地混合的温度就没有特别限制。在熔融法中,为了避免因热导致的农药活性成分A的分解,优选在尽可能低的温度下且在短时间内进行熔融混炼。但是,如果熔融时的温度过低,则熔融物的粘性变高,有时很难形成充分的相溶或均匀的混合状态。因此,优选添加表面活性剂来进行熔融。通过添加表面活性剂,有时即使是粘性高的状态也能够得到均匀的组合物。
溶剂法是具有使农药活性成分A、水难溶性树脂和白炭黑溶解或分散在有机溶剂中匀化后、馏去有机溶剂的工序的制备方法。
作为溶剂法,更具体而言,可例示如下方法:在容器中加入溶剂,分别添加水难溶性树脂和农药活性成分A,边加热边搅拌使水难溶性树脂和农药活性成分A完全溶解在溶剂中,在其中添加白炭黑并使其分散,接着完全馏去溶剂。
溶剂法中使用的溶剂只要是能够溶解所用的水难溶性树脂和农药活性成分A且它们能够稳定存在的溶剂,就没有特别限定。例如可例示二甲苯、甲苯、烷基萘、苯基二甲苯基乙烷、煤油、轻油、己烷、环己烷等芳香族或脂肪族烃类;氯苯、二氯甲烷、二氯乙烷、三氯乙烷等卤代烃类;甲醇、乙醇、异丙醇、丁醇、己醇、乙二醇等醇类;二乙醚、乙二醇二甲醚、四氢呋喃、二烷等醚类;乙酸乙酯、乙酸丁酯等酯类;丙酮、甲基乙基酮、甲基异丁基酮、环己酮等酮类;乙腈、异丁腈等腈类;二甲基亚砜、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等酰胺类;大豆油、棉籽油等植物油等。在它们中,特别优选二氯甲烷、丙酮和甲醇。
溶剂法中使用的溶剂的量只要是可溶解农药活性成分A和水难溶性树脂的量,就没有特别限定,优选相对于农药活性成分A和水难溶性树脂的合计量为10~20质量%的范围。
溶解于尽可能少量的溶剂进行制造的方式可节省馏去溶剂所浪费的成本,因而优选,但少量的溶剂使得粘性增加,有时难以通过搅拌得到相溶或均匀的混合状态的树脂。因此,优选添加表面活性剂使其溶解于溶剂中。通过添加表面活性剂,有时即使是粘性高的状态也能够得到均匀的组合物。
将农药活性成分A和水难溶性树脂溶解在溶剂中时的温度优选是20~40℃以确保农药活性成分A稳定。
作为溶剂的馏去方法,可使用通常的方法。具体而言,可例示减压馏去、加热馏去、减压加热馏去等。另外,可例示使用喷雾干燥造粒机的方法。另外,可例示添加对农药活性成分A和水难溶性树脂的不良溶剂使农药活性成分A和水难溶性树脂析出、进行过滤的方法。
在熔融法和溶剂法中,将农药活性成分A、水难溶性树脂和白炭黑熔融或溶解的顺序没有特别限制,可以同时进行也可以先后进行。另外,也可以分几次熔融或溶解规定量的农药活性成分A、水难溶性树脂和白炭黑。另外,也可以根据组成比来并用溶剂法和熔融法。
pH析出法是具有制备含有水难溶性树脂、农药活性成分A和白炭黑的碱性液体,接着将该液体的pH调成酸性的工序的制备法。
作为pH析出法,更具体而言,可例示如下方法:将水难溶性树脂和农药活性成分添加到氨溶液中使其完全溶解,在其中添加白炭黑使其分散,接着添加盐酸将液体的pH调成酸性使成分析出,过滤、干燥该析出物。
将通过上述方法制备的组合物造粒成适合测定溶出率的平均粒径(10~25μm)。造粒可以用选自转动造粒法、搅拌造粒法、挤出造粒法、压延造粒法、破碎造粒法和流动造粒法中的至少一种方法进行。在组合物的造粒中,可以添加表面活性剂等造粒助剂。
本发明中,为了调节平均粒径,优选采用破碎造粒法的造粒。在破碎造粒法中,可以使用通过挤出成形制造粒剂时使用的破碎机、可湿性粉剂制造中使用的销棒粉碎机(pin mill)或喷射磨等粉碎机。另外,用溶剂法制造含农药树脂组合物时,可以通过使用喷雾干燥造粒机来同时进行溶剂馏去和造粒。
溶出率的测定如下进行。将造粒好的组合物各自含有10mg农药活性成分A的样品精确称量到100ml的管瓶中,在其中添加25℃的蒸馏水80ml和作为内标的4-羟基苯甲酸甲酯溶液(500mg/L蒸馏水)20ml,加盖进行5次颠倒,在25℃的恒温槽静置直到取样。在经过规定时间时进行5次颠倒,接着取样约0.7ml(用0.45μm的过滤器过滤)。用HPLC测定取样的溶液中的农药活性成分A的浓度,以相对于假定组合物中的农药活性成分A全部溶解在水中时的农药活性成分A的浓度的百分率算出溶出率。
通过该测定,得到多个表示以农药活性成分A、水难溶性树脂和白炭黑的合计质量为基准的组合物中农药活性成分A的含有率Ac[质量%]和白炭黑的含有率Ca[质量%]与添加后经过t时间时的实测溶出率Y(t)的关系的数据。
用线性最小二乘法解析这些数据,求出
式(I):Yev(t)=a(t)×AcS+b(t)×CaS+c(t)
(其中,式(I)中的Yev(t)表示添加后经过t时间时的农药活性成分A的推定溶出率[质量%];a(t)、b(t)和c(t)表示用线性最小二乘法求得的经过时间t的系数;自变量t表示添加后的经过时间[小时];AcS和CaS表示以农药活性成分A、水难溶性树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率[质量%]和白炭黑的含有率[质量%])。
用上述的算出方法,可以得到求出添加到25℃的蒸馏水中后经过15分钟时的农药活性成分A的推定溶出率Yev(0-25)的式(Ia);求出添加到25℃的蒸馏水中后经过120小时时的农药活性成分A的推定溶出率Yev(120)的式(IIa)。
式(Ia):
Yev(0.25)=a(0.25)×Ac+b(0.25)×Ca+c(0.25)
式(Ⅱa):
Yev(120)=a(120)×Ac+b(120)×Ca+c(120)
例如,当使用啶虫脒作为农药活性成分A、使用亲水性白炭黑作为白炭黑时,可以通过上述的算出方法得到式1a、式2a。
式1a:YevA(0.25)=0.524×AcSA+1.422×CaSA-6.009
式2a:YevA(120)=1.545×AcSA+2.945×CaSA-7.562
应予说明,式1a和式2a中的、YevA(0.25)是添加到25℃的蒸馏水中后经过15分钟时的啶虫脒的推定溶出率;YevA(120)是添加到25℃的蒸馏水中后经过120小时时的啶虫脒的推定溶出率;AcSA是以啶虫脒、水难溶性树脂和亲水性白炭黑的合计质量为基准的组合物中的啶虫脒的含有率;CaSA是以啶虫脒、水难溶性树脂和亲水性白炭黑的合计质量为基准的组合物中的亲水性白炭黑的含有率。
接着,满足推定溶出率Yev(0.25)≤40质量%、优选满足6质量%≤推定溶出率Yev(0.25)≤20质量%的、以农药活性成分A、水难溶性树脂和白炭黑的合计质量为基准的组合物中的农药活性成分A的含有率AcS从5质量%~35质量%的范围选择、以农药活性成分A、水难溶性树脂和白炭黑的合计质量为基准的组合物中的白炭黑的含有率CaS从0.1质量%以上的范围选择。
例如,当使用啶虫脒作为农药活性成分A、使用亲水性白炭黑作为白炭黑时,从满足推定溶出率YevA(0.25)=0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%的范围分别选择AcSA和CaSA。
例如,当啶虫脒的含有率选择30质量%时,亲水性白炭黑的含有率是0.1质量%~21.30质量%。
同样,当啶虫脒的含有率选择5质量%时,亲水性白炭黑的含有率是0.1质量%~30.51质量%。
同样,当啶虫脒的含有率选择35质量%时,亲水性白炭黑的含有率是0.1质量%~19.46质量%。
最后,混合农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑使其达到以上选择的农药活性成分A的含有率AcS和白炭黑的含有率CaS,制备目标含农药树脂组合物。作为该制备方法,可举出前述的熔融法、溶剂法、pH析出法等。应予说明,为了提高溶出率的控制精度,优选采用与为求出推定溶出率而制备的组合物的制备方法相同的方法来进行目标含农药树脂组合物的制备。
通过以如上所述的推定溶出率Yev(t)为基础的制造方法而得到的本发明的含农药树脂组合物优选是以下组合物,即以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及白炭黑的合计质量为基准的农药活性成分A的含有率是5质量%~35质量%且白炭黑的含有率是0.1质量%以上,将造粒成平均粒径为10~25μm的组合物添加到25℃的蒸馏水中后经过15分钟时农药活性成分A的实测溶出率Y(0.25)是40质量%以下。
本发明的含农药树脂组合物可以制成适度大小的粒子以形成用于农药制剂的原料用药物粉末。含农药树脂组合物的原料用药物粉末的平均粒径依据使用目的而各自不同,没有限定,优选在200μm以下,特别优选为1~100μm。另外,作为用于农药制剂的原料用药物粉末,可以组合使用2种以上粒度、组成不同的本发明的含农药树脂组合物。通过这样进行组合,可以调节农药活性成分A的溶出速度。另外,也可以分别使用2种以上的农药活性成分A、得到与它们相应的含农药树脂组合物,将它们适当混合作为农药制剂用的原料用药物粉末。
[农药制剂]
本发明的农药制剂含有至少一种本发明的含农药树脂组合物。
在本发明的农药制剂中,可以使用与使用目的相应的制剂基材。作为制剂基材,可举出水溶性高分子、表面活性剂等溶出控制剂;碳酸钙、氯化钾、硫酸钠等无机盐类;柠檬酸、苹果酸、富马酸、硬脂酸等有机酸及它们的盐;乳糖、蔗糖等糖类;氧化铝粉、硅胶、沸石、羟磷灰石、磷酸锆、磷酸钛、氧化硅、氧化钛、氧化锌、水滑石、高岭土、蒙脱石、滑石、粘土等无机添加剂;没食子酸正丙酯、丁基羟基茴香醚等抗氧化剂;三聚磷酸钠、磷酸二氢钠、磷酸铵等pH调节剂、缓冲剂;食用蓝色一号、亚甲蓝、颜料红48等着色剂;此外,可举出防腐剂、滑剂、紫外线吸收剂、抗静电剂等。
作为水溶性高分子,可例示淀粉、明胶等源自天然的水溶性高分子;羧甲基纤维素、甲基纤维素、羟丙基纤维素等半合成的纤维素衍生物;或者,聚乙烯基醇、聚丙烯酸系聚合物、聚丙烯酰胺、聚乙二醇等合成系水溶性高分子等。
表面活性剂只要是通常的农药制剂中能够使用的表面活性剂,就没有限定,具体而言,作为非离子性表面活性剂,可举出山梨糖醇酐脂肪酸酯(C12~18)、POE山梨糖醇酐脂肪酸酯(C12~18)、蔗糖脂肪酸酯等糖酯型表面活性剂;POE脂肪酸酯(C12~18)、POE树脂酸酯、POE脂肪酸二酯(C12~18)等脂肪酸酯型表面活性剂;POE烷基醚(C12~18)等醇型表面活性剂;POE烷基(C8~12)苯基醚、POE二烷基(C8~12)苯基醚、POE烷基(C8~12)苯基醚甲醛缩合物等烷基苯酚型表面活性剂;聚氧乙烯·聚氧丙烯嵌段聚合物、烷基(C12~18)聚氧乙烯·聚氧丙烯嵌段聚合物醚等聚氧乙烯·聚氧丙烯嵌段聚合物型表面活性剂;POE烷基胺(C12~18)、POE脂肪酰胺(C12~18)等烷基胺型表面活性剂;POE脂肪酸二苯基醚等双酚型表面活性剂;POA苄基苯基(或苯基苯基)醚、POA苯乙烯基苯基(或苯基苯基)醚等多芳香环型表面活性剂;POE醚和酯型硅和氟系表面活性剂等硅系、氟系表面活性剂;POE蓖麻油、POE硬化蓖麻油等植物油型表面活性剂,
作为阴离子性表面活性剂,可举出烷基硫酸盐(C12~18,Na、NH4、链烷醇胺)、POE烷基醚硫酸盐(C12~18,Na、NH4、链烷醇胺)、POE烷基苯基醚硫酸盐(C12~18,NH4、链烷醇胺、Ca)、POE苄基(或苯乙烯基)苯基(或苯基苯基)醚硫酸盐(Na、NH4、链烷醇胺)、聚氧乙烯·聚氧丙烯嵌段聚合物硫酸盐(Na、NH4、链烷醇胺)等硫酸盐型表面活性剂;石蜡(链烷)磺酸盐(C12~22,Na、Ca、链烷醇胺)、AOS(C14~16,Na、链烷醇胺)、二烷基磺基琥珀酸盐(C8~12,Na、Ca、Mg)、烷基苯磺酸盐(C12,Na、Ca、Mg、NH4、烷基胺、链烷醇、胺、环己基胺)、单或二烷基(C3~6)萘磺酸盐(Na、NH4、链烷醇胺、Ca、Mg)、萘磺酸盐·甲醛缩合物(Na、NH4)、烷基(C8~12)二苯基醚二磺酸盐(Na、NH4)、木素磺酸盐(Na、Ca)、POE烷基(C8~12)苯基醚磺酸盐(Na)、POE烷基(C12~18)醚磺基琥珀酸半酯(Na)等磺酸盐型表面活性剂;羧酸型脂肪酸盐(C12~18,Na、K、NH4、链烷醇胺)、N-甲基-脂肪酸肌氨酸盐(C12~18,Na)、树脂酸盐(Na、K)等POE烷基(C12~18)醚磷酸盐(Na、链烷醇胺);POE单或二烷基(C8~12)苯基醚磷酸盐(Na,链烷醇胺)、POE苄基(或苯乙烯基)化苯基(或苯基苯基)醚磷酸盐(Na,链烷醇胺)、磷脂酰胆碱.磷脂酰乙醇亚胺(卵磷脂)、烷基(C8~12)磷酸盐等磷酸盐型表面活性剂,
作为阳离子性表面活性剂,可举出烷基三甲基氯化铵(C12~18)、甲基·聚氧乙烯·烷基氯化铵(C12~18)、烷基·溴化N-甲基吡啶(C12~18)、单或二烷基(C12~18)甲基化氯化铵、烷基(C12~18)五甲基丙邻二胺二氯化物等铵型表面活性剂;烷基二甲基苄基氯化铵(C12~18)、苄索氯铵[辛基苯氧基乙氧基乙基二甲基苄基氯化铵]等苄基铵型表面活性剂,
作为两性表面活性剂,可举出二烷基(C8~12)二氨基乙基甜菜碱、烷基(C12~18)二甲基苄基甜菜碱等甜菜碱型表面活性剂;二烷基(C8~12)二氨基乙基甘氨酸、烷基(C12~18)二甲基苄基甘氨酸等甘氨酸型表面活性剂。
上述表面活性剂可以单独使用1种,或混合2种以上使用。
在本发明的农药制剂中,除本发明的含农药树脂组合物所含的农药活性成分A以外,还可以含有农药活性成分B。
农药活性成分B并不限定于液体或固体、或者有机化合物或无机化合物、或者单一化合物或混合物等,可从杀菌剂、杀虫剂、杀螨剂、植物生长调节剂、除草剂、杀鼠剂、抗茵剂、防霉剂、抗藻剂等一般作为农药使用的化合物中选择使用。应予说明,这些农药活性成分可以单独使用1种,或者混合2种以上使用。
在作为农药活性成分B的杀菌剂中,可举出碱性氯化铜、碱性硫酸铜等铜剂;秋兰姆、代森锌、代森锰、代森锰锌、福美锌、丙森锌、代森福美锌等硫剂;克茵丹、灭茵丹、苯氟磺胺等多卤代烷基硫剂;百茵清、四氟苯酞等有机氯剂;IBP、EDDP、甲基立枯磷、吡茵磷、乙磷铝等有机磷剂;甲基硫茵灵、苯茵灵、多茵灵、噻茵灵等苯并咪唑剂;异茵脲、腐霉利、乙烯菌核利、氟氯菌核利等二羧酰亚胺剂;氧化萎锈灵、灭锈胺、氟酰胺、叶枯酞、水杨茵胺、戊茵隆等羧酰胺剂;甲霜灵、霜灵、呋霜灵等酰基丙氨酸剂;醚菌酯、嘧茵酯、苯氧茵胺等甲氧基丙烯酸酯剂;艾普林(andoprim)、嘧茵胺、嘧霉胺、嘧菌环胺等苯胺基嘧啶剂;
三唑酮、三唑醇、联苯三唑醇、腈茵唑、己唑醇、丙环唑、氟茵唑、咪鲜胺、稻瘟酯、氯苯嘧啶醇、啶斑肟、嗪氨灵、氟硅唑、乙环唑、苄氯三唑醇、三氟苯唑、粉唑醇、戊菌唑、烯唑醇、抑霉唑、十三吗啉、丁苯吗啉、丁硫啶、氟环唑、叶茵唑等SBI剂;多抗霉素、灭瘟素S、春雷霉素、井岗霉素、硫酸双氢链霉素等抗生素剂;霜霉威盐酸盐、五氯硝基苯、土茵消、磺茵威、敌茵灵、稻瘟灵、烯丙苯噻唑、灭螨猛、二噻农、敌螨普、哒茵酮、嘧茵腙、氟啶胺、咯喹酮、三环唑、喹酸、二氰蒽醌、双胍辛胺乙酸盐、霜脲氰、吡咯尼群、磺茵威、乙霉威、乐杀螨、卵磷脂、碳酸氢钠、敌磺钠、多果定、烯酰吗啉、叶枯净、环丙酰茵胺、磺茵胺、咯茵腈、唑茵酮等。
在作为农药活性成分B的杀虫·杀螨剂中,可举出倍硫磷、杀螟硫磷、二嗪磷、氯蜱硫磷、ESP、蚜灭多、稻丰散、乐果、安果、马拉硫磷(malathion)、敌百虫、甲基乙拌磷、亚胺硫磷、敌敌畏、乙酰甲胺磷、EPBP、甲基对硫磷、砜吸磷、乙硫磷、蔬果磷、杀螟腈、唑磷、哒嗪硫磷、伏杀硫磷、杀扑磷、硫丙磷、毒虫畏、杀虫畏、甲基毒虫畏、丙虫磷、异柳磷、乙拌磷、丙溴磷、吡唑硫磷、久效磷、谷硫磷、涕灭威、灭多威、硫双威、克百威、丁硫克百威、丙硫克百威、呋线威、残杀威、BPMC、MTMC、MIPC、甲萘威、抗蚜威、乙硫苯威、苯氧威等有机磷和氨基甲酸酯系杀虫剂;
氯菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯、甲氰菊酯、除虫菊素、烯丙菊酯、胺菊酯、苄呋菊酯、苄菊酯、甲呋炔菊酯、苯醚菊酯、消虫菊、氟胺氰菊酯、氟氯氰菊酯、氯氟氰菊酯、氟氰戊菊酯、醚菊酯、乙氰菊酯、四溴菊酯、氟硅菊酯、布络凡(brofenprox)、氟丙菊酯等拟除虫菊酯系杀虫剂;除虫脲、氟啶脲、氟铃脲、杀铃脲、氟虫脲、氟环脲、噻嗪酮、吡丙醚、烯虫酯、硫丹、丁醚脲、氟虫腈、杀螟丹、杀虫环、杀虫磺、硫酸烟碱、鱼藤酮、四聚乙醛、机油、BT、昆虫病原病毒等微生物农药、信息素剂等苯甲酰脲系其它杀虫剂;
苯线磷、噻唑硫磷等杀线虫剂;克氯苯、溴螨酯、三氯杀螨醇、双甲脒、BPPS、杀螨特、噻螨酮、苯丁锡、浏阳霉素、灭螨猛、CPCBS、三氯杀螨砜、阿维霉素、密灭汀、四螨嗪、三环锡、达螨灵、唑螨酯、吡螨胺、嘧螨醚、苯硫威、除螨灵等杀螨剂。
在作为农药活性成分B的植物生长调节剂中,可举出赤霉素类(例如赤霉素A3、赤霉素A4、赤霉素A7)、IAA、NAA等。
在作为农药活性成分B的除草剂中,可举出吡氟酰草胺、敌稗等酰苯胺系除草剂;甲草胺、丙草胺等氯乙酰苯胺系除草剂;2,4-D、2,4-DB等芳氧基链烷酸系除草剂;禾草灵、唑禾草灵等芳氧基苯氧基链烷酸系除草剂;麦草畏、嘧草硫醚等芳基羧酸系除草剂;咪唑喹啉酸、咪草烟等咪唑啉系除草剂;敌草隆、异丙隆等脲系除草剂;氯苯胺灵、甜菜宁等氨基甲酸酯系除草剂;禾草丹、EPTC等硫代氨基甲酸酯系除草剂;氟乐灵、二甲戊乐灵等二硝基苯胺系除草剂;三氟羧草醚、氟磺胺草醚等二苯基醚系除草剂;苄嘧磺隆、烟嘧磺隆等磺酰脲系除草剂;嗪草酮、苯嗪草酮等三嗪酮系除草剂;
莠去津、氰草津等三嗪系除草剂;唑嘧磺草胺等三唑嘧啶系除草剂;溴苯腈、敌草腈等腈系除草剂;草甘膦、草丁膦等磷酸系除草剂;百草枯、野燕枯(difenzoquat)等季铵盐系除草剂;氟烯草酸(flumiclorac-pentyl)、嗪草酸甲酯等环状酰亚胺系除草剂;新燕灵、麦草氟乙酯(furanpropethyl)等苯甲酰氨基丙酸系除草剂;异草胺、乙氧呋草黄、草灵、哌草磷、杀草隆、灭草松、呋草黄、燕麦枯(difenzo-quat)、萘丙胺、三唑苯酰胺(triazofenamide)、二氯喹啉酸、异草酮、磺草酮、环庚草醚、氟硫草定、吡唑特、哒草特、氟胺草唑,还有稀禾定、肟草酮等环己烷二酮系除草剂等。
在作为农药活性成分B的增效·解毒剂中,可举出八氯二丙醚、胡椒基丁醚、协力灵、IBTA、解草嗪、解毒喹、解草胺腈、二氯丙烯胺、解草唑、解草啶、解草胺、氟草肟(flaxofenimi)、解草唑、吡唑解草酯、MG191、萘二甲酸酐、解草腈、新烟碱类化合物等。
在作为农药活性成分B的抗茵·防霉·抗藻剂中,可举出三烷基三胺、乙醇、异丙醇、丙醇、三(羟甲基)硝基甲烷、氯丁醇、溴硝醇、戊二醛、甲醛、α-溴代肉桂醛、Skane M-8、凯松CG(Kathon CG)、NS-500W、BIT、正丁基BIT、异硫氰酸烯丙酯、噻茵灵、2-苯并咪唑基氨基甲酸甲酯、十二烷酸二羟丙基酯、BIOBAN、三氯卡班、卤卡班、古拉西西卡鲁(glasisicar)、苯甲酸、山梨酸、辛酸、丙酸、10-十一碳烯酸、山梨酸钾、丙酸钾、苯甲酸钾、邻苯二甲酸一镁、十一碳烯酸锌、8-羟基喹啉、喹啉铜、TMTD、三氯生、苯氟磺胺(diclohelanilide)、甲苯氟磺胺、鱼精蛋白、蛋白溶茵酶、苯噻硫氰、威百亩、三嗪、戊唑醇(tebuconazole)、桧木醇、四氯间苯二甲腈、TEKTAMER38、葡萄糖酸氯己定、盐酸洗必泰、聚六亚甲基双胍、聚双胍盐酸盐、旦特普洛姆(dantobrom)、库利旦特(clidant)、吡硫钠、吡啶硫酮锌、Densil、吡啶硫酮铜、百里酚、异丙基甲基苯酚、OPP、苯酚、对羟基苯甲酸丁酯、对羟基苯甲酸乙酯、对羟基苯甲酸甲酯、对羟基苯甲酸丙酯、间甲酚、邻甲酚、对甲酚、邻苯基苯酚钠、苄氯酚、对氯苯酚、对氯间二甲苯酚(parachloromethaxylate)、对氯甲酚、氟灭菌丹、多聚赖氨酸、BIOBAN P-1487、二碘代甲基对甲苯基砜、聚乙烯吡咯烷酮对氯异氰酸酯、过氧化氢、稳定化二氧化氯、过乙酸、环烷酸铜、Novaron AG300、氯化银、氧化钛、银、磷酸锌钙、Silver S、铝硅酸银锌、银锌沸石、Novaron AGZ330、Holonkiller、Dimer136、苯扎氯铵、二癸基二甲基氯化铵、BARDAC2250/80、苄索氯铵、HYAMINE3500J、十六烷基溴化铵、西曲溴胺、CTAB、塞太弗伦、Dimer38、苯扎氯铵、BARDAC170P、DC-5700、西吡氯铵、壳聚糖、敌草隆、DCMU、Prepentol A6、CMI、2CI-OIT、BCM、ZPT、BNP、OIT、IPBC、TCMSP等。
本发明的农药制剂,可以使用本发明的含农药树脂组合物、根据需要使用的上述制药基材以及农药活性成分B,通过用于得到粉剂、粉粒剂、粒剂、烟熏剂、糊剂、可湿性粉剂、颗粒可湿性粉剂、片剂、悬浮剂等的一般制造方法来进行制造。例如可举出将含农药树脂组合物与根据需要使用的上述制药基材以及农药活性成分B混合、进行破碎·粉碎·造粒的方法。
本发明的农药制剂可以根据使用目的制成各种粒度。例如在用作制剂基材、种子粉衣或粉剂时,优选200μm以下的范围,特别优选1~100μm的范围。另外,可以通过组合使用2种以上不同粒径、组成的本发明农药制剂来调节农药活性成分的溶出速度。
另外,可以使用多种农药活性成分并各自制备成本发明的农药制剂、再将它们适当混合。如果进行这种混合制剂,则可以将在农药活性成分彼此接触时不稳定的物质制成一种制剂、或将物性显著不同的农药活性成分制成一种制剂。
本发明的农药制剂可以作为各种处理剂施用于耕地、非耕地两者。例如,可作为种子处理剂用于对种芋等的喷吹处理、粉衣处理、散布涂布、漫渍处理等;可作为茎叶处理剂用于散布处理、顶肥处理等;可作为土壤处理剂用于表面散布处理、混合处理、灌注处理、熏蒸处理、植穴处理、株根处理、垄沟处理、播沟处理、育苗箱处理、育苗罐处理等;可作为水田处理剂用于粒剂处理、巨型剂处理、悬浮剂处理等;可作为其它处理剂用于熏蒸处理、草坪用处理等。在这些处理中,本发明的农药制剂可优选用于种子处理剂或土壤处理剂。
实施例
以下,列举实施例更详细地说明本发明,但本发明的范围不受这些实施例限定。
(推定式的确定)
按照表1所示的处方量取啶虫脒原药、SMA17352P(苯乙烯马来酸酐共聚物;分子量:7000/Sartomer公司制)和Carplex#80D(亲水性白炭黑/盐野义制药公司制:疏水度=0%),使之溶解和分散在约200ml丙酮中。用蒸发器馏去溶剂,得到固体成分。在研钵中磨碎该固体成分,在40℃的真空干燥机内干燥2.5小时,得到组合物1~9。
[表1]
在44.1g该组合物中加入Newkalgen RX-B(木素磺酸Na/竹本油脂制)0.45g和Newkalgen BX-C(烷基萘磺酸Na/竹本油脂制)0.45g,充分混合。通过用销棒粉碎机粉碎该混合物,将平均粒径造粒在10~25μm的范围。
对于得到的造粒物,将含有10mg啶虫脒原药的各样品精确称量到100ml的管瓶中,在其中添加25℃的蒸馏水80ml和作为内标的4-羟基苯甲酸甲酯溶液(500mg/L蒸馏水)20ml,加盖颠倒5次,静置于25℃的恒温槽直到取样。在经过规定时间时颠倒5次,接着取样约0.7ml(用0.45μm的过滤器过滤)。用HPLC测定取样溶液中的啶虫脒的浓度,以相对于假定该组合物中的啶虫脒全部溶解在水中时的啶虫脒浓度的百分率算出溶出率。进行所述测定直到经过120小时。
应予说明,本发明的实施例的平均粒径是使用日机装株式会社的Microtrac9320-X-100测定体积平均粒径的结果。
以上述测定结果为基础,将各时间的溶出率作为因变数,将啶虫脒的含有率(AcSA)和亲水性白炭黑的含有率(CaSA)作为自变数,通过线性最小二乘法导出推定各时间的溶出率的式A~式E。
式A:经过15分钟时的啶虫脒的推定溶出率
YevA(0.25)=0.524×AcSA+1.422×CaSA-6.009
式B:经过4小时时的啶虫脒的推定溶出率
YevA(4)=0.745×AcSA+2.135×CaSA-7.234
式C:经过24小时时的啶虫脒的推定溶出率
YevA(24)=1.014×AcSA+2.599×CaSA-7.509
式D:经过72小时时的啶虫脒的推定溶出率
YevA(72)=1.313×AcSA+2.838×CaSA-6.968
式E:经过120小时时的啶虫脒的推定溶出率
YevA(120)=1.545×AcSA+2.945×CaSA-7.562
应予说明,各式在统计学上有意义,AcSA和CaSA各自的系数也是99%以上、有意义。
(实施例1)
选择由上述式A计算的推定溶出率YevA(0.25)=-1.97质量%的、啶虫脒的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=1质量%。如下所述制备选择的组成比的含农药树脂组合物(可湿性粉剂1)。
将啶虫脒原药2.5g、SMA17352P(苯乙烯马来酸酐共聚物;分子量:7000/Sartomer公司制)47.0g和Carplex#80D(亲水性白炭黑/盐野义制药公司制;疏水度=0%)0.5g量取到1000ml的茄形烧瓶中,在其中加入约200ml丙酮并用超声波浴溶解·分散。用蒸发器从该溶液中馏去大部分的溶剂,取出烧瓶内的残渣。在研钵中粉碎该残渣,用真空干燥机在40℃干燥2.5小时,得到固态物。
在该固态物44.1g中加入Newkalgen RX-B(木素磺酸Na/竹本油脂制)0.45g和Newkalgen BX-C(烷基萘磺酸Na/竹本油脂制)0.45g,在塑料袋(ビニ一ル袋)中充分混合。通过用销棒粉碎机粉碎全部该混合物,得到含有平均粒径为17.9μm的微粒组合物的可湿性粉剂1。应予说明,由式A求出的推定溶出率YevA(0.25),虽然相对于实测溶出率有约4%的误差,但在含农药树脂组合物的设计中可充分发挥作用。
(实施例2)
选择由上述式A计算的推定溶出率YevA(0.25)=3.72质量%的、啶虫脒的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为15.2μm的微粒组合物的可湿性粉剂2。
(实施例3)
选择由上述式A计算的推定溶出率YevA(0.25)=10.8质量%的、啶虫脒的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=10质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为14.0μm的微粒组合物的可湿性粉剂3。
(实施例4)
选择由上述式A计算的推定溶出率YevA(0.25)=11.1质量%的、啶虫脒的含有率AcSA=30质量%和亲水性白炭黑的含有率CaSA=1质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为12.7μm的微粒组合物的可湿性粉剂4。
(实施例5)
选择由上述式A计算的推定溶出率YevA(0.25)=16.8质量%的、啶虫脒的含有率AcSA=30质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为14.2μm的微粒组合物的可湿性粉剂5。
(实施例6)
选择由上述式A计算的推定溶出率YevA(0.25)=23.9质量%的、啶虫脒的含有率AcSA=30质量%和亲水性白炭黑的含有率CaSA=10质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为16.6μm的微粒组合物的可湿性粉剂6。
(实施例7)
选择由上述式A计算的推定溶出率YevA(0.25)=13.8质量%的、啶虫脒的含有率AcSA=35质量%和亲水性白炭黑的含有率CaSA=1质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为14.9μm的微粒组合物的可湿性粉剂7。
(实施例8)
选择由上述式A计算的推定溶出率YevA(0.25)=19.4质量%的、啶虫脒的含有率AcSA=35质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为17.2μm的微粒组合物的可湿性粉剂8。
(实施例9)
选择由上述式A计算的推定溶出率YevA(0.25)=26.6质量%的、啶虫脒的含有率AcSA=35质量%和亲水性白炭黑的含有率CaSA=10质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为23.2μm的微粒组合物的可湿性粉剂9。
<水中溶出性试验>
对于可湿性粉剂1~9,将含有10mg啶虫脒原药的各样品精确称量到100ml的管瓶中,在其中添加25℃的蒸馏水80ml和作为内标的4-羟基苯甲酸甲酯溶液(500mg/L蒸馏水)20ml,加盖颠倒5次,静置于25℃的恒温槽直到取样。在经过规定时间时颠倒5次,接着取样约0.7ml(用0.45μm的过滤器过滤)。用HPLC测定取样的溶液中的啶虫脒的浓度,以相对于假定可湿性粉剂中的啶虫脒全部溶解于水时的啶虫脒浓度的百分率算出实测溶出率。将结果示于表2。
[表2]
(实施例10)
选择由上述式A计算的推定溶出率YevA(0.25)=11.1质量%的、啶虫脒的含有率AcSA=30.0质量%和亲水性白炭黑的含有率CaSA=1.0质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为7.9μm的微粒组合物的可湿性粉剂10。
(实施例11)
选择由上述式A计算的推定溶出率YevA(0.25)=10.4质量%的、啶虫脒的含有率AcSA=30.0质量%和亲水性白炭黑的含有率CaSA=0.5质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为13.3μm的微粒组合物的可湿性粉剂11。
(实施例12)
选择由上述式A计算的推定溶出率YevA(0.25)=9.85质量%的、啶虫脒的含有率AcSA=30.0质量%和亲水性白炭黑的含有率CaSA=0.1质量%。用与实施例1相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为12.6μm的微粒组合物的可湿性粉剂12。
(比较例1)
选择由上述式A计算的推定溶出率YevA(0.25)=52.2质量%的、啶虫脒的含有率AcSA=93.5质量%和亲水性白炭黑的含有率CaSA=6.5质量%。如下所述地制备选择的组成比的含农药树脂组合物(可湿性粉剂A)。
在研钵中充分混合啶虫脒72.3g、Newkalgen RX-B2.5g、粘土20.2g、以及Carplex#80D5.0g后,用气流粉碎机粉碎,得到可湿性粉剂A。
(比较例2)
选择由上述式A计算的推定溶出率YevA(0.25)=67.7质量%的、啶虫脒的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=50质量%。如下所述地制备含有选择的组成比的含农药树脂组合物的原料用药物粉末B。
将啶虫脒1g、SMA3000(基础树脂为苯乙烯马来酸酐共聚物;分子量:9500/Sartomer公司制)9g和Carplex#80D(亲水性白炭黑/盐野义制药公司制)10g量取到300ml的茄形烧瓶中,在其中加入100ml二氯甲烷并用超声波浴完全溶解。用蒸发器从该溶液中馏去大部分的溶剂,进一步用真空干燥机在40℃干燥2小时,得到固态物。在研钵中充分研磨该固态物使其粉碎,用网眼44μm和105μm的筛子筛选44μm~105μm的部分,由此得到平均粒径为82μm的微粒组合物(原料用药物粉末B)。
对实施例10~12和比较例1、2中得到的组合物,进行与上述相同的水中溶出性试验。对实施例10~12进行试验直到360小时。由于比较例1、2的实测溶出率饱和,所以中途中止试验。将其结果示于表3。
[表3]
如表3所示,推定溶出率YevA(0.25)大于40质量%的可湿性粉剂A,在经过15分钟时实测溶出率达到100%,可能会发生农药急剧作用于农作物等药害,另外,预测没有残效性。另外,推定溶出率YevA(0.25)大于40质量%的原料用药物粉末B,在经过15分钟时实测溶出率达到60%(即,引起初期突释),之后,实测溶出率几乎没有变化。
另一方面,如表2和表3所示,按照本发明的方法制造的、推定溶出率YevA(0.25)≤40质量%的可湿性粉剂1~12抑制了投入水中初期的大量溶出(初期突释),也适当控制了之后的实测溶出率。本实施例中使用的溶出率YevA的推定式是基于直到经过120小时时的数据而决定的,但在经过360小时时实测溶出率也是适当的走势(profile),没有达到滞留(参照实施例10~12)。
(实施例13)
选择由上述式A计算的推定溶出率YevA(0.25)=-1.97质量%的、吡虫啉的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=1质量%。如下所述地制备选择的组成比的含农药树脂组合物(可湿性粉剂13)。
将吡虫啉原药0.5g、SMA17352P(苯乙烯马来酸酐共聚物;分子量:7000/Sartomer公司制)9.4g和Carplex#80D(亲水性白炭黑/盐野义制药公司制;疏水度=0%)0.1g量取到300ml的茄形烧瓶中,在其中加入约50ml二氯甲烷并用超声波浴溶解·分散。用蒸发器从该溶液中馏去大部分的溶剂,取出烧瓶内的残渣。在研钵中粉碎该残渣,用真空干燥机在40℃干燥2.5小时。然后,用网眼44μm的筛子进行筛分,得到44μm以下的固态物。
在固态物4.41g中加入Newkalgen RX-B(木素磺酸Na/竹本油脂制)0.045g和Newkalgen BX-C(烷基萘磺酸Na/竹本油脂制)0.045g,在塑料袋中充分混合,得到含有平均粒径为19.9μm的微粒组合物的可湿性粉剂13。应予说明,由式A求出的推定溶出率YevA(0.25),虽然相对于实测溶出率有约4%的误差,但在含农药树脂组合物的设计中充分发挥作用。
(实施例14)
选择由上述式A计算的推定溶出率YevA(0.25)=3.72质量%的、吡虫啉的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为22.0μm的微粒组合物的可湿性粉剂14。
(实施例15)
选择由上述式A计算的推定溶出率YevA(0.25)=10.8质量%的、吡虫啉的含有率AcSA=5质量%和亲水性白炭黑的含有率CaSA=10质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为24.5μm的微粒组合物的可湿性粉剂15。
(实施例16)
选择由上述式A计算的推定溶出率YevA(0.25)=11.1质量%的、吡虫啉的含有率AcSA=30质量%和亲水性白炭黑的含有率CaSA=1质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为19.2μm的微粒组合物的可湿性粉剂16。
(实施例17)
选择由上述式A计算的推定溶出率YevA(0.25)=16.8质量%的、吡虫啉的含有率AcSA=30质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为21.1μm的微粒组合物的可湿性粉剂17。
(实施例18)
选择由上述式A计算的推定溶出率YevA(0.25)=13.8质量%的、吡虫啉的含有率AcSA=35质量%和亲水性白炭黑的含有率CaSA=1质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为19.9μm的微粒组合物的可湿性粉剂18。
(实施例19)
选择由上述式A计算的推定溶出率YevA(0.25)=19.4质量%的、吡虫啉的含有率AcSA=35质量%和亲水性白炭黑的含有率CaSA=5质量%。用与实施例13相同的方法制备选择的组成比的含农药树脂组合物,得到含有平均粒径为22.5μm的微粒组合物的可湿性粉剂19。
<水中溶出性试验>
对于可湿性粉剂13~19,将含有10mg吡虫啉原药的各样品精确称量到100ml的管瓶中,在其中添加25℃的蒸馏水80ml和作为内标的4-羟基苯甲酸甲酯溶液(500mg/L蒸馏水)20ml,加盖颠倒5次,静置于25℃的恒温槽直到取样。在经过规定时间时颠倒5次,接着取样约0.7ml(用0.45μm的过滤器过滤)。用HPLC测定取样的溶液中的吡虫啉的浓度,以相对于假设可湿性粉剂中的吡虫啉完全溶解在水中时的吡虫啉浓度的百分率算出实测溶出率。将结果示于表4。
[表4]
由此可知,按照本发明的制造方法,能够容易地设计且能够制造抑制了药害、残效性充分的含农药树脂组合物或农药制剂。
产业上的可利用性
依照本发明的含农药树脂组合物的制造方法,能够容易地设计且能够制造将农药活性成分短期内大量溶出的现象、即初期突释抑制在适度的大小且抑制了本来应该溶出的农药活性成分没有全部溶出而残留的现象、即滞留的含农药树脂组合物和农药制剂。而且,本发明的含农药树脂组合物和农药制剂,既维持了残效性又没有因农药活性成分的作物残留量增加而导致发生药害的情况,还可以防止在环境中的残留。另外,除上述效果以外,通过提高光稳定性、控制挥散性、提高耐雨性等,还具有提高农药活性成分的残效性和减少向环境中的流失的效果、减少总散布药量、减少散布次数、降低对散布者的毒性等效果,尤其可用作种子处理剂和土壤处理剂。如上所述,本发明在产业上极其有用。
Claims (12)
1.一种含农药树脂组合物的制造方法,其包括:
以任意组成比混合在25℃的水中的溶解度为100ppm以上且为新烟碱类化合物的农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑来制备多种组合物,
将该组合物各自遣粒成平均粒径为10~25μm,测定将其添加到25℃的蒸馏水中后经过t时间时的农药活性成分A的溶出率Y(t),其中,溶出率单位为质量%,
用线性最小二乘法解析以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的农药活性成分A的含有率Ac和亲水性白炭黑的含有率Ca、与之前测定的溶出率Y(t),求出式(I),其中,含有率Ac和含有率Ca的单位为质量%,
式(I):Yev(t)=a(t)×AcS+b(t)×CaS+c(t)
其中,式(I)中的Yev(t)表示添加后经过t时间时的农药活性成分A的推定溶出率,单位为质量%;a(t)、b(t)和c(t)表示用线性最小二乘法求得的经过时间t的系数;自变量t表示添加后的经过时间,单位为小时;AcS和CaS表示以农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的农药活性成分A的含有率和亲水性白炭黑的含有率,含有率单位为质量%,
所述式(I)中,添加到25℃的蒸馏水中后经过15分钟时的农药活性成分A的推定溶出率Yev(0.25)成为40质量%以下的、农药活性成分A的含有率AcS从5质量%~35质量%的范围选择、亲水性白炭黑的含有率CaS从0.1质量%以上的范围选择;
混合农药活性成分A、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑使其达到以上选择的含有率AcS和含有率CaS。
2.如权利要求1所述的含农药树脂组合物的制造方法,其中,所述农药活性成分A是选自烯啶虫胺、吡虫啉、啶虫脒、噻虫嗪、噻虫胺、噻虫啉和呋虫胺中的至少一种化合物。
3.一种含农药树脂组合物的制造方法,其包括:
从满足0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%的范围分别选择以啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA;
混合啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑使其达到以上选择的含有率AcSA和含有率CaSA。
4.如权利要求1~3中任一项所述的含农药树脂组合物的制造方法,其中,亲水性白炭黑的疏水度为20%以下。
5.如权利要求1~3中任一项所述的含农药树脂组合物的制造方法,其中,所述苯乙烯马来酸酐共聚物混合树脂是苯乙烯马来酸酐共聚物与具有来自松香或其衍生物、或者、水杨酸或其衍生物的重复单元的聚合物的混合物。
6.一种含农药树脂组合物,由权利要求1~5中任一项所述的制造方法制得。
7.一种含农药树脂组合物,其含有啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑,其中,以啶虫脒、苯乙烯马来酸酐共聚物或苯乙烯马来酸酐共聚物混合树脂、以及亲水性白炭黑的合计质量为基准的啶虫脒的含有率AcSA和亲水性白炭黑的含有率CaSA满足0.524×AcSA+1.422×CaSA-6.009≤40质量%、5质量%≤AcSA≤35质量%和CaSA≥0.1质量%。
8.一种原料用药物粉末,由权利要求6或7所述的含农药树脂组合物形成。
9.一种农药制剂,含有权利要求8所述的原料用药物粉末。
10.如权利要求9所述的农药制剂,其中,原料用药物粉末的平均粒径为200μm以下。
11.一种农药制剂的制造方法,包括将权利要求6或7所述的含农药树脂组合物造粒。
12.如权利要求11所述的农药制剂的制造方法,其中,采用选自转动造粒法、搅拌造粒法、挤出造粒法、压延造粒法、破碎造粒法和流动造粒法中的至少一种方法进行造粒。
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