CN117615650A - 树脂制农药容器的变形防止方法 - Google Patents
树脂制农药容器的变形防止方法 Download PDFInfo
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- CN117615650A CN117615650A CN202280048691.5A CN202280048691A CN117615650A CN 117615650 A CN117615650 A CN 117615650A CN 202280048691 A CN202280048691 A CN 202280048691A CN 117615650 A CN117615650 A CN 117615650A
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- acid
- container
- oily
- resin
- pesticide
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Classifications
-
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/34—Nitriles
-
- 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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
- A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
- A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
- A01N47/06—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom containing —O—CO—O— groups; Thio analogues thereof
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
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Abstract
农药油性悬浮剂为液态农药制剂品之中经常被利用的制剂形态,但如果采用树脂制农药容器作为填充其的容器,则有时在保存中、运输中发生容器的变形、破损。着眼于使用特定的抗氧化剂,提供通过抑制农药油性悬浮剂的油性成分的氧化来调制化学上稳定的油性悬浮剂,将其填充于树脂制农药容器,从而防止该容器变形的方法。
Description
技术领域
本发明涉及防止填充了农药油性悬浮剂的树脂制农药容器的变形的方法以及该方法所使用的农药油性悬浮剂。
背景技术
对于农药的液态制剂品的容器,通常多采用了加工的容易性、轻量性、阻气性、如玻璃瓶那样不容易开裂等便利性优异的树脂制容器。另一方面,在农药的液态制剂品中,油性悬浮剂为使农药的有效成分分散于油性成分的制剂,通过在使油性成分在散布液中均匀地分散的目的下加入了的表面活性剂的作用,从而对作物的附着性、渗透性优异,因此在散布液中不需要展着剂的加用,在液态农药制剂品之中经常被利用。
在专利文献1中,记载了使用含有选自甲醛供体化合物、和没食子酸酯、苯酚衍生物、L-抗坏血酸和它们的盐和衍生物、以及生育酚和它们的衍生物中的抗氧化剂的杀菌性组合物,减少燃料、润滑剂那样的工业制品的保存中和运输中的向内弯曲效果的问题的方法。然而,在专利文献1中,没有关于填充了农药油性悬浮剂的树脂制容器的记载。
在专利文献2中,作为将液态药剂装入到塑料容器进行保存时的塑料容器的变形防止方法,记载了使液态药剂的溶解氧浓度为30ppm以下,作为减少溶解氧浓度的具体的方法,记载了在药剂液中吹入氮气等非活性气体的方法、在非活性气体气氛下加热的方法和减压后用非活性气体恢复到常压的方法。
在专利文献3中,记载了通过在调制包含有机溶剂的液态药剂后,进行脱气处理,在常压或加压下静置或搅拌而使气体再溶解于上述液态药剂,将液态药剂内的气体量恢复到一定以上的状态,调整液态药剂内的溶解气体量从而防止容器的变形的方法。
在专利文献4中,记载了在农药油性悬浮剂中可以添加二丁基羟基甲苯、丁基羟基茴香醚、叔丁基氢醌、没食子酸丙酯作为抗氧化剂,在专利文献5中记载了可以添加二丁基羟基甲苯、丁基羟基茴香醚和表氯醇作为稳定剂。然而,专利文献4和专利文献5中,没有关于填充了农药油性悬浮剂的树脂制容器的记载。
现有技术文献
专利文献
专利文献1:日本特开2005-82595号公报
专利文献2:日本特开2002-97103号公报
专利文献3:日本特开2017-114506号公报
专利文献4:中国专利申请公开公报101785455号
专利文献5:中国专利申请公开公报107439578号
发明内容
发明所要解决的课题
农药油性悬浮剂如上所述,为在液态农药制剂品之中经常被利用的制剂形态,但如果采用树脂制容器作为填充其的容器,则有时在保存中、运输中发生容器的变形、破损,防止该情况作为课题而被举出。
用于解决课题的手段
本发明人等为了解决上述课题进行了研究,结果认为,着眼于农药油性悬浮剂中的油性成分具有通过空气中的氧、湿气、热、光、金属离子、微生物等的作用而被氧化的性质,特别是,通过光、热而氧化被促进,根据填充了农药油性悬浮剂的树脂制容器的保存状态,在容器内的空间存在的氧与油性成分反应从而氧被消耗等,容器内变为减压状态,可能发生容器的变形、破损。进而,作为该课题的解决手段,着眼于使用特定的抗氧化剂,获得通过抑制农药油性悬浮剂的油性成分的氧化从而调制化学上稳定的油性悬浮剂,将其填充于树脂制容器,从而可以防止该容器的变形的认识,完成了本发明。
发明的效果
根据本发明,可以提供防止填充了农药油性悬浮剂的树脂制农药容器的变形的方法。
具体实施方式
本发明涉及一种防止树脂制农药容器变形的方法,是防止填充了农药油性悬浮剂的树脂制农药容器变形的方法,其中,填充于该树脂制农药容器的农药油性悬浮剂含有(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂。
此外本发明涉及树脂制农药容器变形防止用的、上述农药油性悬浮剂,是含有(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂的农药油性悬浮剂,被填充于树脂制农药容器后在容器内发生的油性成分的氧化被抑制了。
在本发明中,所谓树脂制农药容器的变形,是指容器的形状从填充了农药油性悬浮剂的时刻的状态发生凹陷、缩小、变形、破损、龟裂等,不能复原的状态。
作为本发明中的农药有效成分,只要是能够调制为油性悬浮剂的物质就没有特别限定,可举出例如烟嘧磺隆、啶嘧磺隆、吡唑草酯(tolpyralate)、氟嘧硫草酯、硝磺草酮、莠去津、溴苯腈、特丁津、乙草胺、异丙甲草胺、氟啶脲、噻唑膦、氟啶虫酰胺、环溴虫酰胺、异丙噻菌胺、氰霜唑、苯啶菌酮、氟啶胺等。
其中,优选为烟嘧磺隆、啶嘧磺隆、吡唑草酯、氟啶虫酰胺、异丙噻菌胺、氰霜唑、苯啶菌酮或氟啶胺,更优选为烟嘧磺隆或吡唑草酯。
作为本发明中的油性成分,只要是在农药油性悬浮剂被填充于树脂制农药容器后,包含不饱和烃作为与容器内的氧反应的部位的物质,就没有特别限定,可举出例如植物油、进行了烷基酯化的植物油、矿物油、芳香族油,可以将它们混合使用。
作为植物油或进行了烷基酯化的植物油,可举出大豆油、菜籽油、妥尔油、橄榄油、蓖麻油、木瓜油、山茶油、椰子油、棕榈油、芝麻油、玉米油、米油、花生油、棉籽油、亚麻籽油、葵花籽油、印楝油、红花油和它们的烷基酯油,其中优选为菜籽油、玉米油、大豆油和它们的甲基酯油。
此外,作为油性成分,可以使用脂肪酸甘油酯。脂肪酸甘油酯能够由例如植物油获得。脂肪酸的取代数为任意的,可举出单甘油酯、二甘油酯或三甘油酯。在为二甘油酯或三甘油酯的情况下,可以相同或不同的脂肪酸在任意的位置取代而得的物质,在不同的脂肪酸取代的情况下,它们可以为不饱和脂肪酸和饱和脂肪酸中的任一者。此外,也可以混用2种以上脂肪酸甘油酯。
作为上述脂肪酸,可举出α-亚麻酸、亚油酸、油酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、硬脂酸、花生酸、二十碳烯酸、山萮酸、芥酸、木蜡酸、芥酸、蓖麻油酸等,其中优选为亚油酸、油酸、棕榈酸、硬脂酸、芥酸。此外,优选为脂肪酸部分被烷基酯化而得的烷基酯化脂肪酸甘油酯,特别优选为甲基化脂肪酸甘油酯。
作为矿物油,可举出机械油、石蜡油和环烷油,其中优选为石蜡油。矿物油主要包含饱和烃,但有时混合存在不饱和烃,成为本发明的对象。
作为芳香族油,可举出溶剂石脑油、二甲苯,其中优选为溶剂石脑油。
作为本申请发明中的抗氧化剂,可举出例如,苯酚衍生物、没食子酸酯和乙氧基喹啉。
抗氧化剂通过添加在制剂中来获得目标的效果,但优选为使抗氧化剂溶解在制剂中的状态,本发明的农药油性悬浮制剂由于为以油作为基础的农药制剂,因此特别优选为亲油性的抗氧化剂。
作为苯酚衍生物,可举出例如二丁基羟基甲苯、丁基羟基茴香醚、2,5-二-叔戊基氢醌、2,5-二-叔丁基氢醌、4,4’-亚丁基双(6-叔丁基-间甲酚)、4,4’-硫代双(6-叔丁基-间甲酚)、双(5-叔丁基-4-羟基-2-甲基苯基)硫醚,其中优选为二丁基羟基甲苯。
作为没食子酸酯,可举出例如没食子酸甲酯、没食子酸乙酯、没食子酸2-羟基乙酯、没食子酸丙酯、没食子酸异丙酯、没食子酸丁酯,其中优选为没食子酸丙酯。
作为抗氧化剂,特别优选为二丁基羟基甲苯。
本发明中的抗氧化剂即使添加量为微量也可获得所希望的效果,但用于长期抑制树脂制农药容器的变形的、抗氧化剂与油性成分的重量比通常为0.0001:99.9999~30:70,优选为0.001:99.999~20:80,更优选为0.01:99.99~15:85。
在本发明中作为填充农药油性悬浮剂的树脂制农药容器,没有特别限定,但优选为例如,由低密度聚乙烯、高密度聚乙烯、聚氯乙烯、聚丙烯、聚酰胺、聚对苯二甲酸乙二醇酯、聚偏1,1-二氯乙烯、腈树脂、聚碳酸酯、聚丙烯酸酯、聚甲基戊烯、聚乙烯乙烯醇树脂、全氟烷氧基氟树脂等材料通过直接吹塑成型法、拉伸吹塑成型法等而工业生产的树脂制农药容器。容量没有特别限定,可举出例如,100mL、500mL、1L、5L、10L、20L、200L和1000L等,优选为500mL、1L和5L。
本发明的农药油性悬浮剂中的农药有效成分、油性成分和抗氧化剂的混配比例有时根据各自的种类、性状等而适当变更,不能笼统地规定,但但例如如以下那样。
农药有效成分为0.1~80重量份,优选为0.5~50重量份,进一步优选为2~35重量份。
油性成分为1~99重量份,优选为5~95重量份,更优选为15~75重量份。
抗氧化剂为0.001~10重量份,优选为0.01~10重量份,更优选为0.1~3重量份。
本发明的农药油性悬浮剂可以根据需要适当添加表面活性剂、防冻剂、抗沉降剂、消泡剂、溶剂等制剂助剂。
作为上述表面活性剂,可举出例如脂肪酸盐、苯甲酸盐、烷基磺基琥珀酸盐、二烷基磺基琥珀酸盐、烷基硫酸酯盐、烷基硫酸盐、烷基二甘醇醚硫酸盐、醇硫酸酯盐、烷基磺酸盐、烷基芳基磺酸盐、烷基二苯基醚二磺酸盐、聚苯乙烯磺酸盐、烷基磷酸酯盐、烷基芳基磷酸盐、苯乙烯基芳基磷酸盐、聚氧乙烯烷基醚硫酸酯盐、聚氧乙烯烷基芳基醚硫酸盐、聚氧乙烯苯乙烯基芳基醚硫酸盐、聚氧乙烯苯乙烯基芳基醚硫酸铵盐、聚氧乙烯烷基芳基醚硫酸酯盐、聚氧乙烯烷基醚磷酸盐、聚氧乙烯烷基芳基磷酸酯盐、聚氧乙烯苯乙烯基芳基醚磷酸酯或其盐那样的阴离子系的表面活性剂;失水山梨糖醇脂肪酸酯、甘油脂肪酸酯、脂肪酸聚甘油酯、脂肪酸醇聚二醇醚、炔属二醇、炔属醇、氧化烯嵌段聚合物、聚氧乙烯烷基醚、聚氧乙烯烷基芳基醚、聚氧乙烯苯乙烯基芳基醚、聚氧乙烯烯丙基苯基醚、聚氧乙二醇烷基醚、聚氧乙烯脂肪酸酯、聚氧乙烯失水山梨糖醇脂肪酸酯、聚氧乙烯山梨糖醇脂肪酸酯、聚氧乙烯甘油脂肪酸酯、聚氧乙烯氢化蓖麻油、聚氧乙烯蓖麻油、聚氧丙烯脂肪酸酯、聚氧乙烯烷基胺、聚氧乙烯烷基醚磷酸酯、聚氧乙烯甲基聚硅氧烷那样的非离子系的表面活性剂;烷氧基化脂肪族胺那样的阳离子系的表面活性剂;等,根据需要,可以混用它们的2种以上。该表面活性剂的混配比例为0~80重量份,优选为5~70重量份。
作为上述防冻剂,优选为2元醇,具体而言,可举出乙二醇、丙二醇等亚烷基二醇,其中优选使用丙二醇。上述2元醇也具有作为减粘剂的作用,除了冷冻防止效果以外,有时使农药油性悬浮剂的粘度降低,流动性被改善。防冻剂的混配比例通常为2~30重量份,优选为5~10重量份。
作为上述抗沉降剂,可举出例如,黄原胶、中性树胶、刺槐豆胶、角叉菜胶、威兰胶等天然多糖类;聚丙烯酸钠等合成高分子类;羧基甲基纤维素等半合成多糖类;硅酸铝镁、蒙脱石、膨润土、锂蒙脱石、干式法二氧化硅、有机膨润土、有机锂蒙脱石等矿物质微粉末、氧化铝溶胶等,根据需要,可以混用它们的2种以上。抗沉降剂的混配比例通常为0.01~10.0重量份,优选为0.1~5.0重量份。
作为消泡剂,可举出例如,包含聚二甲基硅氧烷作为有效成分的有机硅系消泡剂、二氧化硅等。具体而言,可举出商品名SILCOLAPSE432(Bluestar silicones社制)、商品名SILFOAM SC 120(旭化成ワッカーシリコーン社制)、商品名SAG 47、SAG 1538、SAG 1572(モメンティブ社制)等,根据需要,可以混用二氧化硅。消泡剂的混配比例通常为0.01~10重量份,优选为0.1~2.0重量份。
作为溶剂,可举出例如水、二烷、丙酮、异佛尔酮、甲基异丁基酮、氯苯、环己烷、二甲亚砜、二甲基甲酰胺、二甲基乙酰胺、二甲基C8-C12酰胺、N-甲基-2-吡咯烷酮、2-乙基己醇、γ-丁内酯、醇、乙酸、丁酸、乳酸、乙酸异丙酯、乙酸丁酯、乳酸二甲酯、苯、烷基苯、烷基萘等,根据需要,可以混用它们的2种以上。溶剂的混配比例通常为0.1~30重量份,优选为0.5~20重量份。
作为本发明的农药油性悬浮剂的制造方法,可以按照该技术领域中的通常的方法进行,可举出例如,在将表面活性剂与抗沉降剂、稳定剂添加于油性成分而进行了混合后,加入农药有效成分,根据需要也加入其它助剂用均化器等进行预粉碎后,使用锆石珠等,通过湿式粉碎机进行了微粉碎直到规定的粒径后,添加增稠剂等助剂进行混合的方法;将农药有效成分与表面活性剂等助剂一起进行干式粉碎而得的物质,添加于溶解了表面活性剂、抗沉降剂和其它助剂的油性成分,用均化器等进行预粉碎后,使用玻璃珠等通过湿式粉碎机进行了微粉碎直到规定的粒径后,根据需要添加增稠剂、稳定剂等助剂进行混合的方法等。农药有效成分的粒径通常优选粉碎直到0.1~5μm左右,期望根据农药有效成分的物性来改变粒径。
作为在制造本发明的农药油性悬浮剂时可以使用的粉碎机,可举出珠磨机、振动磨机、行星磨机等湿式粉碎机,可以使用例如油漆摇动器(东洋精机制作所制)、粉砕ナノ太郎NP-100(THINKY社制)、戴诺磨KD型(WAB社制)、レディーミルRMH型(アイメックス社制)等。作为可以使用的珠,可举出玻璃珠、氧化锆珠、锆石珠等。作为珠粒径,优选使用0.01~1.5mm的范围的物质,更优选为0.5~1.0mm的范围的物质。通过使用粒径小的珠,从而可以制造平均粒径小的农药油性悬浮剂。
农药有效成分的平均粒径例如可以通过マイクロトラックMT3300-EXII(日机装社制)、Mastersizer 3000(Malvern社制)等激光衍射式粒度分布测定装置测定。在使用マイクロトラックMT3300-EXII的情况下,测定可以使试样分散在正己烷那样的有机溶剂而进行。
本发明的农药油性悬浮剂的粘度例如可以利用TVB-10形粘度计(东机产业社制)、BrookField粘度计(BrookField社制)而测定。在使用TVB-10形粘度计的情况下,测定可以使用试样液体温度20℃、转速60rpm、转子M2或M3而进行。
在本发明中,通过在将农药油性悬浮剂填充于树脂制农药容器后,从盒式氮瓶(ナリカ社制)那样的装置将氮气供给到容器的空间部分,从而可以将容器的空间部分置换为氮气。进行了氮气置换的容器可以用感应衬垫(DGF-500型,ランズワーク社制)那样的装置进行密闭。
以下记载本发明的、期望的方案。
〔1〕一种防止树脂制农药容器变形的方法,是防止填充了农药油性悬浮剂的树脂制农药容器变形的方法,其中,填充于该树脂制农药容器的农药油性悬浮剂含有(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂。
〔2〕根据〔1〕所述的方法,上述抗氧化剂为选自苯酚衍生物和没食子酸酯中的至少1种。
〔3〕根据〔1〕或〔2〕所述的方法,上述苯酚衍生物为选自二丁基羟基甲苯、丁基羟基茴香醚、2,5-二-叔戊基氢醌、2,5-二-叔丁基氢醌、4,4’-亚丁基双(6-叔丁基-间甲酚)、4,4’-硫代双(6-叔丁基-间甲酚)和双(5-叔丁基-4-羟基-2-甲基苯基)硫醚中的至少1种。
〔4〕根据〔1〕或〔2〕所述的方法,上述没食子酸酯为选自没食子酸甲酯、没食子酸乙酯、没食子酸2-羟基乙酯、没食子酸丙酯、没食子酸异丙酯和没食子酸丁酯中的至少1种。
〔5〕根据〔1〕~〔4〕所述的方法,上述油性成分为选自植物油、进行了烷基酯化的植物油、矿物油和芳香族油中的至少1种。
〔6〕根据〔5〕所述的方法,上述植物油或进行了烷基酯化的植物油选自大豆油、菜籽油、妥尔油、橄榄油、蓖麻油、木瓜油、山茶油、椰子油、棕榈油、芝麻油、玉米油、米油、花生油、棉籽油、亚麻籽油、葵花籽油、印楝油、红花油和它们的烷基酯油。
〔7〕根据〔5〕所述的方法,上述矿物油为选自机械油、石蜡油和环烷油中的至少1种。
〔8〕根据〔5〕所述的方法,上述芳香族油为选自溶剂石脑油和二甲苯中的至少1种。
〔9〕根据〔1〕~〔4〕所述的方法,上述油性成分为脂肪酸甘油酯。
〔10〕根据〔9〕所述的方法,上述脂肪酸甘油酯为选自α-亚麻酸、亚油酸、油酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、硬脂酸、花生酸、二十碳烯酸、山萮酸、芥酸、木蜡酸、芥酸和蓖麻油酸中的至少1种脂肪酸的甘油酯。
〔11〕根据〔9〕或〔10〕所述的方法,上述脂肪酸甘油酯为单甘油酯、二甘油酯、三甘油酯或它们的混合物。
〔12〕根据〔1〕~〔11〕所述的方法,上述抗氧化剂与上述油性成分的重量比为0.01:99.99~15:85。
〔13〕根据〔1〕~〔12〕所述的方法,在将上述农药油性悬浮剂填充于树脂制农药容器后,进一步,将容器内的空间部的气体向氮气置换。
〔14〕根据〔1〕~〔13〕所述的方法,上述农药有效成分为烟嘧磺隆、啶嘧磺隆、吡唑草酯、氟嘧硫草酯、硝磺草酮、莠去津、溴苯腈、特丁津、乙草胺、异丙甲草胺、氟啶脲、噻唑膦、氟啶虫酰胺、环溴虫酰胺、异丙噻菌胺、氰霜唑、苯啶菌酮或氟啶胺。
〔15〕根据〔1〕~〔13〕所述的方法,上述农药有效成分为选自烟嘧磺隆和吡唑草酯中的至少1种。
〔16〕上述〔1〕~〔15〕所述的、树脂制农药容器变形防止用的、农药油性悬浮剂。
〔17〕一种防止树脂制农药容器变形的方法,是抑制填充后由树脂制农药容器内部的氧被消耗引起的该树脂制农药容器内减压的方法,其中,将(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂混合而调制农药油性悬浮剂,
接着将该农药油性悬浮剂填充于树脂制农药容器。
〔18〕根据〔17〕所述的方法,上述抗氧化剂为选自苯酚衍生物和没食子酸酯中的至少1种。
实施例
以下,记载本发明涉及的实施例,但它们不限定本发明。首先,记载制剂例。
制剂例
将下述表A所示的量的各成分利用均化器ULTRA-TURRAX T25basic(IKA社制)进行混合粉碎,调制油性悬浮剂。表A中的数字表示重量份。表A中的作为(C)成分的表面活性剂(C1)~(C7)为各自示于表B中的物质,此外,表A中所记载的商品的成分各自为以下物质。
·商品名“SAG47”:有机硅系消泡剂(モメンティブ社制)
·商品名“Agnique ME 18RD-F”:C16-18饱和脂肪酸和C18不饱和脂肪酸的甲基酯(BASF社制)
·商品名“コーンサラダ油”:三酰基甘油(ボーソー油脂社制)
[表1]
表A
[表2]
表A续
[表3]
表B
表述 | 成分名 |
(c)-1 | 聚氧乙烯失水山梨糖醇脂肪酸酯 |
(c)-2 | 聚氧乙烯蓖麻油 |
(c)-3 | 聚氧乙烯烯丙基苯基醚 |
(c)-4 | 聚氧乙烯烷基胺 |
(c)-5 | 聚氧乙烯烷基醚 |
(c)-6 | 烷基苯磺酸钙 |
(c)-7 | 烷基苯磺酸钠 |
接下来记载试验例。
试验例1
如以下那样,调制出有农药有效成分的油性悬浮剂、与无农药有效成分的油性悬浮剂。
[有农药有效成分]
将农药有效成分(吡唑草酯12.0重量份、烟嘧磺隆12.0重量份)、聚氧乙烯失水山梨糖醇脂肪酸酯10.5重量份、聚氧乙烯蓖麻油1.2重量份、烷基苯磺酸钙3.3重量份、有机膨润土1.5重量份、聚氧乙烯单烷基醚3.0重量份、干式法二氧化硅3.0重量份进行混合,加入Agnique ME18RD-F(商品名:C16-18饱和脂肪酸和C18不饱和脂肪酸的甲基酯,BASF社制)54.7重量份以成为1L的方式进行了调制。然后,通过均化器ULTRA-TURRAX T25basic(IKA社制)进行混合粉碎,以农药有效成分的粒径成为5μm以下的方式用珠磨机进一步粉碎而获得了油性悬浮剂。
[无农药有效成分]
加入聚氧乙烯失水山梨糖醇脂肪酸酯6.2重量份、聚氧乙烯蓖麻油0.7重量份、烷基苯磺酸钙1.9重量份、Agnique ME18RD-F(商品名:C16-18饱和脂肪酸和C18不饱和脂肪酸的甲基酯,BASF社制)79.2重量份以成为1L的方式调制后,通过均化器ULTRA-TURRAXT25basic(IKA社制)进行混合粉碎而获得了油性悬浮剂。
在各油性悬浮剂中,添加第1表所示的抗氧化剂(二丁基羟基甲苯或抗坏血酸),进行混合而调制试验样品后,在容量500ml的聚乙烯制瓶容器(型号:NSW-500-2(M)瓶,东都成型株式会社制)中分别填充各200ml。在用感应衬垫将瓶容器密封前将氧浓度测定用芯片安装于空间部,并且一部分样品在瓶容器空间部分使用氮气(盒式实验用气体(ナリカ社制))将瓶容器空间部的气体置换为氮气,用感应衬垫(DGF-500型,ランズワーク社)进行密闭,在室温下保存了863天。在保存后,将瓶容器的外观利用下述基准进行调查,也测定了瓶容器内的氧浓度。调查结果示于第1表中。
瓶容器的外观〇:没有或极少变化,×:瓶身部分具有大的凹陷
[表4]
第1表
根据试验例1的结果,在长期保存条件下,通过包含本发明的抗氧化剂0.2重量份而抑制了瓶容器的变形。此外,通过包含抗氧化剂0.02重量份,将瓶容器内的空气进行氮气置换从而也抑制了瓶容器的变形。此外,在制剂中包含农药有效成分时氧浓度略高。
试验例2
通过与试验例1相同方法调制油性悬浮剂,添加第2表所示的抗氧化剂0.01重量份~3.0重量份并进行了混合后,测定了瓶容器的外观和瓶容器内的氧浓度。调查结果示于第2表中。
[表5]
第2表
根据试验例2的结果,在长期保存条件下(140天),添加作为本发明的抗氧化剂的二丁基羟基甲苯0.01~3.0重量份、没食子酸丙酯0.2重量份或乙氧基喹啉0.2重量份从而抑制了瓶容器的变形,与抗坏血酸那样的亲水性抗氧化剂相比亲油性抗氧化剂时抑制效果高。此外,通过将瓶容器内的空气进行氮气置换从而也抑制了瓶容器的变形。此外,在制剂中包含农药有效成分时氧浓度高,瓶容器的变形防止效果也高。
试验例3
将在试验例2中调制出的油性悬浮剂70g量取到100ml的玻璃瓶中,加入到铝包装容器(ヤナギ社制,型号0401,12×22cm)中,以铝层压的体积成为400~430ml的方式调整内部的空气量,利用热封机(富士インパルス社制,型号PS-310E型)进行密闭,在室温下保存了130天。铝层压容器的体积的变化通过测量在预先装了1.5L的水的2L的量筒中沉入了铝层压容器时的水的体积来调查。调查结果示于第3表中。
[表6]
第3表
根据试验例3的结果,在长期保存条件下(在室温下130天),通过添加二丁基羟基甲苯0.01~3.0重量份、没食子酸丙酯0.2~3.0重量份或乙氧基喹啉0.1~3.0重量份从而抑制了铝层压容器的变形。另一方面,添加了作为亲水性的抗氧化剂的抗坏血酸、D-异抗坏血酸、或生育酚的情况下的容器的变形防止效果低。此外,通过将瓶容器内的空气进行氮气置换从而也抑制了铝层压容器的变形。此外,在制剂中包含农药有效成分时铝层压容器的变形防止效果高。
试验例4
使用第4表所示的农药有效成分,通过与试验例1相同方法而调制油性悬浮剂,添加二丁基羟基甲苯0.01重量份~0.2重量份并进行了混合后,在40℃下保存了28天。为了调查瓶容器的状态,测定瓶容器的外径(中央部和下部(距底2cm),通过下述式算出了外径的变化率CV值。CV值越小则容器的变形越小,变形防止效果越高。调查结果示于第4表中。
CV值=容器外径的标准偏差÷容器外径的平均值×100
[表7]
第4表
根据试验例4的结果,包含除草甘膦以外的农药有效成分的各制剂品通过将二丁基羟基甲苯以每100mL样品0.1重量份以上的添加而抑制了瓶容器的变形。
需要说明的是,将在2021年8月12日申请的日本专利申请2021-131666号的说明书、权利要求书、和摘要的全部内容引用到本文中,作为本发明的说明书的公开而被并入。
Claims (15)
1.一种防止树脂制农药容器变形的方法,是防止填充了农药油性悬浮剂的树脂制农药容器变形的方法,其中,填充于该树脂制农药容器的农药油性悬浮剂含有(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂。
2.根据权利要求1所述的方法,所述抗氧化剂为选自苯酚衍生物和没食子酸酯中的至少1种。
3.根据权利要求1或2所述的方法,所述抗氧化剂为苯酚衍生物。
4.根据权利要求1~3所述的方法,所述苯酚衍生物为选自二丁基羟基甲苯、丁基羟基茴香醚、2,5-二-叔戊基氢醌、2,5-二-叔丁基氢醌、4,4’-亚丁基双(6-叔丁基-间甲酚)、4,4’-硫代双(6-叔丁基-间甲酚)和双(5-叔丁基-4-羟基-2-甲基苯基)硫醚中的至少1种。
5.根据权利要求1~4所述的方法,所述油性成分为选自植物油、进行了烷基酯化的植物油、矿物油和芳香族油中的至少1种。
6.根据权利要求1~5所述的方法,所述油性成分为脂肪酸甘油酯。
7.根据权利要求6所述的方法,所述脂肪酸甘油酯为选自α-亚麻酸、亚油酸、油酸、辛酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、棕榈油酸、硬脂酸、花生酸、二十碳烯酸、山酸、芥酸、木蜡酸、芥酸和蓖麻油酸中的至少1种脂肪酸的甘油酯。
8.根据权利要求6或7所述的方法,所述脂肪酸甘油酯为单甘油酯、二甘油酯、三甘油酯或它们的混合物。
9.根据权利要求1~8所述的方法,所述抗氧化剂与所述油性成分的重量比为0.01:99.99~15:85。
10.根据权利要求1~9所述的方法,在将所述农药油性悬浮剂填充于所述树脂制农药容器后,进一步,将容器内的空间部的气体向氮气置换。
11.一种用于防止树脂制农药容器变形的农药油性悬浮剂,是被填充于树脂制农药容器后抑制了在容器内发生的油性成分的氧化的农药油性悬浮剂,所述农药油性悬浮剂含有(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂。
12.根据权利要求11所述的农药油性悬浮剂,所述抗氧化剂为选自苯酚衍生物和没食子酸酯中的至少1种。
13.一种防止树脂制农药容器变形的方法,是抑制填充后由树脂制农药容器内部的氧被消耗引起的该树脂制农药容器内减压的方法,其中,
将(1)农药有效成分、(2)油性成分以及(3)选自苯酚衍生物、没食子酸酯和乙氧基喹啉中的至少1种抗氧化剂混合而调制农药油性悬浮剂,
接着将该农药油性悬浮剂填充于树脂制农药容器。
14.根据权利要求13所述的方法,所述抗氧化剂为选自苯酚衍生物和没食子酸酯中的至少1种。
15.根据权利要求13或14所述的方法,在填充了所述农药油性悬浮剂后,向所述树脂制农药容器的空间部分供给氮气。
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