CN102111997A - 用于提高杀真菌剂效力的亚磷酸的钙盐 - Google Patents
用于提高杀真菌剂效力的亚磷酸的钙盐 Download PDFInfo
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- CN102111997A CN102111997A CN2009801221831A CN200980122183A CN102111997A CN 102111997 A CN102111997 A CN 102111997A CN 2009801221831 A CN2009801221831 A CN 2009801221831A CN 200980122183 A CN200980122183 A CN 200980122183A CN 102111997 A CN102111997 A CN 102111997A
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- phosphorous acid
- salt
- calcium
- solid formulations
- acid
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Classifications
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- A—HUMAN NECESSITIES
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- 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/26—Phosphorus; Compounds thereof
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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
- A01N25/12—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
- 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
- A01N37/36—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 containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—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 containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
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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
- 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
- A01N43/24—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 two or more hetero atoms
- A01N43/32—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 two or more hetero atoms six-membered rings
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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
- 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
- A01N47/08—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 one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
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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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
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Abstract
本发明涉及亚磷酸的钙盐在农业中提高杀真菌剂效力的用途。此外,本发明涉及固体配制剂,制备所述固体配制剂的方法及其在防治有害真菌中的用途。此外,本发明涉及一种制备亚磷酸的钙盐的方法。
Description
本发明涉及亚磷酸的钙盐在农业中提高杀真菌剂效力的用途。此外,本发明涉及固体配制剂,制备固体配制剂的方法以及它们在防治有害真菌中的用途。此外,本发明涉及一种制备亚磷酸的钙盐的方法。
在农业中长久以来发现亚磷酸及其碱金属和碱土金属盐以及酯提高杀真菌剂的效力。US 4,075,324描述了基于亚磷酸或其盐的杀真菌组合物,该组合物具有亚磷酸盐的通用杀真菌活性。据说它们在与杀真菌剂组合时仅具有加和活性。在实施例中提到了二级亚磷酸钙(CaHPO3)的可湿性粉末。US 5,626,281公开了使用固体或固化形式的亚磷酸盐以水溶性颗粒制备杀真菌组合物。WO 2002/05650公开了包含与由至少一种氨基酸和至少一种藻类提取物组成的有机化合物组合的亚磷酸的衍生物和盐的杀真菌制剂。WO 2004/047540描述了亚磷酸钾对某些合成杀真菌剂的特别强的协同增效作用。WO 2006/128677公开了包含亚磷酸的铜(II)盐、亚磷酸的另一金属盐和杀真菌剂的杀真菌组合物。WO 2007/017220描述了亚磷酸的盐与没有或很少具有杀真菌活性和固有光催化性能的化合物的协同增效混合物。
然而,所述亚磷酸衍生物的配制方案是有限的,且在某些条件下它们的效力也不令人满意。尤其在固体作物保护配制剂如水分散性粉末(WP)或水分散性颗粒(WG)的制备中,所述衍生物不能提供任何适合施用的产品。
在水分散性粉末的制备中,使活性化合物或活性化合物混合物与配制助剂混合,然后在喷射磨机或机械磨机如锤磨机或针磨机中研磨。在研磨之前和之后,粉末必须具有足够流动性,从而可以实现令人满意的产品质量。在混合和研磨工艺过程中,当使用亚磷酸的常规钾和/或钠盐时,由于其高吸湿性而形成重度附聚,这导致加工不可能进行。
在通过喷雾干燥或流化床造粒方法制备水分散性颗粒时,首先生产活性化合物或活性化合物混合物与各种配制助剂的水溶液或研磨悬浮液,然后在以小液滴形式喷雾之后通过对流输入热而干燥。液滴在工艺温度下的尽可能快速干燥对于实现令人满意的造粒是必要的。当使用亚磷酸的常规钾和/或钠盐时,颗粒的生产甚至在高温下是不可能的。甚至在减压下干燥也不能得到任何干燥产品。
在通过挤出机造粒方法制备水分散性颗粒时,首先制备活性化合物或活性化合物混合物与各种配制助剂的粉状研磨预混物,然后用水润湿并捏合,使用挤出机(例如篮式挤出机或径向挤出机)以圆柱形颗粒挤出,然后通过对流输入热而干燥。当使用亚磷酸的常规钾和/或钠盐时,再也不能在干燥步骤中除去加入的水并且稳定颗粒的制备是不可能的。
由于其吸湿性,亚磷酸钾和亚磷酸钠仅能以含水配制剂加工。其他类型的配制剂,尤其是固体配制剂,如水分散性颗粒(WG)或水分散性粉末(WP)被排除在外。迄今为止,在实践中仅使用过基于亚磷酸的钾和/或钠盐的亚磷酸液体配制剂。尤其其高吸湿性,这些盐不能令人满意地以固体形式配制。另一方面,某些活性化合物,如二硫代氨基甲酸盐类,由于化学原因不能永久地稳定于液体配制剂中。若要将该类活性化合物与增效剂组合进行配制,则仅能配制固体配制剂。然而,该类固体配制剂不能用已知的亚磷酸钠和亚磷酸钾稳定地制备。
本发明的目的是提供一种在作物保护中用于杀真菌剂的有效增效剂,其易于配制且广泛可得,以及基于亚磷酸和合适的话其他杀真菌活性化合物的固体配制剂,其中这些配制剂的处理和储存稳定性与已知配制剂相比显著改进。
该目的通过使用亚磷酸的钙盐在农业中提高杀真菌剂的效力而实现。亚磷酸的钙盐优选呈固体配制剂形式。它们特别优选呈颗粒形式。
根据本发明,将亚磷酸的钙盐用于在农业中提高杀真菌剂效力。通常可以同时提高一种或多种,如两种或三种杀真菌剂的效力。优选将亚磷酸的钙盐用于提高为有机合成化合物的杀真菌剂的效力。有机合成杀真菌剂通常由碳和氢构成且此外可以包含杂原子,如氧、氮、硫、卤素和/或磷。该类杀真菌剂由化学品通过化学转化而以目标方式制备。
杀真菌剂此外优选基本不含铜盐。铜盐如包含Cu+或Cu2+的盐是本身已知具有已知杀真菌作用的化合物。然而,将铜盐施用于用于农业的区域具有生态缺点。术语“基本不含”通常指基于杀真菌剂的总量小于3重量%,优选小于1重量%,特别优选小于0.1重量%。
将亚磷酸的钙盐用于在农业中提高杀真菌剂的效力。
“提高杀真菌剂的效力”应理解为指与亚磷酸的钙盐组合时活性以协同增效方式提高。此外,在许多情况下,可以拓宽活性谱或者可以防止耐药性的产生。
“亚磷酸”应理解为指具有式P(OH)3的亚磷酸以及互变异构的膦酸HP(O)(OH)2。“亚磷酸的盐”应理解为指亚磷酸的盐和互变异构的膦酸的盐。亚磷酸的无机盐通常称为亚磷酸盐(或膦酸盐;经验式[HPO3]2-)或亚磷酸氢盐(或膦酸氢盐;经验式[H2PO3]-)。下文中将亚磷酸的盐也称为亚磷酸盐。
合适亚磷酸的钙盐例如为亚磷酸钙CaHPO3或亚磷酸氢钙Ca(H2PO3)2。优选亚磷酸氢钙。在优选实施方案中,在亚磷酸氢钙中钙与磷的摩尔比为1∶2.1-1∶1.8,尤其是1∶2.05-1∶1.9。
亚磷酸的钙盐可以包含结晶水。优选它们尤其以Ca∶H2O摩尔比为0.5∶3-3∶0.5,尤其是0.8∶2-2∶0.8包含结晶水。在一个实施方案中,优选每Ca(CaHPO3*1H2O)具有1mol结晶水的亚磷酸钙。作为1重量%的水溶液它通常具有2-6,优选3-5的pH。在另一实施方案中,优选每Ca(Ca(H2PO3)2*1H2O)具有1mol结晶水的亚磷酸氢钙。尤其优选的亚磷酸的钙盐为Ca(H2PO3)2*1H2O。
亚磷酸的钙盐以一般方式由文献已知。其制备尤其描述于US4,075,324中。这里由碳酸钙和亚磷酸制备亚磷酸氢钙,或者由氯化钙和亚磷酸铵制备亚磷酸钙。Ebert and Vesely(Collection of Czechoslovak Chemical Communications,1959,2,2801-2802)描述了由亚磷酸和固体碳酸盐或氢氧化物开始制备亚磷酸氢钙。未反应的亚磷酸必须使用过量乙醇除去。
我们发现了一种制备亚磷酸的钙盐的特别有利的本发明方法,其中使氢氧化钙Ca(OH)2和/或氧化钙CaO的含水悬浮液与亚磷酸H3PO3和水反应。该方法尤其适于制备亚磷酸氢钙。亚磷酸优选以水溶液存在。该反应例如可以通过将浓度为20重量%的氢氧化钙悬浮液引入浓度为50%的H3PO3溶液中进行,或反之亦然。另一变体是将固体H3PO3引入浓度为20%的氢氧化钙悬浮液中。
通常将亚磷酸H3PO3和水在输入能量下加入氢氧化钙Ca(OH)2和/或氧化钙CaO的悬浮液中。该反应可以在20-100℃的温度下进行。通过调整加料速率和中和热的耗散可以根据需要控制反应温度。取决于温度、中和度和浓度,所形成的亚磷酸的钙盐以溶解和/或悬浮形式存在。
所得亚磷酸的钙盐的含水悬浮液通过常规方法干燥,例如通过在桨叶干燥机中减压蒸发、冷冻干燥、喷雾干燥和转鼓干燥。在另一优选实施方案中,该悬浮液在不干燥下用于本发明制备固体配制剂的方法中。
为了制备亚磷酸氢钙,通常将1mol细碎氢氧化钙含水悬浮液加入2mol亚磷酸中。浓度为1重量%的水溶液的pH为2.0-6.0,优选3.0-5.0。若在100℃以下进行干燥,则得到的通常为包含1mol结晶水的固体亚磷酸氢钙(残留水含量约8%)。优选仅将亚磷酸氢钙的悬浮液干燥到其中在亚磷酸氢钙中残留1mol结晶水/Ca的点。
为了制备亚磷酸钙,通常将1mol氢氧化钙含水悬浮液加入1mol亚磷酸中。浓度为1重量%的水溶液的pH为6-12,优选7-10。
本发明制备亚磷酸的钙盐的方法所具有的优点是高转化率以及短反应时间、水溶液pH的快速调节和低的产热。不要求额外的提纯步骤,如用乙醇萃取未反应的亚磷酸。
术语“农药”或“作物保护剂”是指一种或多种化合物可以选自杀真菌剂、杀虫剂、杀线虫剂、除草剂、安全剂和生长调节剂。还可以使用上述类型中的两种或更多种的混合物。本领域熟练技术人员熟知该类农药,例如它们可以在“Pesticide Manual”,第13版(2003),The British Crop Protection Council,London中找到。
下面所列为可以与亚磷酸的钙盐一起使用的杀真菌剂。该列举用于说明可能的组合,但不限制它们。这些杀真菌剂优选与亚磷酸的钙盐一起使用。A)嗜球果伞素类:
腈嘧菌酯(azoxystrobin)、醚菌胺(dimoxystrobin)、烯肟菌酯(enestroburin)、氟嘧菌酯(fluoxastrobin)、亚胺菌(kresoxim-methyl)、叉氨苯酰胺(metominostrobin)、肟醚菌胺(orysastrobin)、啶氧菌酯(picoxystrobin)、唑菌胺酯(pyraclostrobin)、pyribencarb、肟菌酯(trifloxystrobin)、2-(2-(6-(3-氯-2-甲基苯氧基)-5-氟嘧啶-4-基氧基)苯基)-2-甲氧亚氨基-N-甲基乙酰胺、2-(邻-((2,5-二甲基苯氧基亚甲基)苯基)-3-甲氧基丙烯酸甲酯、3-甲氧基-2-(2-(N-(4-甲氧基苯基)环丙烷亚胺酰硫基甲基)苯基)丙烯酸甲酯、2-(2-(3-(2,6-二氯苯基)-1-甲基亚烯丙基氨基氧甲基)苯基)-2-甲氧亚氨基-N-甲基乙酰胺;
B)羧酰胺类:
-羧酰苯胺类:苯霜灵(benalaxyl)、精苯霜灵(benalaxyl-M)、麦锈灵(benodanil)、bixafen、啶酰菌胺(boscalid)、萎锈灵(carboxin)、呋菌胺(fenfuram)、环酰菌胺(fenhexamid)、氟酰胺(flutolanil)、呋吡唑灵(furametpyr)、isopyrazam、异噻菌胺(isotianil)、kiralaxyl、丙氧灭绣胺(mepronil)、甲霜灵(metalaxyl)、精甲霜灵(metalaxyl-M)、甲呋酰胺(ofurace)、霜灵(oxadixyl)、氧化萎锈灵(oxycarboxin)、吡噻菌胺(penthiopyrad)、叶枯酞(tecloftalam)、溴氟唑菌(thifluzamide)、噻酰菌胺(tiadinil)、2-氨基-4-甲基噻唑-5-甲酰苯胺、2-氯-N-(1,1,3-三甲基-2,3-二氢化茚-4-基)烟酰胺、N-(2′,4′-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′,4′-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′,5′-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′,5′-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′,5′-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′,5′-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′-氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′-氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′,4′,5′-三氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2′,4′,5′-三氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-[2-(1,1,2,3,3,3-六氟丙氧基)苯基]-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-[2-(1,1,2,2-四氟乙氧基)苯基]-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(4′-三氟甲硫基联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3′,4′-二氯-5-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2-(1,3-二甲基丁基)苯基)-1,3,3-三甲基-5-氟-1H-吡唑-4-甲酰胺、N-(4’-氯-3’,5′-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(4’-氯-3’,5′-二氟联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,4’-二氯-5′-氟联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5′-二氟-4’-甲基联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5′-二氟-4’-甲基联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2-双环丙-2-基苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(顺式-2-双环丙-2-基苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(反式-2-双环丙-2-基苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺;
-羧酸吗啉化物:烯酰吗啉(dimethomorph)、氟吗啉(flumorph);
-苯甲酰胺类:氟联苯菌(flumetover)、氟吡菌胺(fluopicolide)、氟吡菌酰胺(fluopyram)、苯酰菌胺(zoxamide)、N-(3-乙基-3,5,5-三甲基环己基)-3-甲酰氨基-2-羟基苯甲酰胺;
-其他羧酰胺类:氯环丙酰胺(carpropamid)、双氯氰菌胺(diclocymet)、双炔酰菌胺(mandipropamid)、土霉素(oxytetracyclin)、硅噻菌胺(silthiofarm)、N-(6-甲氧基吡啶-3-基)环丙烷甲酰胺;
C)唑类:
-三唑类:戊环唑(azaconazole)、双苯三唑醇(bitertanol)、糠菌唑(bromuconazole)、环唑醇(cyproconazole)、醚唑(difenoconazole)、烯唑醇(diniconazole)、烯唑醇M(diniconazole-M)、氧唑菌(epoxiconazole)、腈苯唑(fenbuconazole)、喹唑菌酮(fluquinconazole)、氟硅唑(flusilazole)、粉唑醇(flutriafole)、己唑醇(hexaconazole)、酰胺唑(imibenconazole)、环戊唑醇(ipconazole)、环戊唑菌(metconazole)、腈菌唑(myclobutanil)、oxpoconazole、多效唑(paclobutrazole)、戊菌唑(penconazole)、丙环唑(propiconazole)、丙硫菌唑(prothioconazole)、硅氟唑(simeconazole)、戊唑醇(tebuconazole)、氟醚唑(tetraconazole)、三唑酮(triadimefon)、唑菌醇(triadimenol)、戊叉唑菌(triticonazole)、烯效唑(uniconazole)、1-(4-氯苯基)-2-([1,2,4]三唑-1-基)环庚醇;
-咪唑类:氰霜唑(cyazofamid)、烯菌灵(imazalil)、抑霉唑硫酸盐(imazalil sulfate)、稻瘟酯(pefurazoate)、丙氯灵(prochloraz)、氟菌唑(triflumizole);
-苯并咪唑类:苯菌灵(benomyl)、多菌灵(carbendazim)、麦穗宁(fuberidazole)、涕必灵(thiabendazole);
-其他:噻唑菌胺(ethaboxam)、氯唑灵(etridiazole)、土菌消(hymexazole)、1-(4-氯苯基)-1-(丙炔-2-基氧基)-3-(4-(3,4-二甲氧基苯基)异唑-5-基)丙-2-酮;
D)含氮杂环化合物
-吡啶类:氟啶胺(fluazinam)、啶斑肟(pyrifenox)、3-[5-(4-氯苯基)-2,3-二甲基异唑烷-3-基]吡啶、3-[5-(4-甲基苯基)-2,3-二甲基异唑烷-3-基]吡啶、2,3,5,6-四氯-4-甲磺酰基吡啶、3,4,5-三氯吡啶-2,6-二甲腈、N-(1-(5-溴-3-氯吡啶-2-基)乙基)-2,4-二氯烟酰胺、N-((5-溴-3-氯吡啶-2-基)甲基)-2,4-二氯烟酰胺;
-嘧啶类:磺嘧菌灵(bupirimate)、环丙嘧啶(cyprodinil)、二氟林(diflumetorim)、异嘧菌醇(fenarimol)、嘧菌腙(ferimzone)、嘧菌胺(mepanipyrim)、氯草定(nitrapyrin)、氟苯嘧啶醇(nuarimol)、二甲嘧菌胺(pyrimethanil);
-哌嗪类:嗪氨灵(triforine);
-吗啉类:4-十二烷基-2,6-二甲基吗啉(aldimorph)、吗菌灵(dodemorph)、吗菌灵乙酸酯(dodemorph acetate)、丁苯吗啉(fenpropimorph)、克啉菌(tridemorph);
-哌啶类:苯锈啶(fenpropidin);
-二羧酰亚胺类:氟菌安(fluorimide)、异丙定(iprodione)、杀菌利(procymidone)、烯菌酮(vinclozolin);
-非芳族5员杂环:唑酮菌(famoxadone)、咪唑菌酮(fenamidone)、异噻菌酮(octhilinone)、噻菌灵(probenazole)、5-氨基-2-异丙基-3-氧代-4-邻甲苯基-2,3-二氢吡唑-l-硫代甲酸S-烯丙基酯;
-其他:噻二唑素(acibenzolar-S-methyl)、amisulbrom、敌菌灵(anilazine)、灭瘟素(blasticidin-S)、敌菌丹(captafol)、克菌丹(captan)、灭螨蜢(quinomethionate)、棉隆(dazomet)、咪菌威(debacarb)、哒菌清(diclomezine)、野燕枯(difenzoquat)、野燕枯甲基硫酸酯(difenzoquat methylsulfate)、氰菌胺(fenoxanil)、灭菌丹(folpet)、恶喹酸(oxolinic acid)、粉病灵(piperalin)、丙氧喹啉(proquinazid)、咯喹酮(pyroquilone)、喹氧灵(quinoxyfen)、唑菌嗪(triazoxide)、三环唑(tricyclazole)、2-丁氧基-6-碘-3-丙基苯并吡喃-4-酮、5-氯-1-(4,6-二甲氧基嘧啶-2-基)-2-甲基-1H-苯并咪唑、N-(4-(3-甲氧基-1-(5-甲基-[1,2,3]噻二唑-4-基)萘-2-基)噻唑-2-基)丁酰胺、5-氯-7-(4-甲基哌啶-1-基)-6-(2,4,6-三氟苯基)-[1,2,4]三唑并[1,5-a]嘧啶、6-(3,4-二氯苯基)-5-甲基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、6-(4-叔丁基苯基)-5-甲基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、5-甲基-6-(3,5,5-三甲基己基)-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、5-甲基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、6-甲基-5-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、6-乙基-5-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、5-乙基-6-(3,5,5-三甲基己基)-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、6-辛基-5-丙基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、5-甲氧基甲基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、6-辛基-5-三氟甲基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺和5-三氟甲基-6-(3,5,5-三甲基己基)-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺;
E)氨基甲酸盐和二硫代氨基甲酸盐
-硫代-和二硫代氨基甲酸盐:福美铁(ferbam)、代森锰锌(mancozeb)、代森锰(maneb)、威百亩(metam)、磺菌威(methasulfocarb)、代森联(metiram)、甲基代森锌(propineb)、福美双(thiram)、代森锌(zineb)、福美锌(ziram);
-氨基甲酸盐:乙霉威(diethofencarb)、苯噻菌胺(benthiavalicarb)、异丙菌胺(iprovalicarb)、百维灵(propamocarb)、霜霉威盐酸盐(propamocarb hydrochloride)、valiphenal、N-(1-(1-(4-氰基苯基)乙磺酰基)丁-2-基)氨基甲酸4-氟苯基酯;
F)其他杀真菌剂
-胍类:多果定(dodine)、多果定游离碱、双胍盐(guazatine)、双胍辛胺(guazatine acetate)、双胍辛醋酸盐(iminoctadine)、双胍辛胺三乙酸盐(iminoctadine triacetate)、双八胍盐(iminoctadine tris(albesilate));
-硝基苯基衍生物:乐杀螨(binapacryl)、氯硝胺(dicloran)、敌螨通(dinobuton)、敌螨普(dinocap)、异丙消(nitrothal-isopropyl)、四氯硝基苯(tecnazene);
-含硫杂环化合物:二噻农(dithianon)、稻瘟灵(isoprothiolane);
-有机磷化合物:克瘟散(edifenphos)、藻菌磷(fosetyl)、乙磷铝(fosetylaluminum)、异稻瘟净(iprobenfos)、定菌磷(pyrazophos)、甲基立枯磷(tolclofos-methyl);
-有机氯化合物:百菌清(chlorothalonil)、抑菌灵(dichlofluanid)、双氯酚(dichlorophen)、磺菌胺(flusulfamide)、六氯苯(hexachlorobenzene)、戊菌隆(pencycuron)、五氯酚(pentachlorophenol)及其盐、四氯苯酞(phthalide)、五氯硝基苯(quintozene)、甲基托布津(thiophanate methyl)、对甲抑菌灵(tolylfluanid)、N-(4-氯-2-硝基苯基)-N-乙基-4-甲基苯磺酰胺;
-其他:联苯、拌棉醇(bronopol)、环氟菌胺(cyflufenamid)、清菌脲(cymoxanil)、二苯胺、苯菌酮(metrafenone)、米多霉素(mildiomycin)、调环酸钙(prohexadione-calcium)、螺茂胺(spiroxamine)、对甲抑菌灵、N-(环丙基甲氧亚氨基-(6-二氟甲氧基-2,3-二氟苯基)甲基)-2-苯基乙酰胺、N′-(4-(4-氯-3-三氟甲基苯氧基)-2,5-二甲基苯基)-N-乙基-N-甲基甲脒、N′-(4-(4-氟-3-三氟甲基苯氧基)-2,5-二甲基苯基)-N-乙基-N-甲基甲脒、N′-(2-甲基-5-三氟甲基-4-(3-三甲基硅烷基丙氧基)苯基)-N-乙基-N-甲基甲脒、N′-(5-二氟甲基-2-甲基-4-(3-三甲基硅烷基丙氧基)苯基)-N-乙基-N-甲基甲脒。
可以与本发明化合物一起使用的下列生长调节剂用于说明可能的组合,但不限制它们:
G)脱落酸(abscisic acid)、先甲草胺(amidochlor)、嘧啶醇(ancymidol)、苄胺基嘌呤(6-benzylaminopurine)、油菜素内酯(brassinolide)、地乐胺(butralin)、矮壮素阳离子(chlormequat)(矮壮素(chlormequat chloride))、氯化胆碱(cholin chloride)、环丙酸酰胺(cyclanilide)、丁酰肼(daminozide)、敌草克(dikegulac)、噻节因(dimethipin)、2,6-二甲基吡啶(2,6-dimethylpuridine)、乙烯利(ethephon)、抑芽敏(flumetralin)、呋嘧醇(flurprimidol)、达草氟(fluthiacet)、调吡脲(forchlorfenuron)、九二O(gibberellic acid)、抗倒胺(inabenfid)、吲哚-3-乙酸、抑芽丹(maleic hydrazide)、氟草磺(mefluidide)、助壮素阳离子(mepiquat)(助壮素(mepiquat chloride))、环戊唑菌、萘乙酸、N-6-苄基腺嘌呤、多效唑、调环酸(prohexadione)(调环酸钙)、茉莉酸丙酯(prohydrojasmon)、赛二唑素(thidiazuron)、抑芽唑(triapenthenol)、脱叶磷(tributyl phosphorotrithioate)、2,3,5-三碘苯甲酸、抗倒酯(trinexapac-ethyl)和烯效唑。
可以与亚磷酸的钙盐一起使用的下列除草剂用于说明可能的组合,但不限制它们:
H)除草剂如草甘膦(glyphosate)、草硫膦(sulfosate)、草铵膦(glufosinate)、七氟菊酯(tefluthrin)、特丁磷(terbufos)、毒死蜱(chlorpyrifos)、壤虫氯磷(chlorethoxyfos)、嘧丙磷(tebupirimfos)、双氧威(phenoxycarb)、茂醚(diofenolan)、拒嗪酮(pymetrozine)、咪草烟(imazethapyr)、咪草啶酸(imazamox)、灭草烟(imazapyr)、甲基咪草烟(imazapic)或精噻吩草胺(dimethenamid-P)。
可以与亚磷酸的钙盐一起使用的下列杀虫剂用于说明可能的组合,但不限制它们:
I)杀虫剂如锐劲特(fipronil)、吡虫啉(imidacloprid)、吡虫清(acetamiprid)、硝胺烯啶(nitenpyram)、虫螨威(carbofuran)、丁硫克百威(carbosulfan)、丙硫克百威(benfuracarb)、呋虫胺(dinotefuran)、噻虫啉(thiacloprid)、噻虫嗪(thiamethoxam)、噻虫胺(clothianidin)、氟脲杀(diflubenzuron)、氟虫脲(flufenoxuron)、伏虫隆(teflubenzuron)和甲体氯氰菊酯(alpha-cypermethrin)。
本发明尤其涉及包含亚磷酸的钙盐和至少一种杀真菌剂,例如一种或多种,如一种或两种上述A)-F)组活性化合物的配制剂。它们任选还可以包含其他作物保护剂,例如上述G)-H)组。
这些混合物就降低施用率而言是令人感兴趣的,因为它们中的许多在降低的活性化合物施用总量下对有害真菌,尤其是对某些适应症显示出改进的活性。通过同时联合或分开施用亚磷酸的钙盐和至少一种A)-F)组活性化合物,以超加和方式提高杀真菌效力。
对本发明而言,联合施用是指亚磷酸氢钙和至少一种其他活性化合物同时以足以有效防治真菌生长的量存在于作用位置(即待防治的作物损害性真菌及其栖息地如侵染的植物,植物繁殖材料,尤其是种子,土壤、材料或空间以及要防止真菌侵袭的植物,植物繁殖材料,尤其是种子,土壤、材料或空间)。这可以通过以联合活性化合物制剂一起施用或以至少两种分开的活性化合物制剂同时施用活性化合物和至少一种其他活性物质或者通过在作用位置依次使用活性化合物而实现,其中选择各次活性化合物施用之间的间隔以确保首先施用的活性物质在施用其他活性物质时以足够量存在于作用位置。其中施用活性化合物的时间顺序并不重要。
在双组分混合物,即包含亚磷酸的钙盐和其他活性化合物,例如A)-I)组,优选A)-F)组活性化合物的本发明组合物中,亚磷酸的钙盐与其他活性化合物的重量比通常为1∶50-250∶1,优选1∶20-100∶1,尤其是1∶1-20∶1。
在三组分混合物,即包含亚磷酸的钙盐以及第一种其他活性化合物和第二种其他活性化合物,例如两种不同的A)-I)组,优选A)-F)组活性化合物的组合物中,亚磷酸的钙盐与第一种其他活性化合物的重量比优选为1∶50-250∶1,更优选1∶20-100∶1,尤其是1∶1-20∶1。亚磷酸的钙盐与第二种其他活性化合物的重量比优选为1∶50-250∶1,优选1∶20-100∶1,尤其是1∶1-20∶1。第一种其他活性化合物与第二种其他活性化合物的重量比优选为1∶50-50∶1,尤其是1∶10-10∶1。
本发明组合物的各组分可以单独或作为即混物或多组分成套包装来包装和使用。
在本发明的一个实施方案中,成套包装可以包含一种或多种(包括所有)可以用于制备本发明农化组合物的组分。例如这些成套包装可以包含一种或多种杀真菌剂组分和/或助剂组分和/或杀虫剂组分和/或生长调节剂组分和/或除草剂。一种或多种组分可以相互组合或预配制而存在。在其中两种以上组分提供在成套包装中的那些实施方案中,各组分可以相互组合并包装在单独容器如罐、瓶、桶、袋、囊或箱中。在其他实施方案中,成套包装的两种或更多种组分可以分开包装,即不预配制或混合。成套包装可以包含一个或多个分开的容器如罐、瓶、桶、袋、囊或箱,其中各容器包含农化组合物的单独组分。本发明组合物的各组分可以单独或作为即混物或多组分成套包装来包装和进一步使用。在两种形式中,一种组分可以与其他组分分开或一起或者作为本发明多组分成套包装的成分用于制备本发明混合物。
用户如农夫通常将本发明组合物用于前剂量装置、小背包喷雾器、喷雾罐或喷雾飞机中。这里将该农化组合物用水和/或缓冲剂稀释至所需施用浓度,其中合适的话可以加入其他助剂,从而得到即用喷雾液或本发明农化组合物。每公顷农业利用区通常施用50-500升,优选100-400升即用喷雾液。
根据一个实施方案,用户可以自己在喷雾罐中混合本发明组合物的各组分,例如成套包装的各部分或二元或三元混合物的各部分并且合适的话可以加入其他助剂(桶混合)。在另一实施方案中,用户可以在喷雾罐中混合本发明组合物的各单独组分和部分预混的组分,例如包含亚磷酸的钙盐和/或选自A)-I)组的活性化合物的组分,并且合适的话可以加入其他助剂(桶混合)。在另一实施方案中,用户可以联合(例如作为桶混合物)或依次使用本发明组合物的各单独组分和部分预混的组分,例如包含亚磷酸的钙盐和/或A)-I)组活性化合物的组分。
优选包含亚磷酸的钙盐与至少一种选自A)组嗜球果伞素类,特别优选选自腈嘧菌酯、醚菌胺、氟嘧菌酯、亚胺菌、肟醚菌胺、啶氧菌酯、唑菌胺酯和肟菌酯的活性化合物的固体配制剂。
优选包含亚磷酸的钙盐与至少一种选自B)组羧酰胺类,尤其选自环酰菌胺、甲霜灵、精甲霜灵(mefenoxam)、甲呋酰胺、烯酰吗啉、氟吗啉、氟吡菌胺(picobenzamid)、苯酰菌胺、氯环丙酰胺和双炔酰菌胺的活性化合物的固体配制剂。
优选包含亚磷酸的钙盐与至少一种选自C)组唑类,尤其选自环唑醇、醚唑、氧唑菌、喹唑菌酮、氟硅唑、粉唑醇、环戊唑菌、腈菌唑、戊菌唑、丙环唑、丙硫菌唑、三唑酮、唑菌醇、戊唑醇、氟醚唑、戊叉唑菌、丙氯灵、氰霜唑、苯菌灵、多菌灵和噻唑菌胺的活性化合物的固体配制剂。
优选包含亚磷酸的钙盐与至少一种选自D)组含氮杂环化合物,尤其选自氟啶胺、环丙嘧啶、异嘧菌醇、嘧菌胺、二甲嘧菌胺、嗪氨灵、氟菌、吗菌灵(fodemorph)、丁苯吗啉、克啉菌、苯锈啶、异丙定、烯菌酮、唑酮菌、咪唑菌酮、噻菌灵、丙氧喹啉、噻二唑素、敌菌丹、灭菌丹、氰菌胺和喹氧灵的活性化合物的固体配制剂。
优选包含亚磷酸的钙盐与至少一种选自E)组氨基甲酸盐,尤其选自代森锰锌、代森联、甲基代森锌、福美双、异丙菌胺、flubenthiavalicarb(也已知为苯噻菌胺)和百维灵的活性化合物的固体配制剂。在另一实施方案中,优选的活性化合物是硫代-和二硫代氨基甲酸盐,如福美铁、代森锰锌、代森锰、威百亩、磺菌威、代森联、甲基代森锌、福美双、代森锌、福美锌,尤其是二硫代氨基甲酸盐。
优选包含亚磷酸的钙盐与至少一种选自F)组杀真菌剂,尤其选自二噻农、藻菌磷、乙磷铝、百菌清、抑菌灵、甲基托布津、清菌脲、苯菌酮、螺茂胺和5-氯-7-(4-甲基哌啶-1-基)-6-(2,4,6-三氟苯基)-[1,2,4]-三唑并[1,5-a]嘧啶的活性化合物的固体配制剂。
本发明的优选实施方案涉及表A所列组合物A-1至A-267,尤其呈固体配制剂形式,其中在每种情况下表A的一行对应于包含亚磷酸的钙盐(组分1)和选自所述行中提到的A)-F)组的相应其他活性化合物(组分2)的农化组合物。另一优选实施方案还涉及类似于表A的组合物,其中使用亚磷酸钙CaHPO3代替亚磷酸氢钙Ca(H2PO3)2。所述表A组合物中的活性化合物在每种情况下优选以协同增效有效量存在。
特别优选组合物A-9、A-20、A-186、A-232、A-5、A-66、A-139、A-171、A-196和A-200,组分1在每种情况下为Ca(H2PO3)2。非常特别优选组合物A-9、A-20、A-186和A-232,组分1在每种情况下为Ca(H2PO3)2。
表A:包含亚磷酸的钙盐(组分1)和A)-F)组其他活性化合物(组分2)的活性化合物组合物
行 | 组分1 | 组分2 |
A-223 | Ca(H2PO3)2 | 链霉素 |
A-224 | Ca(H2PO3)2 | 井冈霉素 |
A-225 | Ca(H2PO3)2 | 乐杀螨 |
A-226 | Ca(H2PO3)2 | 氯硝胺 |
A-227 | Ca(H2PO3)2 | 敌螨通 |
A-228 | Ca(H2PO3)2 | 敌螨普 |
A-229 | Ca(H2PO3)2 | 异丙消 |
A-230 | Ca(H2PO3)2 | 四氯硝基苯 |
A-231 | Ca(H2PO3)2 | 三苯锡基盐 |
A-232 | Ca(H2PO3)2 | 二噻农 |
A-233 | Ca(H2PO3)2 | 稻瘟灵 |
A-234 | Ca(H2PO3)2 | 克瘟散 |
A-235 | Ca(H2PO3)2 | 藻菌磷,乙磷铝 |
A-236 | Ca(H2PO3)2 | 异稻瘟净 |
A-237 | Ca(H2PO3)2 | 亚磷酸及衍生物 |
A-238 | Ca(H2PO3)2 | 定菌磷 |
A-239 | Ca(H2PO3)2 | 甲基立枯磷 |
A-240 | Ca(H2PO3)2 | 百菌清 |
A-241 | Ca(H2PO3)2 | 抑菌灵 |
A-242 | Ca(H2PO3)2 | 双氯酚 |
A-243 | Ca(H2PO3)2 | 磺菌胺 |
A-244 | Ca(H2PO3)2 | 六氯苯 |
A-245 | Ca(H2PO3)2 | 戊菌隆 |
A-246 | Ca(H2PO3)2 | 五氯酚及盐 |
A-247 | Ca(H2PO3)2 | 四氯苯酞 |
A-248 | Ca(H2PO3)2 | 五氯硝基苯 |
A-249 | Ca(H2PO3)2 | 甲基托布津 |
A-250 | Ca(H2PO3)2 | 对甲抑菌灵 |
A-251 | Ca(H2PO3)2 | N-(4-氯-2-硝基苯基)-N-乙基-4-甲基苯磺酰胺 |
A-252 | Ca(H2PO3)2 | Bordeaux混合物 |
A-253 | Ca(H2PO3)2 | 联苯 |
A-254 | Ca(H2PO3)2 | 拌棉醇 |
A-255 | Ca(H2PO3)2 | 环氟菌胺 |
A-256 | Ca(H2PO3)2 | 清菌脲 |
A-257 | Ca(H2PO3)2 | 二苯胺 |
A-258 | Ca(H2PO3)2 | 苯菌酮 |
A-259 | Ca(H2PO3)2 | 米多霉素 |
上面作为组分2提到的活性化合物、其制备及其对有害真菌的作用是已知的(参见http://www.alanwood.net/pesticides/);它们可以市购。根据IUPAC命名的化合物、其制备及其杀真菌作用同样是已知的(参见EP-A226 917;EP-A 1 028 125;EP-A 1 035 122;EP-A 1 201 648;WO 98/46608;WO 99/24413;WO 03/14103;WO 03/053145;WO 03/066609;WO04/049804)。
在优选实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂包括至少一种选自二噻农、唑菌胺酯、啶酰菌胺、5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、烯酰吗啉、代森联、代森锰锌、灭菌丹和亚胺菌的杀真菌剂。优选杀真菌剂为至少一种选自二噻农、唑菌胺酯、啶酰菌胺和5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺的杀真菌剂。
在特别优选的实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂为含硫杂环化合物,优选二噻农。亚磷酸氢钙与该杀真菌剂的重量比在大多数情况下为50/1-1/20,优选10/1-1/5,尤其是7/1-1/1。
在另一特别优选的实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂为嗜球果伞素类,优选唑菌胺酯。亚磷酸氢钙与该杀真菌剂的重量比在大多数情况下为3/1-1/500,优选1/10-1/200,尤其是1/80-1/120。
在另一特别优选的实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂为羧酰苯胺类,优选啶酰菌胺。亚磷酸氢钙与该杀真菌剂的重量比在大多数情况下为3/1-1/300,优选1/5-1/100,尤其是1/35-1/65。
在另一特别优选的实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂为杀真菌的[1,2,4]三唑并[1,5-a]嘧啶类,优选5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺。亚磷酸氢钙与该杀真菌剂的重量比在大多数情况下为5/1-1/200,优选1/1-1/50,尤其是1/5-1/25。
在另一特别优选的实施方案中,亚磷酸的钙盐为亚磷酸氢钙且杀真菌剂为二噻农以及选自二噻农、唑菌胺酯、啶酰菌胺、5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、烯酰吗啉、代森联、代森锰锌、灭菌丹和亚胺菌的第二杀真菌剂。亚磷酸氢钙与第二杀真菌剂的重量比在大多数情况下为50/1-1/20,优选15/1-1/5,尤其是10/1-1/1。
农药总量基于固体配制剂为1-40重量%,优选3-30重量%。
活性化合物的总量为固体配制剂中农药和亚磷酸的钙盐的总和。活性化合物的总量基于固体配制剂为至少40重量%,优选至少50重量%,尤其是至少60重量%。
本发明此外还提供了一种用于作物保护的固体配制剂,该配制剂包含亚磷酸的钙盐和杀真菌剂。固体配制剂类型的实例是可溶于水中(可溶性)或可分散于水中(可湿性)的可湿性粉末或粉剂(WP,SP,SS,WS,DP,DS)或颗粒(SG,WG,GR,GG,MG)。本发明的固体配制剂优选呈颗粒形式,尤其是水溶性颗粒或水分散性颗粒形式。颗粒的平均粒度通常为0.05-5mm,优选0.1-1mm。
在固体配制剂中亚磷酸的钙盐可以包含亚磷酸氢钙和/或亚磷酸钙。优选固体配制剂中亚磷酸的钙盐包括亚磷酸氢钙。
此外,本发明固体配制剂还可以包含常用于配制作物保护剂的助剂,助剂的选择取决于特定使用形式和/或活性化合物。常用于配制作物保护剂的助剂实例是溶剂、固体载体、表面活性剂(如加溶剂、保护性胶体、润湿剂和增粘剂)、结块剂、有机和无机增稠剂、杀菌剂、防冻剂、消泡剂、着色剂和粘合剂(例如用于。
溶剂的实例是水,中到高沸点的有机溶剂如矿物油馏分,如煤油和柴油,此外还有煤焦油和植物或动物来源的油,脂族、环状和芳族烃类,例如石蜡,四氢化萘,烷基化萘及其衍生物,烷基化苯及其衍生物,醇类如甲醇、乙醇、丙醇、丁醇和环己醇,二醇类,酮类如环己酮、γ-丁内酯,二甲基脂肪酸酰胺,脂肪酸和脂肪酸酯以及强极性溶剂,例如胺类,如N-甲基吡咯烷酮。原则上还可以使用溶剂混合物,以及上述溶剂和水的混合物。它们优选包含水作为溶剂。本发明固体配制剂通常基本不含有机溶剂。优选固体配制剂包含至多20重量%,更优选至多10重量%,特别优选至多5重量%,特别是至多2重量%,尤其是至多0.5重量%有机溶剂。优选固体配制剂包含至多10重量%,更优选至多5重量%,特别优选至多2重量%,特别是至多1重量%,尤其是至多0.3重量%水,不考虑以结晶水结合在亚磷酸的钙盐中的水。
例如可以提及下列固体载体:a)无机化合物:矿土,如硅胶、硅酸盐、滑石、高岭土、活性粘土(attaclay)、石灰石、石灰、白垩、黄土、粘土、白云石、硅藻土、硫酸钙、硫酸镁、氧化镁、硅镁土、蒙脱土、云母、蛭石、合成硅酸、无定形硅酸和合成硅酸钙或其混合物;b)有机化合物:磨碎的塑料,肥料如硫酸铵、磷酸铵、硝酸铵、硫脲和脲,植物来源的产品如谷粉、树皮粉、木粉和坚果壳粉、纤维素粉。优选的固体载体为硅酸。固体载体还可以用作结块剂,如硅酸。因此,对本发明而言,结块剂为固体载体。
本发明固体配制剂优选包含至多25重量%,特别优选至多20重量%,特别是至多10重量%,尤其是至多5重量%固体载体。该类固体载体的低含量允许活性化合物和其他助剂的更高含量。
合适的表面活性剂(助剂、润湿剂、增粘剂、分散剂或乳化剂)是芳族磺酸如木素磺酸类型,挪威Borregaard)、苯酚磺酸、萘磺酸类型,Akzo Nobel,USA)和二丁基萘磺酸类型,德国BASF)的碱金属、碱土金属和铵盐,以及脂肪酸的盐,烷基-和烷基芳基磺酸盐,烷基、月桂基醚和脂肪醇硫酸盐,还有硫酸化十六-、十七-和十八烷醇的盐,以及脂肪醇乙二醇醚的盐,磺化萘及其衍生物与甲醛的缩合物,萘或萘磺酸与苯酚和甲醛的缩合物,聚氧乙烯辛基酚醚,乙氧基化异辛基酚、辛基酚或壬基酚,烷基苯基聚乙二醇醚,三丁基苯基聚乙二醇醚,烷基芳基聚醚醇,异十三烷醇,脂肪醇/氧化乙烯缩合物,乙氧基化蓖麻油,聚氧乙烯烷基醚或聚氧丙烯烷基醚,月桂醇聚乙二醇醚乙酸酯,山梨醇酯,木素亚硫酸盐废液,以及蛋白质,变性蛋白,多糖(例如甲基纤维素),疏水改性淀粉,聚乙烯醇类型,瑞士Clariant),聚羧酸盐类型,德国BASF),聚烷氧基化物,聚乙烯胺类型,德国BASF),聚乙烯亚胺类型,德国BASF),聚乙烯吡咯烷酮及其共聚物。此外,例如合适的还有脂肪醇烷氧基化物的磷酸酯A-EP,德国BASF)和烷基聚葡糖苷。
优选本发明的固体配制剂包含至少一种芳族磺酸和/或其盐。在一个实施方案中,该配制剂还可以包含不止一种,例如两种或三种。合适的芳族磺酸和/或其盐例如为木素磺酸类型,挪威Borregaard),苯酚磺酸,萘磺酸类型,Akzo Nobel,USA)和二丁基萘磺酸类型,德国BASF),烷基芳基磺酸盐,磺化萘及其衍生物与甲醛的缩合物类型,德国BASF),萘磺酸与苯酚和甲醛的缩合物。合适的盐例如为碱金属、碱土金属或铵盐。芳族磺酸和/或其盐的含量基于固体配制剂的总重量通常为1-40重量%,优选5-30重量%,特别优选10-25重量%。
优选该固体配制剂包含至少两种不同的芳族磺酸和/或其盐。这两种芳族磺酸和/或其盐的重量比通常为10∶1-1∶1,优选5∶1-1∶1,尤其是2∶1-1∶1。特别优选该固体配制剂包含木素磺酸或其盐以及萘磺酸与甲醛和/或苯酚的缩合物或其盐。它尤其包含木素磺酸钠和萘磺酸/甲醛缩合物钠盐。该至少两种不同芳族磺酸和/或其盐的总量基于固体配制剂的总重量通常为10-45重量%,优选15-40重量%,特别优选20-35重量%。
特别优选该固体配制剂包含至少两种不同的芳族磺酸和/或其盐以及至少一种其他表面活性剂。其他表面活性剂优选为脂肪醇烷氧基化物的磷酸酯、烷基萘磺酸酯、烷基葡糖苷、月桂基硫酸酯或其碱金属、碱土金属或铵盐。其他表面活性剂的含量基于固体配制剂的总重量通常为0.1-10重量%,优选0.5-5重量%,特别优选1-3重量%。
表面活性剂的比例基于该固体配制剂的总重量通常为0.5-60重量%,优选10-50重量%,特别优选20-40重量%。
此外,可以将下列物质以本身常规的量用作其他助剂:
水溶性盐,例如水溶性铵盐,如硫酸铵、硫酸氢铵、氯化铵、乙酸铵、甲酸铵、草酸铵、碳酸铵、碳酸氢铵、硫代硫酸铵、二磷酸氢铵、单磷酸二氢铵、磷酸氢钠铵、硫氰酸铵、氨基磺酸铵或氨基甲酸铵;或水溶性硫酸盐,如硫酸钠、硫酸钾、硫酸铵;或其他水溶性盐,如氯化钠、氯化钾、乙酸钠。优选水溶性铵盐或硫酸盐,尤其是硫酸铵;
粘合剂,如聚乙烯吡咯烷酮、聚乙烯醇、部分水解的聚乙酸乙烯酯、羧甲基纤维素、淀粉、乙烯基吡咯烷酮/乙酸乙烯酯共聚物和聚乙酸乙烯酯或其混合物;
配合物形成剂,如乙二胺四乙酸(EDTA)的盐、氨三乙酸的盐或聚磷酸的盐或其混合物;
增稠剂,如多糖以及有机和无机片状矿物,如黄原胶CPKelco,USA),23(法国Rhodia)或(R.T.Vanderbilt,USA)或(Engelhard Corp.,NJ,USA)。本发明固体配制剂通常基本不含增稠剂;
杀菌剂,如基于双氯酚和苄醇半缩甲醛的那些(ICI的或ThorChemie的RS和Rohm & Haas的MK),以及异噻唑啉酮衍生物如烷基异噻唑啉酮类和苯并异噻唑啉酮类(Thor Chemie的MBS)。本发明固体配制剂通常基本不含杀菌剂;
防冻剂,如乙二醇、丙二醇、尿素和甘油。本发明固体配制剂通常基本不含防冻剂;
着色剂(微水溶性颜料和水溶性染料二者),如以下列名称已知的染料和颜料:若丹明B,C.I.颜料红112和C.I.溶剂红1,颜料蓝15:4,颜料蓝15:3,颜料蓝15:2,颜料蓝15:1,颜料蓝80,颜料黄1,颜料黄13,颜料红48:2,颜料红48:1,颜料红57:1,颜料红53:1,颜料橙43,颜料橙34,颜料橙5,颜料绿36,颜料绿7,颜料白6,颜料棕25,碱性紫10,碱性紫49,酸性红51,酸性红52,酸性红14,酸性蓝9,酸性黄23,碱性红10,碱性红108。本发明固体配制剂通常基本不含着色剂。
本发明固体配制剂可以通过已知方法制备:
a)水分散性颗粒和水溶性颗粒(WG,SG)
将50重量份亚磷酸的钙盐细碎研磨并加入50重量份分散剂和润湿剂,借助工业装置(例如挤出机、喷雾塔、流化床)将其制成水分散性或水溶性颗粒。用水稀释得到稳定的活性化合物分散体或溶液。该配制剂的活性化合物含量为50重量%。
b)水分散性粉末和水溶性粉末(WP,SP,SS,WS)
将75重量份亚磷酸的钙盐在转子-定子磨机中研磨并加入25重量份分散剂、润湿剂和硅胶。用水稀释得到稳定的活性化合物分散体或溶液。该配制剂的活性化合物含量为75重量%。
c)粉剂(DP,DS)
将5重量份亚磷酸的钙盐细碎研磨并与95重量份细碎高岭土充分混合。这得到活性化合物含量为5重量%的可撒粉产品。
d)颗粒(GR,FG,GG,MG)
将0.5重量份亚磷酸的钙盐细碎研磨并结合99.5重量份载体。常见方法是挤出、喷雾干燥或流化床方法。这得到活性化合物含量为0.5重量%的不经稀释而施用的颗粒。
有利的是本发明制备包含所用亚磷酸的钙盐的固体配制剂的方法是一种其中干燥包含亚磷酸的钙盐的含水组合物的方法。通常首先提供包含亚磷酸的钙盐、杀真菌剂和任选的配制助剂的含水组合物。该含水组合物优选为悬浮液或淤浆。特别优选该含水组合物包含20-80重量%,优选30-70重量%,特别优选40-60重量%水,在每种情况下基于该含水组合物的总量。该含水组合物可以研磨,例如在球磨机中研磨。
含水组合物可以通过喷雾干燥或其他造粒方法干燥。优选造粒方法如挤出机造粒、流化床造粒、混合机造粒和盘式造粒。合适的温度范围是20-200℃,优选40-100℃的产品温度。特别合适的是流化床造粒(FBG)。取决于配制剂的所需组成,在FBG设备中喷雾并附聚包含该配方的所有成分的水溶液、乳液或悬浮液。干燥使得该固体配制剂的水含量至多为10重量%,优选至多5重量%,特别优选至多2重量%,特别是至多1重量%,尤其是至多0.3重量%水,不考虑亚磷酸的钙盐中作为结晶水结合的水。
然而,任选还可以首先在该设备中加入活性化合物盐和/或无机铵盐,将它们用该配方的剩余成分的溶液或乳液/悬浮液喷雾并由此附聚。此外还可以依次将包含该配方的某些成分的水溶液、乳液或悬浮液施加于活性化合物颗粒、活性化合物盐和/或无机铵盐上,由此得到各种涂层。
通常在流化床造粒过程中充分干燥颗粒。然而,可能有利的是在造粒之后在相同或分开的干燥器中进行分开的干燥步骤。在造粒/干燥之后,将产品冷却和筛分。
其他特别合适的方法是挤出机造粒。适合挤出机造粒的优选是篮式挤出机、径向挤出机或低程度压实颗粒的圆顶挤出机。为了造粒,使用造粒液体在合适的混合机中将固体混合物制成糊,直到形成可挤出材料。将该材料在所提到的挤出机之一中挤出。为了挤出,使用0.3-3mm(优选0.5-1.5mm)的孔尺寸。活性化合物、配制助剂和合适的话水溶性盐的混合物作为固体的混合物使用。通常预研磨这些混合物。在某些情况下,仅在合适磨机中预研磨水不溶性物质就足够了。合适的造粒液体是水、本发明的APG或其水溶液。还合适的是无机盐、非离子表面活性剂、阴离子表面活性剂的水溶液,粘合剂如聚乙烯基吡咯烷酮、聚乙烯醇、羧甲基纤维素、淀粉、乙烯基吡咯烷/乙酸乙烯酯共聚物、糖类、糊精或聚乙二醇的溶液。在挤出机造粒之后,将所得颗粒干燥并且合适的话筛分以除去太粗或太细的颗粒。
所得颗粒为无尘、自由流动的不结块产品,其易溶于或分散于冷水中。
本发明固体配制剂通常包含0.01-95重量%,优选0.1-90重量%,特别优选20-80重量%,尤其是30-70重量%亚磷酸的钙盐。这里它优选以90-100%,优选95-100%的纯度使用。
固体配制剂通常具有下列组成:
20-80重量%亚磷酸的钙盐
1-40重量%杀真菌剂和任选其他农药
0.5-60重量%表面活性剂
其他助剂加至100重量%。
优选下列组成:
20-80重量%亚磷酸的钙盐
1-40重量%杀真菌剂和任选其他农药
5-30重量%木素磺酸或其盐
5-30重量%萘磺酸与苯酚和甲醛的缩合物
其他助剂加至100重量%。
特别优选下列组成:
30-70重量%亚磷酸的钙盐
3-30重量%杀真菌剂和任选其他农药
5-20重量%木素磺酸或其盐
10-25重量%萘磺酸与苯酚和甲醛的缩合物
0-5重量%其他表面活性剂
0-6重量%水溶性盐
0-5重量%固体载体
其他助剂加至100重量%。
在上面以示例方式提到的组合物的一个实施方案中,固体配制剂仅包含杀真菌剂作为活性化合物,在另一实施方案中,它额外包含其他农药。在上面以示例方式提到的组合物的另一实施方案中,固体配制剂包含亚磷酸氢钙作为亚磷酸的钙盐。
本发明还涉及一种防治植物病原性有害真菌的方法,其中将包含协同增效有效量的亚磷酸的钙盐和杀真菌剂的组合物施用于植物、种子或土壤。优选该组合物为本发明的固体配制剂。
为了处理植物繁殖材料,尤其是种子,通常使用粉剂(DS)、水分散性粉末和水溶性粉末(WS,SS)。这些配制剂可以以未稀释形式或优选以稀释形式施用于繁殖材料,尤其是种子上。这里所述配制剂可以稀释2-10倍,从而使用于拌种的配制剂中存在0.01-60重量%,优选0.1-40重量%活性化合物。施用可以在播种之前进行。植物繁殖材料的处理,尤其是种子的处理,对本领域熟练技术人员而言是已知的且通过植物繁殖材料的撒粉、包衣或造粒而进行,优选通过造粒、包衣和撒粉进行处理,从而例如防止种子的早期萌发。
含水使用形式可以通过添加水而由乳液浓缩物、糊或可湿性粉末(可喷雾粉末、油分散体)制备。为了制备乳液、糊或油分散体,可借助润湿剂、增粘剂、分散剂或乳化剂将该物质直接或溶于油或溶剂中后在水中均化。然而,还可以制备由活性物质、润湿剂、增粘剂、分散剂或乳化剂以及合适的话溶剂或油组成的浓缩物且该类浓缩物适于用水稀释。
即用制剂中的活性化合物浓度可以在较宽范围内变化。它们通常为0.0001-10%,优选0.01-1%。活性化合物还可以成功地用于超低容量法(ULV),其中可以施用包含超过95重量%活性化合物的配制剂或甚至施用不含添加剂的活性化合物。
可以将各种类型的油、润湿剂、助剂、除草剂、杀菌剂、其他杀真菌剂和/或农药加入活性化合物或包含它们的组合物中,合适的话甚至在紧临施用前加入(桶混合)。这些组合物可以以1∶100-100∶1,优选1∶10-10∶1的重量比加入本发明组合物中。就此而言合适的助剂尤其为有机改性的聚硅氧烷,例如Break Thru S醇烷氧基化物,例如245,MBA 1303,LF 300和ON 30;EO/PO嵌段聚合物,例如RPE 2035和B;醇乙氧基化物,例如XP80;以及磺基琥珀酸二辛酯钠,例如RA。
当用于作物保护中时,施用率为0.01-2.0kg/ha活性化合物,这取决于所需效果。当用于处理植物繁殖材料如种子时,活性化合物的用量通常为1-2000g/100kg,优选5-100g/100kg繁殖材料或种子。
本发明亚磷酸氢钙与至少一种杀真菌剂的组合以及包含它们的配制剂有利地适合防治有害真菌。它们对宽范围的植物病原性真菌[包括尤其源于根肿菌纲(Plasmodiophoromycetes)、Peronosporomycetes(同义词卵菌纲(Oomycetes))、壶菌纲(Chytridiomycetes)、接合菌纲(Zygomycetes)、子囊菌纲(Ascomycetes)、担子菌纲(Basidiomycetes)和半知菌纲(Deuteromycetes)(同义词不完全菌纲(Fungi imperfecti))的土传真菌]具有优异的活性。它们中的一些内吸有效并且可以作为叶面杀真菌剂、拌种用杀真菌剂和土壤杀真菌剂用于作物保护中。此外,它们适合防治尤其侵袭木材或植物根部的有害真菌。
它们对于在各种农作物如禾谷类,例如小麦、黑麦、大麦、小黑麦、燕麦或稻;甜菜,例如糖用甜菜或饲料甜菜;仁果、核果和浆果,例如苹果、梨、李、桃、杏仁、樱桃、草莓、悬钩子、黑莓或鹅莓;豆科植物,例如菜豆、扁豆、豌豆、苜蓿或大豆;油料植物,例如油菜、芥菜、橄榄、向日葵、椰子、可可、蓖麻豆、油棕、花生或大豆;葫芦科植物,例如南瓜、黄瓜或甜瓜;纤维植物,例如棉花、亚麻、大麻或黄麻;柑桔类水果,例如橙子、柠檬、葡萄柚或橘;蔬菜植物,例如菠菜、莴苣、芦笋、卷心菜、胡萝卜、洋葱、西红柿、土豆、葫芦或柿子椒;月桂类植物,例如鳄梨、肉桂或樟脑;能量和原料植物,例如玉米、大豆、小麦、油菜、甘蔗或油棕;玉米;烟草;坚果;咖啡;茶;香蕉;葡萄藤(食用葡萄和酿酒用葡萄);啤酒花;禾草,例如草坪;橡胶植物;观赏和森林植物,例如花卉、灌木、阔叶树和针叶树,以及植物繁殖材料如种子,以及这些植物的收获材料中防治大量病原性真菌特别重要。
优选将它们用于在农作物,例如土豆、糖用甜菜、烟草、小麦、黑麦、大麦、燕麦、稻、玉米、棉花、大豆、油菜、豆科植物、向日葵、咖啡或甘蔗;水果,葡萄藤以及观赏植物和蔬菜植物如黄瓜、西红柿、菜豆和南瓜以及植物繁殖材料如种子,以及这些植物的收获材料上防治大量真菌病原体。
术语“植物繁殖材料”包括植物的所有繁殖部分如种子,以及可以用于繁殖植物的无性植物部分如秧苗和块茎(例如土豆)。这些包括种子、根、果实、块茎、球茎、地下茎、嫩枝和其他植物部分,包括在萌发后或出苗后由土壤移植的秧苗和幼苗。幼苗可以通过例如通过浸渍或浇灌的完全或部分处理而防止有害真菌。
优选将亚磷酸氢钙和至少一种杀真菌剂的组合以及包含它们的配制剂对植物繁殖材料的处理用于在禾谷类作物如小麦、黑麦、大麦或燕麦;稻、玉米、棉花和大豆中防治大量真菌病原体。
术语“农作物”包括已经通过育种、诱变或基因工程修饰的植物。基因修饰植物是其基因材料以在自然条件下不能通过杂交、突变或自然重组(即基因信息的再组合)发生的方式修饰的植物。这里通常将一个或多个基因整合到植物的基因材料中以改善植物的性能。
因此,术语“农作物”包括已经通过育种和基因工程获得对某些类别除草剂的耐受性的植物,所述除草剂例如羟基苯基丙酮酸双加氧酶(HPPD)抑制剂;乙酰乳酸合成酶(ALS)抑制剂如磺酰脲类(EP-A-0257993,US5,013,659)或咪唑啉酮类(例如参见US 6,222,100,WO 01/82685,WO00/26390,WO 97/41218,WO 98/02526,WO 98/02527,WO04/106529,WO 05/20673,WO 03/14357,WO 03/13225,WO03/14356,WO 04/16073);烯醇丙酮酰莽草酸3-磷酸合成酶(EPSPS)抑制剂如草甘膦(例如参见WO 92/00377);谷氨酰胺合成酶(GS)抑制剂如草铵膦(例如参见EP-A-0242236,EP-A-242246)或oxynil除草剂(例如参见US5,559,024)。
已经借助常规育种(诱变)方法产生耐受咪唑啉酮类如咪草啶酸的许多农作物,例如油菜。已经借助基因工程方法产生耐受草甘膦或草铵膦的农作物如大豆、棉花、玉米、甜菜和油菜,它们以商标名(耐受草甘膦)和Liberty(耐受草铵膦)市购。
因此,术语“农作物”还包括由于通过基因工程的干预而产生一种或多种毒素的植物,该毒素例如为芽孢杆菌属(Bacillus)细菌菌株的那些。由该类基因修饰植物产生的毒素例如包括芽孢杆菌属杀虫蛋白,特别是苏云金芽孢杆菌(B.thuringiensis)杀虫蛋白,例如内毒素如CryIAb、CryIAc、Cry1F、Cry1Fa2、Cry2Ab、Cry3A、Cry3Bb1、Cry9c、Cry34Ab1或Cry35Ab1;或无性杀虫蛋白(VIP)如VIP1、VIP2、VIP3或VIP3A;线虫定居细菌的杀虫蛋白如发光杆菌属(Photorhabdus)或致病杆菌属(Xenorhabdus);动物有机体的毒素如黄蜂、蜘蛛或蝎毒素;真菌毒素如链霉菌属(Streptomycetes)毒素,植物凝集素如豌豆或大麦凝集素;凝集素;蛋白酶抑制剂如胰蛋白酶抑制剂、丝氨酸蛋白酶抑制剂、马铃薯块茎储藏蛋白(patatin)、半胱氨酸蛋白酶抑制剂或木瓜蛋白酶抑制剂;核糖体失活蛋白(RIP)如蓖麻蛋白、玉米-RIP、相思豆毒蛋白、丝瓜籽蛋白、皂草素或异株腹泻毒蛋白(bryodin);类固醇代谢酶如3-羟基类固醇氧化酶、蜕皮甾类-IDP糖基转移酶、胆固醇氧化酶、蜕皮激素抑制剂或HMG-CoA还原酶;离子通道阻断剂如钠通道或钙通道阻断剂;保幼激素酯酶;利尿激素受体(helicokinin受体);茋合成酶,联苄合成酶,壳多糖酶和葡聚糖酶。在植物中,这些毒素作为前毒素、杂合蛋白或截短的或其他方面改性的蛋白产生。杂合蛋白的特征在于不同蛋白域的新组合(例如参见WO02/015701)。该类毒素或产生这些毒素的基因修饰植物的其他实例公开于例如EP-A 374 753、WO 93/007278、WO 95/34656、EP-A 427 529、EP-A451 878、WO 03/18810和WO 03/52073中。生产这些基因修饰植物的方法对本领域熟练技术人员是已知的且例如公开于上述出版物中。许多上述毒素赋予产生它们的植物以对来自所有节肢动物分类学的害虫,尤其是甲虫(鞘翅目(Coeleropta))、双翅目昆虫(双翅目(Diptera))和蝶(鳞翅目(Lepidoptera))以及线虫(线虫纲(Nematoda))的耐受性。
产生一种或多种编码杀虫蛋白的基因的基因修饰植物例如描述于上述出版物中,并且它们中的一些可市购,例如(产生Cry1Ab毒素的玉米栽培品种),Plus(产生Cry1Ab和Cry3Bb1毒素的玉米栽培品种),(产生Cry9c毒素的玉米栽培品种),RW(产生Cry34Ab1、Cry35Ab1和酶膦丝菌素-N-乙酰转移酶[PAT]的玉米栽培品种);33B(产生Cry1Ac毒素的棉花栽培品种),I(产生Cry1Ac毒素的棉花栽培品种),II(产生Cry1Ac和Cry2Ab2毒素的棉花栽培品种);(产生VIP毒素的棉花栽培品种);(产生Cry3A毒素的土豆栽培品种);法国Syngenta Seeds SAS的Bt11(例如CB)和Bt176(产生Cry1Ab毒素和PAT酶的玉米栽培品种),法国Syngenta Seeds SAS的MIR604(产生Cry3A毒素的修饰译本的玉米栽培品种,参见WO 03/018810),比利时Monsanto Europe S.A.的MON 863(产生Cry3Bb1毒素的玉米栽培品种),比利时Monsanto Europe S.A.的IPC 531(产生Cry1Ac毒素的修饰译本的棉花栽培品种)和比利时Pioneer Overseas Corporation的1507(产生Cry1F毒素和PAT酶的玉米栽培品种)。
因此,术语“农作物”还包括借助基因工程产生一种或多种蛋白以增加其对细菌、病毒或真菌病原体的抗性或耐受性的植物,这类蛋白例如为与发病机理相关的蛋白(PR蛋白,例如参见EP-A 0 392 225),抗性蛋白(例如产生两种针对来自野生墨西哥土豆Solanum bulbocastanum的致病疫霉(Phytophthora infestans)的抗性基因的土豆栽培品种)或T4溶菌酶(例如通过产生该蛋白而耐受细菌如Erwinia amylvora的土豆栽培品种)。
因此,术语“农作物”还包括通过借助基因工程方法改进其产量,例如提高潜在产量(例如生物质、谷粒产量、淀粉、油或蛋白含量),对干旱、盐或其他限制性环境因素的耐受性或对害虫以及真菌、细菌和病毒病原体的耐受性的植物。术语“农作物”还包括已经借助基因工程方法而改性其成分以尤其改善人类或动物营养的植物,例如产生促进健康的长链ω-3脂肪酸或单不饱和ω-9脂肪酸的油料作物(例如油菜)。术语“农作物”还包括借助基因工程方法改性以改善原料生产的植物,例如提高支链淀粉含量的土豆(例如土豆)。
本文所用术语“蛋白”还包括寡肽、多肽或具体还掺入前蛋白、杂合蛋白、肽、截短的或其他方面改性的蛋白而由多肽制备的分子,包括由如下方法得到的那些:翻译后修饰如酰化(例如乙酰化:加入乙酰基,通常在蛋白的N-末端)、烷基化、加入烷基(例如加入乙基或甲基,通常在赖氨酸或精氨酸残基处)或脱甲基化、在C-末端处酰胺化、生物素化(用生物素基团酰化保存的赖氨酸残基)、甲酰化、维生素K依赖性γ-羧化、谷氨酰化(谷氨酸残基的共价结合)、糖基化(糖基与天冬酰胺、羟基赖氨酸、丝氨酸或苏氨酸结合形成糖蛋白)、糖化(非酶催糖基化)、甘氨酰化(一个或多个甘氨酸残基的共价结合)、共价加入血红素基团、羟基化、碘化、异戊二烯化(加入类异戊二烯基团,如法呢醇和香叶基香叶醇)、包括异戊烯化在内的硫辛酸化(加入硫辛酸基团)、GPI锚链形成(例如肉豆蔻酰化、法呢基化和香叶基香叶基化)、包括ADP核糖基化和黄素加入在内的核苷酸或其衍生物的共价结合、氧化、聚乙二醇化(pegylation)、共价结合磷脂酰肌醇、磷酸泛酰巯基乙胺化(由辅酶A转移4′-磷酸泛酰巯基乙胺基团)、磷酸化(通常将磷酸基团加入丝氨酸、酪氨酸、苏氨酸或组氨酸)、焦谷氨酸形成、脯氨酸残基外消旋化、氨基酸的tRNA-调节加成如精氨酰化、硫酸盐化(硫酸盐基团加成到酪氨酸残基)、硒化(硒到含硒蛋白中的共翻译掺入)、ISG化(与ISG15蛋白的共价结合[干扰素刺激基因15])、SUMO化(与SUMO蛋白[‘与小遍在蛋白相关的修饰基因’]的共价结合)、遍在蛋白化(共价结合于蛋白质遍在蛋白或多聚遍在蛋白)、瓜氨酸化或脱亚氨基化(精氨酸转化成瓜氨酸)、脱氨基化(谷氨酰胺转化成谷氨酸或天冬酰胺转化成天冬氨酸)、形成二硫化物桥(两个半胱氨酸残基的共价结合)或蛋白酶剪切(蛋白质在肽键处剪切)。
亚磷酸氢钙与至少一种杀真菌剂的组合以及包含它们的配制剂尤其适合防治下列植物病害:
·观赏植物、蔬菜作物(例如白锈菌(A.candida))和向日葵(例如婆罗门参白锈菌(A.tragopogonis))上的白锈菌属(Albugo)(白锈病);
·蔬菜、油菜(例如芸苔生链格孢(A.brassicola)或芸苔链格孢(A.brassicae))、糖用甜菜(例如A.tenuis)、水果、稻、大豆和土豆(例如早疫链格孢(A.solani)或链格孢(A.alternata))以及西红柿(例如早疫链格孢或链格孢)和小麦上的链格孢属(Alternaria)(黑斑病);
·糖用甜菜和蔬菜上的丝囊霉属(Aphanomyces);
·禾谷类和蔬菜上的壳二孢属(Ascochyta),例如小麦上的A.tritici(叶斑病)和大麦上的大麦壳二孢(A.hordei);
·玉米(例如玉蜀黍平脐蠕孢(D.maydis))、禾谷类(例如麦根腐平脐蠕孢(B.sorokiniana):叶褐斑病、斑枯病)、稻(例如稻平脐蠕孢(B.oryzae))和草坪上的平脐蠕孢属(Bipolaris)和内脐蠕孢属(Drechslera)(有性型:旋孢腔菌属(Cochliobolus));
·禾谷类(例如小麦或大麦)上的小麦白粉菌(Blumeria(以前:Erysiphe)graminis)(白粉病);
·葡萄藤上的葡萄座腔菌属(Botryosphaeria(干枯病))(例如葡萄座腔菌(B.obtusa);
·浆果和仁果(尤其是草莓)、蔬菜(尤其是莴苣、胡萝卜、根芹菜和卷心菜)、油菜、花卉、葡萄藤、森林植物和小麦(穗霉病)上的灰葡萄孢(Botrytis cinerea)(有性型:灰葡萄孢霉(Botryotinia fuckeliana):灰霉病);
·莴苣上的莴苣盘梗霉(Bremia lactucae)(霜霉病);
·阔叶树和针叶树上的长喙壳属(Ceratocystis)(同义词线嘴壳属(Ophiostoma))(蓝变),例如榆树上的榆枯萎病菌(C.ulmi)(荷兰榆病);
·玉米、稻、糖用甜菜(例如甜菜生尾孢(C.beticola))、甘蔗、蔬菜、咖啡、大豆(例如大豆灰斑病菌(C.sojina)或大豆紫斑病菌(C.kikuchii))和稻上的尾孢属(Cercospora)(尾孢叶斑病);
·西红柿(例如番茄叶霉菌(C.fulvum):番茄叶霉病、苜蓿叶斑病)和禾谷类上的枝孢属(Cladosporium),例如小麦上的草芽枝孢(C.herbarum)(黑穗病、烟灰霉病);
·禾谷类上的麦角菌(Claviceps purpurea)(麦角病);
·玉米(例如灰色长蠕孢(C.carbonum))、禾谷类(例如禾旋孢腔菌(C.sativus),无性型:麦根腐平脐蠕孢:叶褐斑病、斑枯病)和稻(例如宫部旋孢腔菌(C.miyabeanus),无性型:水稻长蠕孢(H.oryzae))上的旋孢腔菌属(无性型:长蠕孢属(Helminthosporium)或平脐蠕孢属)(叶斑病、斑枯病);
·棉花(例如棉炭疽病菌(C.gossypii))、玉米(例如禾生炭疽病菌(C.Graminicola):茎腐病和叶枯病)、浆果、土豆(例如西瓜炭疽病菌(C.coccodes):枯萎病)、菜豆(例如菜豆炭疽病菌(C.lindemuthianum))和大豆(例如大豆炭疽病菌(C.truncatum))上的剌盘孢属(Colletotrichum)(有性型:围小丛壳菌属(Glomerella)(叶枯病、炭疽病);
·伏革菌属(Corticium),例如稻上的笹木伏革菌(C.sasakii)(纹枯病);
·大豆和观赏植物上的黄瓜褐斑病菌(Corynespora cassiicola)(叶斑病);
·锈斑病菌属(Cycloconium),例如橄榄树上的C.Oleaginum;
·果树、葡萄藤(例如C.liriodendri,有性型:Neonectria liriodendri:乌脚病)和许多观赏树上的人参生柱隔孢属(Cylindrocarpon)(例如果树腐烂病或葡萄藤幼苗衰弱病,有性型:丛赤壳属(Nectria)或杓兰菌根菌属(Neonectria));
·大豆上的白纹羽菌(Dematophora(有性型:Rosellinia)necatrix)(白银腐病/茎腐病);
·北茎溃疡菌属(Diaporthe),例如大豆上的大豆北茎溃疡病菌(D.phaseolorum)(立枯疡);
·玉米、禾谷类如大麦(例如大麦网斑内脐蠕孢(D.teres),网斑病)和小麦(例如D.tritici-repentis:黄斑病)、稻和草坪上的内脐蠕孢属(同义词长蠕孢属,有性型:核腔菌属(Pyrenophora));
·由斑褐孔菌(Formitiporia(同义词Phellinus)punctata)、F.mediterranea、Phaeomoniella chlamydospora(以前为Phaeoacremonium chlamydosporum)、Phaeoacremonium aleophilum和/或葡萄座腔菌(Botryosphaeria obtusa)引起的葡萄藤上的埃斯卡(Esca)(葡萄藤枯萎病,干枯病);
·仁果(E.pyri)、浆果(覆盆子痂囊腔菌(E.veneta):炭疽病、茎斑病)和葡萄藤(葡萄痂囊腔菌(E.ampelina):炭疽病、鸟眼腐病)上的痂囊腔菌属(Elsinoe);
·稻上的稻叶黑粉菌(Entyloma oryzae)(叶黑粉病);
·小麦上的附球菌属(Epicoccum)(黑穗病、烟灰霉病);
·糖用甜菜(甜菜白粉菌(E.betae))、蔬菜(例如豌豆白粉菌(E.pisi))如黄瓜(例如二孢白粉菌(E.cichoracearum))和卷心菜植物如油菜(例如E.cruciferarum)上的白粉菌属(Erysiphe)(白粉病);
·果树、葡萄藤和许多观赏树上的侧弯孢菌(Eutypa lata)(Eutypa溃疡病或枯萎病,无性型:Cytosporina lata,同义词Libertella blepharis);
·玉米(例如玉米大斑病菌(E.turcicum))上的突脐蠕孢属(Exserohilum)(同义词长蠕孢属);
·各种植物上的镰孢霉属(Fusarium)(有性型:赤霉属(Gibberella))(枯萎病,根腐病和茎腐病),例如禾谷类(例如小麦或大麦)上的禾本科镰孢(F.graminearum)或大刀镰孢(F.culmorum)(根腐病和穗枯病或穗霉病),西红柿上的尖镰孢(F.oxysporum),大豆上的茄镰孢(F.solani)和玉米上的轮枝镰孢(F.verticillioides);
·禾谷类(例如小麦或大麦)和玉米上的禾顶囊壳(Gaeumannomycesgraminis)(全蚀病、黑根腐病);
·禾谷类(例如玉蜀黍赤霉(G.zeae))和稻(例如藤仓赤霉(G.fujikuroi):恶苗病)上的赤霉属;
·葡萄藤、仁果和其他植物上的苹果炭疽病菌(Glomerella cingulata)以及棉花上的棉炭疽病菌(G.gossypii);
·稻上的Grainstaining complex;
·葡萄藤上的葡萄黑腐病菌(Guignardia bidwellii)(黑腐病);
·蔷薇科植物和刺柏上的锈菌属(Gymnosporangium),例如梨上的G.sabinae(刺柏-梨锈病);
·玉米、禾谷类和稻上的长蠕孢属(同义词内脐蠕孢属,有性型:旋孢腔菌属);
·驼孢锈菌属(Hemileia),例如咖啡上的咖啡驼孢锈菌(H.vastatrix)(咖啡叶锈病);
·葡萄藤上的褐斑拟棒束孢(Isariopsis clavispora)(同义词Cladosporium vitis);
·大豆和棉花上的菜豆壳球孢(Macrophomina phaseolina(同义词phaseoli))(根腐病和茎腐病);
·禾谷类(例如小麦或大麦)上的雪霉叶枯菌(Microdochium(同义词Fusarium)nivale(雪霉病);
·大豆上的扩散叉丝壳(Microsphaera diffusa)(白粉病);
·丛梗孢属(Monilinia),例如核果和其他蔷薇科植物上的核果链核盘菌(M.laxa)、桃褐腐菌(M.fructicola)和M.fructigena(花腐病);
·禾谷类、香蕉、浆果和花生上的球腔菌属(Mycosphaerella),例如小麦上的禾生球腔菌(M.graminicola)(无性型:小麦壳针孢(Septoria tritici),壳针孢叶斑病)或香蕉上的斐济球腔菌(M.fijiensis)(黑条叶斑病);
·卷心菜(例如芸苔霜霉(P.brassicae))、油菜(例如寄生霜霉(P.parasitica))、球茎植物(例如大葱霜霉(P.destructor))、烟草(烟草霜霉(P.tabacina))和大豆(例如大豆霜霉病菌(P.manshurica))上的霜霉属(Peronospora)(霜霉病);
·大豆上的豆薯层锈菌(Phakopsora pachyrhizi)和山马蟥层锈菌(P.Meibomiae)(大豆锈病);
·例如葡萄藤(例如P.Tracheiphila和P.tetraspora)和大豆(例如大豆茎褐腐病菌(P.gregata):茎病害)上的瓶霉菌属(Phialophora);
·油菜和卷心菜上的黑胫茎点霉(Phoma lingam)(根腐病和茎腐病)以及糖用甜菜上的甜菜茎点霉(P.betae)(叶班病);
·向日葵、葡萄藤(例如葡萄黑腐病菌(P.viticola):茎斑病和叶斑病)和大豆(例如茎溃疡、豆荚凋腐病和蔓枯病:P.phaseoli,有性型:大豆北茎溃疡病菌(Diaporthe phaseolorum))上的拟茎点霉属(Phomopsis);
·玉米上的玉米褐斑病菌(Physoderma maydis)(褐斑病);
·各种植物如柿子椒和黄瓜植物(例如辣椒疫霉(P.capsici))、大豆(例如大豆疫霉(P.megasperma),同义词P.sojae)、土豆和西红柿(例如致病疫霉(P.infestans):晚疫病)和阔叶树(例如栎树猝死病菌(P.ramorum):橡树急死病)上的疫霉属(Phytophthora)(枯萎病,根腐病,叶腐病,茎腐病和果树腐烂病);
·卷心菜、油菜、小萝卜和其他植物上的芸苔根肿菌(Plasmodiophora brassicae)(根肿病);
·霜霉属(Plasmopara),例如葡萄藤上的葡萄生单轴霉(P.viticola)(葡萄藤霜霉病,霜霉病)和向日葵上的霍尔斯单轴霉(P.halstedii);
·蔷薇科植物、啤酒花、仁果和浆果上的叉丝单囊壳属(Podosphaera)(白粉病),例如苹果上的苹果白粉病菌(P.leucotricha);
·例如禾谷类如大麦和小麦(禾谷多粘菌(P.graminis))以及糖用甜菜(甜菜多粘菌(P.betae))上的多粘菌属(Polymyxa)以及由此传播的病毒病害;
·禾谷类如小麦或大麦上的小麦基腐病菌(Pseudocercosporella herpotrichoides)(眼斑病、茎变色,有性型:Tapesia yallundae);
·各种植物上的假霜霉属(Pseudoperonospora)(霜霉病),例如黄瓜植物上的古巴假霜霉(P.cubensis)或啤酒花上的葎草假霜(P.humili);
·葡萄藤上的Pseudopezicula tracheiphila(葡萄角斑叶焦病菌,无性型:瓶霉属(Phialophora));
·各种植物上的柄锈菌属(Puccinia)(锈病),例如禾谷类如小麦、大麦或黑麦上的小麦柄锈菌(P.triticina)(小麦褐锈病),条形柄锈病(P.striiformis)(条锈病),大麦柄锈病(P.hordei)(黄矮叶锈病),禾柄锈菌(P.graminis)(茎锈病、黑锈病)或小麦叶锈菌(P.recondita)(黑麦褐锈病),以及芦笋上的柄锈菌属(例如天门冬属柄锈病(P.asparagi));
·小麦上的小麦黄斑叶枯病菌(Pyrenophora(无性型:Drechslera)tritici-repentis)(黄斑病)或大麦上的大麦网斑内脐蠕孢(P.teres)(网斑病);
·梨孢属(Pyricularia),例如稻上的稻瘟病菌(P.oryzae)(有性型:Magnaporthe grisea,稻瘟病)以及草坪和禾谷类上的稻梨孢菌(P.grisea);
·草坪、稻、玉米、小麦、棉花、油菜、向日葵、大豆、糖用甜菜、蔬菜和其他植物(例如终极腐霉菌(P.ultimum)或瓜果腐霉(P.aphanidermatum))上的腐霉属(Pythium)(立枯病);
·柱隔孢属(Ramularia),例如大麦上的R.collo-cygni(叶斑病/生理叶斑病)和糖用甜菜上的甜菜叶斑病菌(R.beticola);
·棉花、稻、土豆、草坪、玉米、油菜、糖用甜菜、蔬菜和各种其他植物上的丝核菌属(Rhizoctonia),例如大豆上的立枯丝核菌(R.solani)(根腐病和茎腐病),稻上的R.solani(纹枯病)或小麦或大麦上的禾谷丝核菌(R.cerealis)(小麦纹枯病);
·草莓、胡萝卜、卷心菜、葡萄藤和西红柿上的葡枝根霉(Rhizopus stolonifer)(软腐病);
·大麦、黑麦和小黑麦上的黑麦喙孢(Rhynchosporium secalis)(褐斑病);
·稻上的稻帚枝霉(Sarocladium oryzae)和S.attenuatum(叶鞘腐败病);
·蔬菜和农作物如油菜、向日葵(例如核盘菌(Sclerotinia sclerotiorum))和大豆(例如S.rolfsii)上的核盘菌属(Sclerotinia)(茎腐病或白绢病);
·各种植物上的壳针孢属(Septoria),例如大豆上的大豆壳针孢(S.glycines)(褐斑病),小麦上的小麦壳针孢(S.tritici)(壳针孢叶斑病)和禾谷类上的颖枯壳多孢(S.(同义词Stagonospora)nodorum)(叶花斑枯病);
·葡萄藤上的葡萄钩丝壳(Uncinula(同义词Erysiphe)necator)(白粉病,无性型:Oidium tuckeri);
·玉米(例如玉米大斑病菌(S.turcicum),同义词大斑凸脐蠕孢(Helminthosporium turcicum))和草坪上的大斑病菌属(Setospaeria)(叶枯病);
·玉米(例如丝轴黑粉菌(S.reiliana):丝黑穗病)、小米和甘蔗上的轴黑粉菌属(Sphacelotheca)(黑穗病);
·黄瓜植物上的单丝壳白粉菌(Sphaerotheca fuliginea)(白粉病);
·土豆上的粉痂菌(Spongospora subterranea)(粉痂病)以及由此传播的病毒病害;
·禾谷类上的壳多孢属(Stagonospora),例如小麦上的颖枯壳多孢(S.nodorum)(叶花斑枯病,有性型:颖枯球腔菌(Leptosphaeria[同义词Phaeosphaeria]nodorum));
·土豆上的马铃薯癌肿病菌(Synchytrium endobioticum)(土豆癌肿病);
·外囊菌属(Taphrina),例如桃上的畸形外囊菌(T.deformans)(缩叶病)和李上的李外囊菌(T.pruni)(囊果李);
·烟草、仁果、蔬菜作物、大豆和棉花上的根串珠霉属(Thielaviopsis)(黑色根腐病),例如黑色根腐病菌(T.basicola)(同义词Chalara elegans);
·禾谷类上的腥黑粉菌属(Tilletia)(腥黑穗病或光腥黑穗病),例如小麦上的T.tritici(同义词T.caries,小麦腥黑穗病)和T.controversa(矮腥黑穗病);
·大麦或小麦上的肉孢核瑚菌(Typhula incarnata)(灰雪腐病);
·黑粉菌属(Urocystis),例如黑麦上的隐条黑粉菌(U.occulta)(条黑粉病);
·蔬菜植物,如菜豆(例如疣顶单胞锈菌(U.appendiculatus),同义词U.phaseoli)和糖用甜菜(例如甜菜锈病菌(U.betae))上的单孢锈属(Uromyces)(锈病);
·禾谷类(例如麦散黑粉菌(U.nuda)和U.avaenae)、玉米(例如玉蜀黍黑粉菌(U.maydis):玉米黑穗病)和甘蔗上的黑粉菌属(Ustilago)(黑穗病);
·苹果(例如苹果黑星病(V.inaequalis))和梨上的黑星菌属(Venturia)(黑星病);以及
·各种植物如果树和观赏树、葡萄藤、浆果、蔬菜和农作物上的轮生菌属(Verticillium)(叶和枝枯萎病),例如草莓、油菜、土豆和西红柿上的茄黄萎病菌(V.dahliae)。
亚磷酸的钙盐和至少一种其他杀真菌剂的组合以及包含它们的配制剂此外还适合防治有害真菌以保护材料和建筑物(例如木材、纸张、漆分散体、纤维或织物)和保护储藏的产品。在木材和建筑物保护中,特别应注意下列有害真菌:子囊菌纲真菌,例如线嘴壳属,长喙壳属,出芽短梗霉(Aureobasidium pullulans),Sclerophoma spp.,毛壳属(Chaetomium),腐质霉属(Humicola),彼得壳属(Petriella),毛束霉属(Trichurus);担子菌纲真菌,例如粉孢革菌属(Coniophora),革盖菌属(Coriolus),粘褶菌属(Gloeophyllum),香菇属(Lentinus),侧耳属(Pleurotus),卧孔属(Poria),干朽菌属(Serpula)和干酪菌属(Tyromyces),半知菌纲真菌,例如曲霉属(Aspergillus),枝孢属,青霉属(Penicillium),木霉属(Trichorma),链格孢属,拟青霉属(Paecilomyces)和接合菌纲(Zygomycetes)真菌,例如毛霉属(Mucor),此外在材料保护中应注意下列酵母真菌:假丝酵母属(Candida)和酿酒酵母(Saccharomyces cerevisae)。
亚磷酸的钙盐以具有至少一种杀真菌剂的组合物形式通过用杀真菌有效量的化合物I处理有害真菌、其栖息地或需要防止真菌侵染的植物或植物繁殖材料如种子、土壤、区域、材料或空间而施用。施用可以在植物、植物繁殖材料如种子、土壤、区域、材料或空间被真菌侵染之前和之后进行。亚磷酸的钙盐和杀真菌剂的施用可以同时或依次进行。
植物繁殖材料可以在播种或移栽时或甚至在播种或移栽之前直接用亚磷酸氢钙或包含亚磷酸氢钙的组合物预防性地处理。
术语“有效量”指足以在农作物上或在材料和建筑物保护中防治有害真菌且不对被处理农作物引起显著损害的量的农化组合物或化合物I。该量可以在宽范围内变化且受许多因素如待防治的有害真菌、被处理的各种农作物或材料、气候条件和化合物影响。
下列实施例用于说明本发明的实施方案。
实施例
化学品
萘磺酸/甲醛缩合物的钠盐,粉末状,活性物含量约78重量%,硫酸钠含量约17重量%,例如以NH 7519由BASF SE市购。
2-乙基己基葡糖苷,活性化合物含量65重量%,35重量%水,例如以AG6202由Akzo Nobel市购。
杀真菌剂A:5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺(可根据WO2005/087773、WO 2007/012598或WO 2008/087182得到)。
方法:
除非另有指明,试验在受控温室条件下原位(in planta)进行。在温室中的温度、大气湿度和光条件与宿主植物和病原体的特定要求相适应。将肉眼测定的侵染叶面积百分数值转化成以相对于未处理对照的百分数表示的效力。根据Abbott公式按如下计算效力(W):W=(1-a/b)*100。
a=对应于被处理植物的真菌侵染%,和
b=对应于未处理(对照)植物的真菌侵染%。
效力为0时被处理植物的侵染对应于未处理对照植物的侵染;效力为100%时被处理植物未被侵染。
根据Colby(Colby,S.R.“计算除草剂组合的协同增效和拮抗响应”,Weeds 15:20-22,1967)确定各组合的预期效力并与观察到的效力比较。
Colby公式:E=x+y-x*y/100
E=以浓度a和b使用活性化合物A和B的混合物时预期的效力,以未处理对照的%表示
x=以浓度a使用活性化合物A时的效力,以未处理对照的%表示
y=以浓度b使用活性化合物B时的效力,以未处理对照的%表示
实施例1-制备亚磷酸氢钙*水合物[Ca(H
2
PO
3
)
2
*H
2
O]
将22.6g氢氧化钙Ca(OH)2缓慢加入50g H3PO3在100ml水中的溶液中。将所得乳状悬浮液在真空干燥箱中于60℃下干燥。得到67g水合亚磷酸氢钙。
实施例2a-制备亚磷酸氢钙*水合物颗粒
首先将67g亚磷酸氢钙*水合物(来自实施例1)加入200ml水中并加入15g木素磺酸钠、15g萘磺酸/甲醛缩合物和3g脂肪醇烷氧基化物的磷酸酯。使用珠磨机将该悬浮液研磨并在60℃的温度下进行流化床造粒。这得到活性化合物含量为67%的WG配制剂。与水的浓度为1%的混合物的pH为3.9。
实施例2b-制备亚磷酸氢钙*水合物颗粒
首先将50g亚磷酸氢钙*水合物(来自实施例1)加入200ml水中,并加入26g木素磺酸钠、13g萘磺酸/甲醛缩合物和10g硫酸铵。使用珠磨机将该悬浮液研磨并在60℃的温度下进行流化床造粒。这得到活性化合物含量为50%的WG配制剂。与水的浓度为1%的混合物的pH为3.9。
实施例2c-制备亚磷酸氢钙*水合物颗粒
首先将46g亚磷酸氢钙*水合物加入200ml水中,并加入30g木素磺酸钠、13g萘磺酸/甲醛缩合物、10g硫酸铵和1g消泡剂。使用珠磨机将该悬浮液研磨并在60℃的温度下进行流化床造粒。这得到活性化合物含量为46%的WG配制剂。
实施例3a-w-制备包含活性化合物的颗粒(表1)
首先将一种或多种活性化合物和亚磷酸氢钙*水合物(来自实施例1)加入200ml水中,并加入木素磺酸钠、萘磺酸/甲醛缩合物和其他配制助剂。使用珠磨机将该悬浮液研磨并在60℃的温度下进行流化床造粒。这得到WG配制剂。测定在每种情况下该配制剂在水中浓度为1%的溶液的pH。所用材料的量和试验a-w的数据示于下表1。
实施例4-二噻农和Ca(H
2
PO
3
)对抗西红柿上的晚疫病
在温室中用活性组分浓度如下所述的含水悬浮液喷雾栽培品种为′bigbeef tomato St.Pierre′的盆栽植物的叶子至滴流点。5天后将叶子用密度为0.25×106个孢子/ml的致病疫霉的冷含水游动孢子悬浮液侵染。然后将植物置于温度为10-20℃的水蒸气饱和室中。6天候未处理但侵染的对照植物上的晚疫病发展到可以肉眼测定侵染百分数的程度(表2)。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌活性。
表2
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 300 | 31 | - |
B | Ca(H2PO3)2(II) | 750 | 13 | - |
C | I+II | 300+750 | 60 | 41 |
实施例5-杀真菌剂A和Ca(H
2
PO
3
)对抗西红柿上的晚疫病
通过用去离子水稀释杀真菌剂A在DMSO中的溶液和亚磷酸氢钙颗粒的配制剂而制备包含二噻农和亚磷酸氢钙(来自实施例2c)的喷雾液。
在温室中用活性化合物浓度如下所述的含水悬浮液喷雾栽培品种为′big beef tomato St.Pierre′的盆栽植物的叶子至滴流点。7天后将叶子用密度为0.25×106个孢子/ml的致病疫霉的冷含水游动孢子悬浮液侵染,其他程序如实施例4。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌活性(表3)。
表3
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 杀真菌剂A(I) | 50 | 39 | - |
B | Ca(H2PO3)2(II) | 750 | 0 | - |
C | I+II | 50+750 | 44 | 39 |
实施例6-唑菌胺酯和Ca(H
2
PO
3
)对抗葡萄藤上的霜霉病
通过用去离子水稀释唑菌胺酯在DMSO中的溶液和亚磷酸氢钙颗粒的配制剂而制备包含唑菌胺酯和亚磷酸氢钙(来自实施例2c)的喷雾液。
用活性化合物浓度如下所述的含水悬浮液喷雾栽培品种为′Riesling′的盆栽葡萄藤的叶子至滴流点。喷雾涂层干燥之后,将植物置于温室中1天。仅在此时才用葡萄生单轴霉的含水游动孢子悬浮液接种叶子。然后首先将葡萄藤置于24℃的水蒸气饱和室中48小时,然后置于温度为20-30℃的温室中5天。在此期间后,再次将植物置于潮湿室中16小时以促进孢子囊喷发。然后肉眼确定叶子下侧上的侵染发展程度。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,在每种情况下存在协同增效杀真菌作用(表4)。
表4
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 唑菌胺酯(I) | 0.5 | 92 | - |
B | Ca(H2PO3)2(II) | 50 | 3 | - |
C | I+II | 0.5+50 | 95 | 92 |
实施例7-二噻农和Ca(H
2
PO
3
)对抗葡萄藤上的霜霉病
通过用去离子水稀释二噻农在DMSO中的溶液和亚磷酸氢钙颗粒的配制剂而制备包含二噻农和亚磷酸氢钙(来自实施例2c)的喷雾液。如实施例6进行试验。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,在每种情况下存在协同增效杀真菌作用(表5)。
表5
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 10 | 62 | - |
B | Ca(H2PO3)2(II) | 50 | 3 | - |
C | I+II | 10+50 | 87 | 63 |
实施例8-二噻农和Ca(H
2
PO
3
)
2
对抗葡萄藤上的霜霉病
使用来自实施例7的喷雾液。该试验涉及特定施用方式:其中施用的叶面积仅由条形式的小矩形组成。这里发现具有高为1.5cm且宽为7cm的截面的条形式是有利的。所述施用在叶子上侧的下半部上进行。在喷雾涂层干燥之后,将植物置于温室中1天。仅在此时才用葡萄生单轴霉的含水游动孢子悬浮液接种叶子的下侧。然后首先将葡萄藤置于24℃的水蒸气饱和室中48小时,然后置于温度为20-30℃的温室中5天。在此期间后,再次将植物置于潮湿室中16小时以促进孢子囊喷发。然后肉眼确定叶子下侧顶部上的侵染发展程度。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,在每种情况下存在协同增效杀真菌作用(表6)。
表6
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 10 | 6 | - |
B | Ca(H2PO3)2(II) | 50 | 0 | - |
C | I+II | 10+50 | 18 | 6 |
实施例9-杀真菌剂A和Ca(H
2
PO
3
)对抗葡萄藤上的霜霉病(跨层作用)
根据实施例5制备喷雾液并调节至表7中所述活性化合物浓度。如实施例8进行测试;然而,将活性化合物施用于叶子上侧。为了使所述活性化合物被葡萄藤叶子吸收并且合适的话转运,在用葡萄生单轴霉接种之前48小时进行施用。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌作用(表7)。
表7
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 杀真菌剂A(I) | 5 | 1 | - |
B | Ca(H2PO3)2(II) | 100 | 0 | - |
C | I+II | 5+100 | 15 | 1 |
实施例10-杀真菌剂A和Ca(H
2
PO
3
)对抗葡萄藤上的霜霉病
根据实施例5制备包含杀真菌剂A和亚磷酸氢钙(来自实施例2c)的喷雾液。如实施例6进行该试验。然而,在喷雾涂层干燥之后,将植物置于温室中7天而不是1天。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,在每种情况下存在协同增效杀真菌作用(表8)。
表8
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 杀真菌剂A(I) | 100 | 85 | - |
B | Ca(H2PO3)2(II) | 750 | 9 | - |
C | I+II | 100+750 | 92 | 86 |
实施例11-啶酰菌胺和Ca(H
2
PO
3
)对抗大豆上的豆薯层锈菌
通过用去离子水稀释啶酰菌胺在DMSO中的溶液和亚磷酸氢钙颗粒的配制剂而制备包含啶酰菌胺和亚磷酸氢钙(来自实施例2c)的喷雾液。在栽培品种为′Monsoy′的大豆植物(glycine max)上用豆薯层锈菌进行试验。所用植物处于2叶阶段。用活性化合物浓度如下所述的含水悬浮液将叶子喷雾至滴流点。2天后用大豆锈病的夏孢子悬浮液接种被处理的叶子。然后将植物置于高大气湿度(95-99%)和20-22℃的室中24小时。在此期间孢子萌发并且芽管穿透到叶组织中。第二天将测试植物送回温室中并在23-26C的温度和65-70%的相对大气湿度下栽培10-12天。然后以百分数肉眼测定叶子上锈病真菌发展程度。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,在每种情况下存在协同增效杀真菌作用(表9)。
表9
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 啶酰菌胺(I) | 20 | 11 | - |
B | Ca(H2PO3)2(II) | 1000 | 48 | - |
C | I+II | 20+1000 | 79 | 54 |
实施例12-二噻农和Ca(H
2
PO
3
)对抗葡萄藤上的霜霉病
通过用自来水稀释二噻农在DMSO中的溶液和亚磷酸氢钙颗粒的配制剂而制备包含二噻农和亚磷酸氢钙(来自实施例2c)的喷雾液。在德国Rhineland Palatinate的测试场所使用自然侵染室外进行试验。使用GEP标准重复4次进行试验。使用14-16天的喷雾间隔总共在9个日期进行施用。所示结果打分在第6次施用1天后进行。按照EPPO准则PP 1/31(3)肉眼对叶子上的侵染强度%打分。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌活性(表10)。
表10
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 300 | 85 | - |
B | Ca(H2PO3)2(II) | 900 | 18 | - |
C | I+II | 300+900 | 93 | 88 |
实施例13-二噻农和Ca(H
2
PO
3
)
2
对抗葡萄藤上的霜霉病
如实施例12所述,在德国Rhineland Palatinate的测试场所使用自然侵染室外进行试验。使用14-16天的喷雾间隔总共在7个日期进行施用。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌作用(表11)。
表11
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 400 | 48 | - |
B | Ca(H2PO3)2(II) | 1200 | 21 | - |
C | I+II | 400+1200 | 76 | 59 |
实施例14-二噻农和Ca(H
2
PO
3
)
2
对抗葡萄藤上的霜霉病
如实施例12所述,在德国Rhineland Palatinate的测试场所使用自然侵染室外进行试验。使用9-11天的喷雾间隔总共在9个日期进行施用。所示结果打分在第8次施用4天后进行。在该试验中,根据Abbott计算的混合物的效力大于根据Colby计算的效力;因此,存在协同增效杀真菌活性(表11)。
表12
活性化合物 | 喷雾液中的浓度(ppm) | 效力W(%) | Colby预期效力(%) | |
A | 二噻农(I) | 300 | 56 | - |
B | Ca(H2PO3)2(II) | 900 | 24 | - |
C | I+II | 300+900 | 76 | 67 |
Claims (16)
1.亚磷酸的钙盐在农业中提高杀真菌剂效力的用途。
2.根据权利要求1的用途,其中所述亚磷酸的钙盐包括亚磷酸氢钙。
3.根据权利要求1或2的用途,其中所述杀真菌剂包括至少一种选自二噻农、唑菌胺酯、啶酰菌胺、5-乙基-6-辛基-[1,2,4]三唑并[1,5-a]嘧啶-7-基胺、烯酰吗啉、代森联、代森锰锌、灭菌丹或亚胺菌的杀真菌剂。
4.根据权利要求1-3中任一项的用途,其中所述亚磷酸的钙盐呈固体配制剂形式。
5.一种用于作物保护的固体配制剂,包含亚磷酸的钙盐和杀真菌剂。
6.根据权利要求5的固体配制剂,其中所述配制剂呈颗粒形式。
7.根据权利要求5或6的固体配制剂,其中所述亚磷酸的钙盐包括亚磷酸氢钙。
8.根据权利要求5-7中任一项的固体配制剂,其中所述配制剂包含至多25重量%固体载体。
9.根据权利要求5-8中任一项的固体配制剂,其中所述配制剂包含芳族磺酸和/或其盐。
10.根据权利要求5-9中任一项的固体配制剂,其中所述配制剂包含木素磺酸或其盐以及萘磺酸与甲醛和/或苯酚的缩合物或其盐。
11.一种制备包含亚磷酸的钙盐的固体配制剂的方法,其中干燥包含亚磷酸的钙盐的含水组合物。
12.根据权利要求11的方法,其中干燥使用造粒方法进行。
13.一种制备亚磷酸的钙盐的方法,其中将亚磷酸H3PO3加入氢氧化钙Ca(OH)2和/或氧化钙CaO的含水悬浮液中。
14.一种防治植物病原性有害真菌的方法,其中将包含协同增效有效量的亚磷酸的钙盐和杀真菌剂的组合物施用于植物、种子或土壤。
15.根据权利要求14的方法,其中所述组合物为根据权利要求5-10中任一项的固体配制剂。
16.以1-2000g/100kg的量包含根据权利要求5-10中任一项的固体配制剂的种子。
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Cited By (6)
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CN105746542A (zh) * | 2012-12-06 | 2016-07-13 | 陕西汤普森生物科技有限公司 | 一种含唑嘧菌胺的杀菌组合物 |
CN108135160A (zh) * | 2015-07-21 | 2018-06-08 | 瑟拉迪斯有限公司 | 稳定的农用组合物 |
CN109645011A (zh) * | 2019-01-29 | 2019-04-19 | 山东康德源农业科技有限公司 | 一种杀菌药肥及其制剂和应用 |
CN110199613A (zh) * | 2019-07-16 | 2019-09-06 | 黑龙江省农业科学院经济作物研究所 | 一种高钙营养亚麻芽菜的培植方法及其专用浸种方法 |
CN111848295A (zh) * | 2019-04-04 | 2020-10-30 | 宁波三江益农化学有限公司 | 一种含亚磷酸钾的杀菌组合物及应用 |
CN108641962B (zh) * | 2018-03-23 | 2022-02-18 | 湖北省农业科学院植保土肥研究所 | 一种提高小麦白粉菌离体保存时间的方法 |
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US10631542B2 (en) * | 2008-10-31 | 2020-04-28 | Agro-K Corporation | Compositions and methods for providing micronutrients in conjunction with plant growth regulation |
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AP2013006741A0 (en) * | 2010-08-26 | 2013-02-28 | Makhteshim Chem Works Ltd | Synergistic fungicidal composition |
EA201300907A1 (ru) | 2011-02-16 | 2014-02-28 | Басф Се | Способ борьбы с фитопатогенными грибами |
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FR2655816B1 (fr) * | 1989-12-14 | 1994-04-29 | Rhone Poulenc Agrochimie | Granules dispersables de produits fongicides. |
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FR2778314B1 (fr) * | 1998-05-07 | 2002-06-14 | Rhone Poulenc Agrochimie | Composition fongicide synergique comprenant un compose analogue de la strobilurine |
FR2787295A1 (fr) * | 1998-12-22 | 2000-06-23 | Rhone Poulenc Agrochimie | Composition fongicide synergique comprenant un compose analogue de la strobilurine |
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ITMI20051019A1 (it) * | 2005-05-31 | 2006-12-01 | Isagro Spa | Composizioni fungicide sinergiche |
CN1330564C (zh) * | 2005-09-29 | 2007-08-08 | 武汉理工大学 | 一种改性亚磷酸盐微细防锈颜料的制备方法 |
JP5162794B2 (ja) * | 2006-07-17 | 2013-03-13 | ディーエスエム アイピー アセッツ ビー.ブイ. | 新規な抗真菌組成物 |
-
2009
- 2009-06-02 WO PCT/EP2009/056713 patent/WO2009150076A2/de active Application Filing
- 2009-06-02 CN CN2009801221831A patent/CN102111997A/zh active Pending
- 2009-06-02 KR KR1020117000715A patent/KR20110028352A/ko not_active Application Discontinuation
- 2009-06-02 EP EP09761639A patent/EP2296465A2/de not_active Withdrawn
- 2009-06-02 BR BRPI0915043-9A patent/BRPI0915043A2/pt not_active IP Right Cessation
- 2009-06-02 MX MX2010012844A patent/MX2010012844A/es not_active Application Discontinuation
- 2009-06-02 JP JP2011512933A patent/JP2011522851A/ja not_active Withdrawn
- 2009-06-02 AU AU2009256715A patent/AU2009256715A1/en not_active Abandoned
- 2009-06-02 EA EA201100006A patent/EA019069B1/ru not_active IP Right Cessation
- 2009-06-02 CA CA2725594A patent/CA2725594A1/en not_active Abandoned
- 2009-06-02 US US12/997,084 patent/US20110105323A1/en not_active Abandoned
- 2009-06-11 AR ARP090102116A patent/AR072108A1/es not_active Application Discontinuation
-
2010
- 2010-11-25 IL IL209582A patent/IL209582A0/en unknown
- 2010-12-09 CR CR11834A patent/CR11834A/es not_active Application Discontinuation
- 2010-12-30 MA MA33473A patent/MA32427B1/fr unknown
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2011
- 2011-01-10 ZA ZA2011/00243A patent/ZA201100243B/en unknown
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105746542A (zh) * | 2012-12-06 | 2016-07-13 | 陕西汤普森生物科技有限公司 | 一种含唑嘧菌胺的杀菌组合物 |
CN108135160A (zh) * | 2015-07-21 | 2018-06-08 | 瑟拉迪斯有限公司 | 稳定的农用组合物 |
CN108641962B (zh) * | 2018-03-23 | 2022-02-18 | 湖北省农业科学院植保土肥研究所 | 一种提高小麦白粉菌离体保存时间的方法 |
CN109645011A (zh) * | 2019-01-29 | 2019-04-19 | 山东康德源农业科技有限公司 | 一种杀菌药肥及其制剂和应用 |
CN111848295A (zh) * | 2019-04-04 | 2020-10-30 | 宁波三江益农化学有限公司 | 一种含亚磷酸钾的杀菌组合物及应用 |
CN110199613A (zh) * | 2019-07-16 | 2019-09-06 | 黑龙江省农业科学院经济作物研究所 | 一种高钙营养亚麻芽菜的培植方法及其专用浸种方法 |
Also Published As
Publication number | Publication date |
---|---|
AR072108A1 (es) | 2010-08-04 |
EA019069B1 (ru) | 2013-12-30 |
EP2296465A2 (de) | 2011-03-23 |
MA32427B1 (fr) | 2011-06-01 |
AU2009256715A1 (en) | 2009-12-17 |
EA201100006A1 (ru) | 2011-08-30 |
CA2725594A1 (en) | 2009-12-17 |
WO2009150076A2 (de) | 2009-12-17 |
BRPI0915043A2 (pt) | 2015-08-11 |
IL209582A0 (en) | 2011-01-31 |
MX2010012844A (es) | 2010-12-14 |
JP2011522851A (ja) | 2011-08-04 |
KR20110028352A (ko) | 2011-03-17 |
CR11834A (es) | 2011-02-16 |
US20110105323A1 (en) | 2011-05-05 |
WO2009150076A3 (de) | 2011-04-28 |
ZA201100243B (en) | 2012-03-28 |
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