CN1946288B - 含水杀真菌组合物及其在防治有害微生物中的用途 - Google Patents
含水杀真菌组合物及其在防治有害微生物中的用途 Download PDFInfo
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- CN1946288B CN1946288B CN2005800132245A CN200580013224A CN1946288B CN 1946288 B CN1946288 B CN 1946288B CN 2005800132245 A CN2005800132245 A CN 2005800132245A CN 200580013224 A CN200580013224 A CN 200580013224A CN 1946288 B CN1946288 B CN 1946288B
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- 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
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- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-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
- 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
- A01N43/647—Triazoles; Hydrogenated triazoles
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- A—HUMAN NECESSITIES
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- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
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- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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Abstract
本发明涉及含水杀真菌活性物质组合物及其在防治有害微生物中的用途,尤其是在保护含纤维素材料,特别是木材以防微生物,尤其是可能损害木材或纤维素的那些有害真菌侵袭中的用途。本发明活性物质组合物包含a)至少一种在25℃/1013毫巴下的水溶性不超过5g/l的杀真菌有机活性物质和b)由动态光散射测定的平均粒度不超过300nm的细碎聚合物,其中聚合物颗粒包含活性物质,该聚合物由包含如下单体的烯属不饱和单体M形成:基于单体M的总量为至少60重量%的至少一种在25℃下的水溶性不超过30g/l的中性单烯属不饱和单体M1和基于单体M的总量为至多40重量%的一种或多种单体M1以外的烯属不饱和单体M2。
Description
本发明涉及含水杀真菌活性物质组合物及其在防治有害微生物中的用途,尤其是保护含纤维素的材料,特别是木材以免被有害真菌,尤其是可能对木材或纤维素有害的那些有害真菌的侵袭中的用途。
已知木材和其他含纤维素的材料在暴露于促进微生物,尤其是真菌(下文也称为有害真菌)的生长和发育的环境条件下可能被这类微生物侵袭和在极端情况下被其破坏。此外,即使一些类型的木材对该侵袭具有天然抵抗力,但其他类型的木材,尤其是软木类型的木材,极易受侵袭(还参见EN350,第2部分)。为此,通常用木材防腐剂处理木材。
基于焦油的常规木材防腐剂如蒽油由于其固有的气味及其潜在的致癌性而并不非常吸引人。在有些场合下提议将有机杀真菌剂用作木材防腐剂(见E.H.Pommer,Ullmann’s Encyclopedia of Industrial Chemistry(CDRom),第5版,1997,Wiley VCH,Weinheim,木材防腐,第2.3.1章)。因为杀真菌活性物质通常为不溶于水中的物质,因此对于木材防腐而言通常将它们配制成在有机溶剂中的溶液。然而,使用溶剂伴有额外的成本且此外由于工业卫生原因和环境保护原因是不希望的。
在植物保护中,通常将在水中仅具有低溶解度的杀真菌活性物质配制成含水悬浮液或乳液形式。然而,乳液通常仍包含有机溶剂,而悬浮液通常配制成不含溶剂。活性物质以粒度在微米范围内的细颗粒形式存在于这些悬浮液中。若现在用该悬浮液处理木材,则活性物质保留在木材表面,因为其因粒度的原因不能渗入木材的孔中。然而,当希望有效保护木材时这是需要的。此外,活性物质易于因天气的影响而从表面洗去。
在有些场合下也提议将杀真菌的透明清漆用作木材防腐剂。就此而言,这些清漆是基于包含悬浮形式的活性物质的含水聚合物胶乳的含水油漆体系。这里的木材保护也并不令人满意,因为活性物质不渗入木材中而是保留在木材表面上。
在有些场合下提议将水不溶性杀真菌活性物质配制成含水微乳液或纳米乳液形式(例如参见WO 02/082900、WO 02/45507和WO 99/65301)。与常规的通常不透明粗乳液(其中分散相的粒度明显大于1μm)相反,在透明至不透明微乳液或纳米乳液中的活性物质以粒度明显小于1000nm至低至10nm或更小的细碎形式存在[就此而言参见D.J.Shaw,Introduction toColloid and Surface Chemistry,Butterworths,London,1986,第273页]。需要承认的是,制备该类微乳液或纳米乳液需要较大量的乳化剂和有机溶剂。由于乳化剂比例高,存在的危险是活性物质将因水的作用从木材或已处理的包含纤维素的材料中渗出。另一方面,因工业卫生原因和成本原因,溶剂是不希望的。此外,与未处理木材相比,使用乳化剂增加了木材在暴露于湿气时的吸水能力和在潮湿气氛中储存时的平衡含湿量,这使得木材更易受有害真菌侵袭。该类微乳液的另一问题是它们在分层方面不稳定。该分层例如在微乳液因乳化剂对木材的高亲和性而贫含乳化剂时或在出现溶剂减少时发生,这些情况在加压浸渍中容易发生。
因此,本发明的目的是提供一种具有低水溶性,即在25℃/1013毫巴下水溶性低于5g/l,尤其低于1g/l的杀真菌活性物质的杀真菌有效的含水组合物,该组合物有利地适于保护含纤维素材料,尤其是木材以防被有害真菌侵袭。该组合物应尤其仅包含少量挥发性有机化合物如有机溶剂或不包含挥发性有机化合物如有机溶剂。此外,活性物质不应或不以显著程度因水的作用而从已处理材料中渗出。此外,该含水活性物质组合物应比常规悬浮液或微乳液具有更好稳定性。
已经惊人地发现该目的由一种含水活性物质组合物实现,在该组合物中水不溶性或仅水微溶性的杀真菌活性物质存在于细碎的水不溶性聚合物的聚合物颗粒中,所述聚合物的聚合物颗粒具有的平均粒度不超过300nm,且其中该聚合物由基于单体M的总量为至少60重量%的至少一种水溶性在25℃下不超过30g/l的中性单烯属不饱和单体M1和基于单体M的总量为至多40重量%的一种或多种单体M1以外的烯属不饱和单体M2形成。
因此,本发明涉及一种含水活性物质组合物,其包含:
a)至少一种水溶性在25℃/1013毫巴下不超过5g/l的杀真菌有机活性物质,
和
b)通过动态光散射测定的平均粒度不超过300nm的细碎聚合物,其中聚合物颗粒包含该活性物质,
其中该聚合物由包含如下单体的烯属不饱和单体M形成:
-基于单体M的总量为至少60重量%的至少一种水溶性在25℃下不超过30g/l的中性单烯属不饱和单体M1,和
-基于单体M的总量为至多40重量%的一种或多种单体M1以外的烯属不饱和单体M2。
本发明的组合物是水不溶性或仅水微溶性的杀真菌活性物质的稳定含水制剂,它们原则上适用于所有需要实现防止被微生物,尤其是有害真菌侵袭的有效保护的应用。
尽管在聚合物基质中掺入了杀真菌活性物质,但惊人的是有效保护所需的活性物质施用率并不高于使用常规含水活性物质制剂时的施用率且在某些情况下甚至低于使用常规含水活性物质制剂时的施用率。
本发明还涉及该类含水组合物在防治微生物,尤其是防治有害真菌中的用途。术语“防治”在这里和下文中包括防止或避免被微生物,尤其是有害真菌侵袭以及在被侵袭的基底中破坏微生物,尤其是有害真菌。
本发明的组合物特别适于在木材和其他纤维素材料中防治微生物,尤其是有害真菌,且尤其适于保护这些材料以防被微生物,尤其是有害真菌侵袭。因此,本发明的具体实施方案涉及使用该类组合物来保护含纤维素材料以防被微生物侵袭,尤其是被木材破坏性真菌侵袭。
然而,本发明的含水组合物还适于其中例如在植物保护中需要防治微生物,尤其是有害真菌的其他应用,防治植物毒性微生物,用于种子处理以及用于保护材料,用作罐内和薄膜防腐剂,用于防垢以及用于保护皮革和其他有机材料以防有害微生物侵袭。
这里给出的细碎聚合物的粒度是重均粒度,其可以通过动态光散射测定。用于该测定的方法对本领域熟练技术人员而言例如由如下文献熟知:H.Wiese,D.Distler,Polymerdispersionen[聚合物水分散体],Wiley-VCH,1999,第4.2.1章,第40页及随后各页和其中引用的文献,以及H.Auweter,D.Horn,J.Colloid Interf.Sci.,105(1985),399,D.Lilge,D.Horn,Colloid Polym.Sci.,269(1991),704,或H.Wiese,D.Horn,J.Chem.Phys.,94(1991),6429。平均粒度优选为10-250nm,尤其是20-200nm,特别优选30-150nm,非常特别优选30-100nm。
根据本发明,该聚合物由基于形成该聚合物的单体M的总量为至少60重量%,优选60-99.5重量%,特别优选70-99重量%的水溶性在25℃/1013毫巴下不超过30g/l的中性单烯属不饱和单体M1形成。具体而言,单体M1在这些条件下在水中的溶解度为0.1-20g/l。合适的单体M1包括乙烯基芳族单体,如苯乙烯;具有3-8个,尤其是3或4个碳原子的单烯属不饱和一元羧酸和二元羧酸与C1-C10链烷醇或C5-C8环烷醇的酯,尤其是丙烯酸、甲基丙烯酸或巴豆酸的酯,马来酸、富马酸和衣康酸的二酯,特别优选丙烯酸与C2-C10链烷醇的酯(=丙烯酸C2-C10烷基酯),如丙烯酸乙酯、丙烯酸正丁基酯、丙烯酸异丁基酯、丙烯酸叔丁基酯、丙烯酸正己基酯、丙烯酸2-乙基己基酯和丙烯酸3-丙基庚基酯,以及甲基丙烯酸与C1-C10链烷醇的酯,如甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丁基酯、甲基丙烯酸异丁基酯、甲基丙烯酸叔丁基酯、甲基丙烯酸正己基酯等。此外,合适的单体M1是具有2-10个碳原子的脂族羧酸的乙烯基和烯丙基酯,例如乙酸乙烯酯、丙酸乙烯酯和酸的乙烯酯(支链烷烃羧酸乙烯酯);乙烯基卤化物,如氯乙烯和偏二氯乙烯;共轭二烯烃,如丁二烯和异戊二烯;以及C2-C6烯烃,如乙烯、丙烯、1-丁烯和正己烯。优选的单体M1是乙烯基芳族单体,尤其是苯乙烯,丙烯酸C2-C10烷基酯,尤其是丙烯酸C2-C8烷基酯,以及甲基丙烯酸C1-C10烷基酯。
形成聚合物的烯属不饱和单体M有利地还包含至少0.5-40重量%,尤其是1-30重量%的至少一种单体M1以外的烯属不饱和单体M2。
单体M2尤其包括具有至少一个酸基团或至少一个阴离子基团的单烯属不饱和单体M2a,尤其是具有磺酸基团、膦酸基团或一个或两个羧酸基团的单体M2a,以及单体M2a的盐,尤其是碱金属盐,如钠或钾盐以及铵盐。这些单体包括烯属不饱和磺酸,尤其是乙烯基磺酸、2-丙烯酰胺基-2-甲基丙烷磺酸,2-丙烯酰氧基乙烷磺酸、2-甲基丙烯酰氧基乙烷磺酸、3-丙烯酰氧基-和3-甲基丙烯酰氧基丙烷磺酸、乙烯基苯磺酸及其盐,烯属不饱和膦酸,如乙烯基膦酸和乙烯基膦酸二甲酯及其盐,以及α,β-烯属不饱和C3-C8一元羧酸和C4-C8二元羧酸,尤其是丙烯酸、甲基丙烯酸、巴豆酸、马来酸、富马酸和衣康酸。单体M2a的比例基于单体M的总量通常不超过35重量%,优选不超过20重量%,例如0.1-20重量%,尤其是0.5-15重量%。
单体M2额外包括水溶性在25℃下为至少50g/l,尤其是在25℃下为至少100g/l的单烯属不饱和中性单体M2b。这些单体的实例是上述烯属不饱和羧酸的酰胺,尤其是丙烯酰胺和甲基丙烯酰胺,烯属不饱和腈类,如甲基丙烯腈和丙烯腈,上述α,β-烯属不饱和C3-C8一元羧酸和C4-C8二元羧酸的羟烷基酯,尤其是丙烯酸羟乙基酯、甲基丙烯酸羟乙基酯、丙烯酸2-和3-羟基丙基酯以及甲基丙烯酸2-和3-羟基丙基酯,还有上述单烯属不饱和一元羧酸和二元羧酸与C2-C4聚亚烷基二醇的酯,尤其是这些羧酸与聚乙二醇或烷基聚乙二醇的酯,其中(烷基)聚乙二醇残基通常具有100-3000的分子量。此外,单体M2b包括N-乙烯基酰胺,如N-乙烯基甲酰胺、N-乙烯基吡咯烷酮、N-乙烯基咪唑和N-乙烯基己内酰胺。单体M2b的比例基于单体M的总量优选不超过20%,尤其不超过10重量%,例如0.1-10重量%,尤其是0.5-5重量%。
此外,单体M2包括具有至少一个阳离子基团和/或至少一个可在含水介质中质子化的基团的单烯属不饱和单体M2c。单体M2c尤其包括具有可质子化氨基、季铵基团、可质子化亚氨基或季铵化亚氨基的那些。具有可质子化亚氨基的单体实例是N-乙烯基咪唑和乙烯基吡啶。具有季铵化亚氨基的单体实例是N-烷基乙烯基吡啶鎓盐和N-烷基-N’-乙烯基咪唑啉鎓盐,如N-甲基-N’-乙烯基咪唑啉鎓氯化物或甲基硫酸盐。在单体M2c中,尤其优选通式(I)的单体:
其中
R1为氢或C1-C4烷基,尤其是氢或甲基,
R2和R3相互独立地为C1-C4烷基,尤其是甲基,和
R4为氢或C1-C4烷基,尤其是氢或甲基,
Y为氧、NH或NR5,其中R5=C1-C4烷基,
A为C2-C8亚烷基,例如1,2-亚乙基、1,2-或1,3-亚丙基、1,4-亚丁基或2-甲基-1,2-亚丙基,合适的话被1、2或3个非相邻氧原子间隔,和
X-为阴离子等价物,例如Cl-、HSO4 -、1/2SO4 2-或CH3OSO3 -等,
以及对于R4=H,式I单体的游离碱。
该类单体的实例是丙烯酸2-(N,N-二甲氨基)乙基酯、甲基丙烯酸2-(N,N-二甲氨基)乙基酯、2-(N,N-二甲氨基)乙基丙烯酰胺、3-(N,N-二甲氨基)丙基丙烯酰胺、3-(N,N-二甲氨基)丙基甲基丙烯酰胺、2-(N,N-二甲氨基)乙基甲基丙烯酰胺、氯化丙烯酸2-(N,N,N-三甲基铵)乙基酯、氯化甲基丙烯酸2-(N,N,N-三甲基铵)乙基酯、氯化2-(N,N,N-三甲基铵)乙基甲基丙烯酰胺、氯化3-(N,N,N-三甲基铵)丙基丙烯酰胺、氯化3-(N,N,N-三甲基铵)丙基甲基丙烯酰胺、氯化2-(N,N,N-三甲基铵)乙基丙烯酰胺,以及对应的硫酸盐和甲基硫酸盐。
在优选实施方案中,形成聚合物的单体M包括至少一种单体M2c。此时单体M2c的比例基于单体M的总量有利地为0.1-20重量%,尤其是0.5-10重量%,特别优选1-7重量%。
在本发明的特别优选实施方案中,该聚合物呈现净阳离子电荷,即该聚合物中单体M2c的摩尔比例大于单体M2a的摩尔比例且基于单体M2a优选为110mol%,尤其是至少120mol%,特别优选至少150mol%。
此外,单体M2还包括通常可以用于乳液聚合中的所有单体。然而,具有两个或更多个非共轭烯属不饱和双键的单体的比例基于单体总量通常不超过5重量%,尤其不超过2重量%,例如0.01-2重量%,尤其是0.05-1.5重量%。
此外,已经证明有利的是存在于本发明组合物中的聚合物具有的玻璃化转变温度Tg为至少10℃,优选至少20℃,尤其是至少30℃。具体而言,该玻璃化转变温度不超过180℃,特别优选不超过130℃。若本发明的活性物质组合物包含几种具有不同玻璃化转变温度的聚合物,无论它是以阶梯聚合物或核/壳聚合物形式还是以不同聚合物的共混物形式,玻璃化转变温度为至少10℃,优选至少20℃,尤其是至少30℃的聚合物的比例为至少40重量%。
术语“玻璃化转变温度Tg”在这里应理解为由差示扫描量热法(DSC)根据ASTM D 3418-82测定的中点温度(参见Ullmann′s Encyclopedia ofIndustrial Chemistry,第5版,第A21卷,VCH,Weinheim,1992,第169页,和Zosel,Farbe und Lack,82(1976),第125-134页,还参见DIN 53765)。
就此而言,已经证明有利的是估算共聚物P的玻璃化转变温度Tg。根据Fox(T.G.Fox,Bull.Am.Phys.Soc.(Ser.II),1,123[1956]和Ullmann’sEncyclopedia of Industrial Chemistry,Weinheim(1980),第17-18页),下列方程:
非常近似地对具有高摩尔质量的弱交联共聚物的玻璃化转变温度有效,其中符号X1、X2、...、Xn代表单体1、2、...、n的摩尔分数且Tg 1、Tg 2、...、Tg n以Kelvin代表在每种情况下仅由单体1、2、...、n之一形成的聚合物的玻璃化转变温度。后者例如由Ullmann′s Encyclopedia of IndustrialChemistry,VCH,Weinheim,第A 21卷(1992),第169页或由J.Brandrup,E.H.Immergut,Polymer Handbook,第3版,J.Wiley,New York,1989已知。
所有抑制有害真菌的生长或繁殖或破坏后者的具有低水溶性的有机物质原则上均适合作为活性物质。它们在25℃/1013毫巴下的水溶性通常不超过5g/l,常常不超过3g/l,尤其不超过1g/l,例如在25℃/1013毫巴下为0.001-1g/l,尤其是0.002-0.5g/l。
合适的活性物质实例是在the Compendium of Pesticide CommonNames:http://www.hclrss.demon.co.uk/class-fungicides.html(通用名索引)中被列为杀真菌剂的化合物。它们例如包括:
·酰基丙氨酸类,例如苯霜灵(benalaxyl)、甲霜灵(metalaxyl)、甲呋酰胺(ofurace)或噁霜灵(oxadixyl),
·吗啉化合物,例如4-十二烷基-2,6-二甲基吗啉(aldimorph)、多果定(dodine)、吗菌灵(dodemorph)、丁苯吗啉(fenpropimorph)、苯锈啶(fenpropidin)、双胍盐(guazatine)、双胍辛醋酸盐(iminoctadine)、螺噁茂胺(spiroxamine)或克啉菌(tridemorph),
·苯胺基嘧啶类,例如二甲嘧菌胺(pyrimethanil)、嘧菌胺(mepanipyrim)或环丙嘧啶(cyprodinil),
·抗菌素,例如放线菌酮(cycloheximid)、灰黄霉素(griseofulvin)、春雷素(kasugamycin)、多马霉素(natamycin)、多氧霉素(polyoxin)或链霉素(streptomycin),
·唑类,例如戊环唑(azaconazole)、双苯三唑醇(bitertanol)、糠菌唑(bromoconazole)、环唑醇(cyproconazole)、苄氯三唑醇(diclobutrazol)、噁醚唑(difenoconazole)、烯唑醇(diniconazole)、氧唑菌(epoxiconazole)、腈苯唑(fenbuconazole)、喹唑菌酮(fluquinconazole)、氟硅唑(flusilazole)、粉唑醇(flutriafol)、酮康唑(ketoconazole)、己唑醇(hexaconazole)、烯菌灵(imazalil)、环戊唑菌(metconazole)、腈菌唑(myclobutanil)、戊菌唑(penconazole)、丙环唑(propiconazole)、丙氯灵(prochloraz)、丙硫菌唑(prothioconazole)、戊唑醇(tebuconazole)、氟醚唑(tetraconazole)、三唑酮(triadimefon)、唑菌醇(triadimenol)、氟菌唑(triflumizol)或戊叉唑菌(triticonazole),
·二羧酰亚胺类,如异丙定(iprodione)、甲菌利(myclozolin)、杀菌利(procymidone)或烯菌酮(vinclozolin),
·二硫代氨基甲酸盐类,如福美铁(ferbam)、代森钠(nabam)、代森锰(maneb)、代森锰锌(mancozeb)、威百亩(metam)、代森联(metiram)、甲基代森锌(propineb)、福代锌(polycarbamate)、福美双(thiram)、福美锌(ziram)或代森锌(zineb),
·杂环化合物,如敌菌灵(anilazine)、苯菌灵(benomyl)、啶酰菌胺(boscalid)、多菌灵(carbendazim)、萎锈灵(carboxin)、氧化萎锈灵(oxycarboxin)、氰霜唑(cyazofamid)、棉隆(dazomet)、二噻农(dithianon)、噁唑酮菌(famoxadone)、咪唑菌酮(fenamidone)、异嘧菌醇(fenarimol)、麦穗宁(fuberidazole)、氟酰胺(flutolanil)、呋吡唑灵(furametpyr)、稻瘟灵(isoprothiolan)、丙氧灭绣胺(mepronil)、氟苯嘧啶醇(nuarimol)、噻菌灵(probenazole)、丙氧喹啉(proquinazid)、啶斑肟(pyrifenox)、咯喹酮(pyroquilon)、喹氧灵(quinoxyfen)、硅噻菌胺(silthiofam)、涕必灵(thiabendazole)、溴氟唑菌(thifluzamide)、甲基托布津(thiophanate-methyl)、噻酰菌胺(tiadinil)、三环唑(tricyclazole)或嗪氨灵(triforine),
·硝基苯基衍生物,如乐杀螨(binapacryl)、敌螨普(dinocap)、敌螨通(dinobuton)或异丙消(nitrophthal-isopropyl),
·苯基吡咯类,如拌种咯(fenpiclonil)或氟噁菌(fludioxonil),
·嗜球果伞素类(strobilurins),如醚菌胺(dimoxystrobin)、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)和肟菌酯(trifloxystrobin),
·其它杀真菌剂,如噻二唑素(acibenzolar-S-methyl)、苯甲酰苯甲酸酯、十二烷基胍盐酸盐、苯噻菌胺(benthiavalicarb)、氯环丙酰胺(carpropamid)、百菌清(chlorothalonil)、环氟菌胺(cyflufenamid)、清菌脲(cymoxanil)、哒菌清(diclomezine)、双氯氰菌胺(diclocymet)、乙霉威(diethofencarb)、克瘟散(edifenphos)、噻唑菌胺(ethaboxam)、环酰菌胺(fenhexamid)、薯瘟锡(fentin acetate)、氰菌胺(fenoxanil)、嘧菌腙(ferimzone)、氟啶胺(fluazinam)、藻菌磷(fosetyl)、乙膦铝(fosetyl-aluminum)、异丙菌胺(iprovalicarb)、六氯苯(hexachlorobenzene)、苯菌酮(metrafenone)、戊菌隆(pencycuron)、百维灵(propamocarb)、四氯苯酞(phthalide)、甲基立枯磷(tolclofos-methyl)、五氯硝基苯(quintozene)或苯酰菌胺(zoxamid),
·次磺酸衍生物,如敌菌丹(captafol)、克菌丹(captan)、抑菌灵(dichlofluanid)、灭菌丹(folpet)或对甲抑菌灵(tolylfluanid),
·肉桂酰胺及类似化合物,如烯酰吗啉(dimethomorph)、氟联苯菌(flumetover)或氟吗啉(flumorph)。
此外,它们还包括:
·碘化合物,如二碘甲基对甲苯基砜、3-碘-2-丙炔醇、4-氯苯基-3-碘炔丙基缩甲醛、碳酸3-溴-2,3-二碘-3-丙烯基·乙基酯、2,3,3-三碘烯丙醇、3-溴-2,3-二碘-2-丙烯醇、正丁基氨基甲酸3-碘-2-丙炔基酯、正己基氨基甲酸3-碘-2-丙炔基酯、苯基氨基甲酸3-碘-2-丙炔基酯、丁基氨基甲酸O-1-(6-碘-3-氧代己-5-炔基)酯、苯基氨基甲酸O-1-(6-碘-3-氧代己-5-炔基)酯或napcocide;
·苯酚衍生物,如三溴苯酚、四氯苯酚、3-甲基-4-氯苯酚、二氯芬、邻苯基苯酚、间苯基苯酚或2-苄基-4-氯苯酚;
·异噻唑啉酮,如N-甲基异噻唑啉-3-酮、5-氯-N-甲基异噻唑啉-3-酮、4,5-二氯-N-辛基异噻唑啉-3-酮或N-辛基异噻唑啉-3-酮;
·(苯并)异噻唑啉酮,如1,2-苯并异噻唑-3(2H)-酮、4,5-三甲基异噻唑-3-酮或2-辛基-2H-异噻唑-3-酮;
·吡啶,如1-羟基-2-吡啶硫酮(及其Na、Fe、Mn和Zn盐),或四氯-4-甲基磺酰基吡啶;
·金属皂,如锡、铜或锌的环烷酸盐、辛酸盐、2-乙基己酸盐、油酸盐、磷酸盐或苯甲酸盐;
·有机锡化合物,如三丁基锡(TBT)化合物,如三丁基锡和三丁基(单环烷酰氧基)锡衍生物;
·二烷基二硫代氨基甲酸酯以及二烷基二硫代氨基甲酸酯的Na和Zn盐,四甲基秋兰姆二硫化物;
·腈类,如2,4,5,6-四氯间苯二甲腈;
·苯并噻唑,如2-巯基苯并噻唑;
·喹啉类,如8-羟基喹啉,及其Cu盐;
·三(N-环己基二氮烯鎓二氧基)铝、(N-环己基二氮烯鎓二氧基)三丁基锡或二(N-环己基二氮烯鎓二氧基)铜;
·3-苯并[b]噻吩-2-基-5,6-二氢-1,4,2-氧杂噻嗪4-氧化物(bethoxazin)。
对于本发明组合物在保护含纤维素材料以免被与木材防腐相关的微生物,主要是霉菌、木材变色真菌和木材破坏性真菌侵袭中的用途,尤其优选例如对下列类别的微生物有效的那些杀真菌剂:
木材变色真菌:
·子囊菌纲(Ascomycetes),如线嘴壳属(Ophiostoma)(例如Ophiostomapiceae,Ophiostoma piliferum),长喙壳属(Ceratocystis)(例如天蓝色长喙壳(Ceratocystis coerulescens)),出芽短梗霉(Aureobasidium pullulans)或Sclerophoma属(例如Sclerophoma pityophila);
·半知菌纲(Deuteromycetes),如曲霉属(Aspergillus)(例如黑曲霉(Aspergillus niger)),枝孢霉属(Cladosporium)(例如Cladosporiumsphaerospermum),青霉属(Penicillium)(例如绳状青霉(Penicilliumfuniculosum)),木霉属(Trichoderma)(例如绿色木霉(Trichodermaviride)),链格孢属(Alternaria)(例如赤星病菌(Alternaria alternata))或拟青霉属(Paecilomyces)(例如宛氏拟青霉(Paecilomyces variotii));
·接合菌纲(zygomycetes),如毛霉属(Mucor)(例如冻土毛霉(Mucorhiemalis));
木材破坏性真菌:
·子囊菌纲,如毛壳属(Chaetomium)(例如球毛壳菌(Chaetomiumglobosum)),腐殖霉属(Humicola)(例如灰色腐殖霉(Humicola grisea)),Petriella属(例如Petriella setifera)或毛束霉属(Trichurus)(例如Trichurus spiralis);
·担子菌纲(Basidiomycetes),如粉孢革菌属(Coniophora)(例如粉孢革菌(Coniophora puteana)),革盖菌属(Coriolus)(例如彩绒革盖菌(Coriolusversicolor)),褐褶菌属(Gloeophyllum)(例如密粘褶菌(Gloeophyllumtrabeum)),香菇属(Lentinus)(例如豹皮香菇(Lentinus lepideus)),侧耳属(Pleurotus)(例如糙皮侧耳(Pleurotus ostreatus)),Poria属(例如棉腐卧孔菌(Poria placenta),Poria vaillantii),龙介属(Serpula)(例如干朽菌(Serpula lacrymans))和干酪菌属(Tyromyces)(例如瘤盖干酪菌(Tyromyces palustris))。
优选的活性物质因此选自康唑类(conazoles)、吗啉类、嗜球果伞素类、噻唑类、亚磺酰胺类和碘化合物类。
尤其优选在欧盟生物杀伤剂法规(COMMISSION REGULATION(EC)No.2032/2003,2003年11月4日)中在类别08(木材防腐剂)中提到的那些杀真菌剂。
本发明的含水活性物质制剂通常基于组合物中存在的聚合物或基于用于制备聚合物的单体M的总量以0.1-50重量%,优选0.2-30重量%,尤其是0.5-20重量%的量包含杀真菌活性物质。
除了杀真菌活性物质外,本发明组合物还可以包含一种或多种杀虫活性物质。在优选实施方案中,杀虫活性物质与至少一种杀真菌活性物质一起存在于聚合物颗粒中。此时杀虫活性物质优选为在25℃/1013毫巴下具有不超过5g/l,优选不超过3g/l,尤其不超过1g/l,例如0.001-1g/l或0.002-0.5g/l的低水溶性的有机活性物质。合适的杀虫活性物质是在Compendium of Pesticide Common Names:http://www.hclrss.demon.co.uk/class-insecticides.html(通用名索引)中列为杀虫剂的化合物。这些化合物例如包括:
·有机(硫代)磷酸酯类:高灭磷(acephate)、唑啶磷(azamethiphos)、谷硫磷(azinphos-methyl)、毒死蜱(chlorpyrifos)、甲基毒死蜱(chlorpyriphos-methyl)、毒虫畏(chlorfenvinphos)、二嗪农(diazinon)、敌敌畏(dichlorvos)、百治磷(dicrotophos)、乐果(dimethoate)、乙拌磷(disulfoton)、乙硫磷(ethion)、杀螟松(fenitrothion)、倍硫磷(fenthion)、异噁唑磷(isoxathion)、马拉硫磷(malathion)、甲胺磷(methamidophos)、杀扑磷(methidathion)、甲基一六零五(methyl-parathion)、速灭磷(mevinphos)、久效磷(monocrotophos)、砜吸磷(oxydemeton-methyl)、对氧磷(paraoxon)、一六零五(parathion)、稻丰散(phenthoate)、伏杀磷(phosalone)、亚胺硫磷(phosmet)、磷胺(phosphamidon)、甲拌磷(phorate)、辛硫磷(phoxim)、虫螨磷(pirimiphos-methyl)、丙溴磷(profenofos)、丙硫磷(prothiofos)、乙丙硫磷(sulprophos)、三唑磷(triazophos)或敌百虫(trichlorfon);
·氨基甲酸酯类:棉铃威(alanycarb)、丙硫克百威(benfuracarb)、噁虫威(bendiocarb)、甲奈威(carbaryl)、丁硫克百威(carbosulfan)、双氧威(fenoxycarb)、呋线威(furathiocarb)、噁二唑虫(indoxacarb)、灭虫威(methiocarb)、灭多虫(methomyl)、甲氨叉威(oxamyl)、抗蚜威(pirimicarb)、残杀威(propoxur)、硫双威(thiodicarb)或唑蚜威(triazamate);
·合成除虫菊酯类:丙烯菊酯(allethrin)、氟氯菊酯(bifenthrin)、氟氯氰菊酯(cyfluthrin)、苯醚氰菊酯(cyphenothrin)、氯氰菊酯(cypermethrin)以及α-、β-、θ-和ξ-异构体、溴氰菊酯(deltamethrin)、高氰戊菊酯(esfenvalerate)、醚菊酯(ethofenprox)、甲氰菊酯(fenpropathrin)、杀灭菊酯(fenvalerate)、(RS)氯氟氰菊酯(cyhalothrin)、氯氟氰菊酯(lambda-cyhalothrin)、咪炔菊酯(imiprothrin)、氯菊酯(permethrin)、炔酮菊酯(prallethrin)、除虫菊酯I(pyrethrin I)、除虫菊酯II(pyrethrin II)、灭虫硅醚(silafluofen)、氟胺氰菊酯(tau-fluvalinate)、七氟菊酯(tefluthrin)、胺菊酯(tetramethrin)、四溴菊酯(tralomethrin)、四氟菊酯(transfluthrin)或己体氯氰菊酯(zeta-cypermethrin);
·节肢动物生长调节剂:a)几丁质合成抑制剂;例如苯甲酰脲类,如定虫隆(chlorfluazuron)、cyromacin、氟脲杀(diflubenzuron)、氟螨脲(flucycloxuron)、氟虫脲(flufenoxuron)、氟铃脲(hexaflumuron)、氟丙氧脲(lufenuron)、双苯氟脲(novaluron)、伏虫隆(teflubenzuron)、杀虫隆(triflumuron);噻嗪酮(buprofezin)、噁茂醚(diofenolan)、噻螨酮(hexythiazox)、特苯噁唑(etoxazole)或四螨嗪(clofentazine);b)蜕皮激素拮抗剂,如特丁苯酰肼(halofenozide)、甲氧苯酰肼(methoxyfenozide)或双苯酰肼(tebufenozide);c)保幼激素类似物:蚊蝇醚(pyriproxyfen)、蒙五一五(methoprene)或双氧威(fenoxycarb);d)类脂生物合成抑制剂:螺螨酯(spirodiclofen);
·新类烟碱(neonicotinoids),如氟啶虫酰胺(flonicamid)、噻虫胺(clothianidin)、呋虫胺(dinotefuran)、吡虫啉(imidacloprid)、噻虫嗪(thiamethoxam)、硝胺烯啶(nitenpyram)、硝虫噻嗪(nithiazine)、吡虫清(acetamiprid)或噻虫啉(thiacloprid);
·吡唑类杀虫剂,如acetoprole、乙虫清(ethiprole)、锐劲特(fipronil)、吡螨胺(tebufenpyrad)、唑虫酰胺(tolfenpyrad)和氟吡唑虫(vaniliprole);
·此外还有齐墩螨素(abamectin)、灭螨醌(acequinocyl)、虫螨脒(amitraz)、艾扎丁(azadirachtin)、联苯肼酯(bifenazate)、杀螟丹(cartap)、氟唑虫清(chlorfenapyr)、杀虫脒(chlordimeform)、灭蝇胺(cyromazine)、杀螨硫隆(diafenthiuron)、噁茂醚(diofenolan)、甲氨基阿维菌素(emamectin)、硫丹(endosulfan)、喹螨醚(fenazaquin)、伐虫脒(formetanate)、伐虫脒盐酸盐(formetanate hydrochloride)、灭蚁腙(hydramethylnon)、噁二唑虫(indoxacarb)、增效醚(piperonyl butoxide)、哒螨酮(pyridaben)、拒嗪酮(pymetrozine)、艾克敌105(spinosad)、噻虫嗪(thiamethoxam)、硫环杀(thiocyclam)、啶虫丙醚(pyridalyl)、fluacyprim、米尔螨素(milbemectin)、季酮甲螨酯(spiromesifen)、flupyrazofos、安百亩(NCS 12)、flubendiamide、双三氟虫脲(bistrifluron)、benclothiaz、pyrafluprole、pyriprole、amidoflumet、flufenerim、cyflumetofen、lepimectin、丙氟菊酯(profluthrin)、四氟甲醚菊酯(dimefluthrin)和metaflumizone。
其中优选对木材破坏性昆虫有效且尤其对下列木材破坏性昆虫有效的那些杀虫剂:
鞘翅目(Coleoptera(甲虫)):
·天牛科(Cerambycidae),如家天牛(Hylotrupes bajulus)或蓝扁天牛(Callidium violaceum);
·粉蠹科(Lyctidae),如抱扁蠹(Lyctus linearis)或褐粉蠹(Lyctus brunneus);
·长蠹科(Bostrichidae),如竹长蠹(Dinoderus minutus);
·窃蠹科(Anobiidae),如Anobium punctatum或Xestobium rufovillosum;
·筒蠹科(Lymexylidae),如Lymexylon navale;
·长小蠹科(Platypodidae),如柱体长小蠹(Platypus cylindrus);
·拟天牛科(Oedemeridae),如黑尾拟天牛(Nacerda melanura);
膜翅目(Hymenoptera)(膜翅类昆虫(hymenopterans)):
·蚁科(Formicidae),如Camponotus abdominalis、黄毛蚁(Lasius flavus)、
Lasius brunneus或亮毛蚁(Lasius fuliginosus);
等翅目(Isoptera)(白蚁):
·木白蚁科(Kalotermitidae),如欧洲木白蚁(Kalotermes flavicollis)或Cryptothermes brevis;
·草白蚁科(Hodotermitidae),如美古白蚁(Zootermopsis angusticollis)或内华达古白蚁(Zootermopsis nevadensis);
·鼻白蚁科(Rhinotermitidae),如北美散白蚁(Reticulitermes flavipes)、欧洲散白蚁(Reticulitermes lucifugus)、家白蚁(Coptotermes formosanus)或短刀乳白蚁(Coptotermes acinaciformis);
·澳白蚁科(Mastotermitidae),如达尔文澳白蚁(Mastotermesdarwiniensis)。
这些尤其包括选自如下类别的杀虫活性物质:合成除虫菊酯类,节肢动物生长调节剂如几丁质生物合成抑制剂,蜕皮激素拮抗剂,保幼激素类似物或类脂生物合成抑制剂,新类烟碱,吡唑杀虫剂和氟唑虫清。
尤其优选在欧盟生物杀伤剂法规(COMMISSION REGULATION(EC)No.2032/2003,2003年11月4日)中在类别08(木材防腐剂)和类别18(防治其他节肢动物的杀虫剂、杀螨剂和产品)中提到的那些杀虫活性物质。
需要的话,杀虫活性物质通常基于形成聚合物的单体M以0.1-50重量%,优选0.2-30重量%,尤其是0.5-20重量%的量存在于本发明的活性物质组合物中。
活性物质在本发明组合物的聚合物中的总量基于该聚合物或形成该聚合物的单体M优选为0.2-50重量%,尤其是0.5-30重量%,特别优选1-20重量%。
本发明的含水组合物通常包含表面活性物质以稳定含水介质中的聚合物颗粒。这些物质包括保护性胶体和低分子量乳化剂,后者与保护性胶体相反的是通常具有低于2000g/mol,尤其低于1000g/mol的分子量(重均)。保护性胶体和乳化剂均可以是阳离子性、阴离子性或中性的和两性离子的。
阴离子表面活性物质的实例是阴离子乳化剂,如烷基苯基磺酸盐、苯基磺酸盐、烷基硫酸盐、烷基磺酸盐、烷基醚硫酸盐、烷基酚醚硫酸盐、烷基聚乙二醇醚磷酸盐、烷基二苯基醚磺酸盐、聚芳基苯基醚磷酸盐、烷基磺基琥珀酸盐、烯烃磺酸盐、链烷烃磺酸盐、石油磺酸盐、氨基乙磺酸盐、肌氨酸金属盐、脂肪酸、烷基萘磺酸或萘磺酸,包括其碱金属、碱土金属、铵和胺盐。阴离子保护性胶体的实例是木素磺酸,磺化萘与甲醛或与甲醛和苯酚以及需要的话脲的缩合产物,还有苯酚磺酸、甲醛和脲的缩合产物,木素亚硫酸盐废液和木素磺酸盐,以及聚羧酸盐,如聚丙烯酸盐,马来酸酐/烯烃共聚物(例如CP9,BASF),还有上述保护性胶体的碱金属、碱土金属、铵和胺盐。
非离子乳化剂例如为烷基酚烷氧基化物、醇烷氧基化物、脂肪胺烷氧基化物、聚氧乙烯甘油脂肪酸酯、蓖麻油烷氧基化物、脂肪酸烷氧基化物、脂肪酸酰胺烷氧基化物、脂肪酸聚二乙醇酰胺、羊毛脂乙氧基化物、脂肪酸聚乙二醇酯、异十三烷醇、脂肪酸酰胺、甲基纤维素、脂肪酸酯、硅油、烷基聚苷和甘油脂肪酸酯。非离子保护性胶体的实例为聚乙二醇、聚丙二醇、聚乙二醇/聚丙二醇嵌段共聚物、聚乙二醇烷基醚、聚丙二醇烷基醚、聚乙二醇/聚丙二醇醚嵌段共聚物及其混合物。
阳离子乳化剂的实例是季铵盐,例如三甲基-和三乙基(C6-C30烷基)铵盐,如椰油烷基三甲基铵盐和三甲基鲸蜡基铵盐,二甲基-和二乙基二(C4-C20烷基)铵盐,如二癸基二甲基铵盐和二椰油烷基二甲基铵盐,甲基-和乙基三(C4-C20烷基)铵盐,如甲基三辛基铵盐,(C1-C20烷基)二(C1-C4烷基)苄基铵盐,如三乙基苄基铵盐和椰油烷基苄基二甲基铵盐,甲基-和乙基二(C4-C20烷基)聚(氧乙基)铵盐,例如二癸基甲基聚(氧乙基)铵盐,N-(C6-C20烷基)吡啶鎓盐,例如N-月桂基吡啶鎓盐,N-甲基-和N-乙基-N-(C6-C20烷基)吗啉鎓盐,以及N-甲基-和N-乙基-N’-(C6-C20烷基)咪唑啉鎓盐,尤其是卤化物、硼酸盐、碳酸盐、甲酸盐、乙酸盐、丙酸盐、碳酸氢盐、硫酸盐和甲基硫酸盐。
阳离子保护性胶体的实例是上述单体M2c的均聚物和共聚物,其中单体M2c的含量为至少20重量%,尤其是至少30重量%,例如N-乙烯基-N-甲基咪唑啉鎓盐或N-烷基乙烯基吡啶鎓盐的均聚物以及这些单体与优选水混溶性中性单体M2b的共聚物。
两性离子乳化剂是具有甜菜碱结构的那些。该类物质对本领域熟练技术人员是已知的且可以从相关现有技术中找到(例如参见R.Heusch,Ullmann’s Encyclopedia of Industrial Chemistry,第5版,CD-ROM,Wiley-VCH,1997,“乳液”,第7章,表4)。
本发明组合物通常包含至少一种乳化剂,优选至少一种离子乳化剂以及合适的话一种或多种非离子乳化剂。对于在木材防腐中的应用,已经证明有用的是本发明组合物包含至少一种阳离子乳化剂,尤其在不使用单体M2c来制备聚合物时。
乳化剂的量基于单体M或聚合物P通常为0.1-15重量%,尤其是0.2-12重量%,特别优选0.7-10重量%。离子乳化剂的量基于构成聚合物的单体M优选为0.3-10重量%,尤其是0.5-8重量%。非离子乳化剂的量基于构成聚合物的单体M优选为0.2-12重量%,尤其是0.5-10重量%。
本发明含水组合物的制备包括单体M的水包油乳液的自由基水乳液聚合,其中乳液的单体液滴包含至少一种杀真菌活性物质和合适的话杀虫活性物质。聚合类似于常规乳液聚合方法进行,其中不同在于待聚合的单体乳液包含溶于单体液滴中的活性物质。
活性物质/单体溶液的水包油乳液可以通过将活性物质在待聚合单体M中的溶液加入在聚合条件下的聚合容器中而就地制备。然而,优选将活性物质溶于单体M中并将如此得到的单体溶液转化成单体水乳液,然后将如此得到的单体/活性物质乳液供入聚合反应中。
聚合通常根据“单体进料方法”进行,即在聚合反应过程中将较大部分,优选至少70%,尤其至少90%的活性物质在单体M中的溶液或较大部分,优选至少70%,尤其至少90%的单体/活性物质乳液供入聚合容器中。单体/活性物质溶液或乳液的加入优选在至少0.5小时,优选至少1小时,例如1-10小时,尤其2-5小时内进行。单体/活性物质溶液或乳液的加入可以恒定或可变加料速率进行,例如以具有恒定加料速率或可变加料速率的间隔进行或以可变加料速率连续进行。单体/活性物质溶液或乳液的组成可以在加料过程中保持恒定或可以变化,其中可以改变单体组成以及活性物质类型或活性物质浓度。
在本发明的优选实施方案中,在单体加料过程中改变单体组成以在聚合物颗粒中得到具有不同玻璃化转变温度的聚合物范围。这通过“逐步聚合”实现。为此,首先在第一步中聚合单体组成对应于玻璃化转变温度Tg 1的第一单体/活性物质溶液或乳液,然后对其提供单体组成对应于玻璃化转变温度Tg 2的第二单体/活性物质溶液或乳液(第二步)并且适当的话在其后对其依次提供一种或多种单体组成在每种情况下对应于玻璃化转变温度Tg n的额外单体/活性物质溶液或乳液,其中n为各步骤。在依次聚合步骤中得到的聚合物的各玻璃化转变温度优选相差至少10K,尤其至少20K,特别优选至少30K,例如30-200K,尤其是40-160K。通常而言,聚合的单体量在两步聚合中为至少5重量%,优选至少10重量%,例如5-95重量%,尤其是10-90重量%,而在三步或更多步聚合中为5-90或5-85重量%,尤其是10-80重量%。
已经证明对于制备本发明活性物质组合物且对于活性物质组合物的性能有利的是在种子聚合物(种子胶乳)存在下进行乳液聚合。此时它为细碎的聚合物胶乳,平均粒度通常不超过100nm,尤其不超过80nm,特别优选不超过50nm。构成该种子胶乳的单体优选至少90重量%,尤其至少95重量%,常常大于99重量%选自单体M1,其中种子胶乳还可以包含用于稳定的少量,例如0.1-10重量%,尤其0.1-5重量%,特别是0.1-1重量%的不同单体M2,例如单体M2a。该种子胶乳通常具有的玻璃化转变温度为至少10℃,尤其至少50℃,常常为至少80℃。种子胶乳的量基于待聚合单体MI通常为0.01-5重量%,尤其0.1-4重量%。优选在聚合开始时将大部分,尤其是所有种子胶乳完全放入反应容器中。种子胶乳还可以在聚合容器中通过使形成该种子胶乳的单体自由基乳液聚合而就地产生,其中形成该种子胶乳的单体选自上述单体MI和M2,尤其是至少90重量%选自单体M1。该种子胶乳的所需粒度可以经由单体/乳化剂比例而以本身已知的方式控制。
适于本发明乳液聚合的引发剂是适于且常用于乳液聚合的引发单体M的自由基聚合的聚合引发剂。它们包括偶氮化合物,如2,2′-偶氮二异丁腈、2,2′-偶氮二(2-甲基丁腈)、2,2’-偶氮二[2-甲基-N-(2-羟乙基)丙酰胺]、1,1’-偶氮二(1-环己基甲腈)、2,2’-偶氮二(2,4-二甲基戊腈)、2,2’-偶氮二(N,N’-二亚甲基异丁脒)二盐酸盐和2,2’-偶氮二(2-脒基丙烷)二盐酸盐,有机或无机过氧化物,如过氧化二乙酰、过氧化二(叔丁基)、过氧化二戊基、过氧化二辛酰、过氧化二癸酰、过氧化二月桂酰、过氧化二苯甲酰、过氧化二(邻甲苯甲酰)、过氧化琥珀酰、过乙酸叔丁酯、过马来酸叔丁酯、过异丁酸叔丁酯、过新戊酸叔丁酯、过辛酸叔丁酯、过新癸酸叔丁酯、过苯甲酸叔丁酯、过氧化叔丁基、氢过氧化叔丁基、氢过氧化枯烯、过氧化(2-乙基己酸)叔丁酯和过氧二氨基甲酸二异丙基酯、过二硫酸的盐和氧化还原引发剂体系。
优选使用水溶性引发剂,例如阳离子偶氮化合物,如偶氮二(二甲基脒基丙烷),过二硫酸的盐,尤其是钠、钾或铵盐,或氧化还原引发剂体系,其中作为氧化剂的是过二硫酸的盐、过氧化氢或有机过氧化物,如氢过氧化叔丁基。作为还原剂它们优选包含尤其选自如下的硫化合物:亚硫酸氢钠、羟基甲烷亚磺酸钠和丙酮的亚硫酸氢盐加合物。额外的合适还原剂是含磷化合物,如亚磷酸、次磷酸盐和次膦酸盐,以及肼或水合肼和抗坏血酸。此外,氧化还原引发剂体系可以包括少量氧化还原金属盐如铁盐、钒盐、铜盐、铬盐或锰盐的加入,例如氧化还原引发剂体系抗坏血酸/硫酸铁(II)/过二硫酸钠。
引发剂通常基于单体M的量以0.02-2重量%,尤其是0.05-1.5重量%的量使用。引发剂的最佳量自然取决于所用引发剂体系且可以由本领域熟练技术人员通过常规试验确定。引发剂可以部分或全部引入反应容器中。优选在聚合过程中将大部分引发剂,尤其是至少80%,例如80-99.5%的引发剂提供给聚合反应器。
压力和温度对于制备本发明活性物质组合物是次要的。温度通常取决于所用引发剂体系且最佳聚合温度可以通过常规试验由本领域熟练技术人员确定。聚合温度通常为20-110℃,常常为50-95℃。聚合通常在标准压力或环境压力下进行。然而,还可以在加压,例如高达3巴,或在稍微减压,例如>800毫巴下进行。
已经在上面作为本发明活性物质配制剂的成分提到的常用于乳液聚合的乳化剂和保护性胶体适合作为表面活性物质。常用于乳液聚合的表面活性物质的量通常位于上述范围内,从而经由乳液聚合提供本发明组合物中的所有或部分表面活性物质。然而,还可以在乳液聚合中仅使用一部分,例如10-90重量%,尤其是20-80重量%在本发明组合物中存在的表面活性物质并在乳液聚合之后、在乳液聚合的任选除臭(随后皂化)之前或之后加入剩余量的表面活性物质。
聚合物的分子量显然可以通过加入少量,例如基于聚合的单体M为0.01-2重量%的调节剂而调节。具体而言,有机硫代化合物以及烯丙基醇和醛适合作为调节剂。
在实际聚合反应之后,可能需要从本发明的聚合物水分散体中基本除去恶臭物质如残留单体和其他挥发性有机成分。以本身已知的方式,这可以通过蒸馏除去(尤其经由蒸汽蒸馏)或通过用惰性气体汽提而以物理方式进行。此外,残留单体可以通过自由基后聚合而以化学方式减少,该后聚合尤其在例如如DE-A 44 35 423、DE-A 44 19 518和DE-A 44 35 422所述的氧化还原引发剂体系下进行。后聚合优选使用由至少一种有机过氧化物和一种有机亚硫酸酯组成的氧化还原引发剂进行。
在聚合结束之后,通常将所用聚合物分散体在根据本发明使用之前调节到碱性值,优选调节到pH值为7-10。可以将氨或有机胺以及优选氢氧化物如氢氧化钠、氢氧化钾或氢氧化钙用于中和。
这样得到稳定的聚合物水分散体,其包含在该分散体的聚合物颗粒中的至少一种杀真菌活性物质以及合适的话一种或多种杀虫活性物质。此外,如此得到的分散体包含上述表面活性物质。如此得到的活性物质制剂的特征在于高稳定性和低挥发性有机化合物含量,所述含量基于该组合物的总重量通常不超过1重量%,常常不超过0.1重量%,尤其不超过500ppm。挥发性化合物在这里及以后是指所有在标准压力下沸点低于200℃的有机化合物。
本发明组合物的固体含量最近似地由活性物质和聚合物决定且通常为10-60重量%,尤其是20-50重量%。
可如此得到的活性物质组合物可以直接使用或在稀释之后使用。此外,本发明组合物还可含有常规添加剂,如粘度改性添加剂(增稠剂)、消泡剂、杀菌剂和防冻剂。
合适的增稠剂是赋予配制剂以假塑性流动性能,即在静止时具有高粘度且在搅拌状态下具有低粘度的化合物。就此而言可以提到例如多糖或有机层状矿物,如Xanthan (Kelco的 23或(R.T.Vanderbilt),或(Engelhardt),优选使用
合适的防冻剂为有机多元醇,例如乙二醇、丙二醇或甘油。这些试剂通常基于活性物质组合物的总重量以不超过10重量%的量使用。
合适的话,本发明的活性物质组合物可以基于制备的配制剂总量包含1-5重量%缓冲剂,以调节pH,其中所用缓冲剂的量和类型取决于活性物质的化学性能。缓冲剂的实例是弱无机或有机酸如磷酸、硼酸、乙酸、丙酸、柠檬酸、富马酸、酒石酸、草酸和琥珀酸的碱金属盐。
此外,本发明的含水组合物可以用常规粘合剂如聚合物水分散体或水溶性树脂如水溶性醇酸树脂或用蜡配制。
为了用于保护含纤维素材料,尤其是用于木材防腐,本发明的含水活性物质组合物还可以用常规水溶性木材防腐剂,尤其是其水溶液配制,以改进对木材破坏性生物体的总体有效性。就此而言,这些试剂例如为常规木材保护性盐的含水制剂,所述盐例如为基于硼酸的盐和硼酸碱金属盐,基于季铵化合物的盐如三甲基-和三乙基(C6-C30烷基)铵盐,如椰油烷基三甲基氯化铵或三甲基鲸蜡基铵盐,二甲基-和二乙基二(C4-C20烷基)铵盐,如二癸基二甲基氯化铵、二癸基二甲基溴化铵或二椰油烷基二甲基氯化铵,(C1-C20烷基)二(C1-C4烷基)苄基铵盐,如椰油烷基苄基二甲基氯化铵,或甲基-和乙基二(C4-C20烷基)聚(氧乙基)铵盐,例如二癸基甲基聚(氧乙基)氯化铵和二癸基甲基聚(氧乙基)丙酸铵,还有硼酸盐、碳酸盐、甲酸盐、乙酸盐、碳酸氢盐、硫酸盐和甲基硫酸盐,或为铜-胺配合物的含水制剂,尤其是包含铜乙醇胺的盐,如Cu-HDO的含水制剂。显而易见的是,本发明的含水活性物质制剂还可以与其他含水杀真菌和杀虫活性物质组合物配制,例如与上述活性物质如上述唑类和嗜球果伞素类杀真菌剂或上述杀虫剂的常规乳油、悬浮浓缩液或悬浮乳液浓缩液配制,或与开头所提到的上述杀真菌剂和杀虫剂的微乳液配制。通过将本发明的含水活性物质组合物与上述活性物质的常规含水制剂混合,首先实现了活性谱的拓宽,若常规制剂包含与本发明含水活性物质组合物不同的活性物质的话。其次,本发明活性物质组合物的优点并没有因与常规含水活性物质制剂配制而失去,尤其是对含纤维素材料,特别是木材的改进粘附性。因此,常规含水活性物质制剂的应用性能可以通过与相同活性物质的本发明含水活性物质组合物配制而改进。
本发明的活性物质组合物具有许多优点。首先,这些组合物是水不溶性或仅水微溶性杀真菌活性物质的稳定含水配制剂。具体而言,没有观察到在活性物质的常规配制剂和微分散体或纳米分散体中观察到的相分离问题且没有观察到活性物质的沉降,甚至当使用苛刻条件时,例如在用杀真菌活性物质浸渍木材时所用的方法中出现的苛刻条件时。在常规添加下挥发性有机化合物的含量低于相当的常规配制剂,且与活性物质的微分散体或纳米分散体相比,乳化剂的比例基于所用活性物质而言更低。与其他配制剂相比,在水的作用下活性物质以显著更低的程度从被处理材料中渗出。此外,没有观察到例如在常规配制剂中经常发生的活性物质与其他配制成分或额外活性物质的相互作用。再有,活性物质因基材或环境如介质的pH值或UV辐射而发生的分解减缓或甚至完全消除。惊人的是,没有观察到通过掺入聚合物基质中而降低活性物质的效力。
本发明还涉及一种保护含纤维素材料,尤其是木材以防有害真菌侵袭,尤其是上述木材破坏性真菌侵袭的方法,其中用本发明的组合物处理含纤维素材料,尤其是木材。
除了木材和下游产品外,含纤维素材料例如为木坯,胶合板,粗纸板,MDF板或OSB板,还有造纸中的纸浆和中间体,基于纤维素如棉花的织物,基于一年生木材的材料,例如由油菜渣形成的模制品,bargasse板,稻草板等。此外,含纤维素材料包括由含纤维素的纤维材料形成的制品,如织物、成型织物、纸张、板、绝热材料、绳、缆等。对本发明方法合适的纤维材料包括纺织纤维,如胡麻、亚麻、大麻、黄麻、棉花和苎麻,纸纤维,如胡麻、亚麻或大麻,竹纤维,纸桑和木素纤维素纤维,以及刺麻纤维,马尼拉麻,剑麻、洋麻和椰子纤维。
处理可以取决于基材类型通过用未稀释的本发明活性物质组合物或用水稀释的本发明活性物质组合物喷雾、上漆、浸涂或浸渍基材或通过将基材淹没在未稀释的本发明含水活性物质组合物或用水稀释的本发明含水活性物质组合物中而以本身已知的方式进行。本发明组合物还可以例如作为粘合剂或作为施胶剂存在于含纤维素材料的制造中。
若本发明基材为木材,则可以使用木材防腐中的常用方法,例如由Ullmann’s Encyclopedia of Industrial Chemistry,木材防腐,第5版,CD-ROM,Wiley VCH,Weinheim,1997,第7章已知的方法。这些方法尤其包括借助压差浸渍木材的方法,例如真空-加压方法和二次真空浸渍。
用本发明的活性物质组合物处理该类材料可以根据常用于此的方法进行且以本身已知的方式在每种情况下与技术现实相适应。此时的施用浓度和掺入取决于该材料的危险程度和相应的处理方法且通常为0.05mg-10g活性物质/kg材料。
包含活性物质的未稀释组合物通常例如与所用粘合剂一起作为辅助粘合剂用于木材下游产品和含纤维素材料。显而易见的是,在制造过程中或制造之后的单独处理如施胶也是可能的。
除了所述基于纤维素的材料外,本发明的含水活性物质组合物还可以用于材料保护的其他领域以防有害真菌侵袭以及合适的话防止动物害虫侵袭。例如,可以用本发明的含水组合物有效保护皮肤、毛皮或皮革以防微生物和动物害虫侵袭,尤其是防止上述有害真菌侵袭。此外,本发明的含水组合物还可以用作防垢漆,例如用于造船中,或用作建筑物立面和屋顶瓦的藻类杀伤漆体系,在每种情况下取决于其中所存在的活性物质。此外,本发明组合物可以用作罐内和薄膜防腐剂。
下列实施例用于阐明本发明,但不限制本发明:
所给粘度按照ISO 2555在23℃下在布氏(Brookfield)旋转粘度计中测量。
所给粒度根据上述方法在稀分散体(0.01-0.1重量%)中通过准弹性光散射测定。给出通过所测量的自校准函数的累计分析测定的平均直径。
玻璃化转变温度按照ASTM D 3418使用差示扫描量热法测定。
I.制备活性物质组合物
实施例1a(具有3重量%活性物质的聚合物水分散体,分散体D1)
将300g去离子水和13.6g 33重量%聚苯乙烯水分散体(平均粒度为30nm)引入装有搅拌器的反应容器中,用氮气吹扫该容器,然后加热到75℃。在搅拌并维持温度下同时开始在3小时内加入进料1并在3.15小时内加入进料2。在进料2加料结束之后,将温度再维持30分钟,然后加入3.0g 25重量%氨水溶液。然后为了进行化学除臭,在90分钟内在维持温度下加入进料3和进料4,然后将反应混合物冷却到室温。然后一次加入进料5并将反应混合物搅拌10分钟,然后用氨将pH值调节到7-7.5,再滤过网眼尺寸为125μm的网筛。
所得分散体具有38.7重量%的固含量和30mPa·s的粘度。该聚合物的玻璃化转变温度为+16℃。借助光散射测定的平均粒度为146nm。
进料1:
400.0g 去离子水
25.7g 阴离子乳化剂E11)的28重量%溶液
21.0g 非离子乳化剂E22)的28重量%溶液
7.8g 丙烯酸
292.0g 苯乙烯
237.0g 丙烯酸正丁酯
60.0g 丙烯酸乙酯
3.0g 丙烯酰胺
18.0g 氧唑菌
进料2:
100g 去离子水
2.4g 过二硫酸钠
进料3:
22.0g 去离子水
2.6g 氢过氧化叔丁基(70重量%)
进料4:
25.0g 去离子水
1.7g 羟基甲烷亚磺酸钠
进料5:
37.0g 去离子水
30.0g 乳化剂溶液E2
1)月桂基硫酸钠
2)每分子平均具有18个氧化乙烯单元的C16/C18脂肪醇乙氧基化物实施例1b(具有2重量%杀真菌活性物质和1重量%杀虫活性物质的聚合物水分散体,分散体D2)
类似于实施例1a的程序进行制备,进料1具有下列组成:
进料1:
400.0g 去离子水
25.7g 阴离子乳化剂E11)的28重量%溶液
21.0g 非离子乳化剂E22)的28重量%溶液
7.8g 丙烯酸
322.0g 苯乙烯
177.0g 丙烯酸正丁酯
60.0g 丙烯酸乙酯
30.0g 丙烯腈
3.0g 丙烯酰胺
12.0g 氧唑菌
6.0g 氟唑虫清
所得分散体具有39重量%的固含量和45mPa·s的粘度。该聚合物的玻璃化转变温度为31℃。借助光散射测定的平均粒度为151nm。
实施例2(具有不同活性物质的阶梯聚合物,分散体D3-D8)
通用程序:
将183g水和75.8g聚苯乙烯水分散体(33重量%,平均粒径为30nm)引入反应容器中,将该容器用氮气吹扫并加热到85℃。在维持该温度下将1.5g过二硫酸钠在21.4g水中的25重量%溶液(进料4)加入其中。在10分钟后同时开始加入进料1和剩余量的进料4。在维持该温度下将进料1在90分钟内加入,进料4在255分钟内加入。在进料1加料结束之后,将该温度维持30分钟,然后在60分钟内加入进料2,将该温度再维持45分钟,然后在维持该温度下在30分钟内加入进料3。在进料3加料结束之后,将该温度再维持30分钟,然后将反应混合物冷却至室温。
进料1:
220.1g 水
220.8g 苯乙烯
1.6g 甲基丙烯酸烯丙酯
11.1g 乳化剂溶液E3
xg 活性物质(见表1)
进料2:
135.6g 水
180.4g 丙烯酸正丁酯
2.1g 甲基丙烯酸烯丙酯
7.2g 乳化剂溶液E3
yg 活性物质(见表1)
进料3:
92.5g 水
19.7g 苯乙烯
75.5g 甲基丙烯酸甲酯
1.7g 乳化剂溶液E3
z g 活性物质(见表1)
乳化剂溶液E3:(C16烷基)二苯基醚磺酸的钠盐的45重量%水溶液
表1
分散体 | 活性物质 | x[g] | y[g] | z[g] |
D3 | 环戊唑菌 | 26.4 | 14.4 | 12.0 |
D4 | 环唑醇 | 21.6 | 10.8 | 10.8 |
D5 | 氧唑菌 | 30.0 | 6.0 | 6.0 |
D6 | 戊唑醇 | 15.0 | 18.0 | - |
D7 | IPBC1) | 21.0 | 4.2 | 6.0 |
D8 | 氧唑菌+氟唑虫清 | 4.02.0 | 4.02.0 | 4.02.0 |
1)IPBC=丁基氨基甲酸3-碘-2-丙基酯。
所得分散体的固体含量为45重量%且粘度为115mPa·s。聚合物具有借助DSC测定在-31℃和+99℃的2个玻璃化转变温度。借助光散射测定的平均粒度为95-105nm。
实施例3(具有不同活性物质的阳离子分散体D9-D13)
通用制备程序:
将465g去离子水、5重量%进料1和10重量%进料2加热到80℃。在10分钟之后加入剩余量的进料1和进料2。加料时间为3.5小时。在进料加料结束之后,将混合物在80℃下再维持30分钟并冷却到室温。
进料1:
496.1g 去离子水
7.6g 硫酸(50重量%)
361.0g 甲基丙烯酸甲酯
19.0g 甲基丙烯酸二甲氨基乙酯
57.0g 乳化剂溶液E4
xg 活性物质(见表2)
进料2:
1.5g 2,2′-偶氮二(N,N’-二甲基异丁脒)在63.3g去离子水中的溶液
乳化剂溶液E4:通过用4-5mol氧化乙烯依次乙氧基化硬脂胺并随后用硫酸二甲酯季铵化而得到的阳离子乳化剂的40重量%水溶液。
表2
分散体 | 活性物质 | x[g] |
D9 | 环戊唑菌 | 61.8 |
D10 | 环唑醇 | 42.9 |
D11 | 氧唑菌 | 0.4 |
D12 | 戊唑醇 | 19.0 |
D13 | IPBC | 18.2 |
所得分散体的固体含量为29.5重量%且粘度为100mPa·s。该聚合物具有借助DSC测定为87℃的玻璃化转变温度。借助光散射测定的平均粒度为157-175nm。
实施例4(具有不同活性物质的阳离子分散体D14-D18)
通用制备程序:
将465g去离子水、进料1和10重量%进料2加热到80℃。在10分钟之后开始加入剩余量的进料2和进料3。进料2和进料3的加料时间为3.5小时。在进料的加料结束之后,将混合物在80℃下再维持30分钟,然后冷却到室温。
进料1:
46.1g 去离子水
38.0g 苯乙烯
7.6g 3-(N,N-二甲氨基)丙基甲基丙烯酰胺
14.2g 乳化剂溶液E4(见上文)
进料2:
1.5g 2,2’-偶氮二(N,N’-二甲基异丁脒)在63.3g去离子水中的溶液
进料3:
450.1g 去离子水
7.6g 丙烯酸
270.0g 甲基丙烯酸甲酯
57.0g 甲基丙烯酸二甲氨基乙酯
42.8g 乳化剂溶液E4(见上文)
xg 活性物质(见表3)
表3
分散体 | 活性物质 | x[g] |
D14 | 环戊唑菌 | 61.8 |
D15 | 环唑醇 | 42.9 |
D16 | 氧唑菌 | 0.4 |
D17 | 戊唑醇 | 19.0 |
D18 | IPBC1) | 18.2 |
所得分散体具有的固体含量为29.8重量%且粘度为105mPa·s。该聚合物具有借助DSC测定为110℃的玻璃化转变温度。借助光散射测定的平均粒度为155-175nm。
II.应用研究:
在尺寸为40×15×4mm3的松属(Pinus)木材试样(南方黄松)上测定本发明组合物对木材破坏性担子菌纲真菌的有效性限度。已知为Bravery试验的对碎木试样的测试方法近似地基于EN 113并用于测定木材防腐剂对木材破坏性真菌的防治效果(就此而言可以参见A.F.Bravery,Intern.Res.Group Wood Pres.,Doc.No.IRG/WP/2113,5S.,Stockholm,1978)。在无渗出或根据EN 84有渗出下测试用本发明组合物浸渍的木材试样。使用6种不同活性物质浓度进行研究,所述浓度为0.4-4重量%活性物质(氧唑菌)或0.63-6.3重量%活性物质(戊唑醇),并且对每个活性物质浓度和测试真菌每次取5个平行试样。将粉孢革菌(Coniophora puteana)BAM Ebw.15和棉腐卧孔菌(Poria placenta)FPRL 280用作测试真菌。由测试木材的重量损失反映由真菌侵袭引起的木材破坏,所述重量损失在6周后测定。若重量损失基于试样的起始干重低于3重量%,则认为该防腐剂在特定活性物质浓度下实现的木材保护属于满意。以两个浓度给出有效性的浓度限度。较低浓度反映木材不再受到满意保护的值,而较高浓度对应于实现完全保护的最小浓度。
测试了根据实施例2的程序制备的活性物质含量为5.52重量%氧唑菌(基于固体含量,或2.4重量%,基于分散体)、固体含量为43.7重量%且平均粒度为107nm的分散体和根据实施例2的程序制备的活性物质含量为4.69重量%戊唑醇(基于固体含量,或2.05重量%,基于分散体)、固体含量为43.8重量%且平均粒度为98nm的分散体。
有效性的限度列于表4中。为了对比,给出的是对活性物质在丙酮中的溶液测定的值。
表4:
在实践中,渗出之后的上限值尤其对木材防腐剂的评价具有决定性。表4的结果证明本发明的活性物质组合物对木材破坏性真菌的有效性至少相当于在有机溶剂中的配制剂,在氧唑菌的情况下甚至更好。
在测试条件下,为对比目的而仅用不含活性物质的但具有其他相同组成的分散体处理的木材试样显示出真菌侵袭对木材物质的严重损害,与未处理木材试样相比仅稍低。
Claims (21)
1.一种含水活性物质组合物,其包含:
a)至少一种水溶性在25℃且1013毫巴下不超过5g/l的杀真菌有机活性物质,和
b)通过动态光散射测定的平均粒度不超过300nm的细碎聚合物,其中聚合物颗粒包含所述活性物质,
其中所述聚合物由包含如下单体的烯属不饱和单体M形成:
-基于单体M的总量为60-99.5重量%的至少一种水溶性在25℃下不超过30g/l的中性单烯属不饱和单体M1,其中单体M1选自乙烯基芳族单体、丙烯酸C2-C10烷基酯和甲基丙烯酸C1-C10烷基酯,和
-基于单体M的总量为0.5-40重量%的一种或多种单体M1以外的烯属不饱和单体M2,所述单体M2选自:
-具有至少一个酸基团或至少一个阴离子基团的单烯属不饱和单体M2a;
-水溶性在25℃下为至少50g/l的单烯属不饱和中性单体M2b;和
-具有至少一个阳离子基团和/或至少一个可以在含水介质中质子化的基团的单烯属不饱和单体M2c,
其中,基于单体M的总量,所述杀真菌有机活性物质的量为0.1-30重量%;所述含水活性物质组合物进一步包含至少一种乳化剂,乳化剂的量基于单体M的总量为0.1-15重量%。
2.根据权利要求1的活性物质组合物,其中单体M包括至少一种单体M2c。
4.根据权利要求1-3中任一项的活性物质组合物,其中所述聚合物具有至少10℃的玻璃化转变温度Tg。
5.根据权利要求1-3中任一项的活性物质组合物,其中杀真菌活性物质选自如下类杀真菌剂:康唑类,吗啉类,嗜球果伞素类,噻唑类,亚磺酰胺类和碘化合物类。
6.根据权利要求4的活性物质组合物,其中杀真菌活性物质选自如下类杀真菌剂:康唑类,吗啉类,嗜球果伞素类,噻唑类,亚磺酰胺类和碘化合物类。
7.根据权利要求1-3中任一项的活性物质组合物,其中聚合物颗粒额外包含杀虫活性物质,所述杀虫活性物质为在25℃且1013毫巴下的水溶性不超过5g/l的有机活性物质,其中活性物质的总量基于单体M的总量为0.5-30重量%。
8.根据权利要求6的活性物质组合物,其中聚合物颗粒额外包含杀虫活性物质,所述杀虫活性物质为在25℃且1013毫巴下的水溶性不超过5g/l的有机活性物质,其中活性物质的总量基于单体M的总量为0.5-30重量%。
9.根据权利要求7的活性物质组合物,其中杀虫活性物质选自合成除虫菊酯类,节肢动物生长调节剂,氟唑虫清和新类烟碱。
10.根据权利要求8的活性物质组合物,其中杀虫活性物质选自合成除虫菊酯类,节肢动物生长调节剂,氟唑虫清和新类烟碱。
11.根据权利要求1-3中任一项的活性物质组合物,其中聚合物可以通过单体M的水包油乳液的自由基水乳液聚合得到,其中待聚合的水包油乳液的单体液滴包含溶解形式的杀真菌活性物质。
12.根据权利要求10的活性物质组合物,其中聚合物可以通过单体M的水包油乳液的自由基水乳液聚合得到,其中待聚合的水包油乳液的单体液滴包含溶解形式的杀真菌活性物质。
13.根据权利要求1-3中任一项的活性物质组合物,其中挥发性有机成分的含量基于该组合物的总重量低于1重量%。
14.根据权利要求12的活性物质组合物,其中挥发性有机成分的含量基于该组合物的总重量低于1重量%。
15.根据权利要求1-3中任一项的活性物质组合物,其中固体含量为10-60重量%。
16.根据权利要求14的活性物质组合物,其中固体含量为10-60重量%。
17.一种制备根据权利要求1-16中任一项的活性物质组合物的方法,包括单体M的水包油乳液的自由基水乳液聚合,其中该乳液的单体液滴包含至少一种杀真菌活性物质和任选杀虫活性物质。
18.根据权利要求1-16中任一项的活性物质组合物在防治有害真菌中的用途。
19.根据权利要求1-16中任一项的活性物质组合物在保护含纤维素材料以防被有害真菌侵袭中的用途。
20.一种保护含纤维素材料以防被有害真菌侵袭的方法,包括用根据权利要求1-16中任一项的组合物处理含纤维素材料。
21.根据权利要求20的方法,其中含纤维素材料为木材。
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