CN102647911B - 用于防治蜂巢中的螨的含聚酯膜的分配器 - Google Patents
用于防治蜂巢中的螨的含聚酯膜的分配器 Download PDFInfo
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- CN102647911B CN102647911B CN201080040662.1A CN201080040662A CN102647911B CN 102647911 B CN102647911 B CN 102647911B CN 201080040662 A CN201080040662 A CN 201080040662A CN 102647911 B CN102647911 B CN 102647911B
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- 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
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
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Abstract
本发明涉及一种填充有包含C1-C10羧酸和增稠剂的凝胶的分配器,其包含聚酯膜。本发明进一步涉及所述凝胶。还涉及制备所述分配器的方法,包括:a)将C1-C10羧酸与增稠剂混合,和b)将步骤a)的混合物填充至所述分配器中。本发明进一步涉及一种防治蜂巢中的螨的方法,包括将所述分配器置于蜂巢内部或附近。还涉及所述分配器或凝胶在农业、工业或家庭环境中防治螨或孢子虫中的用途。
Description
本发明涉及一种填充有包含C1-C10羧酸和增稠剂的凝胶的分配器,其包含聚酯膜。本发明进一步涉及所述凝胶。还涉及一种制备所述分配器的方法,包括:a)将C1-C10羧酸与增稠剂混合,和b)将步骤a)的混合物填充到分配器中。本发明进一步涉及一种防治蜂巢中的螨的方法,包括将所述分配器置于蜂巢内部或附近。还涉及所述分配器或凝胶在农业、工业或家庭环境中防治螨的用途。优选实施方案与其他优选实施方案的组合处于本发明的范围之内。
用于防治蜂巢中螨的有机酸的各种分配器是公知的:
Kochansky和Shimanuki,Journal of Agri.Food Chem.1999,47,3850-3853公开了用于防治蜜蜂的寄生性螨的甲酸凝胶配制剂。公开了各种胶凝剂,例如热解法二氧化硅、聚丙烯酸、黄原胶、瓜尔胶、阿拉伯树胶、膨润粘土或淀粉接枝聚合物。作为分配器,使用由聚乙烯、聚丙烯、聚乙烯/聚酯层压材料、Barex膜(通常为改性丙烯腈-丙烯酸甲酯共聚物),或Valeron/Surlyn(后者通常为部分中和的乙烯-甲基丙烯酸共聚物)制成的预填充包。为了分配甲酸,在分配器中切出四条缝。
US6,037,374公开了一种用于处理蜜蜂的寄生性螨的分配器,其包含甲酸以及选自热解法二氧化硅和聚丙烯酸的胶凝剂的凝胶组合物。作为分配器,使用聚乙烯袋,其中切出四条缝以用于分配。还提出了多孔容器。
Daniels等,Journal of Apiculture Research 1999,38,63-69公开了用于蜜蜂的螨防治中甲酸的隔膜阻挡递送。作为膜装置,使用膜厚度为71-650μm的胶乳避孕套。
WO2002/30181公开了一种包含毛细细胞状结构的泡沫芯的处理流体分配器,所述泡沫芯包封在流体不可渗透的皮层中。当将泡沫芯切成两半并用甲酸饱和时,其可垂直悬挂于蜜蜂空间中并向下置于泡沫芯的暴露面上。由此使甲酸蒸发。
WO1997/47193公开了一种用于防治蜂巢中侵染的缓释凝胶配制剂,其包含精油或有机酸。所述凝胶可呈具有例如由铝或塑料箔制成的气密密封盖的浅盘分配器的形式。
这些已知装置具有各种缺点,所述缺点应由本发明克服。因此,本发明的目的是寻找一种用于提高蜂群健康的装置,所述装置允许容易且可靠的处理:养蜂人应容易地操作所述装置,尤其是不与活性成分如腐蚀性甲酸接触。活性成分的分配应在各种气候条件下是可靠的,例如在美国南方或加利福尼亚的温暖气候中也是可靠的。所有配制剂添加剂(优选包括分配器)应对蜜蜂是无毒的。所述分配器和配制剂应为可生物降解的。
该目的通过一种填充有包含C1-C10羧酸和增稠剂的凝胶的分配器实现,所述分配器包括聚酯膜。
所述分配器包括聚酯膜。这类分配器可通过所述聚酯膜将凝胶分配到环境中。所述分配器可具有适于容纳凝胶的任何三维中空形式,例如圆柱形、球形、立方体,或囊。所述分配器可由任何分配器材料如金属、塑料、纸、玻璃或木材构成,优选由塑料构成。所述分配器材料通常对甲酸稳定。所述分配器材料对甲酸蒸气而言可为可透的。所述分配器填充有凝胶。通常,分配器内部容积的至少50%,优选至少80%填充有所述凝胶。内部可存在例如一些空气。
分配器中空形状的一部分可包括膜。例如由分配器材料制成的圆柱底部可由聚酯膜构成;或者由分配器材料制成的立方体的一面可由聚酯膜构成。通常,聚酯膜覆盖分配器表面的至少10%。优选所述膜覆盖分配器表面的至少30%,更优选至少50%,最优选至少95%。在尤其优选的实施方案中,所述分配器为由膜构成的囊。例如聚酯膜形成可填充有凝胶的囊。通常,该囊具有5-5000ml,优选30-1000ml,更优选80-300ml的容积。
所述聚酯膜通常具有3-500μm,优选10-200μm,更优选20-150μm,甚至更优选20-120μm的厚度。所述膜可由至少一层,例如1、2或3层构成。所述层通常包含本领域熟知的各种加工添加剂,例如防粘连或防滑添加剂。优选所述膜中所存在的所有层均由聚酯,优选半芳族聚酯构成。
所述膜可通过常规膜挤出方法生产。
所述聚酯膜可结合至涂覆基质上。涂覆基质通常涂有聚酯,从而形成层压体。优选涂覆基质为可堆肥或腐烂的那些,例如纸、纤维素或淀粉的模制品。优选涂覆基质为纸或纤维素。所述聚酯膜可通过辊压、涂布、喷涂或倾注而结合至涂覆基质上。优选的涂覆方法描述于2008年9月29日提交的EP08165372.7和2009年8月12日提交的EP09010388.8中,通过引用将二者并入本文中。
所述聚酯膜通常包含聚酯。聚酯为公知的聚合物。其包含聚合形式的单体,如二醇和二酸(或二酯),或羟基酸(或羟基酯)。优选聚酯为脂族或半芳族聚酯,更优选半芳族聚酯。
合适的聚酯为脂族聚酯。这些包括脂族羟基羧酸或内酯的均聚物,以及不同羟基羧酸或内酯的共聚物或嵌段共聚物,或这些的混合物。这些脂族聚酯也可含有二醇和/或异氰酸酯单元。脂族聚酯还可含有衍生自三-或多官能化合物,例如衍生自环氧化物、酸或三醇的单元。脂族聚酯可含有后者单元作为单独的单元,或大量这些单元(可能的话与二醇和/或异氰酸酯一起)。脂族聚酯的制备方法是本领域技术人员所已知的。在制备脂族聚酯中,当然也可使用由两种或更多种共聚单体和/或其他单元(例如环氧化物或多官能脂族或芳族酸或多官能醇)构成的混合物。脂族聚酯通常具有10,000-100,000g/mol的摩尔质量(数均)。
脂族聚酯的实例为乳酸、聚-3-羟基丁酸酯的聚合反应产物,或由脂族或脂环族二羧酸与脂族或脂环族二醇构成的聚酯。脂族聚酯也可为含有其他单体的无规或嵌段共聚酯。所述其他单体的比例通常为至多10重量%。优选的共聚单体为羟基羧酸或内酯或这些的混合物。
乳酸的聚合反应产物本身是已知的或可通过本身已知的方法制备。除聚交酯外,也可使用基于乳酸与其他单体的那些共聚物或嵌段共聚物。大多使用线性聚交酯。然而,也可使用支化乳酸聚合物。支化剂的实例为多官能酸或醇。可作为实例提及的聚交酯为可基本由乳酸或其C1-C4烷基酯或这些的混合物与至少一种脂族C4-C10二羧酸以及与至少一种具有3-5个羟基的C3-C10链烷醇得到的那些。
聚-3-羟基丁酸酯为3-羟基丁酸或其与4-羟基丁酸以及与3-羟基戊酸,特别是与至多30%,优选至多20%重量比的最后所提酸的混合物的均聚物或共聚物。合适的这类聚合物还包括具有R-有规立构构型的那些。聚羟基丁酸酯或这些的共聚物可微生物制备。由各种细菌和真菌制备的方法以及制备有规立构聚合物的方法是已知的。也可使用上述羟基羧酸或内酯,或其混合物、低聚物或聚合物的嵌段共聚物。
由脂族或脂环族二羧酸以及脂族或脂环族二醇构成的聚酯为由脂族或脂环族二羧酸或由这些的混合物以及由脂族或脂环族二醇或由这些的混合物构成的那些。根据本发明,可使用无规或嵌段共聚物。本发明合适的脂族二羧酸通常具有2-10个碳原子,优选4-6个碳原子。它们可为线性或支化的。就本发明而言,可使用的脂环族二羧酸的通常为具有7-10个碳原子的那些,特别是具有8个碳原子的那些。然而,原则上也可使用具有更大碳原子数,例如具有至多30个碳原子的二羧酸。应提及的实例为:丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、壬二酸、癸二酸、富马酸、2,2-二甲基戊二酸、辛二酸、1,3-环戊烷二甲酸、1,4-环己烷二甲酸、1,3-环己烷二甲酸、二甘醇酸、衣康酸、马来酸和2,5-降冰片烷二甲酸,优选己二酸。还应提及的是同样可使用的上述脂族或脂环族二羧酸的成酯衍生物,特别是二-C1-C6烷基酯,例如二甲酯、二乙酯、二正丙酯、二异丙酯、二正丁酯、二异丁酯、二叔丁酯、二正戊酯、二异戊酯和二正己酯。同样可使用二羧酸的酐。二羧酸或这些的成酯衍生物可单独或作为这些中两种或更多种的混合物使用。
合适的脂族或脂环族二醇通常具有2-10个碳原子,优选4-6个碳原子。其可为线性或支化的。实例为1,4-丁二醇、乙二醇、1,2-或1,3-丙二醇、1,6-己二醇、1,2-或1,4-环己二醇或这些的混合物。
可使用的脂族聚酯的实例为如WO94/14870所述的脂族共聚酯,特别是由琥珀酸、其二酯,或由其与其他脂族酸或相应的二酯如戊二酸和丁二醇的混合物,或由该二醇与乙二醇、丙二醇或己二醇构成的混合物或这些的混合物制备的脂族共聚酯。在另一实施方案中,优选的脂族聚酯包括聚己内酯。
根据本发明,术语半芳族聚酯是指包含聚合形式的脂族和芳族单体的聚酯。术语半芳族聚酯还意欲包括聚酯衍生物,如聚醚酯、聚酯酰胺或聚醚酯酰胺。其中合适的半芳族聚酯为线性非扩链聚酯(WO92/09654)。优选扩链和/或支化半芳族聚酯。后者公开于开头所提及的说明书、WO96/15173、WO96/15174、WO96/15175、WO96/15176、WO96/21689、WO96/21690、WO96/21691、WO96/21689、WO96/25446、WO96/25448和WO98/12242中,通过引用明确地将其并入本文中。也可使用不同半芳族聚酯的混合物。特别地,术语半芳族聚酯意欲指产品如(BASFAktiengesellschaft)和Bio和Origo-Bi(Novamont)。
其中特别优选的半芳族聚酯为包含如下显著组分的聚酯:
A)由如下组分构成的酸组分:
a1)30-99mol%的至少一种脂族、或至少一种脂环族二羧酸、或其成酯衍生物或这些的混合物,
a2)1-70mol%的至少一种芳族二羧酸、或其成酯衍生物、或这些的混合物,和
a3)0-Smol%的包含磺酸盐基团的化合物,和
B)选自至少一种C2-C12链烷二醇和至少一种C5-C10环烷二醇或这些的混合物的二醇组分。
如果需要的话,所述半芳族聚酯还可包含一种或多种选自C)和D)的组分,其中:
C)为选自如下的组分:
c1)至少一种包含醚官能且具有式I的二羟基化合物:
HO-[(CH2)n-O]m-H (I)
其中n为2、3或4且m为2-250的整数,
c2)至少一种式IIa或IIb的羟基羧酸:
其中p为1-1500的整数且r为1-4的整数,且G为选自亚苯基、
-(CH2)q-(其中q为1-5的整数)、-C(R)H-和-C(R)HCH2(其中R为甲基或乙基)的基团,
c3)至少一种氨基-C2-C12链烷醇、或至少一种氨基-C5-C10环烷醇或这些的混合物,
c4)至少一种二氨基-C1-C8链烷烃,
c5)至少一种式III的2,2’-双唑啉:
其中R1为单键、(CH2)z-亚烷基(其中z=2、3或4)或亚苯基,c6)至少一种选自如下组的氨基羧酸:天然存在的氨基酸,可通过使具有4-6个碳原子的二羧酸与具有4-10个碳原子的二胺缩聚而获得的聚酰胺,式IVa和IVb的化合物:
其中s为1-1500的整数且t为1-4的整数,T为选自亚苯基、-(CH2)u-(其中u为1-12的整数)、-C(R2)H-和-C(R2)HCH2-(其中R2为甲基或乙基)的基团,
以及具有重复单元V的聚唑啉:
其中R3为氢、C1-C6烷基、C5-C8环烷基、未被取代或被至多3个C1-C4烷基取代的苯基,或四氢呋喃基,
或由c1-c6构成的混合物,
和其中:
D)为选自如下的组分:
d1)至少一种具有至少3个能形成酯的基团的化合物,
d2)至少一种异氰酸酯,
d3)至少一种二乙烯基醚,
或由d1)-d3)构成的混合物。
在一个优选实施方案中,半芳族聚酯的酸组分A包含30-70mol%,特别是40-60mol%a1,和30-70mol%,特别是40-60mol%a2。
可使用的脂族酸和相应的衍生物a1通常为具有2-10个碳原子,优选4-6个碳原子的那些。其可为线性或支化的。可用于本发明的脂环族二羧酸通常为具有7-10个碳原子的那些,特别是具有8个碳原子的那些。然而,原则上也可使用具有更大碳原子数,例如具有至多30个碳原子的二羧酸。
可提及的实例为:丙二酸、琥珀酸、戊二酸、2-甲基戊二酸、3-甲基戊二酸、己二酸、庚二酸、壬二酸、癸二酸、富马酸、2,2-二甲基戊二酸、辛二酸、1,3-环戊烷二甲酸、1,4-环己烷二甲酸、1,3-环己烷二甲酸、二甘醇酸、衣康酸、马来酸、十三烷二酸和2,5-降冰片烷二甲酸。
也可使用并可提及的上述脂族或脂环族二羧酸的成酯衍生物特别地为二-C1-C6烷基酯,例如二甲酯、二乙酯、二正丙酯、二异丙酯、二正丁酯、二异丁酯、二叔丁酯、二正戊酯、二异戊酯或二正己酯。也可使用二羧酸的酐。
此时,二羧酸或其成酯衍生物可单独或以由这些中两种或更多种组成的混合物形式使用。
优选使用琥珀酸、己二酸、壬二酸、癸二酸、十三烷二酸,或其相应的成酯衍生物,或这些的混合物。特别优选使用琥珀酸、己二酸或癸二酸,或其相应的成酯衍生物,或这些的混合物。特别优选使用己二酸或其成酯衍生物,例如其烷基酯,或其混合物。如果制备具有“硬”或“脆性”组分ii),例如聚羟基丁酸酯,特别是聚交酯的聚合物混合物,则所用脂族二羧酸优选包含癸二酸,或癸二酸与己二酸的混合物。如果制备具有“软”或“韧性”组分ii),例如聚羟基丁酸酯-共聚-戊酸酯的聚合物混合物,则所用脂族二羧酸优选包含琥珀酸或琥珀酸与己二酸的混合物。
琥珀酸、壬二酸、癸二酸和十三烷二酸的另一优点是它们是易得的可再生原料。
可提及的芳族二羧酸a2通常为具有8-12个碳原子的那些,优选为具有8个碳原子的那些。例如可提及对苯二甲酸、间苯二甲酸、2,6-萘甲酸和1,5-萘甲酸,以及这些的成酯衍生物。此处可特别提及二-C1-C6烷基酯,例如二甲酯、二乙酯、二正丙酯、二异丙酯、二正丁酯、二异丁酯、二叔丁酯、二正戊酯、二异戊酯或二正己酯。二羧酸a2的酐也是合适的成酯衍生物。
然而,原则上也可使用具有更大碳原子数,例如至多20个碳原子的芳族二羧酸a2。
芳族二羧酸或这些的成酯衍生物a2可单独或作为这些中两种或更多种的混合物使用。特别优选使用对苯二甲酸或其成酯衍生物,例如对苯二甲酸二甲酯。
所用包含磺酸盐基团的化合物通常为一种含磺酸根的二羧酸或其成酯衍生物的碱金属或碱土金属盐,优选5-磺基间苯二甲酸的碱金属盐或这些的混合物,特别优选钠盐。
在一个优选实施方案中,酸组分A包含40-60mol%a1,40-60mol%a2和0-2mol%a3。在另一优选实施方案中,酸组分A包含40-59.9mol%a1,40-59.9mol%a2和0.1-1mol%a3,特别是40-59.8mol%a1,40-59.8mol%a2和0.2-0.5mol%a3。
二醇B通常选自具有2-12个碳原子,优选4-6个碳原子的支化或线性链烷二醇,或选自具有5-10个碳原子的环烷二醇。
合适链烷二醇的实例为乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,4-丁二醇、1,5-戊二醇、2,4-二甲基-2-乙基-1,3-己二醇、2,2-二甲基-1,3-丙二醇、2-乙基-2-丁基-1,3-丙二醇、2-乙基-2-异丁基-1,3-丙二醇和2,2,4-三甲基-1,6-己二醇,特别是乙二醇、1,3-丙二醇、1,4-丁二醇或2,2-二甲基-1,3-丙二醇(新戊二醇);环戊二醇、1,4-环己二醇、1,2-环己烷二甲醇、1,3-环己烷二甲醇、1,4-环己烷二甲醇或2,2,4,4-四甲基-1,3-环丁二醇。特别优选1,4-丁二醇,特别是与己二酸组合作为组分a1),和1,3-丙二醇,特别是与癸二酸组合作为组分a1)。1,3-丙二醇的另一优点为其是可得的可再生原料。也可使用不同链烷二醇的混合物。
取决于需要酸基团过量还是OH端基过量,组分A或组分B可过量使用。在一个优选的实施方案中,所用组分A与B的摩尔比可为0.4∶1-1.5∶1,优选0.6∶1-1.1∶1。
除组分A和B之外,本发明聚酯混合物所基于的聚酯可包含其他组分。
优选使用的二羟基化合物c1为二甘醇、三甘醇、聚乙二醇、聚丙二醇和聚四氢呋喃(聚THF),特别优选二甘醇、三甘醇和聚乙二醇,也可使用这些的混合物,如可能具有不同变量n(参见式I)的化合物,例如包含丙烯单元(n=3)的聚乙二醇,其可例如通过使用本身已知的聚合方法并首先与氧化乙烯聚合,然后与氧化丙烯聚合而得到,特别优选基于具有不同变量n的聚乙二醇的聚合物,其中由氧化乙烯形成的单元占优势。聚乙二醇的摩尔质量(Mn)通常选自250-8000g/mol,优选600-3000g/mol。
在制备半芳族聚酯的一个优选实施方案中,可例如使用基于B和c1的摩尔量为15-98mol%,优选60-99.5mol%的二醇B和0.2-85mol%,优选0.5-30mol%的二羟基化合物c1。
在一个优选实施方案中,所用羟基羧酸c2)为:羟基乙酸、D-、L-或D,L-乳酸、6-羟基己酸,这些的环状衍生物如乙交酯(1,4-二烷-2,5-二酮)、D-或L-二丙交酯(3,6-二甲基-1,4-二烷-2,5-二酮),对羟基苯甲酸或其低聚物和聚合物如3-聚羟基丁酸、聚羟基戊酸、聚交酯(例如可以以4042D(NatureWorks)获得)或3-聚羟基丁酸与聚羟基戊酸的混合物(可由PHB Industrial,Tianan或Metabolix获得),以及为了制备半芳族聚酯,特别优选其低分子量和环状衍生物。
可使用的羟基羧酸的量的实例基于A和B的量为0.01-50重量%,优选0.1-40重量%。
就还包括4-氨甲基环己烷甲醇的本发明而言,所用氨基-C2-C12链烷醇或氨基-C5-C10环烷醇(组分c3)优选为氨基-C2-C6链烷醇,例如2-氨基乙醇、3-氨基丙醇、4-氨基丁醇、5-氨基戊醇或6-氨基己醇,或氨基-C5-C6环烷醇如氨基环戊醇和氨基环己醇,或这些的混合物。
所用二氨基-C1-C8链烷烃(组分c4)优选为二氨基-C4-C6链烷烃,例如1,4-二氨基丁烷、1,5-二氨基戊烷或1,6-二氨基己烷(六亚甲基二胺,“HMD”)。
在用于制备半芳族聚酯的一个优选实施方案中,可使用基于B的摩尔量为0.5-99.5mol%,优选0.5-50mol%的c3,和基于B的摩尔量为0-50mol%,优选0-35mol%的c4。
式III的2,2’-双唑啉c5通常可通过Angew.Chem.Int.Edit.,第11卷(1972),第287-288页的方法获得。特别优选的双唑啉为其中R1为单键、(CH2)z-亚烷基(其中z=2、3或4,例如亚甲基、乙烷-1,2-二基、丙烷-1,3-二基或丙烷-1,2-二基)或苯基的那些。可提及的特别优选的双唑啉为2,2’-双(2-唑啉)、双(2-唑啉基)甲烷、1,2-双(2-唑啉基)乙烷、1,3-双(2-唑啉基)丙烷和1,4-双(2-唑啉基)丁烷,特别是1,4-双(2-唑啉基)苯、1,2-双(2-唑啉基)苯或1,3-双(2-唑啉基)苯。
在制备半芳族聚酯中,可使用例如70-98mol%B、至多30mol%c3和0.5-30mol%c4和0.5-30mol%c5,在每种情况下基于组分B、c3、c4和c5的摩尔量之和。在另一优选实施方案中,可使用基于A和B的总重量为0.1-5重量%,优选0.2-4重量%c5。
所用组分c6可以为天然氢基羧酸。这些包括缬氨酸、亮氨酸、异亮氨酸、苏氨酸、蛋氨酸、苯基丙氨酸、色氨酸、赖氨酸、丙氨酸、精氨酸、天冬氨酸、半胱氨酸、谷氨酸、甘氨酸、组氨酸、脯氨酸、丝氨酸、酪氨酸、天冬酰胺和谷氨酰胺。
优选的式IVa和IVb的氨基羧酸为其中s为1-1000的整数且t为1-4的整数,优选1或2,且t选自亚苯基和-(CH2)u-(其中u为1、5或12)的那些。
c6也可为式V的聚唑啉。然而,c6也可为不同氨基羧酸和/或聚唑啉的混合物。
在一个优选实施方案中,c6的用量可基于组分A和B的总量为0.01-50重量%,优选0.1-40重量%。
其中,如果需要的话可用于制备半芳族聚酯的其他组分为包含至少3个能形成酯的基团的化合物d1。
化合物d1优选包含3-10个能形成酯键的官能团。特别优选的化合物d1在分子中具有3-6个这类官能团,特别是3-6个羟基和/或羧基。应提及的实例为:酒石酸、柠檬酸、马来酸;三羟甲基丙烷、三羟甲基乙烷;季戊四醇;聚醚三醇;甘油;苯均三酸;偏苯三酸、偏苯三酸酐;苯均四酸、苯均四酸二酐和羟基间苯二甲酸。
化合物d1的用量基于组分A通常为0.01-15mol%,优选0.05-10mol%,特别优选0.1-4mol%。
所用组分d2为异氰酸酯或不同异氰酸酯的混合物。可使用芳族或脂族二异氰酸酯。然而,也可使用较高官能度的异氰酸酯。就本发明而言,芳族二异氰酸酯d2尤其为甲苯-2,4-二异氰酸酯、甲苯-2,6-二异氰酸酯、二苯基甲烷-2,2’-二异氰酸酯、二苯基甲烷-2,4’-二异氰酸酯、二苯基甲烷-4,4’-二异氰酸酯、萘-1,5-二异氰酸酯或二甲苯二异氰酸酯。例如可使用可以以由BASF Aktiengesellschaft获得的异氰酸酯。
在这些中,特别优选二苯基甲烷-2,2’-、2,4’-和4,4’-二异氰酸酯作为组分d2。后者二异氰酸酯通常作为混合物使用。
还可使用的三环异氰酸酯d2为三(4-异氰酸酯基苯基)甲烷。多环芳族二异氰酸酯例如在单环或二环二异氰酸酯的制备过程中产生。
组分d2还可包含次要量,例如基于组分d2的总重量为至多5重量%的脲二酮基团,例如以封闭异氰酸酯基团。
就本发明而言,脂族二异氰酸酯d2主要为具有2-20个碳原子,优选3-12个碳原子的线性或支化亚烷基二异氰酸酯或亚环烷基二异氰酸酯,例如六亚甲基-1,6-二异氰酸酯、异佛尔酮二异氰酸酯或亚甲基双(4-异氰酸酯基环己烷)。六亚甲基-1,6-二异氰酸酯和异佛尔酮二异氰酸酯是特别优选的二异氰酸酯d2。
其中,优选的异氰脲酸酯为衍生自C2-C20,优选C3-C12亚环烷基二异氰酸酯或亚烷基二异氰酸酯如异佛尔酮二异氰酸酯或亚甲基双(4-异氰酸酯基环己烷)的脂族异氰脲酸酯。此时,亚烷基二异氰酸酯可为线性或支化的。特别优选基于正己烷二异氰酸酯的异氰脲酸酯,例如正己烷二异氰酸酯的环化三聚物、五聚物或更高级低聚物。
组分d2的用量基于A和B的摩尔量之和通常为0.01-5mol%,优选0.05-4mol%,特别优选0.1-4mol%。
可使用的二乙烯基醚d3通常为任何常规和市售二乙烯基醚。优选使用1,4-丁二醇二乙烯基醚、1,6-己二醇二乙烯基醚或1,4-环己烷二甲醇二乙烯基醚或这些的混合物。
优选使用的二乙烯醚的量基于A和B的总重量为0.01-5重量%,尤其为0.2-4重量%。
优选的半芳族聚酯的实例基于如下组分:A、B、d1;A、B、d2;A、B、d1、d2;A、B、d3;A、B、c1;A、B、c1、d3;A、B、c3、c4;A、B、c3、c4、c5;A、B、d1、c3、c5;A、B、c3、d3;A、B、c3、d1;A、B、c1、c3、d3;或A、B、c2。在这些中,特别优选基于A、B和d1,或A、B和d2,或基于A、B、d1和d2的半芳族聚酯。在另一优选实施方案中,所述半芳族聚酯基于A、B、c3、c4和c5或A、B、d1、c3和c5。
如果需要的话,上述聚酯还可含有填料,所述填料可在聚合工艺期间在任何阶段或随后,例如在聚酯熔体中掺入。可加入基于聚酯为0-80重量%的填料。合适填料的实例为炭黑、淀粉、木素粉、纤维素纤维、天然纤维如剑麻和大麻、氧化铁、粘土矿物、矿石、碳酸钙、硫酸钙、硫酸钡和二氧化钛。
聚酯可包含其他添加剂,所述添加剂可在聚合工艺期间在任何阶段或随后,例如在聚酯熔体中掺入。可加入基于聚酯为0-80重量%,优选0-5重量%的填料。合适添加剂的实例为稳定剂如生育酚(维生素E)、有机磷化合物、单-、二-和多酚、氢醌、二芳基胺、硫醚、UV稳定剂;成核剂如滑石;和基于烃的润滑剂和脱模剂,脂肪醇、高级羧酸、高级羧酸的金属盐如硬脂酸钙和锌,和褐煤蜡。聚酯还可以以任何所需方式通过加入有机或无机染料而着色。
聚酯通常为可生物降解的。就本发明而言,如果该物质或物质的混合物在DIN V 54900-2(1998年9月的初级标准)定义的三种方法的至少一种中具有至少60%的百分比生物降解度,则该物质或物质混合物符合称为“可生物降解”的特征。
生物降解性的结果通常是聚酯或聚酯混合物在合适且可验证的期间内分解。降解可由酶、水解、氧化和/或通过暴露于电磁辐射如UV辐射而发生,且大部分主要由暴露于微生物如细菌、酵母、真菌和藻类下而导致。量化生物降解性的方法实例是将聚酯与堆肥混合并将其储存特定的时间。例如,根据DIN EN 13432或DIN V 54900-2,方法3,使不含CO2的空气在堆肥期间通过成熟的堆肥并使堆肥经历所定义的温度曲线。此时,生物降解性定义为由试样所释放的净CO2量(在扣除无试样的堆肥所释放的CO2量之后)与试样最大可能释放出的CO2量(由试样的碳含量计算)之比,该比值以百分比生物降解性定义。甚至在堆肥数日以后,可生物降解的聚酯或可生物降解的聚酯混合物通常显示出明显的降解信号,例如真菌生长、断裂和穿孔。
测定生物降解性的其他方法例如描述于ASTM D5338和ASTM D6400中。
半芳族聚酯的制备本身是已知的或可通过本身已知的方法进行。
优选的半芳族聚酯的特征可为1000-100000g/mol,特别是9000-75000g/mol,优选10000-50000g/mol的摩尔质量(Mn)。优选的半芳族聚酯的特征也可为60-170℃,优选80-150℃的熔点。
可将聚酯任选与其他聚合物,优选与聚乳酸混合。本文所用术语“聚交酯”包括聚乳酸和所有共聚物以及聚交酯均聚物和共聚物的共混物且缩写为PLA。PLA的聚合物结构可变化,并因此影响性能。结构的变化由合成中所用的乳酸对映体D(-)和L(+)的不同比例导致。这些乳酸可产生三类交酯以用于聚合:D、L和内消旋。含有大于93%L-乳酸单元的PLA树脂为半晶体,而具有50-93%L-乳酸的PLA为严格无定形的。均聚物聚(D-交酯)或聚(L-交酯)和高D-或L-共聚物具有非常规整的结构并形成晶相。内消旋和D-交酯形式的存在导致晶体结构不完美,从而降低结晶度。聚乳酸例如由NatureWorks LLC,Minnetonka,Minn.,美国以所谓的4020或4042D获得。PLA可以以基于聚酯和PLA的总质量为至多60重量%,优选至多50重量%存在。优选PLA可以基于聚酯和PLA的总质量为10-60重量%,优选30-50重量%的量存在。这种半芳族聚酯和PLA的混合物可商购获得,例如获自BASF SE的L BX 8145(获自BASF的半芳族聚酯F BX 7011与45重量%PLA的混合物)。
所述凝胶包含C1-C10羧酸和增稠剂。C1-C10羧酸通常包含1-10个碳原子。分子中可存在1、2或3个羧酸基团。优选将所述羧酸溶解或乳化,优选溶解于溶剂,优选水中。优选所述羧酸为甲酸、乙酸、草酸、苹果酸、酒石酸、羟基乙酸、乳酸、柠檬酸、扁桃酸或其混合物。更优选所述羧酸为甲酸、乙酸、乳酸、草酸或其混合物。最优选甲酸。
所述增稠剂可为通常用于提高流体粘度的任何类型的化学或天然化合物。合适增稠剂的实例为多糖、蛋白质(例如酪蛋白、明胶)、合成聚合物,优选多糖,或无机粘土(例如硅酸或层状硅酸盐)。上述增稠剂分别可单独或作为混合物使用。
合成聚合物例如为聚乙烯醇、聚(甲基)丙烯酸或其盐、聚丙烯酰胺、聚乙烯吡咯烷酮、聚乙二醇、苯乙烯-马来酸酐共聚物或其盐。
多糖例如为淀粉(天然或改性的)、改性纤维素(例如羟乙基纤维素、羟丙基甲基纤维素、羟丙基纤维素、乙基羟乙基纤维素、羧甲基纤维素、甲基纤维素、微晶纤维素(通过将木浆用盐酸水解而制备的部分解聚形式的纤维素))、琼脂、果胶、藻酸盐或基于多糖的天然树胶(例如刺槐豆胶、瓜尔胶、阿拉伯树胶、角叉菜胶、黄原胶、结冷胶)。优选所述增稠剂包括天然淀粉或改性淀粉。更优选,所述增稠剂为天然淀粉。多糖如天然或改性淀粉通常以粉末形式使用。
术语“天然淀粉”是指呈在将其与本发明凝胶的其他组分混合以前的状态的淀粉。天然淀粉随后可与C1-C10羧酸反应并形成天然淀粉的衍生物。这类反应由Wolff等,J.Am.Chem.Soc.1957,79,3860-3862或Gottlieb等,J.Am.Chem.Soc.1940,62,3342-3344中已知。
天然淀粉,通常称为未改性淀粉或珍珠型淀粉,可通过湿磨法生产且以大的工业量作为淀粉粉末商购获得。天然淀粉的实例选自玉米淀粉、土豆淀粉、小麦淀粉、米淀粉、木薯淀粉、西米淀粉、高粱淀粉、卡巴萨甜瓜(cassaba)淀粉、豌豆淀粉以及所述天然淀粉的混合物。天然淀粉也可预胶凝化。优选未改性淀粉为玉米淀粉。
合适的改性淀粉为水解或酶降解的淀粉,例如糊精如白色或黄色糊精和麦芽糖糊精,或氧化淀粉如双醛淀粉。其他实例为用无机或有机酸酯化的淀粉,特别是磷酸化和乙酰化淀粉,以及用有机卤化合物、环氧化物或硫酸盐醚化的淀粉也是合适的。淀粉及其降解和化学改性方法描述于Ullmann′s Encyclopedia of Industrial Chemistry,第5版,第A25卷,第2页及随后各页中,通过引用将其并入本文中。
所述凝胶还可包含糖。糖可为任何已知的单糖或二糖或其混合物,优选可由天然来源获得的那些。实例为蔗糖、葡萄糖、乳糖、果糖、右旋糖、麦芽糖。也可使用包含糖的工业混合物,例如黑糖、红糖、蜂蜜、糖浆。优选所述糖为二糖,更优选蔗糖。
所述凝胶还可包含精油。精油应当理解为包含可由植物提取的油或其精油组分,其有时为固体。精油的实例为单萜如薄荷醇、香叶醇、百里酚、月桂烯、柠檬醛、苧烯、蒈烯、樟脑、丁子香酚或桉油酚(桉树脑);天然油如来自柠檬、冬青、桉树、楝树、留兰香、肉桂的油。凝胶中精油的浓度并不重要,但合理地为凝胶总重量的1-50重量%。优选浓度为10-40重量%。
所述凝胶通常包含基于凝胶总重量为15-85重量%的纯C1-C10羧酸,更优选35-65重量%,甚至更优选45-55重量%。所述凝胶通常包含基于凝胶总重量为1-50重量%的增稠剂,更优选5-40重量%,甚至更优选20-30重量%。如果增稠剂包含水分,则所述浓度涉及增稠剂的干重。所述凝胶任选包含基于凝胶总重量为至多50重量%的糖,更优选至多30重量%,甚至更优选至多20重量%。在另一实施方案中,所述凝胶任选包含基于凝胶总重量为1-50重量%的糖,更优选3-30重量%,甚至更优选10-20重量%。所述凝胶通常包含水,优选基于凝胶总重量为至多100重量%。
所述凝胶可包含其他组分如配制剂添加剂。实例为溶剂、糖、染料、分散剂或乳化剂(例如增溶剂、保护性胶体、表面活性剂)、杀菌剂、防冻剂或消泡剂。
所述农业化学组合物还可包含常用于农业化学组合物中的助剂。所用助剂分别取决于具体施用形式和活性物质。合适助剂的实例为溶剂、固体载体、分散剂或乳化剂(例如其他增溶剂、保护性胶体、表面活性剂和粘合剂)、杀菌剂、防冻剂、着色剂或消泡剂。
合适溶剂为水,有机溶剂如中至高沸点的矿物油馏分如煤油或柴油,此外还有煤焦油和植物或动物来源的油,脂族、环状和芳族烃如甲苯、二甲苯、链烷烃、四氢化萘、烷基化萘或其衍生物,醇类如甲醇、乙醇、丙醇、丁醇和环己醇,二醇类,酮类如环己酮和γ-丁内酯,脂肪酸二甲基酰胺,脂肪酸和脂肪酸酯和强极性溶剂如胺类如N-甲基吡咯烷酮。优选溶剂为水。
合适的表面活性剂(辅助剂、润湿剂、增粘剂、分散剂或乳化剂)为芳族磺酸如木素磺酸(型,Borregard,挪威)、苯酚磺酸、萘磺酸(型,Akzo Nobel,美国)、二丁基萘磺酸(型,BASF,德国)和脂肪酸的碱金属盐、碱土金属盐和铵盐,烷基磺酸盐,烷基芳基磺酸盐,烷基硫酸盐,月桂醚硫酸盐,脂肪醇硫酸盐,和硫酸化十六-、十七-和十八烷酸盐,硫酸化脂肪醇乙二醇醚,此外还有萘或萘磺酸与苯酚和甲醛的缩合物,聚氧乙烯辛基苯基醚,乙氧基化异辛基酚,辛基酚,壬基酚,烷基苯基聚乙二醇醚,三丁基苯基聚乙二醇醚,三硬脂基苯基聚乙二醇醚,烷基芳基聚醚醇,醇和脂肪醇/氧化乙烯缩合物,乙氧基化蓖麻油,聚氧乙烯烷基醚,乙氧基化聚氧丙烯,月桂醇聚乙二醇醚缩醛,山梨醇酯、木素亚硫酸盐废液和蛋白质,变性蛋白,多糖(例如甲基纤维素),疏水改性淀粉,聚乙烯醇(型,Clariant,瑞士),聚羧酸盐(型,BASF,德国),聚烷氧基化物,聚乙烯胺(型,BASF,德国),聚乙烯吡咯烷酮及其共聚物。
可加入杀菌剂以用于组合物的防腐和稳定。合适杀菌剂的实例为基于双氯酚和苄醇半缩甲醛的那些(ICI的或Thor Chemie的RS和Rohm & Haas的MK)和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)。合适防冻剂的实例为乙二醇、丙二醇、尿素和甘油。消泡剂的实例为硅酮乳液(例如SRE,Wacker,德国或Rhodia,法国)、长链醇、脂肪酸、脂肪酸盐、含氟有机化合物及其混合物。
着色剂的实例为染料或颜料,例如若丹明B、C.I.颜料红112、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112、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、苋菜红、苋菜红铝色淀、赤藓红、赤藓红铝色淀、胭脂红、焰红染料、玫瑰红、acid eed、酒石黄、酒石黄铝色淀、日落黄FCF、日落黄FCF铝色淀、坚牢绿FCF、坚牢绿FCF铝色淀、亮蓝FCF、亮蓝FCF铝色淀、靛蓝胭脂红、靛蓝胭脂红铝色淀、β-胡萝卜素、叶绿素铜。
本发明进一步涉及一种本发明凝胶。所述凝胶包含C1-C10羧酸和如上所述增稠剂。
一种制备本发明分配器的方法,其包括:
a)将C1-C10羧酸与增稠剂混合,和
b)将步骤a)的混合物填充至所述分配器中。
优选步骤a)包括将所述增稠剂与所述C1-C10羧酸在低于35℃的温度下混合。
优选步骤a)包括:
a1)将C1-C10羧酸与糖混合,和
a2)将所述增稠剂加入a1)的混合物中。
为了更容易地在步骤b)中将所述混合物填入分配器中,可将所述混合物加热至高达90℃,优选高达60℃。
步骤a)的混合物通常包含基于步骤a)中所得混合物的总重量为15-85重量%的纯C1-C10羧酸,更优选35-65重量%,甚至更优选45-55重量%。所述C1-C10羧酸可作为纯化合物或优选作为水溶液加入。更优选所述C1-C10羧酸作为70-99重量%,更优选80-97重量%的甲酸水溶液加入。
步骤a)的混合物通常包含基于步骤a)中所得混合物的总重量为1-50重量%的增稠剂,更优选5-40重量%,甚至更优选20-30重量%。如果所述增稠剂包含水分,则所述浓度涉及增稠剂的干重。
步骤a)的混合物任选包含基于步骤a)中所得混合物的总重量为1-50重量%的糖,更优选3-30重量%,甚至更优选10-20重量%。
步骤a)的混合物通常包含基于凝胶的总重量为至多100重量%的水。
本发明进一步涉及一种防治蜂巢中的螨的方法,包括将本发明分配器置于蜂巢内部或附近,优选内部。术语“蜂巢”对应于所有用于保存蜜蜂(包括蜂王的交尾)的装置。施用时间基于已广为人知的有害生物综合治理原则。优选的施用时间为在蜜蜂采蜜期间(例如当贮蜜箱(用于储存蜂蜜的木箱)置于蜂巢上时)。通常每次处理和每个蜂巢使用10-500g,优选50-300g的量的凝胶。所述量取决于蜂巢的尺寸且可容易地由本领域技术人员根据需要采用。
本发明还涉及本发明分配器在防治蜂巢中的螨中的用途。
本发明还涉及本发明分配器或本发明凝胶在农业、工业或家庭环境中防治螨中的用途。
本发明进一步涉及一种防治蜂巢中的孢子虫的方法,包括将本发明分配器置于蜂巢内部或附近,优选内部。施用时间基于已广为人知的有害生物综合治理原则。孢子虫(也称为小孢子虫病)是养蜂业中公知的病害。孢子虫的侵染通常是由微孢子虫蜜蜂微孢子虫(Nosema apis)或东方蜜蜂微孢子虫(Nosema ceranae)所导致的(Bourgeois等,Journal of InvertebratePathology,2010,103,53-58)。由WO2005/110384中已知例如用包含乙酰水杨酸或抗生素烟曲霉素防治蜜蜂中的孢子虫。
本发明还涉及本发明分配器在防治蜂巢中的孢子虫中的用途。
本发明还涉及本发明分配器或本发明凝胶在防治农业、工业或家庭环境中的孢子虫中的用途。
本发明的优点在于其显著提高了蜂群的健康。例如可有效地防治瓦螨。所述分配器可容易地由养蜂人处理,因为腐蚀性甲酸被很好地保护于分配器内部。由于存在容许甲酸可控扩散的特定聚酯膜,无需在甲酸垫料中冲孔或切缝以释放甲酸。本发明的另一优点是其可在全年,甚至在炎热的夏季月份也可施用。所述凝胶对蜜蜂是无毒的。所述装置和/或凝胶是可生物降解的。又一优点是避免了用于防治孢子虫的抗生素。
下文本发明实施例进一步阐述了本发明,但本发明不限于这些实施例。
实施例
实施例1:甲酸凝胶的制备
将甲酸溶液(56.9重量份的85重量%水溶液;相当于48.4重量份纯甲酸)加热至40-50℃。加入颗粒状蔗糖(16.1重量份)并搅拌直至溶解。将甲酸/蔗糖溶液冷却。加入(任选加入食品染料)粉状玉米淀粉(27.0重量份;水分含量10重量%)并混合。将溶液冷却直至形成糊。
实施例2:囊的制备
然后将实施例1制备的糊计量(50g、100g、150g或200g)并倾入或泵入可透膜囊中。使用蒸气可透膜囊以包封凝胶。将该囊密封并将所述糊挤压成型为条。将所述条包装于外袋中并置于HDPE桶中储存。在室温下会形成非常硬的半透明凝胶,基本为固态。如果通过加热将其液化(例如至多100℃),则其在室温下恢复成硬凝胶。
所述囊由可生物降解的聚酯膜制成,其由脂族-芳族共聚酯(1,4-丁二醇、己二酸和对苯二甲酸的缩聚物,通过DSC测定其熔点为110-120℃;通过ISO 527测定其拉伸强度为34N/mm2;通过ISO 527测定其极限伸长率(MD)为560%;通过DIN 53122测定其水渗透率为140g/(m2·d))制成。所述膜的膜厚度为32μm。
实施例3:田间试验(佛罗里达)
34个蜜蜂群中的功效和群体健康试验于2009年3-4月在Gainesville,佛罗里达进行,处理施用后进行为期一个月的后续评估。
当群体在蜂团区域内接纳有单个200g囊(如实施例2所制备)时,瓦螨水平降低至远低于处理阈值并保持那样。在至少4个月内无需设计进一步的处理。群体健康完全没有显示出受到影响。
甲酸以使得其在72小时结束时由初始的48.4重量%降至10重量%浓度的速率由囊扩散至群体区域中。该递送体系完全可堆肥且蜜蜂可通过咀嚼将其除去。养蜂人无需冒着危害其健康的风险移除废弃产物。
实施例4:田间试验(加拿大)
12个蜂群中的应力和群体健康试验于2009年5月在Frankford,安大略省进行。对该群体施用多达3次的200g囊(如实施例2所制备)。在最初24小时内打开入口渐缩管(entrance reducer)并置于群体上,然后移除。在试验中,7个蜂巢施用200g处理的1.5倍、2倍和3倍,加上1个不具有入口减缩器的经200g水平处理的蜂巢。四个群体为不具有入口渐缩管的未处理对照例。
蜂王都很健康。一些较小的幼虫损害,成蜂死亡率以较高量发生,但如果在试验开始时将入口减缩器关闭,则这可缓解。群势对结果没有影响。
在施用以后一星期检查雄蜂幼虫:将具有封盖雄蜂幼虫的蜂巢放置于平坦清洁的表面上。用蜜盖叉将封盖雄蜂幼虫水平刺穿并举起。幼虫显示为健康的。有时在蛹上看见死亡瓦螨。当缓慢转动框架以使得拉出雄蜂幼虫的一面现在朝下面向平坦表面并突然摇动时,死亡瓦螨落下。其中一些仅剩空壳。
携播螨(Phoretic Varroa):在试验中在群体上实施醇洗(3个具有幼虫的框架由幼虫巢穴中心摇到桶中,200-300只蜜蜂/试样,12个群体)。处理的群体在处理后没有出现任何瓦螨。与此相对照,瓦螨存在于对照蜂巢的醇洗液中。
当在200g推荐剂量的至多三倍下测试时,甲酸软糖配制剂不能成功杀灭蜂王,即使在最初24小时内入口降至越冬尺寸下。当携播和处于化蛹雄蜂上时,瓦螨显示出对处理高度敏感。
实施例5:田间试验(法国)
选择39个蜂巢(每个具有13个蜂巢的3个养蜂场,每种模式下使用4-5个蜂巢,每个蜂巢具有约35,000只蜜蜂)用于该试验,该试验于8月至10月在法国进行。邻近区域的主要开花作物为苜蓿。将甲酸囊施用于两种模式中:装有贮蜜箱的蜂巢内部,和不具有贮蜜箱的蜂巢内部。在这两种模式中,在0天时(D0)将各自为100g的三个囊(总剂量300g)置于巢脾顶部,然后在三天后(D+3)除去。在每个养蜂场中,将4-5个蜂巢用作对照。它们未用所述囊处理,但在相同条件下进行试验以用于对比。由这些群体得出证实试验性能的数据。
模式的描述和识别:
模式1:不具有贮蜜箱的对照蜂巢(非本发明)
模式2:具有贮蜜箱的处理蜂巢(3囊/蜂巢)
模式3:不具有贮蜜箱的处理蜂巢(3囊/蜂巢)
在蜂巢中施用囊后28天期间,没有发现对群势和发育的不利影响。
A)瓦螨死亡率的评估
瓦螨死亡率用在粘板上计数的方法评估。记录在D-3、D0(囊的施用日)、D+3、D+7、D+10、D+13、D+16、D+19和D+22天进行(参见表1)。在未处理模式(#1)下,粘板上螨虫数量在D0至D+22期间非常平稳。在处理模式(#2和3)下,在D0天施用囊引发D+3天的瓦螨死亡率峰值。对瓦螨死亡率的影响持续至D+13。在试验结束时(D+22),两种处理模式的平均瓦螨死亡率低于未处理的那些。在三个养蜂场中两个中,“具有贮蜜箱”的模式(#2)的瓦螨死亡率高于“不具有贮蜜箱”的模式(#3)中所记录的死亡率。蜂巢上的贮蜜箱的存在似乎提高了试验项目的功效。这可通过当将蜜蜂置于蜂巢与贮蜜箱之间时,蜜蜂与囊之间的接触增加而解释。
粘板法:将板用油脂覆盖并粘面朝上地放置在用于瓦螨计数的具体蜂巢底板(栅格底板)下。在3-4天后将板滑出并直接计数自然掉落的螨并除去。
表1:通过粘板法测定的平均掉落的瓦螨
日期 | 模式1a) | 模式2 | 模式3 |
D-3 | 4.3 | 5.3 | 4.4 |
D-3 | 13.9 | 22.8 | 17.3 |
D0 | 43.9 | 39.9 | 39.9 |
D+3 | 43.3 | 568.2 | 488.6 |
D+7 | 46.0 | 183.9 | 181.6 |
D+10 | 54.0 | 135.6 | 93.9 |
D+13 | 38.4 | 112.3 | 75.6 |
D+16 | 79.0 | 54.7 | 50.5 |
D+19 | 30.2 | 36.8 | 66.5 |
D+22 | 47.0 | 18.8 | 26.0 |
D+28 | 10.6 | 0.5 | 1.1 |
a)对照模式,非本发明。
B)侵染水平
蜜蜂的侵染水平用醇洗法在D-3和D+28天评估(表2)。未处理模式下的侵染平均由4%受侵染蜜蜂升高至10%的受侵染蜜蜂。在“具有贮蜜箱”的模式2(平均96.5%功效)下和“不具有贮蜜箱”的模式3(平均89.5%功效)下,功效优异。功效用Henderson和Tilton公式计算:100×(1-(Pt×Ta)/(Pa×Tt)),其中Pa=处理模式下施用前的%侵染;Pt=处理模式下施用后的%侵染;Ta=未处理模式下施用前的%侵染;Tt=未处理模式下施用后的%侵染。
醇洗法:将蜂巢打开并取样一满杯成蜂(约300只蜜蜂),放入充有一半约50%醇溶液的瓶中。将瓶温和摇动,然后将内容物在滤筛中过滤以保留蜜蜂。螨通过滤筛,然后保留在细网筛上以进行计数。
表2:通过醇洗法测定的平均侵染水平
日期 | 模式1a) | 模式2 | 模式3 |
D-3 | 4.3 | 5.3 | 4.4 |
D+28 | 10.6 | 0.5 | 1.1 |
功效[%] | 0.0 | 96.5 | 89.5 |
a)对照模式,非本发明。
C)幼虫中的瓦螨
在施用后第三天(D+3),在每个蜂巢中对幼虫试样进行取样以评估每只蜜蜂幼虫和每只雄蜂幼虫的瓦螨数。不幸的是,出于后一季节(8月)的原因,雄蜂幼虫减少或缺失。平均数据列于表3中。
在未处理模式(#1)下,幼虫试样上的计数显示每100只蜜蜂幼虫上具有相同数量的存活或死亡瓦螨(分别为5.1和5.6),并且显示出雄蜂幼虫上的存活瓦螨比死亡瓦螨稍多(分别0.4和1.9)。
在处理模式(#2和3)下,在蜜蜂幼虫上观察到多得多的死亡瓦螨:在“具有贮蜜箱”的模式下,每100只蜜蜂幼虫上具有约21只死螨和1只活螨,在“不具有贮蜜箱”的模式下每100只蜜蜂幼虫上具有约11只死螨。对于雄蜂幼虫,观察到死螨比活螨多约2倍。
表3:蜜蜂和雄蜂幼虫上瓦螨的平均数
模式 | 1a) | 2 | 3 | |
每100只蜜蜂幼虫 | 死亡 | 5.1 | 21.6 | 11.6 |
存活 | 5.6 | 1.0 | 1.2 | |
每20只雄蜂幼虫 | 死亡 | 0.4 | 3.1 | 2.2 |
存活 | 1.9 | 1.3 | 1.2 |
a)对照模式,非本发明。
D)孢子虫分析
在每种模式下,在施用日(D0)和施用后三天(D+3)在蜂巢的正前方捕捉25只外勤蜂。将蜜蜂冷冻直至进行孢子虫孢子分析。与模式1的未处理对照蜂巢相比,模式2和模式3的处理蜂巢的孢子水平要低得多。
Claims (22)
1.一种填充有包含C1-C10羧酸和增稠剂的凝胶的分配器,其包含聚酯膜,其中所述聚酯为半芳族共聚酯。
2.根据权利要求1的分配器,其中所述增稠剂为选自淀粉、改性纤维素、琼脂、果胶、藻酸盐或基于多糖的天然树胶的多糖。
3.根据权利要求1的分配器,其中所述增稠剂为天然淀粉。
4.根据权利要求1-3中任一项的分配器,其中所述分配器为由膜制成的囊。
5.根据权利要求1-3中任一项的分配器,其中所述凝胶包含至少5重量%增稠剂。
6.根据权利要求4的分配器,其中所述凝胶包含至少5重量%增稠剂。
7.根据权利要求1-3中任一项的分配器,其中所述聚酯包含聚合形式的1,4-丁二醇、己二酸和对苯二甲酸。
8.根据权利要求6的分配器,其中所述聚酯包含聚合形式的1,4-丁二醇、己二酸和对苯二甲酸。
9.根据权利要求1-3中任一项的分配器,其中所述聚酯膜结合至涂覆基质上。
10.根据权利要求8的分配器,其中所述聚酯膜结合至涂覆基质上。
11.根据权利要求1-3中任一项的分配器,其中所述凝胶包含选自单糖或二糖或其混合物的糖。
12.根据权利要求10的分配器,其中所述凝胶包含选自单糖或二糖或其混合物的糖。
13.根据权利要求1-3中任一项的分配器,其中所述羧酸为甲酸、乙酸、草酸、苹果酸、酒石酸、羟基乙酸、乳酸、柠檬酸、扁桃酸或其混合物。
14.根据权利要求12的分配器,其中所述羧酸为甲酸、乙酸、草酸、苹果酸、酒石酸、羟基乙酸、乳酸、柠檬酸、扁桃酸或其混合物。
15.根据权利要求11的分配器,其中所述凝胶包含至少3重量%所述糖。
16.根据权利要求12的分配器,其中所述凝胶包含至少3重量%所述糖。
17.一种制备根据权利要求1-16中任一项的分配器的方法,包括:
a)将C1-C10羧酸与增稠剂混合,和
b)将步骤a)的混合物填充至分配器中。
18.根据权利要求17的方法,其中步骤a)包括将所述增稠剂与C1-C10羧酸在低于30℃的温度下混合。
19.一种防治蜂巢中的螨的方法,包括将根据权利要求1-16中任一项的分配器置于蜂巢内部或附近。
20.根据权利要求1-16中任一项的分配器在农业、工业或家庭环境中防治螨中的用途。
21.一种防治蜂巢中的孢子虫的方法,包括将根据权利要求1-16中任一项的分配器置于蜂巢内部或附近。
22.根据权利要求1-16中任一项的分配器在农业、工业或家庭环境中防治孢子虫中的用途。
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2010
- 2010-09-01 CN CN201080040662.1A patent/CN102647911B/zh active Active
- 2010-09-01 AU AU2010294356A patent/AU2010294356B2/en active Active
- 2010-09-01 US US13/395,142 patent/US9101132B2/en not_active Expired - Fee Related
- 2010-09-01 EP EP10747637.6A patent/EP2498614B1/en active Active
- 2010-09-01 BR BR112012005583-6A patent/BR112012005583A2/pt not_active Application Discontinuation
- 2010-09-01 WO PCT/EP2010/062776 patent/WO2011029754A2/en active Application Filing
- 2010-09-01 ES ES10747637.6T patent/ES2659350T3/es active Active
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Also Published As
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WO2011029754A3 (en) | 2011-12-22 |
CN102647911A (zh) | 2012-08-22 |
WO2011029754A2 (en) | 2011-03-17 |
AU2010294356B2 (en) | 2014-12-04 |
EP2498614A2 (en) | 2012-09-19 |
US9101132B2 (en) | 2015-08-11 |
ES2659350T3 (es) | 2018-03-14 |
US20120171268A1 (en) | 2012-07-05 |
CA2772986C (en) | 2017-11-28 |
AU2010294356A1 (en) | 2012-04-12 |
BR112012005583A2 (pt) | 2020-11-03 |
CA2772986A1 (en) | 2011-03-17 |
EP2498614B1 (en) | 2017-11-15 |
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