CN106028820A - 高负载拟除虫菊酯包封的种子处理制剂 - Google Patents
高负载拟除虫菊酯包封的种子处理制剂 Download PDFInfo
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical group COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
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- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 description 1
- LMNZTLDVJIUSHT-UHFFFAOYSA-N phosmet Chemical compound C1=CC=C2C(=O)N(CSP(=S)(OC)OC)C(=O)C2=C1 LMNZTLDVJIUSHT-UHFFFAOYSA-N 0.000 description 1
- RGCLLPNLLBQHPF-HJWRWDBZSA-N phosphamidon Chemical compound CCN(CC)C(=O)C(\Cl)=C(/C)OP(=O)(OC)OC RGCLLPNLLBQHPF-HJWRWDBZSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- NAYYNDKKHOIIOD-UHFFFAOYSA-N phthalamide Chemical class NC(=O)C1=CC=CC=C1C(N)=O NAYYNDKKHOIIOD-UHFFFAOYSA-N 0.000 description 1
- 150000004885 piperazines Chemical class 0.000 description 1
- 229960005235 piperonyl butoxide Drugs 0.000 description 1
- YFGYUFNIOHWBOB-UHFFFAOYSA-N pirimicarb Chemical compound CN(C)C(=O)OC1=NC(N(C)C)=NC(C)=C1C YFGYUFNIOHWBOB-UHFFFAOYSA-N 0.000 description 1
- QHOQHJPRIBSPCY-UHFFFAOYSA-N pirimiphos-methyl Chemical group CCN(CC)C1=NC(C)=CC(OP(=S)(OC)OC)=N1 QHOQHJPRIBSPCY-UHFFFAOYSA-N 0.000 description 1
- 239000005648 plant growth regulator Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000205 poly(isobutyl methacrylate) Polymers 0.000 description 1
- 229920000196 poly(lauryl methacrylate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920000184 poly(octadecyl acrylate) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000197 polyisopropyl acrylate Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000182 polyphenyl methacrylate Polymers 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 235000021039 pomes Nutrition 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000473 propyl gallate Substances 0.000 description 1
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- DDIQWGKUSJOETH-UHFFFAOYSA-N pyrafluprole Chemical compound ClC=1C=C(C(F)(F)F)C=C(Cl)C=1N1N=C(C#N)C(SCF)=C1NCC1=CN=CC=N1 DDIQWGKUSJOETH-UHFFFAOYSA-N 0.000 description 1
- AEHJMNVBLRLZKK-UHFFFAOYSA-N pyridalyl Chemical group N1=CC(C(F)(F)F)=CC=C1OCCCOC1=C(Cl)C=C(OCC=C(Cl)Cl)C=C1Cl AEHJMNVBLRLZKK-UHFFFAOYSA-N 0.000 description 1
- MIOBBYRMXGNORL-UHFFFAOYSA-N pyrifluquinazon Chemical compound C1C2=CC(C(F)(C(F)(F)F)C(F)(F)F)=CC=C2N(C(=O)C)C(=O)N1NCC1=CC=CN=C1 MIOBBYRMXGNORL-UHFFFAOYSA-N 0.000 description 1
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 description 1
- JYQUHIFYBATCCY-UHFFFAOYSA-N quinalphos Chemical compound C1=CC=CC2=NC(OP(=S)(OCC)OCC)=CN=C21 JYQUHIFYBATCCY-UHFFFAOYSA-N 0.000 description 1
- 229950010630 quintiofos Drugs 0.000 description 1
- 108020003175 receptors Proteins 0.000 description 1
- 102000005962 receptors Human genes 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- MSHXTAQSSIEBQS-UHFFFAOYSA-N s-[3-carbamoylsulfanyl-2-(dimethylamino)propyl] carbamothioate;hydron;chloride Chemical compound [Cl-].NC(=O)SCC([NH+](C)C)CSC(N)=O MSHXTAQSSIEBQS-UHFFFAOYSA-N 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 231100000161 signs of toxicity Toxicity 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 229960003885 sodium benzoate Drugs 0.000 description 1
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
- 235000010334 sodium propionate Nutrition 0.000 description 1
- 239000004324 sodium propionate Substances 0.000 description 1
- 229960003212 sodium propionate Drugs 0.000 description 1
- 229940001482 sodium sulfite Drugs 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229940014213 spinosad Drugs 0.000 description 1
- CLSVJBIHYWPGQY-GGYDESQDSA-N spirotetramat Chemical compound CCOC(=O)OC1=C(C=2C(=CC=C(C)C=2)C)C(=O)N[C@@]11CC[C@H](OC)CC1 CLSVJBIHYWPGQY-GGYDESQDSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004548 suspo-emulsion Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- UBCKGWBNUIFUST-YHYXMXQVSA-N tetrachlorvinphos Chemical compound COP(=O)(OC)O\C(=C/Cl)C1=CC(Cl)=C(Cl)C=C1Cl UBCKGWBNUIFUST-YHYXMXQVSA-N 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- AMFGTOFWMRQMEM-UHFFFAOYSA-N triazophos Chemical compound N1=C(OP(=S)(OCC)OCC)N=CN1C1=CC=CC=C1 AMFGTOFWMRQMEM-UHFFFAOYSA-N 0.000 description 1
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 239000004061 uncoupling agent Substances 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000000664 voltage gated sodium channel blocking agent Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- 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
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- 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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
-
- 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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
包含多个微胶囊的杀虫剂组合物,其中每一微胶囊包括包封含拟除虫菊酯的核的外部聚合物壳。
Description
相关申请的交叉参考
本申请要求2014年02月19日提交的美国临时申请号61/941,943的优先权,其全文通过引用结合于此。
发明领域
本发明涉及农用化学品组合物和制剂领域。具体来说,本发明提供包含微米尺寸或纳米尺寸胶囊的杀虫制剂,以及制备它们用于用作种子处理物的方法。
背景技术
使用农作物保护剂处理农作物植物、草和草皮,从而控制害虫诱导的对农作物、草和草皮的损坏是非常重要的。已在制药、特种化学品和农业工业中描述了使用微胶囊来用于缓慢或受控地或者快速或迅速释放液体、固体和溶解于溶剂中或悬浮于溶剂中的固体。在农业中,这些释放技术改善了活性剂的效率和递送。
一般来说,捕获的材料的扩散是胶囊壁和其孔隙率以及周围介质和环境影响的函数。因此,通过改变壁中的交联,微胶囊可设计成受控地将材料释放到周围介质,或者遵循延迟的或受控的释放形式。此外,微胶囊壁可用作将与水互溶的液体分散进入水介质以易于输送的阻挡层。这样,在控制农耕计划的产出时,微观包封的活性成分(ai)提供显著的益处。
但是,在制备微胶囊技术中的至少一个缺陷与不良的装载容量有关。换句话说,不能容易地将有效量的活性成分进行包封以提供其预期的应用。通常,活性成分的较低装载无法支持用于制备微观包封杀虫剂的经济性。因此,仍然需要在微胶囊制剂中装载杀虫剂的更有效的方法。另一方面,高装载的活性物质将通常增加产品的毒性水平,因此使得监管标签被归类于不理想的类别。
用于农业作物的种子组合物也是已知的。但是,许多种子处理基于具有某些不利特征的组合物,且在现代农业中,可称作非环境友好。例如,引起溢流的组合物导致环境问题,例如地下水的富营养化、硝酸盐污染、磷酸盐污染等,不尽人意。而在另一方面,在工业中不同参与者担心低效活性成分装载、高制造成本和损坏种子处理设备等。
甚至当进行组合时,现有技术也没有给本领域普通技术人员提供制备革新性制剂以解决工业担心的任何有用信息,也没有暗示制剂的高效率,其令人惊讶地优于现今可得的组合和种子处理选择。本发明针对满足这些需求,并克服工业所面临的两难境地。
发明内容
本发明涉及杀虫组合物,特别是用聚合物壳包封的液体杀虫材料,与现有技术的对应杀虫组合物相比,本发明的杀虫组合物提供多种益处。此外,本发明涉及用于制备这种微胶囊的方法,包括中间方法,及其应用方法。虽然无意受限于任何理论,但本发明的另一方面是提供可解决现有技术中不足的种子处理组合物。
在本发明的一方面中,描述了微胶囊,其包含包封活性杀虫剂的聚合物壁。在该实施方式中,微胶囊包含多层或单层设计的壳。外部聚合物壳包含可生物降解的至少一种聚合物。在至少一个实施方式中,聚合物壳包含选自下组的聚合物:聚脲、聚氨酯、聚酰胺、聚酯等。
本发明的至少另一个方面描述液体农业制剂,其包含多个微胶囊,所述微胶囊在合适的溶剂中包封除虫菊酯(pyrethrin)或合成拟除虫菊酯(pyrethroid)杀虫剂。在一种实施方式中,杀虫剂是选自下组的拟除虫菊酯:联苯菊酯、ζ-氯氰菊酯、α-氯氰菊酯、苄氯菊酯(permethrin)、λ-氯氟氰菊酯和七氟菊酯。在一个更优选的实施方式中,所述杀虫剂是联苯菊酯。在另一种实施方式中,本发明涉及多个微胶囊,其中每一微胶囊包含外部聚合物壳,所述外部聚合物壳包封含联苯菊酯的液体或固体核。在一种实施方式中,所述制剂还包含溶剂、共溶剂、油、乳化剂、粘度改性剂、消泡剂、胺和pH改性剂。
在本发明的另一方面中,微胶囊具有0.1-500微米的直径尺寸。在更优选的实施方式中,制剂中至少90%的微胶囊具有0.5-50微米的直径。在另一种实施方式中,至少90%的微胶囊具有1-50微米的直径。
本发明的另一方面包括提供高负载和高效杀虫剂制剂的方法。根据本发明的另一种实施方式,发明人开发了可用于递送基本上不溶于水或不溶于水的杀虫剂以及其它活性成分的组合物,所述其它活性成分选自下组:杀节肢动物剂(arthropodicide)、杀虫剂、杀螨药(miticide)、杀螨剂(acaricide)、杀线虫剂(nematocide)、杀真菌剂(fungicide)、选择性除草剂、植物生长调节剂或这些生物活性物质中两种或更多种的组合。
本发明的另一方面涉及制备含高负载杀虫剂的微胶囊组合物的方法。在至少一个实施方式中,通过下述步骤来制备高负载杀虫剂微胶囊:(a)混合农用化学品与有机溶剂、至少一种单体和油,以制备有机混合物相,(b)在水性溶剂中溶解有效量的乳化剂、聚乙烯醇和增稠剂,以形成水相,和(c)在均质器中匀化有机相与水相,和(d)使界面聚合进行足够的时间段。在更优选的实施方式中,在25℃-约65℃的温度下进行界面聚合。
在本发明的另一方面中,可将本发明的微胶囊组合物作为种子处理组合物直接施加到种子,由此与其它种子处理组合物相比,预料之外地产生显著更高的农作物产率。这种农作物可包括小麦、玉米、大麦、大豆、谷物、柑橘、可可(cocoas)、椰子、咖啡、玉米、棉花、纤维作物、花卉、饲料作物(forge corp)、林业、落花生(groundnut)、花生(peanut)、啤酒花、园艺、非陆地作物(non-land crop)、油棕、油菜、豌豆、梨果(pomes)、土豆、水稻、核果(stonefruit)、香料、甘蔗向日葵、茶、烟草、番茄、树生坚果(tree nut)、草皮(turf)、蔬菜作物、藤本植物(vine)和葡萄等。
附图简述
图1(A)-(D)是联苯菊酯CS制剂微胶囊的示例性SEM图像。
图1(E)-(F)是在处理的玉米种子上的联苯菊酯CS制剂的微胶囊的示例性SEM图像。
图1(G)是在处理的小麦种子上的联苯菊酯CS制剂的微胶囊的示例性SEM图像。
图2(A)-(B)是使用高负载联苯菊酯CS制剂(左)和联苯菊酯SC制剂(右)处理的玉米种子的光学照片。
图3(A)-(B)是使用高负载联苯菊酯CS制剂(左)和高负载联苯菊酯SC制剂(右)处理的小麦种子的光学照片。
图4(A)-(B)显示使用高负载联苯菊酯CS制剂(左)和高负载联苯菊酯SC制剂(右)处理小麦种子之后,海格(Hege)处理器的鼓表面。
图5(A)-(B)显示使用高负载联苯菊酯CS制剂(左)和高负载联苯菊酯SC制剂(右)处理玉米种子之后,海格(Hege)处理器的鼓表面。
图6提供生物田野试验数据,其显示植物计数随处理的变化。
优选实施方式详述
本发明满足用于农作物处理的高负载杀虫剂微观包封制剂的需求。因此,通过下述描述了高度精确地施加农业活性成分:提供制剂,其能将活性高至少5-48倍的的活性成分递送到感兴趣的位置。本发明描述杀虫剂组合物,其用于递送容纳在具有聚合物壳的微胶囊之内的水溶性活性剂。聚合物壳可为可生物降解的聚合物,其任选地在交联剂存在下是交联的。在一种实施方式中,微胶囊包含基本上不溶于水的杀虫剂化合物,其悬浮成水包油乳液。
如本文所使用,术语“微胶囊”指球形微观颗粒,其由作为成壁材料的聚合物壳以及位于壳之内的包封的活性物质组成。这个术语与分散在溶剂中的活性物质或聚合物的其它球形颗粒不同。本发明的微胶囊可由单一聚合物壳组成或为单一层,其中活性物质位于微胶囊的内核或中心之内。本发明的微胶囊还可指“多层微胶囊”,其由内核微胶囊和一个或多个外部聚合物壳组成。在任一情况下,本发明的微胶囊具有0.1微米-500微米的直径。
如本文所使用,术语“成壁聚合物”指聚合物或可聚合的单体单元或两种或更多种不同聚合物可聚合单体单元的组合,其形成微胶囊的外部壁或层或壳的组分。
术语“聚合物壳”指层,所述层包含成壁聚合物和任选的其它组分,例如增塑剂、油、成孔组分和/或矿物。
本发明的一方面涉及微胶囊,所述微胶囊包含包封杀虫剂的聚合物壳。本发明的第二方面涉及微胶囊,所述微胶囊包含(a)拟除虫菊酯,(b)油或溶剂,和(c)至少另一种活性成分。
在本发明的另一方面中,所述制剂包含多个微胶囊,其中至少一群微胶囊具有小于约500微米的有效粒度(D90);在一种实施方式中,D90小于约100微米,且又在另一种实施方式中,D90是最高达或小于20,18,15或10微米。在具体的实施方式中,微胶囊群具有约1-约7微米、优选2-6微米的通过D90限定的粒度。
在另一种实施方式中,上述微胶囊群中的每一微胶囊包含(a)杀虫剂,(b)一种或多种油组分,和(c)一种或多种粘度改性剂。在至少一个实施方式中,包含粘度改性剂有助于防止胶囊和其它悬浮的组分的沉降。选择粘度改性剂是本技术领域技术人员所公知的,且粘度改性剂可包含多种组分,包括但不限于凹凸棒石粘土、黄原胶和改性纤维素衍生物。在具体实施方式中,每一微胶囊包含联苯菊酯。在一种实施方式中,以最高达480克/升或比常规微观包封制剂更高约50%的量装载联苯菊酯比例。在另一种实施方式中,使用3号纺锤体,将最终产品的粘度调节到使用布氏(Brookfield)LVT旋转粘度计测量时的200-5000厘泊(mPa·s)的测量结果。
在本发明的一种实施方式中,存在的杀虫剂的总量是总制剂的约0.1重量%-约50重量%。在另一种实施方式中,存在的粘度改性剂是总制剂的约0.01重量%-约15重量%。
本发明的至少一个方面涉及可渗透固体的壳,其由通过异氰酸酯聚合制备的聚合物。在一种实施方式中,通过与异氰酸酯部分反应的表面改性化合物促进聚合。合适的异氰酸酯包括但不限于芳族异氰酸酯例如甲苯二异氰酸酯的异构体、苯二异氰酸酯的异构体和衍生物、联苯二异氰酸酯的异构体和衍生物、聚亚甲基聚亚苯基异氰酸酯(polymethylenepolyphenyleneisocyanate)(PMPPI)、含4,4'亚甲基双苯基异氰酸酯(Methylene bisphenyl isocyanate)的聚亚甲基聚苯基异氰酸酯;脂族异氰酸酯例如1,6-己二异氰酸酯(HMDI);环状脂族异氰酸酯例如异佛尔酮二异氰酸酯(isophoronediisocyanate)(IPDI)和HMDI的三聚体或它们的混合物。
在微胶囊壳的结构中,还可使用其它可生物降解的或不可生物降解的其它聚合物。它们包括合成纤维素或其它纤维素部分例如乙酸丁酸纤维素、乙酸邻苯二甲酸纤维素、羧乙基纤维素、三乙酸纤维素和纤维素硫酸钠盐(cellulose sulphate sodium salt);含酯的丙烯酸、甲基丙烯酸的聚合物或它们的共聚物或衍生物,聚(甲基丙烯酸甲酯)、聚(甲基丙烯酸乙酯)、聚(甲基丙烯酸丁酯)、聚(甲基丙烯酸异丁酯)、聚(甲基丙烯酸己酯)、聚(甲基丙烯酸异癸酯)、聚(甲基丙烯酸月桂酯)、聚(甲基丙烯酸苯酯)、聚(丙烯酸甲酯)、聚(丙烯酸异丙酯)、聚(丙烯酸异丁酯)、和聚(丙烯酸十八酯)、聚丙烯酸、聚(丁酸)、聚(戊酸)、和聚(丙交酯-共聚-己内酯)、它们的共聚物和共混物。
不可生物降解的聚合物的示例包括乙烯乙酸乙烯酯、聚(甲基)丙烯酸、聚酰胺、它们的共聚物和混合物。
可生物降解的聚合物的示例包括羟基酸例如乳酸和乙醇酸的聚合物,聚丙交酯、聚乙交酯、聚丙交酯共乙交酯,以及与PEG的共聚物、聚酸酐、聚(原酸)酯、聚氨酯、聚(丁酸)、聚(戊酸)和聚(丙交酯-共聚-己内酯)。
在至少一个实施方式中,本发明的微胶囊设计成在一时间段中缓慢释放核材料,或足够强烈释放,或经干燥再分散。一般来说,壁材料与微胶囊(核加上壁)的重量比例大于1重量%。通常,重量比例是1%-70%,或具体来说,3%-15%。
在另一种实施方式中,本发明的制剂包含成孔材料,其允许杀虫剂渗透出微胶囊。在一种实施方式中,异氰酸酯可与胺部分反应以形成聚脲或者与二-或三-甘醇反应以形成聚氨酯。在本文所述的方法中,异氰酸酯分子通常容纳在油相之内。可在油相中或在油-水界面处产生氨基团。可通过包含交联剂例如乙酸乙烯酯(acetic acid ethenyl ester)来实现交联。
在另一种实施方式中,描述了聚脲微胶囊。在至少一个实施方式中,微胶囊的壳是聚脲,其通过乳液聚合过程形成并与乙酸乙烯酯交联。在至少一种实施方式中,通过将乳液加热到升高的温度来引发成壁反应,在该温度下有些异氰酸酯基团在界面处水解以形成胺,其进而与未水解的异氰酸酯基团反应以形成聚脲微胶囊。
在至少一种实施方式中,以下述方式制备微胶囊:提供5纳米-1000纳米的微胶囊壳厚度。在更优选的实施方式中,微胶囊的壳壁厚是10-200纳米,或者15-100纳米,从而减少微胶囊在处理设备上累积的量。
在至少一种实施方式中,使得进行聚合反应,从而形成适用于本发明的预期目的的微胶囊壁厚。在一种实施方式中,改变油相中聚合的异氰酸酯的浓度以及其与胺部分的相关比例可得到不同的壁厚。例如,在至少一个实施例中,当油相中的含4,4'亚甲基双苯基异氰酸酯的聚亚甲基聚苯基异氰酸酯(27)浓度是3.9%且胺与27比例分别是0.89-1.0时,那么所得微胶囊的壁厚比其中27在油相中以7.5%的量存在时的情况下所得微胶囊的壁厚更小得多。类似地,改变胺:27比例影响最终壁厚。任何这种改变预料之外地得到独特的这种微胶囊的物理和物化性质,这种微胶囊根据活性成分的选择而定制。
在另一种实施方式中,可任选地使用分散剂来悬浮或溶解基本上不溶于水的活性剂。设想用于实施本发明的分散剂包含能悬浮或溶解活性杀虫剂但不与用于制备活性剂的聚合物或活性剂自身反应的任何非水相溶剂
这种溶剂的示例包括植物油例如大豆油、环氧大豆油、椰子油、橄榄油、红花(safflower)油、棉花籽油、玉米油、菜籽油等。其它这样的液体包括脂族、环脂族或芳族烃,例如十二烷、正癸烷、正己烷、环己烷、甲苯、苯等;以及,脂族或芳族醇,例如庚醇、辛醇等,或者它们中任意两种或更多种的组合。合适的溶剂的其它示例包括耗尽重质芳族萘的石油蒸馏物(阿拉马替克(Aromatic)200,100,150),其沸点是100℃-400℃。
在至少一种实施方式中,杀虫剂可为下述一组活性成分中的任一种:
A1)氨基甲酸酯类,包括涕灭威、棉铃威(alanycarb)丙硫克百威、甲萘威(carbaryl)、克百威、丁硫克百威(carbosulfan)、甲硫威、灭多威、杀线威、抗蚜威、残杀威和硫双威(thiodicarb);
A2)有机磷酸酯类,包括乙酰甲胺磷、益棉磷(azinphos-ethyl)、保棉磷(azinphos-methyl)、毒虫畏、毒死蜱、甲基毒死蜱、甲基内吸磷(demeton-S-methyl)、二嗪农、敌敌畏/DDVP、百治磷、乐果、乙拌磷、乙硫磷、杀螟硫磷、倍硫磷、异恶唑磷(isoxathion)、马拉硫磷、甲胺磷(methamidaphos)、杀扑磷、速灭磷、久效磷、氧乐果(oxymethoate)、甲基亚砜磷(oxydemeton-methyl)、对硫磷、甲基对硫磷、稻丰散(phenthoate)、甲拌磷、伏杀硫磷(phosalone)、亚胺硫磷、磷胺、甲基嘧啶磷、喹硫磷(quinalphos)、特丁硫磷、杀虫畏(tetrachlorvinphos)、三唑磷、敌百虫;
A3)环二烯有机氯化合物,例如硫丹(endosulfan);
A4)苯基吡唑(fiprole)类,其由下述组成:乙虫清(ethiprole)、氟虫腈(fipronil)、匹弗普罗(pyrafluprole)和哌普罗(pyriprole);
A5)新烟碱类,其由下述组成:啶虫脒、噻虫胺(chlothianidin)、呋虫胺(dinotefuran)、吡虫啉、烯啶虫胺(nitenpyram)、噻虫啉(thiacloprid)和噻虫嗪(thiamethoxam);
A6)多杀菌素类,例如多杀菌素(spinosad)和斯哌特姆(spinetoram);
A7)来自菌素(mectins)类的氯通道活化剂,其由下述组成:阿巴菌素、甲氨基阿维菌素-苯甲酸盐、双氢除虫菌素、勒皮菌素和弥拜菌素;
A8)仿生的保幼激素(juvenile hormone mimics),例如化保幼素(hydroprene)、丙诺保幼素(kinoprene)、美赐平(methoprene)、苯氧威和吡丙醚;
A9)选择性同翅类取食阻滞剂(selective homopteran feeding blockers),例如吡蚜酮(pymetrozine)、氟啶虫酰胺(flonicamid)和氟虫吡喹(pyrifluquinazon);
A10)螨生长抑制剂例如四螨嗪(clofentezine)、噻螨酮(hexythiazox)和乙螨酮(etoxazole);
Al1)线粒体ATP合酶的抑制剂,例如丁醚脲(diafenthiuron)、苯丁锡氧(fenbutatin oxide)和克螨特(propargite);氧化磷酸化的解偶联剂,例如虫螨腈(chlorfenapyr);
Al2)烟碱乙酰胆碱受体通道阻断剂,例如杀虫磺(bensultap)、杀螟丹盐酸盐(cartap hydrochloride)、杀虫环(thiocyclam)、杀虫双(thiosultap sodium);
A13)来自苯甲酰脲类的0型几丁质生物合成抑制剂,包括:双三氟虫脲(Bistrifluron)、二氟脲、氟虫脲、氟铃脲、虱螨脲、氟酰脲和氟苯脲;
A14)1型几丁质生物合成抑制剂,例如噻嗪酮(buprofezin);
A15)蜕皮干扰剂,例如灭蝇胺(cyromazine);
A16)蜕皮激素受体激动剂,例如甲氧虫酰肼(methoxyfenozide)、虫酰肼(tebufenozide)、氯虫酰肼(halofenozide)和环虫酰肼(chromafenozide);
A17)章鱼胺(octopamin)受体激动剂,例如双甲脒(amitraz);
A18)线粒体复合物电子转移抑制剂,哒螨灵(pyridaben)、吡螨胺(tebufenpyrad)、唑虫酰胺(tolfenpyrad)、嘧虫胺(flufenerim)、腈吡螨酯(cyenopyrafen)、丁氟螨酯(cyflumetofen)、伏蚁腙(hydramethylnon)、灭螨醌(acequinocyl)或嘧螨酯(fluacrypyrim);
A19)电压依赖性钠通道阻断剂,例如茚虫威(indoxacarb)和氰氟虫腙(metaflumizone);
A20)脂合成抑制剂,例如季酮螨酯(spirodiclofen)、螺甲螨酯(spiromesifen)和螺虫乙酯(spirotetramat);
A21)来自二酰胺类的雷诺定受体调节剂,包括:氟虫双酰胺、邻苯二甲酰胺化合物(R)-3-氯-N1-{2-甲基-4-[1,2,2,2-四氟1-(三氟甲基)乙基]苯基}-N2-(1-甲基-2-甲基磺酰基乙基)邻苯二甲酰胺和(S)-3-氯-N1-{2-甲基1-4[1,2,2,2-四氟-1-(三氟甲基)乙基]苯基}-N2-(1-甲基-2-甲基磺酰基乙基)邻苯二甲酰胺、氯虫酰胺(chlorantraniliprole)和氰虫酰胺(cyantraniliprole);
A22)作用模式未知或不确定的化合物,例如印苦楝子素、酰胺弗门特(amidoflumet)、联苯肼酯(Bifenazate)、联氟砜(fluensulfone)、胡椒基丁醚、啶虫丙醚、杀弗乐(Sulfoxaflor),或者
A23)来自拟除虫菊酯类的钠通道调节剂,包括氟酯菊酯、丙烯菊酯、联苯菊酯、氟氯氰菊酯、λ-氯氟氰菊酯、氯氰菊酯、α-氯氰菊酯、β-氯氰菊酯、ζ-氯氰菊酯、溴氰菊酯、顺式氰戊菊酯、醚菊酯、甲氰菊酯、氰戊菊酯、氟氰戊菊酯、τ-氟胺氰菊酯、氯菊酯、氟硅菊酯、七氟菊酯和四溴菊酯。
在一种实施方式中,拟除虫菊酯选自下组:联苯菊酯、ζ-氯氰菊酯、α-氯氰菊酯、氯菊酯(permethrin)、λ-氯氟氰菊酯和七氟菊酯。在至少一种实施方式中,拟除虫菊酯可以25%-60%重量/重量的量存在。在一种实施方式中,联苯菊酯的量是35%-50%重量/重量。
在另一种实施方式中,本发明的制剂还可包含消泡剂和制孔剂。
本发明的制剂还可包含分散剂、粘度改性剂、pH改性剂和/或防腐剂,它们的选择是本领域普通技术人员在制备分散体、悬浮乳剂(suspoemulsion)和其它类似产品时已知的。
合适的分散剂包含非离子和/或离子物质,例如来自下述类型:醇-POE和/或醇-POP醚,酸和/或POP POE酯,烷基芳基和/或POP POE醚,脂和/或POP POE加合物,POE-和/或POP-多元醇衍生物,POE-和/或POP-失水山梨醇或-糖加合物,烷基硫酸酯或芳基硫酸酯,烷基磺酸酯或芳基磺酸酯,和烷基磷酸酯或芳基磷酸酯,或相应的PO-醚加合物,和它们的混合物。烷基多聚葡萄糖苷和磷酸酯是优选的分散剂。
合适的防腐剂包括但不限于苯甲酸C12-C15烷基酯、对羟基苯甲酸烷基酯、芦荟提取物、抗坏血酸、苯扎氯铵、苯甲酸、C9-C15醇的苯甲酸酯、丁羟甲苯、叔丁基羟基茴香醚、叔丁基氢醌、蓖麻油、鲸蜡醇、氯甲酚、柠檬酸、可可油、椰子油、重氮烷基脲(diazolidinylurea)、己二酸二异丙基酯、二甲基聚硅氧烷、DMDM乙内酰脲、乙醇、乙二胺四乙酸,脂肪酸、脂肪醇、十六烷基醇、羟基苯甲酸酯、碘代丙炔基丁基氨基甲酸酯(iodopropynylbutylcarbamate)、异壬酸异壬酯、荷荷芭油、羊毛脂油、矿物油、油酸、橄榄油、尼泊金(paraben)、聚醚、聚环氧丙烷丁基醚、聚环氧丙烷鲸蜡基醚、山梨酸钾、没食子酸丙酯、硅酮油、丙酸钠、苯甲酸钠、亚硫酸氢钠、山梨酸、硬脂脂肪酸、二氧化硫、以及它们的衍生物、酯、盐和混合物。优选的防腐剂包含邻苯基苯酚钠,5-氯-2-甲基-4-异噻唑啉-3-酮,2-甲基-4-异噻唑啉-3-酮,和1,2-苯并异噻唑啉-3-酮(1,2-benzisothiazolin-3-one)。
合适的粘度改性剂包括但不限于甘油、角叉菜胶、黄原胶、瓜尔胶、阿拉伯胶(gum Arabic)、黄芪胶、聚环氧乙烷(polyox)、褐藻胶、凹凸棒石粘土、蒙脱土粘土和海藻酸钠。黄原胶是特别优选的。制剂中粘度增强剂的总浓度可占总制剂的0.01%-15%,更优选地0.1%-5%(重量/重量)。
合适的pH调节剂包括乙酸、盐酸、柠檬酸、磷酸、缓冲液等。
在更优选的实施方式中,微胶囊是核壳结构,其包含拟除虫菊酯例如联苯菊酯以及溶剂和农作物油的合适的组合。在该实施方式中,微胶囊的壳壁是聚脲(polyuria),其通过乳液聚合过程形成并与乙酸乙烯酯交联。交联剂是乙酸乙烯酯(聚乙烯醇和聚醋酸乙烯酯)。这种实施方式的至少一个另一方面是提供降低的口服毒性,同时增加操作者的安全。
现有技术中描述了制备聚合物微胶囊的各种方法。这种方法包括溶剂提取、热熔包封、溶剂蒸发和喷涂干燥。在优选的实施方式中,根据下面的一般步骤来制备本发明的微胶囊:(1)通过混合农用化学品与选定的溶剂/油来制备有机混合物相,(2)通过使用选定的表面活性剂、单体和其它添加剂来制备乳液,(3)添加单体来活化激活界面聚合,(4)以及使界面聚合进行足够量的时间,优选地在预定温度下和2-5的pH下进行5-24小时。在本发明的另一方面中,在25-65℃的温度下进行界面聚合。在更优选的实施方式中,在45℃-约60℃的温度下进行界面聚合。
在至少另一种实施方式中,联苯菊酯负载可为5%到最高达约48%。在优选的实施方式中,联苯菊酯可以最终产品中约10%,20%,30%,40%,50%或60%的量存在。在本发明的另一方面中,联苯菊酯负载的目标量是约300-约600克活性成分/升。
在至少一种示例性实施方式中,通过下述来制备有机混合物:混合熔融工业级联苯菊酯与预定量的玉米油、阿拉马替克200ND溶剂和27,在匀化之前将混合物保持在烘箱(65℃)中。以类似的方式,通过下述来制备水性混合物:在去离子水中溶解预定量的88B,24-203和S,将混合物保持在烘箱(65℃)中。然后,通过混合预定量的例如1,6-六亚甲基二胺与去离子水来制备胺溶液。然后,可使用PolytronPT6100均质器和PT-DA3030-6060分散集合器匀化产品:将有机混合物(I相)缓慢加入水性混合物(II相),在19K rpm下匀化2分钟。在下一步骤中,将胶囊浆料通过夹套(jacked)加入有夹套的反应器(温度设定为52℃)。然后,在200rpm下开始搅拌混合物,且缓慢地(逐滴)将胺溶液(III相)添加进而反应器中的浆料。混合物的搅拌应在52℃下继续5小时,然后将水浴温度设定到室温,并继续搅拌3小时。然后,使用85%磷酸或乙酸,将pH调节到中性。然后,添加其它成分例如Proxel GXL和Kelzan S(2%)/水,从而将粘度和活性负载调节到所需水平。在一种实施方式中,联苯菊酯:玉米油:阿拉马替克200ND的比例分别是81.5%:13.5%:4%,而在另一种实施方式中,该比例是87%:7.6%:5.4%。
在另一种实施方式中,本发明提供处理种子来保护种子免受昆虫和可能的其它害虫影响的方法。本发明的至少一个益处可在其操作影响和设备上来实现。本领域普通技术人员可理解由于在设备上的成分累积,联苯菊酯和其它杀虫剂会损坏设备。这种不足降低了操作效率。本领域普通技术人员可理解,与以常规悬浮液浓缩物的形式施加相反,包封联苯菊酯减少在处理设备上累积的量(参见图5(A)-(B))。在那种程度上,这种优势提供显著的操作效率。
在另一种实施方式中,本发明可用于保护农作物,例如小麦、玉米、大麦、大豆、谷物、柑橘、可可、椰子、咖啡、玉米、棉花、纤维作物、花卉、饲料作物、林业、落花生、花生、啤酒花、园艺、非陆地作物、油棕、油菜、豌豆、梨果、土豆、水稻、核果、香料、甘蔗、向日葵、茶、烟草、番茄、树生坚果、草皮、蔬菜作物、藤本植物和葡萄等。
在至少另一种实施方式中,与可比拟的常规悬浮液相比,本发明提供优异的毒性结果。这样,所要求保护的微观包封过程降低了制剂的毒性,由此不仅改善相对于消费者而言的安全性,还改善当地环境的安全性。
在至少另一种实施方式中,与含聚合物包封的杀虫剂的其它产品相比,本发明实现递送具有更高活性成分含量的产品。本领域普通技术人员可理解这种特征在种子处理操作中提供附加的益处,且显著降低包装要求。
在本发明的至少另一个方面中,提供包含种子和涂层的涂覆的种子,其中所述涂层是多个微胶囊,其中每一胶囊包括包封核的外部聚合物壳,所述核包括活性成分。在优选的实施方式中,这种活性成分是拟除虫菊酯联苯菊酯。在更优选的实施方式中,使用具有外部聚合物壳的微胶囊涂覆本发明的涂覆的种子,所述外部聚合物壳包括选自下组的至少一种聚合物:聚脲、聚氨酯、聚酰胺和聚酯。
在另一种实施方式中,本发明的涂覆的种子具有由聚脲制成的外部聚合物壳。又在另一种实施方式中,使用微胶囊涂覆本发明的涂覆的种子,所述微胶囊在其核中具有活性成分、溶剂和/或油。在另一种实施方式中,溶剂是选自下组的有机溶剂:石油(阿拉马替克200ND),或其它疏水性溶剂,且涂覆制剂还包含(a)共溶剂;(b)有效量的异氰酸酯;(c)分散剂;(d)聚乙烯醇;(e)粘度改性剂;(f)消泡剂(例如硅酮乳液混合物);(g)杀生物剂(例如1,3-苯并异噻唑-3-酮);(h)胺;和(i)pH改性剂。
通过下面的实施例进一步阐述本发明的组合物和方法。这些实施例只是用来说明本发明的具体实施方式,而不以任何方式对本发明的范围构成限制。批露的发明包含的其它改变对于本领域普通技术人员而言是显而易见的。所有这种改变都认为在如本发明的说明书和权利要求所限定的本发明的范围之内。
实施例
实施例1.制备高负载联苯菊酯微观包封的制剂的方法
表1列出了本发明的高负载微胶囊制剂的成分。制备高负载微胶囊的方法遵循下述一般步骤:(1)通过混合农用化学品与选定的溶剂/油来制备有机混合物相,(2)通过使用选定的表面活性剂、单体和其它添加剂来制备乳液,(3)添加单体来激活界面聚合,(4)在预设的温度和pH下,使界面聚合进行2-24小时。
步骤A-制备有机相
将35-48%重量/重量的工业级联苯菊酯与6.4%玉米油、2.7%阿拉马替克200ND溶剂(石油,耗尽重质芳烃、萘)以及2.0%的含4,4'亚甲基双苯基异氰酸酯的聚亚甲基聚苯基异氰酸酯。在匀化之前,随后将混合物保持在温度为65℃的烘箱中。所有重量测量都以重量百分数(%重量/重量)计。
步骤B-制备水性混合物
在高速下,将1.1%重量/重量的高度磺化的硫酸盐法木质素(Kraft lignin)(88B)与溶解于去离子水中的0.8%的24-203和0.05%的S进行混合,并保持在温度为65℃的烘箱中。
步骤C-匀化混合物
在19K rpm下,使用Polytron PT6100均质器和PT-DA3030-6060分散集合器将水性混合物和有机混合物缓慢混合2分钟。
步骤D-匀化后处理
然后,将混合物转移进入有夹套的反应器,该反应器设定为52℃且在200rpm下搅拌。将约70%的1,6六亚甲基二胺与去离子水的胺混合物缓慢加入到搅拌中的混合物。将混合物在52℃下继续搅拌至少2小时。然后,使用85%磷酸或乙酸,将混合物的pH调节到中性(约pH=7)。然后,在水中添加黄原胶(含0.5%1,3-苯并异噻唑-3-酮杀生物剂的水中的2%溶液),从而将粘度和活性物质负载调节到所需水平。
表1.高负载联苯菊酯微观包封制剂的示例
以与实施例1步骤A-D相同的方式制备额外制剂,并在下文的表2和3中总结。表2和3总结了与这些制剂相关的各种化学和物理性质。
表2.高负载联苯菊酯微观包封制剂的物理和化学性质:
表3.
毒性评估
如下文的表4所示,快速毒性研究表明微观包封的联苯菊酯相比高负载联苯菊酯制剂口服LD50毒性降低,这进而提供消费者和中间处理人员安全性的显著改善。
表4.毒性研究结果
实施例2:联苯菊酯种子处理对蛴螬(grub)和线虫损坏春小麦的影响。
首先,作为对照处理,通过在水中稀释杀真菌剂来制备种子处理组合物,浆化到325毫升/100千克,并与杀虫剂同时施加,杀虫剂也稀释到325毫升/100千克浆料。例外是与杀真菌剂进行槽混合,然后用水稀释到最终的325毫升/100千克的浆料速度。在海格处理器中处理种子。然后将以400克/升的包封的联苯菊酯和以550克/升包封的丁硫克百威用于与未包封的和其它市售产品比较种子处理的效率。下文的表5中提供了测试的比例(rate)和制剂。
表5:-测试处理
在田野实验中,在密耳福德淤泥质粘土壤土(Milford Silt Clay Loam)类土壤中的0.11英亩(acers)土地上对比包封和未包封处理的种子。还在相同环境中将包封和未包封处理的种子与未处理的种子进行对比。在田野实验中,以1英寸的深度种植24颗种子/英尺/排(约110磅种子/英亩)。测试的农作物是小麦(Triticum aestivum)(春小麦)。
然后,在50、75和120的联苯菊酯施加速率以及在18、45和90的丁硫克百威施加速率下,测量各测试产品针对西方线虫和白色蛴螬的效率。观察到与杀真菌剂对照处理相比,所有杀虫剂种子处理的评估都显著更好。
下面的表6、7和8提供了与具体田野结果相关的细节:
第一计数报道成具有4个不同单位,全部从单一计数转换而来。与杀真菌剂相比,所有的杀虫剂种子处理都显著改善。通过线虫喂料显著降低其出现。
第二计数报道成具有4个不同单位,全部从单一计数转换而来。除了可流动的联苯菊酯以外,与杀真菌剂对照相比,所有的杀虫剂种子处理都显著改善。处理2和3包含施加到种子的相同负载的联苯菊酯。观察到的差异可能是因为包封的优势,或者因为可流动制剂由于不良的制剂性质在种子上覆盖率不佳。同样地,通过线虫喂料显著降低其出现。
然后,在第一评估时机中测量活力。与杀真菌剂对照相比,所有杀虫剂种子处理都改善。在第二时机中,除了处理1(可流动的联苯菊酯)和处理6(噻虫嗪,低比例10g ai/100kg)以外,在第二评估时机中,所有的杀虫剂种子处理都改善活力。
处理2和处理10具有比杀真菌剂更低的因线虫喂料导致的损坏,但也提供比其它处理更低的保护水平。在最高比例包封的联苯菊酯(50g ai/100kg)中损坏最低。
结果综览表明处理2和处理10具有比杀真菌剂更低的损坏,但也提供比其它处理更低的保护水平。在最高比例的包封的联苯菊酯(50g ai/100kg)观察到最低损坏。
结果进一步特别显示因蛴螬喂料而造成的损坏通常较低,但是通过最高比例的联苯菊酯、最高比例的丁硫克百威和噻虫嗪加上联苯菊酯造成最大的数值下降。
除了低比例的联苯菊酯可流动制剂(处理2)以外,所有的杀虫剂种子处理增加蒲式耳重量。因为喂料损坏造成的活力更低的植物可导致植物种子更轻(更低重量)。
除了处理2以外,与杀真菌剂对照(check)相比,所有的杀虫剂种子处理得到显著更高的产率。与处理2,3,6,7和10相比,50g ai/100kg下的联苯菊酯提供优异的产率。与在相同活性负载下施加的噻虫嗪相比,这个比例的联苯菊酯提供优异的产率。与更高比例相比,最低比例的丁硫克百威的产率更低。这个研究支持了在50g ai/100kg的更高速率下的联苯菊酯的益处,其提供优于30g ai/100kg保护。最后,在任何处理中,都没有观察到植物毒性症状。
根据这个实验的结果,本发明的独特的包封的联苯菊酯制剂提供等于或优于噻虫嗪的保护。相反,因为未知的原因,与包封的制剂相比,可流动形式的联苯菊酯提供更低的保护。包封制剂的至少一个益处在于与可流动制剂相比其提供在处理器上更少的累积,所述可流动制剂在处理器上显示更多的累积。这个观察将支持下述结论:与使用微观包封的制剂相比在种子上获得更低的目标比例。无论如何,本领域普通技术人员将理解本发明的包封的制剂带来优异效率的事实。
本领域普通技术人员可对在本说明书中描述的发明进行修改。所有这种变化和修改都在本发明的精神之内,且用于包含在权利要求中。
Claims (44)
1.一种包含多个微胶囊的杀虫剂组合物,其特征在于,每一微胶囊包括外部聚合物壳,所述外部聚合物壳包封含杀虫剂的核。
2.如权利要求1所述的组合物,其特征在于,所述微胶囊是多层微胶囊或单层微胶囊。
3.如权利要求1所述的组合物,其特征在于,所述外部聚合物壳包括选自下组的至少一种聚合物:聚脲、聚氨酯、聚酰胺和聚酯。
4.如权利要求3所述的组合物,其特征在于,所述外部聚合物壳的聚合物是聚脲。
5.如权利要求1所述的组合物,其特征在于,所述核还包含活性成分、溶剂和/或油。
6.如权利要求5所述的组合物,其特征在于,所述溶剂是选自下组的有机溶剂:石油(阿拉马替克200ND),或其它疏水性溶剂。
7.如权利要求6所述的组合物,其特征在于,所述溶剂的是石油蒸馏物,重质芳烃溶剂(阿拉马替克200,100,150),其沸点是100℃-400℃。
8.如权利要求5所述的组合物,其特征在于,所述油选自下组:玉米油、农作物油、大豆油、玉米油、环氧大豆油、菜籽油或其混合物。
9.如权利要求8所述的组合物,其特征在于,所述油是玉米油。
10.如权利要求5所述的组合物,其特征在于,还包含(a)共溶剂;(b)有效量的异氰酸酯;(c)分散剂;(d)聚乙烯醇;(e)粘度改性剂;(f)消泡剂(例如硅酮乳液混合物);(g)杀生物剂(例如1,3-苯并异噻唑-3-酮);(h)胺;和(i)pH改性剂。
11.如权利要求10所述的组合物,其特征在于,所述共溶剂选自下组:阿拉马替克100,阿拉马替克150和阿拉马替克200。
12.如权利要求11所述的组合物,其特征在于,所述共溶剂是阿拉马替克200。
13.如权利要求10所述的组合物,其特征在于,所述粘度改性剂/增强剂选自下组:黄原胶、甘油、角叉菜胶、黄原胶、瓜尔胶、阿拉伯胶、黄芪胶、聚环氧乙烷、褐藻胶、凹凸棒石粘土、蒙脱土粘土和海藻酸钠。
14.如权利要求13所述的组合物,其特征在于,所述粘度改性剂是黄原胶。
15.如权利要求10所述的组合物,其特征在于,所述分散剂是木质素磺酸盐。
16.如权利要求15所述的组合物,其特征在于,所述盐是磺甲基化木质素磺酸钠盐。
17.如权利要求10所述的组合物,其特征在于,所述聚乙烯醇以约0.05%-约2%重量/重量的量存在。
18.如权利要求10所述的组合物,其特征在于,所述胺是己二胺。
19.如权利要求10所述的组合物,其特征在于,所述pH改性剂是选自下组的酸:磷酸、乙酸、盐酸和柠檬酸。
20.如权利要求2所述的组合物,其特征在于,所述微胶囊具有0.1-1000微米的直径尺寸。
21.如权利要求22所述的组合物,其特征在于,至少90%的所述微胶囊具有2-10微米的直径。
22.如权利要求1所述的组合物,其特征在于,所述杀虫剂选自下组:氨基甲酸酯、有机磷酸酯、环二烯有机氯苯基吡唑、新烟碱、多杀菌素、氯通道活化剂、仿生的保幼激素、选择性同翅类取食阻滞剂、螨生长抑制剂、线粒体ATP合酶的抑制剂、烟酸乙酰胆碱受体通道阻滞剂、几丁质生物合成抑制剂、蜕皮干扰剂、蜕皮激素受体激动剂、章鱼胺受体激动剂、线粒体络合电子传输抑制剂、依赖于电压的钠通道阻滞剂、脂质体合成抑制剂、雷诺定受体调节剂和钠通道调节剂。
23.如权利要求22所述的组合物,其特征在于,所述杀虫剂是拟除虫菊酯。
24.如权利要求23所述的组合物,其特征在于,所述拟除虫菊酯选自下组氟酯菊酯、烯丙菊酯、联苯菊酯、氟氯氰菊酯、λ-氯氟氰菊酯、氯氰菊酯、α-氯氰菊酯、β-氯氰菊酯、ζ-氯氰菊酯、溴氰菊酯、顺式氰戊菊酯、醚菊酯、甲氰菊酯、氰戊菊酯、氟氰戊菊酯、τ-氟胺氰菊酯、苄氯菊酯、氟硅菊酯、和四溴菊酯。
25.如权利要求24所述的组合物,其特征在于,所述拟除虫菊酯是联苯菊酯。
26.一种组合物,所述组合物包含(a)联苯菊酯;(b)阿拉马替克200ND;(c)玉米油;(d)聚异氰酸酯;(e)磺甲基化木质素磺酸钠盐;(f)具有乙醇的乙酸乙烯乙酯聚合物;(g)黄原胶;(h)硅酮乳液混合物;(i)1,3-苯并异噻唑-3-酮;(j)六亚甲基二胺;(k)磷酸;和(l)水。
27.一种制备高负载杀虫剂微胶囊组合物的方法,所述方法包括下述步骤:(a)混合农用化学品与有机溶剂、至少一种单体和油,以制备有机混合物相,(b)在水性溶剂中溶解钠盐、聚乙烯醇和增稠剂,以形成水相,和(c)在均质器中匀化有机相与水相,和使界面聚合进行最高达至少24小时。
28.如权利要求27所述的方法,其特征在于,在25℃-65℃的温度下进行所述界面聚合。
29.如权利要求28所述的方法,其特征在于,在45℃-60℃的温度下进行所述界面聚合。
30.如权利要求27所述的方法,其特征在于,还包含使用3号纺锤体,将所述组合物的粘度调节到使用布氏LVT旋转粘度计测量时的200-5000厘泊(mPa·s)的测量结果。
31.如权利要求27所述的方法,其特征在于,在所述微胶囊中包封的杀虫剂的量是至少8%重量/重量。
32.一种用于保护种子和生长中植物免受害虫影响的方法,所述方法包括:(a)将组合物施加到种子,其中所述组合物包含:多个微胶囊,所述微胶囊包括聚合物壳和包封至少一种杀虫剂或杀虫剂组合的核,其中杀虫剂的总浓度是40-约450克/升。
33.一种种子涂覆组合物,其包含水溶液和多个微胶囊,其特征在于,所述微胶囊中的每一个包含含有具有油相的杀虫剂的核以及环绕所述油的聚合物壳,所述聚合物壳包括选自下组的至少一种聚合物:聚脲、聚氨酯、聚酰胺和聚酯。
34.如权利要求33所述的组合物,其特征在于,所述外部聚合物壳的聚合物是聚脲。
35.如权利要求34所述的组合物,其特征在于,所述核还包含溶剂。
36.如权利要求33所述的组合物,其特征在于,所述微胶囊的平均粒度(D50)是小于或等于10微米。
37.如权利要求33所述的组合物,其特征在于,所述聚合物壁的厚度是5纳米-约20纳米。
38.一种涂覆的种子,其包含种子和涂层,其中所述突出包含多个微胶囊,其特征在于,每一微胶囊包括包封含拟除虫菊酯的核的外部聚合物壳。
39.如权利要求38所述的涂覆的种子,其特征在于,所述外部聚合物壳包括选自下组的至少一种聚合物:聚脲、聚氨酯、聚酰胺和聚酯。
40.如权利要求39所述的涂覆的种子,其特征在于,所述外部聚合物壳的聚合物是聚脲。
41.如权利要求39所述的涂覆的种子,其特征在于,所述核还包含溶剂和/或油。
42.如权利要求41所述的涂覆的种子,其特征在于,所述溶剂是选自下组的有机溶剂:石油(阿拉马替克200ND),或其它疏水性溶剂。
43.如权利要求39所述的涂覆的种子,其特征在于,所述拟除虫菊酯是联苯菊酯。
44.如权利要求43所述的涂覆的种子,其特征在于,所述微胶囊还包含(a)共溶剂;(b)有效量的异氰酸酯;(c)分散剂;(d)聚乙烯醇;(e)粘度改性剂;(f)消泡剂(例如硅酮乳液混合物);(g)杀生物剂(例如1,3-苯并异噻唑-3-酮);(h)胺;和(i)pH改性剂。
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- 2017-06-13 HK HK17105855.4A patent/HK1232074A1/zh unknown
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2019
- 2019-03-20 AU AU2019201948A patent/AU2019201948A1/en not_active Abandoned
Patent Citations (3)
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CN101163401A (zh) * | 2005-04-22 | 2008-04-16 | 恩德拉(共同)股份公司 | 新制剂 |
CN102123590A (zh) * | 2008-01-04 | 2011-07-13 | 恩杜拉有限公司 | 用于调节微囊化的活性成分的释放速率的方法 |
CN103081896A (zh) * | 2011-11-04 | 2013-05-08 | 恩杜拉有限公司 | 具有杀虫活性的制剂的应用 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112449572A (zh) * | 2018-06-18 | 2021-03-05 | Upl有限公司 | 苯甲酰脲与拟除虫菊酯的稳定共制剂 |
CN110876378A (zh) * | 2019-12-11 | 2020-03-13 | 利民化学有限责任公司 | 一种智能微胶囊悬浮剂及其制备方法 |
CN111109254A (zh) * | 2019-12-19 | 2020-05-08 | 安徽伟创聚合材料科技有限公司 | 一种新型聚氨酯微胶囊环保杀虫剂及其制备方法 |
Also Published As
Publication number | Publication date |
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RU2016134726A (ru) | 2018-03-20 |
WO2015127051A1 (en) | 2015-08-27 |
RU2016134726A3 (zh) | 2018-03-20 |
UA117168C2 (uk) | 2018-06-25 |
AU2019201948A1 (en) | 2019-04-11 |
AR099478A1 (es) | 2016-07-27 |
CA2937809C (en) | 2023-02-14 |
RU2667775C2 (ru) | 2018-09-24 |
CA2937809A1 (en) | 2015-08-27 |
HK1232074A1 (zh) | 2018-01-05 |
US20170105418A1 (en) | 2017-04-20 |
AU2015219004B2 (en) | 2018-12-20 |
CL2016002012A1 (es) | 2017-03-24 |
EP3107397A1 (en) | 2016-12-28 |
UY36002A (es) | 2016-08-31 |
AU2015219004A1 (en) | 2016-09-08 |
MX2016010850A (es) | 2017-04-13 |
EP3107397A4 (en) | 2017-08-09 |
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