CN110049675A - 由四甲基苯二亚甲基二异氰酸酯和具有至少3个胺基团的聚胺制备的壳的环庚草醚微胶囊 - Google Patents
由四甲基苯二亚甲基二异氰酸酯和具有至少3个胺基团的聚胺制备的壳的环庚草醚微胶囊 Download PDFInfo
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- CN110049675A CN110049675A CN201780075636.4A CN201780075636A CN110049675A CN 110049675 A CN110049675 A CN 110049675A CN 201780075636 A CN201780075636 A CN 201780075636A CN 110049675 A CN110049675 A CN 110049675A
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- 229920000768 polyamine Polymers 0.000 title claims abstract description 27
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 125000003277 amino group Chemical group 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title description 6
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- 125000005442 diisocyanate group Chemical group 0.000 claims description 4
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
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- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 5
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
Landscapes
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- 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)
- Catching Or Destruction (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明涉及一种包含微胶囊的组合物，所述微胶囊包含聚脲壳和核，其中所述核包含环庚草醚且所述壳包含四甲基苯二亚甲基二异氰酸酯和具有至少3个胺基团的聚胺的聚合产物，其中所述聚合产物包含基于四甲基苯二亚甲基二异氰酸酯重量小于5重量％聚合形式的其他异氰酸酯单体；包括使水、环庚草醚、四甲基苯二亚甲基二异氰酸酯和聚胺接触的步骤的制备所述组合物的方法；一种防治不希望的植物生长的方法，其中使所述组合物作用于土壤上和/或作用于不希望的植物上和/或作用于作物植物和/或其环境上。
Description
本发明涉及一种包含微胶囊的组合物，所述微胶囊包含聚脲壳和核，其中所述核包含环庚草醚(cinmethylin)且所述壳包含四甲基苯二亚甲基二异氰酸酯和具有至少3个胺基团的聚胺的聚合产物；包括使水、环庚草醚、四甲基苯二亚甲基二异氰酸酯和聚胺接触的步骤的制备所述组合物的方法；一种防治不希望的植物生长的方法，其中使所述组合物作用于待保护以防相应有害物的作物植物上、作用于土壤上和/或作用于不希望的植物上和/或作用于作物植物和/或其环境上。本发明包括优选特征与其他优选特征的组合。
包含环庚草醚的包含聚脲壳和核的农业化学微胶囊是已知的，但仍然需要一定改进。WO 94/13139公开了包含环庚草醚的微胶囊，其壳由通过己二胺与2027(来自Dow Chemical的多亚甲基多苯基异氰酸酯)的反应获得的聚氨酯制成。
WO 2015/165834公开了包含环庚草醚的微胶囊，其壳由通过XP2547(基于己二异氰酸酯的阴离子型水分散性多异氰酸酯)、二环己基甲烷二异氰酸酯和聚乙烯亚胺的反应获得的聚氨酯制成。
目的通过包含微胶囊的组合物实现，其中所述微胶囊包含聚脲壳和核，其中所述核包含环庚草醚且所述壳包含a)四甲基苯二亚甲基二异氰酸酯和b)具有至少3个胺基团的聚胺的聚合产物。
环庚草醚是可用于控制例如稻中的一年生禾本科杂草的选择性芽前内吸性除草剂。本文中的通用名环庚草醚是指外消旋混合物(±)-2-外-(2-甲基苄氧基)-1-甲基-4-异丙基-7-氧杂双环[2.2.1]庚烷(也称为"外(exo)-(±)-异构体"，CAS RN 87818-31-3)
它的任何独立对映体或任何非外消旋混合物。该外消旋混合物含有等份数的两种对映体(+)-2-外-(2-甲基苄氧基)-1-甲基-4-异丙基-7-氧杂双环[2.2.1]庚烷(也称为"外-(+)-异构体"，CAS RN 87818-61-9)和(-)-2-外-(2-甲基苄氧基)-1-甲基-4-异丙基-7-氧杂双环[2.2.1]庚烷(也称为"外-(-)-异构体"，CAS RN 87819-60-1)。外-(±)-异构体、外-(+)-异构体和外-(-)-异构体，包括它们的制备和除草性质公开在EP 0 081 893 A2中(参见实施例29、34、35和62)。这些化合物的另一些制备方法描述在US 4,487,945中(参见实施方案46和48)。外消旋混合物(±)-2-外-(2-甲基苄氧基)-1-甲基-4-异丙基-7-氧杂双环[2.2.1]庚烷也描述在The Pesticide Manual，第14版，编辑:C.D.S.Tomlin,BritishCrop Production Council,2006,entry 157,第195-196页中，以其IUPAC命名(1RS,2SR,4SR)-1,4-环氧基-p-薄荷-2-基2-甲基苄基醚及其Chemical Abstracts命名外-(±)-1-甲基-4-(1-甲基乙基)-2-[(2-甲基苯基)甲氧基]-7-氧杂双环[2.2.1]庚烷。环庚草醚是液体，其几乎不溶于水(在20℃下0,063g·L-1)，但可溶于有机溶剂。其具有312℃的沸点(Pesticide Science,1987,21,Nr.2,143–153)。
合适的四甲基苯二亚甲基二异氰酸酯可以是间位或对位取代的四甲基苯二亚甲基二异氰酸酯。优选四甲基苯二亚甲基二异氰酸酯为式(II)化合物：
聚合产物包含基于四甲基苯二亚甲基二异氰酸酯的重量小于5重量％，优选小于3重量％，尤其是小于1重量％的聚合形式的其他异氰酸酯单体。在另外的形式中，聚合产物基本不含聚合形式的其他异氰酸酯单体。术语“其他异氰酸酯单体”可涉及包含至少一种(优选至少两种)异氰酸酯基团且可适合作为制备聚脲的单体的任何化合物。
聚胺具有至少3个胺基团。不同聚胺的混合物也是可能的。优选聚胺为脂族聚胺，其具有两个伯氨基和至少一个仲氨基和/或叔氨基。合适的聚胺为乙烯胺，其通常可由Huntsman Corp.，USA或Dow Chemical Co.，USA市购。更优选聚胺为二亚乙基三胺(DETA)、线性或支化三亚乙基四胺(TETA)、N,N'-双(2-氨基乙基)哌嗪)(BisAEP)、四亚乙基五胺(TEPA)、4-(2-氨基乙基)-N-(2-氨基乙基)-N'-{2-{(2-氨基乙基)氨基}乙基}-1,2-乙二胺)(AETETA)、1-(2-氨基乙基)-4-[(2-氨基乙基)氨基]乙基]-哌嗪)(AEPEEDA)、五亚乙基六胺(PEHA)、六亚乙基七胺(HEHA)或其混合物。甚至更优选三亚乙基四胺(TETA)、四亚乙基五胺(TEPA)、五亚乙基六胺(PEHA)、六亚乙基七胺(HEHA)及其混合物。
在另外优选的形式中，聚胺为式(I)化合物：
其中m为1-8的整数，且R1为H或甲基。指数m优选为2-5的整数，更优选3-4的整数，尤其是3。R1优选为H。优选m为2-5的整数，且R1为H。
聚脲壳包含通常至少45重量％，优选至少55重量％，特别是至少65重量％的四甲基苯二亚甲基二异氰酸酯。聚脲壳包含通常45-90重量％，优选55-85重量％，特别是65-78重量％的四甲基苯二亚甲基二异氰酸酯。聚脲壳中四甲基苯二亚甲基二异氰酸酯的重量％可涉及单体的总量。
聚脲壳包含通常至多55重量％，优选至多45重量％，特别是至多35重量％的聚胺(例如具有式(I)，其中n为1-8的整数)。聚脲壳包含通常15-55重量％，优选20-45重量％，特别是25-35重量％的聚胺(例如具有式(I)，其中n为1-8的整数)。聚脲壳中聚胺的重量％可涉及单体的总量。
聚合产物可包含基于聚胺的重量至多30重量％，优选至多10重量％，尤其是至多5重量％的聚合形式的其他胺单体。术语“其他胺单体”可涉及包含至少一种(优选至少两种)胺基团且可适合作为制备聚脲的单体的任何化合物。
核与聚脲壳的重量比为通常50:1-5:1，优选40:1-10:1，特别是30:1-15:1。核的重量可基于环庚草醚、任选地水不混溶性有机溶剂和任选地其他溶剂的量。聚脲壳的重量可基于四甲基苯二亚甲基二异氰酸酯和聚胺的量。
在另外的优选形式中，聚脲壳包含45-90重量％四甲基苯二亚甲基二异氰酸酯、15-55重量％聚胺(例如具有式(I)，其中m为2-5的整数)和小于5重量％的其他异氰酸酯单体，且核与聚脲壳的重量比为50:1-5:1。
在另外的优选形式中，聚脲壳包含55-85重量％四甲基苯二亚甲基二异氰酸酯、20-45重量％聚胺(例如具有式(I)，其中m为2-5的整数)和小于3重量％的其他异氰酸酯单体，且核与聚脲壳的重量比为40:1-10:1。
在另外的优选形式中，聚脲壳包含65-75重量％四甲基苯二亚甲基二异氰酸酯、25-35重量％聚胺(例如具有式(I)，其中m为2-5的整数)且不含其他异氰酸酯单体，且核与聚脲壳的重量比为30:1-15:1。
具有聚脲壳的微胶囊可类似于现有技术制备。它们优选通过合适的聚合物壁形成材料(如二异氰酸酯和二胺)的界面聚合方法制备。界面聚合通常在包含溶解在其中的至少一部分聚合物壁形成材料的核材料的水包油含水乳液或悬浮液中进行。在聚合期间，聚合物从核材料分离到核材料和水之间的边界表面，由此形成微胶囊的壁。由此可得到微胶囊材料的含水悬浮液。在现有技术中已经公开合适的制备含有环庚草醚的微胶囊的界面聚合方法。通常，聚脲通过使至少一种二异氰酸酯与至少一种二胺反应形成，以形成聚脲壳。
微胶囊的平均尺寸(借助光散射的z-平均值；优选D4,3平均值)为0.5-50μm，优选0.5-20μm，更优选1-15μm，尤其是2-10μm。
微胶囊的核可包含水不混溶性有机溶剂。水不混溶性有机溶剂的合适实例是
-烃溶剂如脂族、环状和芳族烃(例如甲苯、二甲苯、链烷烃、四氢化萘、烷基化萘或其衍生物，中至高沸点的矿物油馏分(如煤油、柴油、煤焦油))；
-植物油如玉米油、菜籽油；
-脂肪酸酯如C10-C22脂肪酸的C1-C10烷基酯；或
-植物油的甲基或乙基酯如菜籽油甲基酯或玉米油甲基酯。
上述水不混溶性有机溶剂的混合物也是可能的。水不混溶性有机溶剂通常可市购，例如烃以商品名200、200或28市购。芳族烃可以贫萘品质的形式使用。优选的水不混溶性有机溶剂为烃类，特别是芳族烃类。
优选地，水不混溶性有机溶剂在水中在20℃下具有至多20g/L，更优选至多5g/L，特别是至多0.5g/L的溶解度。
通常，水不混溶性有机溶剂具有100℃以上，优选150℃以上，特别是180℃以上的沸点。
在一个优选形式中，微胶囊的核可包含至多10重量％，优选至多5重量％，特别是至多1重量％的水不混溶性有机溶剂。
在一个更优选形式中，微胶囊的核可包含小于1重量％，优选小于0.5重量％，特别是小于0.1重量％的水不混溶性有机溶剂。在另外更优选的形式中，微胶囊的核不含水不混溶性有机溶剂。
微胶囊的核可包含其他溶剂，例如至多30重量％，优选至多15重量％，基于核中所有溶剂的总量。在另外的优选形式中，微胶囊的核不含其他溶剂。其他溶剂可为水或水混溶性溶剂。水混溶性有机溶剂可在水中在20℃下具有至少0.5g/L，更优选至少5g/L，特别是至少20g/L的溶解度。
在一个更优选形式中，微胶囊的核可包含小于1重量％，优选小于0.5重量％，特别是小于0.1重量％的有机溶剂。在另外更优选的形式中，微胶囊的核不含有机溶剂。合适的有机溶剂为水不混溶性有机溶剂和其他溶剂。
微胶囊的核可包含至少90重量％，优选至少95重量％，特别是至少99重量％的环庚草醚、任选地水不混溶性有机溶剂和任选地其他溶剂的总和。在另外的形式中，微胶囊的核可由环庚草醚、任选地水不混溶性有机溶剂和任选地其他溶剂组成。在另一形式中，微胶囊的核可由环庚草醚组成。
在一个优选形式中，微胶囊的核可包含至少90重量％，优选至少95重量％，特别是至少99重量％的环庚草醚。
该组合物可为含水组合物，其可包含水相(例如连续水相)。含水组合物可包含至少10重量％，优选至少25重量％，特别是至少35重量％的水。通常，微胶囊悬浮于含水组合物的水相中。
优选地，该组合物为含水组合物，且水相包含木素磺酸盐。合适的木素磺酸盐是碱金属盐和/或碱土金属盐和/或铵盐，例如木素磺酸的铵盐、钠盐、钾盐、钙盐或镁盐。非常特别优选使用钠盐、钾盐和/或钙盐。当然术语木素磺酸盐也包括不同离子的混合盐，例如木素磺酸钾/钠、木素磺酸钾/钙等，特别是木素磺酸钠/钙。
木素磺酸盐可基于硫酸盐浆木素。硫酸盐浆木素在使用氢氧化钠和硫化钠的木质素制浆方法中获得。可将硫酸盐浆木素磺化而获得木素磺酸盐。
木素磺酸盐的分子量可以为500-20000g/mol。优选地，木素磺酸盐的分子量为700-10000g/mol，更优选900-7000g/mol，特别是1000-5000g/mol。
木素磺酸盐通常可溶于水(例如在20℃下)，例如以至少5重量％，优选至少10重量％，特别是至少20重量％溶于水。
含水组合物包含通常0.1-5.0重量％，优选0.3-3.0重量％，特别是0.5-2.0重量％的木素磺酸盐。
该组合物(例如含水组合物)通常包含至少1重量％，优选至少3重量％，特别是至少10重量％的包封的环庚草醚。
该组合物还可含有水溶性无机盐，其可由微胶凝的制备得到或其可在此后加入。如果存在，则水溶性无机盐的浓度可为1-200g/L，优选2-150g/L，尤其是10-130g/L。盐的水溶性意指在水中的溶解度在20℃下为至少50g/L，尤其是至少100g/L或甚至至少200g/L。
该类无机盐优选选自碱金属的硫酸盐、氯化物、硝酸盐、磷酸单氢盐和磷酸二氢盐，氨的硫酸盐、氯化物、硝酸盐、磷酸单氢盐和磷酸二氢盐，碱土金属的氯化物和硝酸盐以及硫酸镁。实例包括氯化锂、氯化钠、氯化钾、硝酸锂、硝酸钠、硝酸钾、硫酸锂、硫酸钠、硫酸钾、磷酸单氢钠、磷酸单氢钾、磷酸二氢钠、磷酸二氢钾、氯化镁、氯化钙、硝酸镁、硝酸钙、硫酸镁、氯化铵、硫酸铵、磷酸单氢铵和磷酸二氢铵等。优选的无机盐为氯化钠、氯化钾、氯化钙、硫酸铵和硫酸镁，其中特别优选硫酸铵和硫酸镁。
在另外的实施方案中，该组合物不含或含有小于10g/L，尤其是小于1g/L的水溶性无机盐。
该组合物可包含二醇，例如乙二醇、丙二醇。该组合物可包含1-250g/L，优选10-150g/L，尤其是30-100g/L二醇。
该组合物可在微胶囊外侧，例如在含水组合物的水相中包含其他辅助剂。合适辅助剂的实例为表面活性剂、分散剂、乳化剂、润湿剂、助剂、加溶剂、渗透提高剂、保护性胶体、粘合剂、增稠剂、保湿剂、趋避剂、引诱剂、进食刺激剂、增容剂、杀菌剂、消泡剂、着色剂、增粘剂和粘结剂。
合适的表面活性剂为表面活性化合物，例如阴离子、阳离子、非离子和两性表面活性剂、嵌段聚合物、聚电解质及其混合物。该类表面活性剂可用作乳化剂、分散剂、加溶剂、润湿剂、渗透提高剂、保护性胶体或助剂。表面活性剂的实例列于McCutcheon’s，第1卷：Emulsifiers&Detergents，McCutcheon’s Directories，Glen Rock，USA，2008(国际版或北美版)中。
合适的阴离子表面活性剂为磺酸、硫酸、磷酸、羧酸及其混合物的碱金属、碱土金属或铵盐。磺酸盐的实例为烷基芳基磺酸盐、二苯基磺酸盐、α-烯烃磺酸盐、脂肪酸和油的磺酸盐、乙氧基化烷基酚的磺酸盐、烷氧基化芳基酚的磺酸盐、缩合萘的磺酸盐、十二烷基-和十三烷基苯磺酸盐、萘和烷基萘的磺酸盐、磺基琥珀酸盐或磺基琥珀酰胺酸盐。硫酸盐的实例为脂肪酸和油的硫酸酯盐、乙氧基化烷基酚的硫酸酯盐、醇的硫酸酯盐、乙氧基化醇的硫酸酯盐、脂肪酸酯的硫酸盐。磷酸盐的实例为磷酸酯盐。羧酸盐的实例为烷基羧酸盐和羧化醇或烷基酚乙氧基化物。术语磺酸盐是指与木素磺酸盐不同的化合物。
合适的非离子表面活性剂为烷氧基化物，N-取代的脂肪酸酰胺，胺氧化物，酯，糖基表面活性剂，聚合物表面活性剂及其混合物。烷氧基化物的实例为诸如已经被1-50当量烷氧基化的醇、烷基酚、胺、酰胺、芳基酚、脂肪酸或脂肪酸酯的化合物。可将氧化乙烯和/或氧化丙烯用于烷氧基化，优选氧化乙烯。N-取代的脂肪酸酰胺的实例是脂肪酸葡糖酰胺或脂肪酸链烷醇酰胺。酯的实例为脂肪酸酯，甘油酯或甘油单酯。糖基表面活性剂的实例为脱水山梨醇、乙氧基化脱水山梨醇、蔗糖和葡萄糖酯或烷基多葡糖苷。聚合物表面活性剂的实例为乙烯基吡咯烷酮、乙烯醇或乙酸乙烯酯的均聚物或共聚物。
合适的阳离子表面活性剂为季型表面活性剂，例如具有1或2个疏水性基团的季铵化合物，或长链伯胺的盐。合适的两性表面活性剂为烷基甜菜碱和咪唑啉类。合适的嵌段聚合物为包含聚氧化乙烯和聚氧化丙烯嵌段的A-B或A-B-A型嵌段聚合物，或包含链烷醇、聚氧化乙烯和聚氧化丙烯的A-B-C型嵌段聚合物。合适的聚电解质为聚酸或聚碱。聚酸的实例为聚丙烯酸的碱金属盐或聚酸梳状聚合物。聚碱的实例是聚乙烯基胺或聚乙烯胺。
合适的助剂是本身具有可忽略的农药活性或者本身甚至没有农药活性且改善化合物I对目标物的生物学性能的化合物。实例为表面活性剂，矿物油或植物油以及其他辅助剂。其他实例由Knowles，Adjuvants and Additives，Agrow Reports DS256，T&F InformaUK，2006，第5章列出。
合适的增稠剂为多糖(例如黄原胶、羧甲基纤维素)、无机粘土(有机改性的或未改性的)、聚羧酸盐和硅酸盐。
合适的杀菌剂为拌棉醇(bronopol)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。
合适的消泡剂为聚硅氧烷、长链醇和脂肪酸的盐。
本发明还涉及一种制备该组合物的方法，该方法包括使水、环庚草醚、四甲基苯二亚甲基二异氰酸酯和聚胺接触的步骤。接触可通过混合各组分，例如在20-100℃的温度下进行。
在一个实施方案中，制备所述组合物的方法包括使包含至少一种分散剂的水相与包含环庚草醚和四甲基苯二亚甲基二异氰酸酯的油相接触的步骤；然后使用高剪切设备乳化该混合物；在用低剪切搅拌器继续搅拌的同时向所得乳液中加入聚胺。乳化和后续搅拌可在20-80℃的温度下进行。
由高剪切搅拌产生的粒度分布通常以下列参数为特征：0.5-20μm的D50和5-30μm的D90，更优选1-15μm的D50和5-20μm的D90；最优选2-10μm的D50和8-15μm的D90(借助光散射得出的z-平均值)。
在本发明的一个优选实施方案中，如下制备该组合物：
步骤1)在20-80℃的温度下将包含环庚草醚和四甲基苯二亚甲基二异氰酸酯的油相添加到水相中；这种水相包含至少一种分散剂；例如，该分散剂可选自如本文定义的木素磺酸盐、缩合烷基萘磺酸盐或缩合酚磺酸盐；然后使用高剪切设备乳化该混合物，以使该乳液的所得粒度分布以2-10μm的D50和8-15μm的D90(借助光散射得出的z-平均值)为特征。
任选地，水相另外包含如下文定义的水溶性无机盐，而所述盐优选选自氯化钠、氯化钾、氯化钙、硫酸铵和硫酸镁；和/或防冻剂，而所述防冻剂优选选自乙二醇和丙二醇；和/或防沫剂，例如有机硅消泡剂。
步骤2)在乳化后，将乳化设备换成低剪切搅拌器并加入聚胺，优选作为水溶液(基于加入的水溶液计5-50重量％，优选15-35重量％)。随后，该分散体在20-80℃下流畅搅拌优选30-150分钟，更优选60-120分钟。
任选地，在第三步骤中，在搅拌下用包含例如分散剂体系、防冻剂、增稠剂、消泡剂或杀生物剂或其组合的成品水溶液处理该胶囊分散体；可以通过加入无机或有机酸，例如乙酸将pH调节到pH 6-8。
步骤1)中的水相中的水溶性无机盐浓度可为2-150g/L，优选10-130g/L，尤其是50-100g/L不等。该盐的水溶性意味着在20℃下至少50g/L，特别是至少100g/L或甚至至少200g/L的在水中的溶解度。
该类无机盐优选选自碱金属的硫酸盐、氯化物、硝酸盐、磷酸单氢盐和磷酸二氢盐，氨的硫酸盐、氯化物、硝酸盐、磷酸单氢盐和磷酸二氢盐，碱土金属的氯化物和硝酸盐以及硫酸镁。实例包括氯化锂、氯化钠、氯化钾、硝酸锂、硝酸钠、硝酸钾、硫酸锂、硫酸钠、硫酸钾、磷酸单氢钠、磷酸单氢钾、磷酸二氢钠、磷酸二氢钾、氯化镁、氯化钙、硝酸镁、硝酸钙、硫酸镁、氯化铵、硫酸铵、磷酸单氢铵和磷酸二氢铵等。优选的无机盐为氯化钠、氯化钾、氯化钙、硫酸铵和硫酸镁，其中特别优选硫酸铵和硫酸镁。
此外，本发明涉及一种防治不希望的植物生长的方法，其中使本发明的组合物作用于土壤上和/或作用于不希望的植物和/或作物植物和/或其环境。
合适作物的实例为禾谷类，例如小麦、黑麦、大麦、小黑麦、燕麦或稻；甜菜，例如糖用甜菜或饲用甜菜；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，例如蚕豆、兵豆、豌豆、苜蓿或大豆；油料作物，例如油菜籽油菜、芥菜、橄榄、向日葵、椰子、可可豆、蓖麻豆、油棕、花生或大豆；葫芦科植物，例如南瓜、黄瓜或甜瓜；纤维作物，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、南瓜或或柿子椒；月桂科植物，例如鳄梨、肉桂或樟脑；能量作物和工业原料作物，例如玉米、大豆、小麦、油菜籽油菜、甘蔗或油棕；玉米；烟草；坚果；咖啡；茶；香蕉；葡萄(食用葡萄和酿酒用葡萄)；啤酒花；禾草，例如草坪；甜叶菊(Stevia rebaudania)；橡胶植物和森林植物，例如花卉、灌木、落叶树和针叶树；和植物繁殖材料，例如种子；以及这些植物的收获产品。
术语作物还包括已经通过育种、诱变或重组方法修饰的那些植物，包括上市销售或处于开发过程中的农业生物技术产品。基因修饰植物是其基因材料以在自然条件下无法通过杂交、突变或自然重组(即基因材料的重组)进行的方式修饰的植物。此时，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。该类重组修饰还包括蛋白质、寡肽或多肽的翻译后修饰，例如通过糖基化或连接聚合物，例如异戊二烯化、乙酰化或法呢基化基团或PEG基团。
用户通常由预剂量装置、背包式喷雾器、喷雾桶、喷雾飞机或灌溉系统施用本发明的组合物。通常用水、缓冲剂和/或其他辅助剂将所述农业化学组合物配制至所需的施用浓度，由此获得即用喷雾液或本发明的农业化学组合物。每公顷农业利用区通常施用20-2000升，优选50-400升即用喷雾液。
可向包含它们作为预混物的农化组合物中加入各种类型的油、润湿剂、助剂、肥料或微量营养素和其他农药(例如除草剂、杀虫剂、杀真菌剂、生长调节剂、安全剂)，或者合适的话在紧临使用前加入(桶混)。这些试剂可以以1:100-100:1，优选1:10-10:1的重量比与本发明的组合物混合。
当用于植物保护中时，环庚草醚的施用量取决于所需的效果类型为0.001-2kg/ha，优选0.005-2kg/ha，更优选0.05-0.9kg/ha，特别是0.05-0.6kg/ha。
本发明具有各种优点：该组合物在长时间的储存期间稳定，例如甚至在宽温度范围；该组合物可用水稀释之后施加而不堵塞喷嘴；该组合物在用水稀释之后稳定；该组合物可与各种其他作物保护产品混合并提供与包含非包封环庚草醚的混合物相比更好的活性组分相容性(例如降低的沉降、絮凝、结晶)；环庚草醚的挥发性降低；紫外线敏感性降低；环庚草醚在施加于作物后更稳定；该组合物使得环庚草醚更好地迁移到土壤中。
Claims (15)
1.一种包含微胶囊的组合物，其中所述微胶囊包含聚脲壳和核，其中所述核包含环庚草醚且所述壳包含a)四甲基苯二亚甲基二异氰酸酯和b)具有至少3个胺基团的聚胺的聚合产物。
2.根据权利要求1的组合物，其中所述聚胺为式(I)化合物：
其中m为1-8的整数，且R1为H或甲基。
3.根据权利要求1或2的组合物，其中m为2-5的整数，且R1为H。
4.根据权利要求1-3中任一项的组合物，其中所述四甲基苯二亚甲基二异氰酸酯为式(II)化合物：
5.根据权利要求1-4中任一项的组合物，其中所述核与聚脲壳的重量比为50:1-5:1，优选40:1-10:1，特别是30:1-15:1。
6.根据权利要求1-5中任一项的组合物，其中所述聚合产物包含基于四甲基苯二亚甲基二异氰酸酯重量小于5重量％聚合形式的其他异氰酸酯单体。
7.根据权利要求1-6中任一项的组合物，其中所述聚脲壳包含至少55重量％的四甲基苯二亚甲基二异氰酸酯。
8.根据权利要求1-7中任一项的组合物，其中所述聚脲壳包含至多45重量％的聚胺。
9.根据权利要求1-8中任一项的组合物，其中所述组合物为含水组合物且水相包含木素磺酸盐。
10.根据权利要求9的组合物，其中所述木素磺酸盐具有至多10000g/mol的分子量。
11.根据权利要求9或10的组合物，其中所述组合物包含0,3-3,0重量％的木素磺酸盐。
12.根据权利要求1-11中任一项的组合物，其中所述核包含小于1重量％水不混溶性有机溶剂。
13.根据权利要求1-11中任一项的组合物，其中所述核包含小于0.5重量％水不混溶性有机溶剂。
14.一种制备如权利要求1-13中任一项所定义的组合物的方法，包括使水、环庚草醚、四甲基苯二亚甲基二异氰酸酯和聚胺接触的步骤。
15.一种防治不希望的植物生长的方法，其中使如权利要求1-13中任一项所定义的组合物作用于土壤上和/或作用于不希望的植物上和/或作用于作物植物和/或其环境。
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