CN1141875C - 气凝胶在农业中的用途 - Google Patents

气凝胶在农业中的用途 Download PDF

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CN1141875C
CN1141875C CNB961920866A CN96192086A CN1141875C CN 1141875 C CN1141875 C CN 1141875C CN B961920866 A CNB961920866 A CN B961920866A CN 96192086 A CN96192086 A CN 96192086A CN 1141875 C CN1141875 C CN 1141875C
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����˼��G������ʲ
G·弗里什
A·齐默曼
��طƸ�
F·施沃特菲格
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—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 containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06—Aerosols
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • 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
    • A01N25/02—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 containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/143—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin

Abstract

本发明涉及气凝胶作为活性物质的载体材料在农业和/或兽药中的用途。

Description

凝胶在农业中的用途
本发明涉及气凝胶例如作为活性物质的载体在农业和兽药中的用途。
气凝胶，特别是那些孔隙率大于60％和密度低于0.6g/cm3的气凝胶具有特别低的导热性和因此正如在EP-A-0171 722中描述的一样被用作绝热材料。
在广义上，例如在“具有空气作为分散介质的气凝胶”的意义上讲的气凝胶是通过干燥合适的凝胶制备的。术语“气凝胶”在这种意义上包括狭义上的气凝胶、干凝胶和冷凝胶。这里，如果在高于临界温度的温度下和从高于临界压力的压力开始除去凝胶中的大部分液体，那么干燥的凝胶被称为狭义上的气凝胶。然而，如果低于临界温度除去凝胶的液体，例如同时形成液/气界相时，那么所得到的凝胶被称为干凝胶。
当在本发明中使用术语气凝胶时，涉及的是广义上的，例如在“具有空气作为分散介质的凝胶”意义上的气凝胶。
此外，气凝胶基本上被划分为无机和有机气凝胶。
自从1931年就已经知道无机气凝胶(S.S.Kistler，自然(Nature)1931，127，741)。从那时起，已经使用各种不同的原材料制备气凝胶。例如已经制备了SiO2、Al2O3、TiO2、ZrO2、SnO2、Li2O、CeO2和V2O5气凝胶及它们的混合物(H.D.Gesser，P.C.Goswami，化学综述(Chem.Rev.)1981，89，756ff)。多年来，同样已知由各种不同的原材料例如用蜜胺甲醛制备有机气凝胶(R.W.Pekala，材料科学杂志(J.Mater.Sci.)1989，24，3221)。
可以以各种不同的方法制备无机气凝胶。
例如，可以通过酸解和在乙醇中冷凝原硅酸四乙酯制备SiO2气凝胶。在这种方法中，所得到凝胶在保持结构下可以通过超临界温度干燥法干燥。例如从EP-A-0 396 176或WO92/03378已知基于这种干燥技术的制备方法。
如果在干燥之前SiO2凝胶与含氯的甲硅烷基化试剂反应，那么可以提供另一种低临界温度干燥SiO2凝胶的方法来代替。这里例如可以通过四烷氧基硅烷借助于水在合适的有机溶剂中酸解制备SiO2凝胶。在使用合适的有机溶剂代替该溶剂后，所得到的凝胶在另一步骤中与甲硅烷基化试剂反应。然后，在空气中，从有机溶剂中干燥出SiO2凝胶。在这种方法中得到孔隙率大于60％和密度低于0.4g/cm3的气凝胶。在WO94/25149中详细描述了基于这种干燥技术的制备方法。
此外，为了提高凝胶网络强度，正如在WO92/20623中描述的一样，可以在酒精水溶液中干燥之前使用四烷氧基硅烷处理和陈化上述凝胶。
此外，也可以以水玻璃为基础制备SiO2凝胶。由DE-A-43 42 548中已知基于这种技术的制备方法。
德国专利申请19502453.2描述了无氯的甲硅烷基化试剂的使用。
根据专门采用的方法，由超临界干燥得到的气凝胶是亲水的，或在短期内是疏水的。然而，从长远来看，它们仍然是亲水的。
这种亲水特性可以在超临界干燥期间通过憎水化步骤得到。由EP-A-0396 076已知这样的方法。
由于它们的制备方法(在干燥前硅烷化)，低临界干燥的气凝胶是永久性疏水的。
本发明的目的是寻找气凝胶的新用途。
现在，已经令人惊奇地发现气凝胶适合作为载体材料用于农业和兽药的活性物质中。
这些活性材料可以是杀虫剂、杀真菌剂、除草剂、杀螨剂、杀鱼剂、灭鼠剂、灭软体动物剂、杀线虫剂、杀细菌剂和/或杀寄生虫药。同样地，气凝胶可以作为载体材料用于病毒、细菌和/或杆菌如苏云金芽孢杆菌来生物控制不希望的生物体。
活性物质可以以溶解的形式和/或悬浮在液态载体材料中的形式，单独的或混合地涂在气凝胶上或被气凝胶吸附，其中，在所述的气凝胶的空隙中还保存着准液体相。液体活性材料也可以被吸收，而不用附加载体材料。为此，这些液体介质可以附加地带有离子和非离子型的乳化试剂。同样，优选地在活性制剂被吸收之后加入润湿剂和分散剂。气凝胶颗粒的尺寸优选地大于0.1μm，特别优选大于1μm，和更优选大于5μm。例如，负载的气凝胶可以与至少一种其它的载体物质例如滑石、白垩、高岭土和/或优选与水和/或油混合和/或用它稀释之后，例如，涂在植物、动物或陆地或水域的表面上。
优选使用无机气凝胶。在本申请中气凝胶被理解为其制备是基于无机材料的气凝胶。
术语“基于无机材料的气凝胶”特别地也指那些例如通过甲硅烷化改性的气凝胶。
优选的是主要包括SiO2、Al2O3、TiO2、ZrO2或它们的混合物的气凝胶。根据用途，它们可以具有亲水和/或疏水的表面基团(例如OH、OR、R)。具有亲水和/或疏水的表面基团的气凝胶的制备这里可以通过本领域普通技术人员已知的各种不同的方法完成。含有SiO2的亲水和/或疏水气凝胶，特别是SiO2气凝胶是特别优选的。
此外，已经令人惊奇地发现通过选择合适的亲水或疏水气凝胶可以使被气凝胶载负的物质以加速或延缓的形式被释放。另外，气凝胶可以作为分散剂用于在固体或液体介质中分散固态、液态或气态物质。加之，特别地，为了在亲水气凝胶的帮助下，将疏水(例如亲油)物质加到液体和/或准固态亲水分散介质中，和在疏水气凝胶的帮助下，为了将亲水物质加到液态疏水分散介质中，载以亲水和/或疏水物质的亲水和/或疏水气凝胶可以毫无问题的溶和到亲水和/或疏水的液态、准固态或固态介质中。例如，疏水气凝胶漂浮在亲水的含水溶液中。此外，甚至可以将液态的亲水或疏水物质转化为固态的可自由流动的粉末和颗粒。
下面借助于实施例进一步详细地描述本发明，但本发明并不限于此。
首先分别描述亲水和疏水气凝胶的制备。在下述的实施例1～39(表1～5)中，这些气凝胶均被使用。
在表中，单个组份用重量％(以总配方为基计)表示。
制备实施例
实施例1
制备永久性疏水气凝胶
将1升的钠水玻璃溶液(含有7重量％的SiO2和SiO2∶SiO2为1∶3.3)与0.5升的酸性离子交换树脂(具有磺酸基团的苯乙烯-二乙烯基苯的共聚物，商业上可得到，其商品名是Duolite C20)一起搅拌直到水溶液的PH值为2.3。然后，过滤出离子交换树脂和使用1摩尔NaOH溶液调节水溶液使PH值为5.0。然后，在85℃下将所得到的凝胶陈化3小时和接着用丙酮置换水，使用了3升的丙酮。然后用三甲基氯硅烷(5重量％三甲基氯硅烷/克湿凝胶)使含有丙酮的凝胶硅烷化。在空气中干燥该凝胶(在40℃下3小时，然后，在50℃下2小时和150℃下12小时)。
所得到的透明的气凝胶的密度是0.15g/cm3，根据BET所测的比表面积是480m2/g，和它是永久性疏水的。
实施例2
制备亲水性气凝胶
在600℃下，在温和的空气流中，用管式炉热解实施例1中制备的永久性疏水气凝胶1小时。所得到的透明的气凝胶的密度是0.18g/cm3，根据BET所测的比表面积是450m2/g，和它是亲水的。
表1
实施例   1   2   3   4   5  6  7  8
三唑磷   20
庚烯磷   15
马拉硫磷   18
对硫磷   12
溴氰菊酯   3
氯氰菊酯   4
莎稗磷   10
倍硫磷   5
气凝胶   36.5   46   49   54   53   50   40   51
二甲苯   30   25   10
Genapol X060   2   1   1
Solvesso 150   20   20   20   30   30
Emulsogen EL 400   6   5.5   4   4.5   3   2   6   5
十二烷基苯磺酸钙   3   3.0   2   2   1   1   3   2
Vanisperse CB   4   4.5   4   3   6   8   4   3
霍斯塔蓬T   0.5   1.0   1.0   0.5   1   1   1   1
Soprophor FL   3   2   4   1   2
Solvesso 200   20   10   5
Morwet D 425   1
表2
实施例   9  10   11   12   13  14  15  16
硫丹   15
Silafluofen  10
禾草灵   20
高噁唑禾草灵   18
气凝胶   39  62   41   38   38   35  50   39
二甲苯   25
Genapol X060  3   1   2   1  2   3
Solvesso 150   35  15   28   32   35  20   30
Emulsogen EL 400   4   4   2   4   4  4   4
十二烷基苯磺酸钙   2   2   1   2   2  2   2
Vanisperse CB  1   4   6   10  12   4
霍斯塔蓬  T   1  1   1   1   1   1  2   1
Soprophor FL  4   2   5   1   1
Solvesso 200   10
Morwet D 425   4  4   5
咪鲜安   16
氟草烟   12
乙氧氟草醚  8
BAS 480 F   6
表3
实施例 17 18 19 20 21 22 23
气凝胶 46.4 43.2 49 39 54 52 41
二甲苯 25
Genapol X060 4 3 4 4
Solvesso 150 30 27.3 20.5
Emulsogen EL 400 6 6 4
十二烷基苯磺酸钙 3 3 2
Vanisperse CB 5 6
霍斯塔蓬T 0.6 0.8 0.7 0.5 0.9 0.8 0.8
Soprophor FL 4 5 5 3 3 3
Solvesso 200 25.1 27.2 34.2
Morwet D 425 6 6 5 5 5
吡嘧磷 10
4-羟基-3，5-二碘苯甲腈辛酸酯 11
溴苯腈 9
2甲4氯丙酸丁酯 25
除虫脲 8
丙环唑 8
环唑醇 10
表4
实施例 24 25 26 27 28 29 30  31  32
气凝胶 38 52 56 47 58 58 59  48  44
二甲苯 5
Genapol X060 2 1 4 2  1
Solvesso 150 24 25 28 25  25
Emulsogen EL 400 4 6 8 2  5  6
十二烷基苯磺酸钙 2 3 4 1  2  3
Vanisperse CB 5 6 5  6
霍斯塔蓬T 0.7 0.4 1 1 1 1 1  1  1
Soprophor FL 3 2 4 2 5
Solvesso 32.3 33.6 30  30
Morwet D 425 5 4 6 5  5
丁苯吗啉 15
乙烯菌核利 10
氯氟氰菊酯 6
吡氟禾草灵 8
噻草酮 9
乙羧氟草醚 6
三唑醇 8
十三吗啉  8
异丙甲草胺  15
表5
实施例  33  34  35  36  37  38  39
气凝胶  52  55  42  42  52  48  38
Genapol X060  1  2  1  2  1  2
Solvesso 150  25  25  10  8  5  20
异佛尔酮  10  24  25  25  20
Emulsogen EL 400  4  4  6  6  6  6
十二烷基苯磺酸钙  2  2  3  3  3  3
Vanisperse CB  10  6
霍斯塔蓬T  1  1  1  1  1  1  1
Soprophor FL  5  1  1  2  5
Solvesso  25
Morwet D 425  4  4  5
苄草丹  5
氟氯氰菊酯  6
抑霉唑  8
乙呋草黄  8
甜菜宁  PMP  5
驱蚊油  DMP  5
苯嗪草酮  5

Claims (8)

1、气凝胶作为活性物质的载体材料在农业和/或兽药中的用途，其特征在于所述气凝胶通过硅烷化进行表面改性。
2、根据权利要求1的用途，其中表面改性的气凝胶具有疏水性表面基团。
3、根据权利要求1或2的气凝胶的用途，其作为载体材料用于杀虫剂、杀真菌剂、除草剂、杀螨剂、杀鱼剂、灭鼠剂、灭软体动物剂、杀线虫剂、杀细菌剂和/或杀寄生虫药。
4、根据权利要求1或2的气凝胶的用途，其作为载体材料用于病毒、细菌和/或杆菌。
5、一种制剂，其包括至少一种气凝胶和至少一种农业和/或兽药中的活性物质，并且所述气凝胶通过硅烷化进行表面改性。
6、根据权利要求5的制剂，其中活性物质以液体、溶解和/或悬浮的形式存在于该载体介质中。
7、根据权利要求5或6的制剂，其中该制剂含有至少一种乳化试剂。
8、根据权利要求5或6的制剂，其中该制剂含有至少一种润湿剂和分散剂。
CNB961920866A 1995-02-22 1996-02-22 气凝胶在农业中的用途 Expired - Fee Related CN1141875C (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19506141A DE19506141A1 (de) 1995-02-22 1995-02-22 Verwendung von Aerogelen in der Pharmazie, in der Kosmetik und im Pflanzenschutz
DE19506141.1 1995-02-22

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