CN107494528B - 氟环唑悬浮剂及其制备方法 - Google Patents
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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
- 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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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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
- A01N25/08—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 solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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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
- A01N25/30—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 characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
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Abstract
本发明公开了一种氟环唑悬浮剂及其制备方法，属于农药制剂加工领域。上述氟环唑悬浮剂由下述重量百分比原料组成：氟环唑10‑15％、表面活性剂8‑14％、藻朊酸钠0.2‑0.5％、尿素0.2‑1％、醋酸钠0.5‑1％、皂角粉0.2‑0.6％、聚氧乙烯甘油醚0.02‑0.05％、余量为水；所述表面活性剂由蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠组成。本发明利用蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠的协同作用，可有效防止原药颗粒的聚集；本发明添加尿素提高介质的密度，有助于保持悬浮剂的悬浮稳定性；本发明的氟环唑悬浮剂具有高悬浮率、长期贮存稳定等优点。
Description
技术领域
本发明涉及农药制剂加工技术领域，尤其涉及一种氟环唑悬浮剂及其制备方法。
背景技术
氟环唑如下所示，是一种内吸性三唑类杀菌剂，主要是抑制病菌麦角甾醇的合成，阻碍病菌细胞壁的形成，并且氟环唑分子对一种真菌酶 (14-dencthylase)有强力亲和性，与目前已知的杀菌剂相比，能更有效抑制病菌原真菌。氟环唑可提高作物的几丁质酶活性，导致真菌吸器的收缩，抑制病菌侵入，这是氟环唑在所有三唑类产品中独一无二的特性。对香蕉、葱蒜、芹菜、菜豆、瓜类、芦笋、花生、甜菜等作物上的叶斑病、白粉病、锈病以及葡萄上的炭疽病、白腐病等病害有良好的防效。
农药悬浮剂以水为分散介质，不溶或微溶于水的固体原药经研磨粉碎，并借助表面活性剂及其它助剂的作用，使之均匀分散，形成一种颗粒细小的高悬浮、能流动的比较稳定的液固态体系。与乳油相比，可避免使用大量的有机溶剂；与可湿性粉剂相比，则无粉尘飞散飘移；对人畜的毒性和刺激性都比较低，并能减轻对作物的药害，也不会因有机溶剂而在贮藏运输过程中燃烧，安全性较高；对用户和整个环境所造成的危险性减少到相当低的程度。并且，其性能优异，分散性好，悬浮率高，在植物体表面的展着力和粘着力都比较强，耐雨水冲刷，药效比较显著而且比较持久。但是现有悬浮剂存在悬浮率低、悬浮稳定差等问题。
《农药》2011年12月第50卷第12期“12.5％氟环唑悬浮剂配方的筛选和优化”公开了最优配方：氟环唑12.5％，分散剂NNO 3％，分散剂 JH 2％，农乳600#1％，EL-60 1％，白炭黑2％，黄原胶0.3％，乙二醇5％，消泡剂WJX 0.5％，蒸馏水补足100％。通过选取特定的助剂得到悬浮稳定、悬浮率高的氟环唑悬浮剂。
发明内容
本发明提供一种氟环唑悬浮剂及其制备方法，通过特定的助剂之间的作用，得到悬浮率高、悬浮稳定性好的悬浮剂。
具体通过下述技术方案得以实现：
本发明提供一种氟环唑悬浮剂，由下述重量百分比原料组成：
所述表面活性剂由蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠组成。
优选的，氟环唑悬浮剂，由下述重量百分比原料组成：
优选的，氟环唑悬浮剂，由下述重量百分比原料组成：
根据实际需要还可以在配方中添加pH调节剂。
优选的，所述水为自来水或去离子水。
本发明的氟环唑悬浮剂可以采用超微粉碎法进行制备，具体包括以下步骤：
(1)根据配方把氟环唑、表面活性剂、藻朊酸钠、尿素、醋酸钠、皂角粉、聚氧乙烯甘油醚和水搅拌混合成浆状物，置于球磨机中粉碎。
(2)置于磨砂机进行超微粉碎，控制平均粒径2-4μm。
(3)置于均质机中均质，使粒子均匀化。
本发明还提供一种氟环唑悬浮剂用于防治叶斑以及葡萄上的炭疽病、白腐病的应用。
众所周知，由于悬浮剂始终以浓缩悬浮液的形态存在，在贮存期间，尤其是长期贮存，可能会出现物理稳定性问题。要保持农药悬浮剂贮存期物理稳定性，就必须通过配方和加工工艺控制悬浮物积聚、沉降和晶体生长。也就是要使悬浮剂在贮存过程中粒子间不发生合并聚结，分散粒子的粒度及其分布保持不变；并且，分散相粒子能稳定地悬浮于分散介质中而不沉降。
农药悬浮剂是一种热力学和动力学均不稳定的体系。其分散相粒子很小，分散相与分散介质间存在相当大的相接口和接口能，粒子会自动聚集，从而使总介面积缩小，界面能降低，以至整个悬浮体系遭受破坏。本发明通过向悬浮剂体系中加入非离子表面活性剂蔗糖脂肪酸酯和阴离子表面活性剂双十三醇磺基琥珀酸酯钠，并利用亲油基团吸附在氟环唑颗粒表面，一方面蔗糖脂肪酸酯吸附于原药粒子的表面并形成较密集的保护层以“位阻”的相互作用使粒子相互排斥，阻止聚结；另一方面，双十三醇磺基琥珀酸酯钠具有两条疏水链，能更好在氟环唑颗粒表面吸附，同时其亲水基团较多，利于氟环唑颗粒在水中分散；当其在原药颗粒上吸附，后使其表面带有负电荷，相邻原药颗粒由于静电相互作用的排斥力，再者，双十三醇磺基琥珀酸酯钠具有一定的空间位阻，存在“位阻”排斥力，可有效防止颗粒聚集。
另外，表面活性剂在悬浮剂中的抗聚集作用与其在原药粒子上的吸附量、吸附层的厚度以及吸附的稳定性等密切相关。本发明发明人通过不断试验，确定由蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠组成的表面活性剂能有效提高原药颗粒的悬浮率，且优选的蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠的重量比为1:3。
同时悬浮剂的黏度对于悬浮剂的稳定性是一个很重要的影响因素。但是悬浮剂黏度也不是越高越好，悬浮剂的黏度太大会影响悬浮剂的加工和使用，使悬浮剂不容易流动、易于结块、在水中不容易分散等，因此选择正确的增稠剂是加工悬浮剂的关键。在悬浮剂体系中加入藻朊酸钠，能够增大介质的黏度，进一步保持悬浮剂的悬浮稳定性。
综上所述，本发明具有以下有益效果：
(1)本发明利用蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠的协同作用，可有效防止原药颗粒的聚集；
(2)本发明添加藻朊酸钠提高介质的黏度，有助于保持悬浮剂的悬浮稳定性；
(3)本发明的氟环唑悬浮剂具有高悬浮率、长期贮存稳定等优点。
具体实施方式
为使本发明的实施例要解决的技术问题、技术方案和优点更加清楚，下面将结合具体实施例进行详细描述。但本发明绝非限于这些例子。以下所述仅为本发明较好的实施例，仅仅用以解释本发明，并不能因此而理解为本发明专利范围的限制。应当指出的是，凡在本发明的精神和原则之内所做的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。因此，本发明专利的保护范围应以所附权利要求为准。
本发明针对现有技术中，悬浮剂悬浮率低、悬浮稳定性差等问题，本发明提供一种氟环唑复配的农药悬浮剂及其制备方法。
实施例1
(1)根据表1中实施例1的配方把氟环唑、蔗糖脂肪酸酯、双十三醇磺基琥珀酸酯钠、藻朊酸钠、尿素、醋酸钠、皂角粉、聚氧乙烯甘油醚和水搅拌混合成浆状物，置于球磨机中粉碎。
(2)置于磨砂机进行超微粉碎，控制平均粒径2-4μm。
(3)置于均质机中均质，使粒子均匀化。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.4μm。
表1：氟环唑悬浮剂配方表单位：公斤
实施例2
按表1对应实施例2数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.4μm。
实施例3
按表1对应实施例3数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.3μm。
实施例4
按表1对应实施例4数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.4μm。
实施例5
按表1对应实施例5数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.5μm。
对比例1
按表1对应对比例1数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.9μm。
对比例2
按表1对应对比例2数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为3.1μm。
对比例3
按表1对应对比例3数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为3.5μm。
对比例4
按表1对应对比例4数据称取原料，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.6μm。
对比例5
将实施例3中的双十三醇磺基琥珀酸酯钠替换成丁二酸二异辛酯磺酸钠，其余试剂及用量与实施例3相同，按实施例1的方法进行制备。
制得的悬浮剂，外观粘稠均相的液体，经马尔文激光粒度分布仪测定，其平均粒径(D50)为2.9μm。
将上述实施例和对比例制备的悬浮剂分别在室温贮存14天、54℃±2℃条件下高温贮存14天，采用《GB/T14825-2006农药悬浮率测定方法》测悬浮率，具体数据见下表2。当悬浮率>85％时，则认为该产品为合格品。
表2：农药悬浮率测定数据表单位：％
悬浮性是指分散的原药粒子在悬浮液中保持悬浮时间长短的能力，通常用悬浮率来表示。一个好的悬浮剂，应具有良好的储存稳定性，即较高的悬浮率。
由表2可知，本发明的氟环唑悬浮剂(实施例1-5)，悬浮率高，产品性能稳定。这是由于双十三醇磺基琥珀酸酯钠与蔗糖脂肪酸酯协同作用，有效提高了原药颗粒的悬浮效果。
以实施例3为例构建的对比例1-4，与实施例3相比，缺少蔗糖脂肪酸酯(对比例1)、缺少双十三醇磺基琥珀酸酯钠(对比例2)，其悬浮率都有所下降，这说明单组份的表面活性剂使用时，其悬浮性能不如两者配合使用效果好；而同时缺少蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠 (对比例3)，其悬浮率急剧降低，这是由于，悬浮体系中氟环唑颗粒表面不存在阻止其聚集的基团或氟环唑表面不存在静电排斥作用，导致氟环唑颗粒聚集，其悬浮率降低。缺少藻朊酸钠(对比例4)，其悬浮率稍微降低，这是由于悬浮剂的黏度较低，原药颗粒沉降，影响了悬浮剂的悬浮率。将双十三醇磺基琥珀酸酯钠替换成丁二酸二异辛酯磺酸钠(对比例5)，其悬浮率降低，这是由于不同链长的表面活性剂，对悬浮剂悬浮性能有影响，导致悬浮稳定性降低。
本发明利用蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠的协同作用，可有效防止原药颗粒的聚集；同时通过添加藻朊酸钠提高介质的黏度，有助于保持悬浮剂的悬浮稳定性；本发明的氟环唑悬浮剂具有高悬浮率、长期贮存稳定等优点。
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明所述原理的前提下，还可以作出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种氟环唑悬浮剂，其特征在于，由下述重量百分比原料组成：
所述表面活性剂由重量比为1:3的蔗糖脂肪酸酯和双十三醇磺基琥珀酸酯钠组成。
2.根据权利要求1所述的氟环唑悬浮剂，其特征在于，由下述重量百分比原料组成：
3.根据权利要求2所述的氟环唑悬浮剂，其特征在于，由下述重量百分比原料组成：
4.根据权利要求1所述的氟环唑悬浮剂，其特征在于，所述水为自来水或去离子水。
5.权利要求1-4任一所述的氟环唑悬浮剂的制备方法，其特征在于，将氟环唑、表面活性剂、藻朊酸钠、尿素、醋酸钠、皂角粉、聚氧乙烯甘油醚和水搅拌混合成浆状物，置于球磨机中粉碎；然后置于磨砂机进行超微粉碎，控制平均粒径2-4μm；置于均质机中均质，使粒子均匀化，即得氟环唑悬浮剂。
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| CN103039441A (zh) * | 2013-01-24 | 2013-04-17 | 凤台县精华助剂有限公司 | 水乳型l40表面活性剂 |
| CN103429077A (zh) * | 2011-03-18 | 2013-12-04 | 日本曹达株式会社 | 水悬浮状农园艺用杀菌剂组合物 |
| CN104705304A (zh) * | 2013-12-11 | 2015-06-17 | 上海中冠生物科技有限公司 | 一种复配杀菌剂及其制备方法 |
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| CN103429077A (zh) * | 2011-03-18 | 2013-12-04 | 日本曹达株式会社 | 水悬浮状农园艺用杀菌剂组合物 |
| CN103039441A (zh) * | 2013-01-24 | 2013-04-17 | 凤台县精华助剂有限公司 | 水乳型l40表面活性剂 |
| CN104705304A (zh) * | 2013-12-11 | 2015-06-17 | 上海中冠生物科技有限公司 | 一种复配杀菌剂及其制备方法 |
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