CN114868743A - 一种农药微囊悬浮剂及其制备方法 - Google Patents

一种农药微囊悬浮剂及其制备方法 Download PDF

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CN114868743A
CN114868743A CN202210710392.5A CN202210710392A CN114868743A CN 114868743 A CN114868743 A CN 114868743A CN 202210710392 A CN202210710392 A CN 202210710392A CN 114868743 A CN114868743 A CN 114868743A
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pesticide
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李志清
辛艳
王伟昌
王建伟
康瑞雪
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Shandong Weifang Rainbow Chemical Co Ltd
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Abstract

本发明公开了一种农药微囊悬浮剂及其制备方法，组成为：农药活性组分1～50%，油相壁材0.5～4.0％，有机溶剂0～20.0％，水相壁材1.5～12.0％，分散剂2.0～6.0％，防冻剂2.0～5.0％，防腐剂0～0.5％，水补足100%。本发明首次提出以聚乙烯醇作为农药微囊悬浮剂的水相壁材，较现有的多元胺水相壁材，能适用于更多的农药活性组分，尤其是咪鲜胺、稻瘟灵、甲草胺等，这些农药很难通过多元胺水相壁材制备成功，工艺稳定，生产成功率高，工业普适性更强。

Description

一种农药微囊悬浮剂及其制备方法
技术领域
本发明涉及一种农药领域的微囊悬浮剂，具体涉及以聚乙烯醇为水相壁材的微囊悬浮剂及其制备方法，属于农药制剂技术领域。
背景技术
农药微囊悬浮剂较常规剂型有独有的优点：降低有效成分对非靶标生物的毒性、降低有效成分对高等动物的刺激、掩蔽囊芯的不良气味、减缓有效成分的分解、使有效成分缓慢释放、增加农药淋溶，农药微囊悬浮剂在拌种使用时，能有效提高对作物种子的安全性，提高发芽势和发芽率。在制备过程中，农药微囊悬浮剂使用水作为制剂的连续相，大量降低有机溶剂的用量，成为乳油制剂的一个重要替代产品，发展前景广阔。
微囊悬浮剂因为其特有的优点，成为如今的研究热点，多家公司和科研院所研究开发了多种制备方法。常见微囊制备方法有十几种，大体分为物理法、化学法、物理化学法及生物法等，其中最常用的是化学法。化学法制备微囊的方法主要有：界面聚合法、原位聚合法。
原位聚合法是将壁材单体预先加入分散相或连续相中，将油相入水相剪切，得到粒径均一、分布范围合格的乳状液后，在搅拌的条件下，通过改变温度或pH值等引发壁材单体在油水界面的聚合，并固化，最终得到质量指标合格的微囊悬浮剂。原位聚合法根据原材料的不同分为以尿素和甲醛为原材料的脲醛树脂和以三聚氰胺和甲醛为原材料的密胺树脂，因为大多用甲醛，导致生产和使用中安全系数较低，逐渐被淘汰。界面聚合法是将一种水溶性的壁材和一种油溶性壁材分别分散在连续相和分散相中，在油水界面两种壁材相互接触并反应形成一层致密的高分子膜，产品最终通过升温固化得到最终的水包油型的微囊悬浮剂。
界面聚合法是目前应用最为广泛的工艺，其中最常用的水相壁材为多元胺(华乃震.农药微囊悬浮剂的加工和进展(Ⅰ)[J].现代农药,2010,9(3):10-14(18).)。但是，该工艺也存在一些不足，例如：为得到更高的包封率，一般会提高水相壁材多元胺的用量，成囊后多余的壁材在配方中不仅不会稳定配方，甚至影响制剂的pH值，导致产品不符合质量控制标准。此外，许多有效成分如咪鲜胺、稻瘟灵、甲草胺等在微囊化过程中，受有效成分和壁材的反应活性影响，使用多元胺作为水相壁材时，极易出现体系爆聚导致膏化，导致生产失败。也就是说，多元胺的使用局限性很大，有效成分普适性差。
聚乙烯醇(PVA)是一种无色的水溶性合成树脂，目前有报道聚乙烯醇可以作为微胶囊壁材使用。专利CN106999894A公开了一种包含胶囊核和胶囊壳的微胶囊，该胶囊壳包含核周围的聚乙烯醇层和相邻聚噁唑啉层。该微胶囊壳的制备原理是利用聚乙烯醇和聚噁唑啉在不同溶液中的溶解度差异，使用复凝聚法形成微胶囊，该反应是物理反应，形成的两层微胶囊壳是物理组合在一起，最终的微胶囊壳为聚乙烯醇层和相邻聚噁唑啉层。该方法制备的微囊不仅有效成分含量偏低，也很难得到稳定的微囊悬浮剂，因而阻碍了其在农药领域的应用。CN113174245A公开了一种聚乙烯醇包覆的纳米二氧化钒光热响应微胶囊及其制备方法，该专利是将聚乙烯醇作为壁材，对分布有发光有机分子的油相进行包覆，也是使用的物理法，最终的微囊壳仅是聚乙烯醇。该微胶囊在后续的干燥过程中容易产生缝隙，导致微囊的包覆率普遍偏低，因而制约了该方法在农药领域的应用。这些现有技术中，聚乙烯醇包裹的有效成分并非为农药，聚乙烯醇是否可用于农药微胶囊的制备不得而知。
发明内容
针对农药领域中微胶囊悬浮剂在制备过程中存在的壁材普适性差、包覆率较低、壁材过量使用影响产品质量控制等的不足，本发明提供了一种农药微囊悬浮剂，该农药微囊悬浮剂以聚乙烯醇为水相壁材，减少了乳化剂和增稠剂的使用，农药适用范围更广，降低了成本和工艺难度，性能优异，合格率高。
本发明具体技术方案如下：
一种农药微囊悬浮剂，其由以下重量百分含量的成分组成：农药活性组分1～50％，油相壁材0.5～4.0％，有机溶剂0～20.0％，水相壁材1.5～12％，分散剂2.0～6.0％，防冻剂2.0～5.0％，防腐剂0～0.5％，水补足100％。
进一步的，所述农药活性组分可以为一种，也可以为多种，本发明配方可以适用于多种农药活性组分，农药普适性更强。本发明农药活性组分为油溶性成分，在常温下为固态或液态。在常温下为固态的农药活性组分包括毒死蜱、稻瘟灵、咪鲜胺、甲草胺、高效氯氟氰菊酯、阿维菌素、二甲戊灵、吡唑醚菌酯、异噁草松、联苯菊酯、氯氰菊酯、精高效氯氟氰菊酯、高效氯氰菊酯、氟氯氰菊酯等，在常温下为液态的农药活性组分包括噻唑磷、辛硫磷、乙草胺、三唑磷、精异丙甲草胺、甲基嘧啶磷、丁草胺等。
优选的，农药活性组分的含量为5～30wt％。
进一步的，所述油相壁材为脂肪族异氰酸酯或芳香族异氰酸酯或它们的改性物，脂肪族异氰酸酯可以为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、十亚甲基二异氰酸酯、2-甲基戊烷二异氰酸酯等，芳香族异氰酸酯可以为甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、对苯二异氰酸酯等，它们的改性物指的是利用化学合成等工艺将脂肪族异氰酸酯或芳香族异氰酸酯进行改性加工，例如TDI-TMP加成物是甲苯二异氰酸酯与三羟甲基丙烷的加成物；此外常见的还有HDI三聚体，是一种最常见的HDI均聚物，它是含异氰脲酸酯杂环结构的三异氰酸酯。
优选的，油相壁材为二苯基甲烷二异氰酸酯，油相壁材的含量为1.5～3.0wt％。
进一步的，有机溶剂的作用是为了溶解农药活性组分，当农药活性组分为固态时，需要用有机溶剂溶解后再与油相壁材混合，当农药活性组分为液态时，可以不用有机溶剂，直接与油相壁材混合。因此，当农药活性组分为液态时，有机溶剂用量优选为0％，当农药活性组分为固态时，有机溶剂用量优选为1～20wt％，更优选为5～10wt％。
进一步的，有机溶剂可以为二甲苯、100#溶剂油、150#溶剂油、200#溶剂油、环己酮等中的一种或多种，优选为二甲苯。
进一步的，水相壁材为水溶性聚乙烯醇，本发明用聚乙烯醇代替传统的多元胺水相壁材，聚乙烯醇与油相壁材搭配组合能适用于更多的农药活性组分，且聚乙烯醇能作为乳化剂和增稠剂，减少了这两个助剂的加入，也不会影响产品的稳定性，生产成功率更高。
进一步的，聚乙烯醇的聚合度范围为1000～30000，优选为聚合度范围1000～2000，进一步的，使用聚乙烯醇为聚乙烯醇17-88。
优选的，水相壁材的含量为6.0～9.0wt％。
进一步的，分散剂为木质素磺酸钠、木质素磺酸钙、烷基萘磺酸盐甲醛缩合物、烯酸甲酯聚羧酸共聚物等中的至少一种，优选为木质素磺酸钠；优选的，分散剂的含量为3.0～5.0％。
进一步的，防冻剂为乙二醇、1,2-丙二醇、丙三醇中的一种或多种，优选为乙二醇；优选的，防冻剂的含量为2.0～4.0wt％。
进一步的，防腐剂为各种常规的农药防腐剂，例如甲基异噻唑琳酮等；优选的，防腐剂的含量为0.1～0.5wt％。
本发明还提供了上述农药微囊悬浮剂的制备方法，该方法为界面聚合法，包括以下步骤：
(1)当农药活性组分为固态时，将农药活性组分用有机溶剂溶解，然后与油相壁材混合，得到油相；当农药活性组分为液态时，直接将农药活性组分与油相壁材混合，得到油相；
(2)将水相壁材、一部分分散剂和水混合，得到水相；
(3)将油相加入水相中，高速剪切乳化，得到乳化液；
(4)将乳化液升温，进行界面聚合反应，反应后加入防冻剂、防腐剂和剩余的分散剂，保温，得农药微囊悬浮剂。
进一步的，步骤(2)中的分散剂为分散剂总质量的40～75％。
进一步的，步骤(3)中，高速剪切的转速为3000～15000r/min，优选的，高速剪切转速为9000～11000r/min。
进一步的，步骤(4)中，乳化液加热至65～75℃进行界面聚合反应，反应时间为3.0～3.5h，然后加入防冻剂、防腐剂和剩余的分散剂，继续保温0.5～1h，得农药微囊悬浮剂。
本发明具有以下有益效果：
1、本发明首次提出以聚乙烯醇作为农药微囊悬浮剂的水相壁材，较现有的多元胺水相壁材，能适用于更多的农药活性组分，例如：毒死蜱，稻瘟灵，咪鲜胺，甲草胺，高效氯氟氰菊酯，阿维菌素，二甲戊灵，噻唑磷，辛硫磷，吡唑醚菌酯，异噁草松，联苯菊酯，乙草胺，三唑磷，精异丙甲草胺，甲基嘧啶磷，氯氰菊酯，精高效氯氟氰菊酯，高效氯氰菊酯，氟氯氰菊酯，丁草胺等，尤其是咪鲜胺、稻瘟灵、甲草胺等，这些农药很难通过多元胺水相壁材制备成功，工艺稳定，生产成功率高，工业普适性更强。
2、成囊后多余的水溶性聚乙烯醇可以作为乳化剂，增强乳液稳定性，聚乙烯醇还可以作为增稠剂，增强微囊悬浮剂的物理稳定性，聚乙烯醇同时发挥水相壁材、增稠剂、乳化剂的作用，配方中不加入增稠剂、乳化剂，降低了生产难度，降低了投料工作强度，减少了备料劳动力输出，降低了投料失误几率，提升了产品生产合格率。
3、本发明微囊悬浮剂选择聚乙烯醇为水相壁材，不仅不会影响制剂的稳定性，还能起到乳化剂和增稠剂的作用，在与其他助剂共同搭配的作用下，所得微囊悬浮剂包封率高，粒径分布范围窄，释放性能合格，自发分散性良好，粘度适中，热贮稳定性、冻融稳定性良好。
4、本发明制备方法工艺流程简单，省时省力，设备要求低，工业化简便，市场广阔。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合实施例对本发明中的技术方案进行清楚、完整地描述。需要说明的是，以下记载的实施例只是本申请的一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本申请保护的范围。
下述实施例中，如无特别说明，所述浓度均为质量百分浓度。
实施例1
制备5％的二甲戊灵微囊悬浮剂，配方如下表所示：
Figure BDA0003707710170000041
制备方法为：
(1)将原药用有机溶剂溶解，然后加入油相壁材混合，得到油相；
(2)将水相壁材、一部分分散剂和水混合，得到水相；
(3)将油相加入水相中，按照10000r/min的速度高速剪切乳化，得到乳化液；
(4)将乳化液升温，达到70℃保温，保温3.5h后加入防冻剂、防腐剂和剩余的分散剂，继续保温0.5h，得农药微囊悬浮剂。
实施例2
制备30％咪鲜胺微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000042
Figure BDA0003707710170000051
制备方法同实施例1。
实施例3
制备15％稻瘟灵微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000052
制备方法同实施例1。
实施例4
制备50％二甲戊灵微囊悬浮剂，配方如下表所示：
Figure BDA0003707710170000053
制备方法同实施例1。
实施例5
制备30％咪鲜胺微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000061
制备方法同实施例1。
实施例6
制备1％稻瘟灵微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000062
制备方法同实施例1。
实施例7
制备30％毒死蜱微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000063
Figure BDA0003707710170000071
制备方法同实施例1。
实施例8
制备40％甲草胺微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000072
制备方法同实施例1。
实施例9
制备9％吡唑醚菌酯微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000073
Figure BDA0003707710170000081
制备方法同实施例1。
实施例10
制备32.4％异噁草松微囊悬浮剂，配方如下表所示：
Figure BDA0003707710170000082
制备方法同实施例1。
实施例11
制备25％高效氯氟氰菊酯微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000083
Figure BDA0003707710170000091
制备方法同实施例1。
实施例12
制备30％噻唑膦微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000092
制备方法同实施例1。
实施例13
制备30％辛硫磷微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000093
Figure BDA0003707710170000101
制备方法同实施例1。
实施例14
制备45％精异丙甲草胺微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000102
制备方法同实施例1。
实施例15
制备25％甲基嘧啶磷微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000103
制备方法同实施例1。
对比例1
制备5％二甲戊灵微囊悬浮剂，配方如下表所示：
Figure BDA0003707710170000104
Figure BDA0003707710170000111
制备方法为：
(1)将原药用有机溶剂溶解，然后加入油相壁材混合，得到油相；
(2)将水相壁材、一部分分散剂、乳化剂和水混合，得到水相；
(3)将油相加入水相中，按照10000r/min的速度高速剪切乳化，得到乳化液；
(4)将乳化液升温，达到70℃保温，保温3.5h后加入防冻剂、防腐剂、增稠剂和剩余的分散剂，继续保温0.5h，得农药微囊悬浮剂。
对比例2
制备30％咪鲜胺微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000112
制备方法同对比例1。
对比例3
制备15％稻瘟灵微囊悬浮剂悬浮剂，配方如下表所示：
Figure BDA0003707710170000121
制备方法同对比例1。
对比例4
制备5％二甲戊灵微囊悬浮剂，配方如下表所示：
Figure BDA0003707710170000122
制备方法同实施例1。
测试例
参照国家标准或CIPAC中要求的方法对上述实施例和对比例制备的微囊悬浮剂的性能进行测试。
悬浮率参照GB/T14825-2006方法检测；
持久起泡性参照GB/T28137-2011方法检测；
pH值参照GB/T 1601-1993方法检测；
湿筛试验参照GB/T 16150-1995方法检测；
热贮稳定性按GB/T 19136-2003方法检测；
冻融稳定性试验在室温(20℃±2℃)与(-10℃±2℃)之间做4个循环，每个循环为冷冻18h，融化6h。
自发分散性参照CIPAC方法中的MT160检测。
粒径参照CIPAC方法中的MT187检测。
倾倒性参照CIPAC方法中的MT148.1检测。
包封率测试方法为：称取含0.05g(精确至0.000 2g)试样，置于50mL烧杯中，用10mL乙二醇50％水溶液稀释样品，经玻璃纤维滤纸(49型，孔径约1.0μm)过滤，再用10mL乙二醇50％水溶液(分两次)洗涤烧杯和滤纸，然后将滤纸及残囊置于50mL容量瓶中加甲醇溶解，在超声波中振荡10min，冷却至室温，用流动相(具体由有效成分检测方法决定)稀释至刻度，摇匀，过滤。待高效液相色谱仪稳定后，进行囊内有效成分含量(％)测定。样品包封率按下式进行计算：
包封率(％)＝囊内有效成分含量/有效成分总含量*100％
缓释速率测试方法为：称取0.5g(精确至0.000 2g)试样置于100mL容量瓶中，用甲醇：水＝80:20溶液进行定容，摇匀后在1000rpm条件下，30±1℃，不停搅拌，定时取样，进行囊外含量检测，计算其缓释速率。
检测结果如下表1、表2和表3所示。
表1实施例1-6样品制剂配方稳定性检测结果
Figure BDA0003707710170000131
Figure BDA0003707710170000141
表2实施例7-15样品制剂配方稳定性检测结果
Figure BDA0003707710170000142
Figure BDA0003707710170000151
表3对比例1-4样品制剂配方稳定性检测结果
Figure BDA0003707710170000152
Figure BDA0003707710170000161
从表1和表3可以看出，实施例1与对比例1相比，制剂各项指标均合格，样品经热贮、冻融加速贮存处理后质量稳定，而对比例1的常温和冻融样品悬浮率、包封率、湿筛实验、自发分散性、粒径、倾倒性等指标性能变差，热贮后，样品悬浮率、包封率、湿筛实验、自发分散性不合格，主要是由于多元胺壁材的使用导致的样品分散性变差，微囊颗粒相互聚集导致的，且对比例1样品pH明显高于实施例1，意味着对作物和环境压力更大。实施例2与对比例2相比，制剂各项指标均合格，样品经热贮、冻融加速贮存处理后质量稳定，而对比例不合格，分析主要原因同样是由于多元胺壁材的使用导致的样品分散性变差，微囊颗粒相互聚集且游离有效成分偏高导致的。实施例3与对比例3相比，受有效成分的影响，对比例3制备过程中出现严重质量问题，样品膏化、结块。对比例4在对比例1基础上去掉乳化剂和增稠剂，与实施例1配方组分一致，常温样品检测发现除粒径较大外，其它指标与对比例1差异不大，这是因为不使用乳化剂导致剪切乳化不合格导致的；值得注意的是，样品热贮和冻融后样品顶部严重淅水，热贮样品底部结块膏化，外观不合格，同时失去使用价值和检测意义，这是因为缺乏增稠剂而导致的样品内部微囊下沉，体系稳定性结构丧失导致的，说明使用多元胺作为水相壁材时，乳化剂和增稠剂必须要添加、使用。相比之下，本发明配方和方法所得的样品各项检测指标合格，样品经热贮、冻融加速贮存处理后质量依然稳定。以上对比说明，使用聚乙烯醇替代多元胺的微囊悬浮剂性能合格，贮存稳定，可以满足生产、贮存、运输及使用要求。同时证明，使用聚乙烯醇作为水相壁材能适用于更多的活性成分，生产过程更加稳定。
另外，通过实施例1-6的对比可以看出，实施例1-3使用了优选的助剂，实施例4-6使用的普通助剂，通过表1的实验结果看，实施例1-3的样品在悬浮率、包封率、缓释速率、自发分散性、倾倒性等方面具有更好的表现，性能更佳。
由表1和表2中的实施例1-15检测结果说明，使用本发明的方法制备微囊悬浮剂，质量稳定，普适性强，应用前景广阔。

Claims (10)

1.一种农药微囊悬浮剂，其特征是由以下重量百分含量的成分组成：农药活性组分1～50%，油相壁材0.5～4.0％，有机溶剂0～20.0％，水相壁材1.5～12.0％，分散剂2.0～6.0％，防冻剂2.0～5.0％，防腐剂0～0.5％，水补足100%。
2.根据权利要求1所述的农药微囊悬浮剂，其特征是：所述农药活性组分为一种或多种，农药活性组分为油溶性成分，在常温下为固态或液态；优选的，在常温下为固态的农药活性组分包括毒死蜱、稻瘟灵、咪鲜胺、甲草胺、高效氯氟氰菊酯、阿维菌素、二甲戊灵、吡唑醚菌酯、异噁草松、联苯菊酯、氯氰菊酯、精高效氯氟氰菊酯、高效氯氰菊酯、氟氯氰菊酯，在常温下为液态的农药活性组分包括噻唑磷、辛硫磷、乙草胺、三唑磷、精异丙甲草胺、甲基嘧啶磷、丁草胺。
3.根据权利要求1或2所述的农药微囊悬浮剂，其特征是：农药活性组分的含量为5～30wt%。
4.根据权利要求1所述的农药微囊悬浮剂，其特征是：所述油相壁材为脂肪族异氰酸酯或芳香族异氰酸酯或它们的改性物，所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、十亚甲基二异氰酸酯或2-甲基戊烷二异氰酸酯，所述芳香族异氰酸酯为甲苯二异氰酸酯、二苯基甲烷二异氰酸酯或对苯二异氰酸酯，所述改性物为TDI-TMP加成物或HDI三聚体。
5.根据权利要求4所述的农药微囊悬浮剂，其特征是：油相壁材为二苯基甲烷二异氰酸酯；优选的，油相壁材的含量为1.5～3.0wt％。
6.根据权利要求1所述的农药微囊悬浮剂，其特征是：水相壁材为水溶性聚乙烯醇，聚乙烯醇的聚合度范围为1000～30000，优选聚合度范围为1000～2000；优选的，聚乙烯醇为聚乙烯醇17-88，水相壁材的含量为6.0～9.0wt％。
7.根据权利要求1所述的农药微囊悬浮剂，其特征是：有机溶剂为二甲苯、100#溶剂油、150#溶剂油、200#溶剂油、环己酮中的一种或多种，优选为二甲苯；分散剂为木质素磺酸钠、木质素磺酸钙、烷基萘磺酸盐甲醛缩合物、烯酸甲酯聚羧酸共聚物中的至少一种，优选为木质素磺酸钠；防冻剂为乙二醇、1,2-丙二醇、丙三醇中的一种或多种，优选为乙二醇；防腐剂为甲基异噻唑琳酮。
8.根据权利要求1或7所述的农药微囊悬浮剂，其特征是：农药活性组分为液态时，有机溶剂用量为0%，农药活性组分为固态时，有机溶剂用量为1～20wt%，优选为5～10wt%；分散剂的含量为3.0～5.0％；防冻剂的含量为2.0～4.0wt％。
9.一种农药界面聚合法制备权利要求1-8中任一项所述的农药微囊悬浮剂的方法，其特征是包括以下步骤：
（1）当农药活性组分为固态时，将农药活性组分用有机溶剂溶解，然后与油溶性壁材混合，得到油相；当农药活性组分为液态时，直接将农药活性组分与油相壁材混合，得到油相；
（2）将水相壁材、一部分分散剂和水混合，得到水相；
（3）将油相加入水相中，高速剪切乳化，得到乳化液；
（4）将乳化液升温，进行界面聚合反应，反应后加入防冻剂、防腐剂和剩余的分散剂，保温，得农药微囊悬浮剂。
10.根据权利要求9所述的方法，其特征是：步骤（2）中的分散剂为分散剂总质量的40～75%；步骤（3）中，高速剪切的转速为3000～15000r/min，优选为9000～11000r/min；步骤（4）中，乳化液加热至65～75℃进行界面聚合反应，反应时间为3.0～3.5h，然后加入防冻剂、防腐剂和剩余的分散剂，继续保温0.5～1h，得农药微囊悬浮剂。
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