CN110663686B - 一种环保型农药乳化剂 - Google Patents
一种环保型农药乳化剂 Download PDFInfo
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Abstract
本发明公开了一种环保型农药乳化剂,由以下质量百分比的组分组成:脂肪醇聚氧烷基醚:30%~75%;阴离子表面活性剂:10%~40%;防冻剂:5%~20%;消泡剂:1%~2%;水:余量;所述脂肪醇聚氧烷基醚的结构式为:R‑O‑(AO)a‑[(EO)m‑(PO)n]‑H或R‑O‑[(EO)m‑(PO)n]‑(AO)a‑H,其中,R为碳原子数6~18的烷基或烯基,A为‑CH2CH2‑、‑CH2CH2CH2‑或‑CH2CH2CH2CH2‑,(EO)m‑(PO)n为‑CH2CH2O‑单元和‑CH2CH2CH2O‑单元以嵌段、交替或无规则分布构成的聚氧烷基链,a为1~10的整数,m和n为0~10的整数。本发明的乳化剂乳化效果优异,不含APEO,安全环保,将其用于农药水剂可以保持农药水剂长期稳定。
Description
技术领域
本发明涉及一种环保型农药乳化剂。
背景技术
中国是世界上主要的农药生产和使用大国,据统计,2018年我国化学农药原药产量高达208.3万吨。随着人们环保意识的提高,对农药制剂的要求也越来越高,逐步要求农药制剂高效安全、环境友好化,而且国家也出台了相关的政策和规划。2010年8月国家工业和信息化部等四部门便联合出台了《农药产业政策》,指出“国家通过科技扶持、技术改造、经济政策引导等措施,支持高效、安全、经济、环境友好的农药新产品发展,加快高污染、高风险产品的替代和淘汰,促进品种结构不断优化”、“大力推动农用剂型向水基化、无尘化、控制释放等高效、安全的方向发展……严格控制有毒有害溶剂和助剂的使用”。2014年国家工信部出台了《农药工业“十二五”发展规划》,指出“严格控制含甲苯、二甲苯等有毒有害溶剂和助剂的使用,开发和推广水基化等剂型”。
农药可以分为乳油、悬浮剂、水剂、可湿性粉剂等多种剂型。乳油剂型是目前常用的农药剂型,据统计,我国每年用于制造乳油剂型农药所使用的二甲苯类溶剂就高达30~40万吨,随着农药的喷洒,这些溶剂首先会挥发到空气中,接着会渗透到食品、土壤和地下水中,不仅会造成生态环境的污染,而且还会对食品安全和人们身体健康造成损害。农药水剂(农药微乳剂的一种)更加安全环保,是国家鼓励发展的方向,近年来发展迅速,但农药水剂中普遍使用烷基酚聚氧乙烯醚(APEO)作为乳化剂。APEO虽然具有良好的润湿、渗透、乳化、分散、增溶等效果,但其毒性大、生物降解性差,对人体和生态环境的危害不容忽视,一些发达国家在很多领域都已经禁止使用APEO。
可见,有必要开发一种不含APEO、安全环保、乳化效果优异、适用于农药水剂的乳化剂。
发明内容
本发明的目的在于提供一种环保型农药乳化剂。
本发明所采取的技术方案是:
一种环保型农药乳化剂,由以下质量百分比的组分组成:
脂肪醇聚氧烷基醚:30%~75%;
阴离子表面活性剂:10%~40%;
防冻剂:5%~20%;
消泡剂:1%~2%;
水:余量。
优选的,一种环保型农药乳化剂,由以下质量百分比的组分组成:
脂肪醇聚氧烷基醚:40%~50%;
阴离子表面活性剂:10%~20%;
防冻剂:5%~15%;
消泡剂:1%~2%;
水:余量。
优选的,所述脂肪醇聚氧烷基醚的结构式为:
R-O-(AO)a-[(EO)m-(PO)n]-H或R-O-[(EO)m-(PO)n]-(AO)a-H,其中,R为碳原子数6~18的烷基或烯基,A为-CH2CH2-、-CH2CH2CH2-或-CH2CH2CH2CH2-,(EO)m-(PO)n为-CH2CH2O-单元和-CH2CH2CH2O-单元以嵌段、交替或无规则分布构成的聚氧烷基链,a为1~10的整数,m和n为0~10的整数。
优选的,所述阴离子表面活性剂为十二烷基苯磺酸钠、乙氧基化烷基硫酸钠、脂肪酸甲酯磺酸盐、α-烯基磺酸盐、仲烷基磺酸钠中的至少一种。
优选的,所述防冻剂为乙二醇、丙二醇、丙三醇、聚乙二醇、山梨醇中的至少一种。
优选的,所述聚乙二醇的数均分子量为200~600g/mol。
优选的,所述消泡剂为有机硅消泡剂、高碳醇消泡剂中的至少一种。
一种农药水剂,包含上述环保型农药乳化剂。
优选的,所述农药水剂中环保型农药乳化剂的质量百分含量为5%~15%。
优选的,所述农药水剂中的农药活性成分为啶虫脒、氯虫苯甲酰胺、噻虫嗪、氰氟草酯、氟虫腈、莠去津、硝磺草酮中的至少一种。
优选的,所述农药活性成分的质量百分含量为1%~15%。
本发明的有益效果是:本发明的乳化剂乳化效果优异,不含APEO,安全环保,将其用于农药水剂可以保持农药水剂长期稳定。
具体实施方式
下面结合具体实施例对本发明作进一步的解释和说明。
实施例1:
一种环保型农药乳化剂,其组成如下表所示:
表1一种环保型农药乳化剂的组成表
原料 | 质量百分比(%) |
支链型C<sub>12</sub>H<sub>25</sub>-O-(EO)<sub>4</sub>-[(EO)<sub>3</sub>-(PO)<sub>3</sub>]-H | 40 |
十二烷基苯磺酸钠 | 10 |
乙二醇 | 10 |
有机硅消泡剂 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述环保型农药乳化剂,具体组成如下表所示:
表2一种农药水剂的组成表
原料 | 质量百分比(%) |
环保型农药乳化剂 | 10 |
啶虫脒 | 2 |
去离子水 | 余量 |
实施例2:
一种环保型农药乳化剂,其组成如下表所示:
表3一种环保型农药乳化剂的组成表
原料 | 质量百分比(%) |
直链型C<sub>14</sub>H<sub>29</sub>-O-[(EO)<sub>2</sub>-(PO)<sub>4</sub>]-(EO)<sub>4</sub>-H | 50 |
十二烷基聚乙烯醚硫酸钠 | 12 |
丙二醇 | 10 |
有机硅消泡剂 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述环保型农药乳化剂,具体组成如下表所示:
表4一种农药水剂的组成表
原料 | 质量百分比(%) |
环保型农药乳化剂 | 7 |
氯虫苯甲酰胺 | 3 |
去离子水 | 余量 |
实施例3:
一种环保型农药乳化剂,其组成如下表所示:
表5一种环保型农药乳化剂的组成表
原料 | 质量百分比(%) |
直链型C<sub>12</sub>H<sub>25</sub>-O-(EO)<sub>3</sub>-[(EO)<sub>2</sub>-(PO)<sub>3</sub>]-H | 40 |
α-烯基磺酸盐 | 12 |
丙二醇 | 10 |
有机硅消泡剂 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述环保型农药乳化剂,具体组成如下表所示:
表6一种农药水剂的组成表
原料 | 质量百分比(%) |
环保型农药乳化剂 | 10 |
噻虫嗪 | 2 |
去离子水 | 余量 |
实施例4:
一种环保型农药乳化剂,其组成如下表所示:
表7一种环保型农药乳化剂的组成表
原料 | 质量百分比(%) |
支链型C<sub>13</sub>H<sub>27</sub>-O-[(EO)<sub>2</sub>-(PO)<sub>4</sub>]-(EO)<sub>4</sub>-H | 45 |
脂肪酸甲酯磺酸盐 | 15 |
聚乙二醇(数均分子量400g/mol) | 10 |
有机硅消泡剂 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述环保型农药乳化剂,具体组成如下表所示:
表8一种农药水剂的组成表
实施例5:
一种环保型农药乳化剂,其组成如下表所示:
表9一种环保型农药乳化剂的组成表
原料 | 质量百分比(%) |
支链型C<sub>13</sub>H<sub>27</sub>-O-(EO)<sub>3</sub>-[(EO)<sub>4</sub>-(PO)<sub>4</sub>]-H | 50 |
脂肪酸甲酯磺酸盐 | 10 |
丙三醇 | 10 |
十二醇 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述环保型农药乳化剂,具体组成如下表所示:
表10一种农药水剂的组成表
原料 | 质量百分比(%) |
环保型农药乳化剂 | 8 |
氟虫腈 | 5 |
去离子水 | 余量 |
对比例1:
一种农药乳化剂,其组成如下表所示:
表11一种农药乳化剂的组成表
原料 | 质量百分比(%) |
蓖麻油聚氧乙烯醚 | 40 |
失水山梨醇脂肪酸酯 | 20 |
丙三醇 | 5 |
十二醇 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述农药乳化剂,具体组成如下表所示:
表12一种农药水剂的组成表
对比例2:
一种农药乳化剂,其组成如下表所示:
表13一种农药乳化剂的组成表
原料 | 质量百分比(%) |
月桂醇聚氧乙烯醚 | 50 |
直链十醇聚氧乙烯醚 | 30 |
丙二醇 | 5 |
有机硅消泡剂 | 1 |
去离子水 | 余量 |
一种农药水剂,包含上述农药乳化剂,具体组成如下表所示:
表14一种农药水剂的组成表
原料 | 质量百分比(%) |
农药乳化剂 | 10 |
氯虫苯甲酰胺 | 3 |
去离子水 | 余量 |
对比例3:
一种农药乳化剂,其组成如下表所示:
表15一种农药乳化剂的组成表
原料 | 质量百分比(%) |
月桂醇聚氧乙烯醚磺酸钠 | 40 |
十醇聚氧乙烯醚羧酸钠 | 20 |
丙二醇 | 5 |
有机硅消泡剂 | 2 |
去离子水 | 余量 |
一种农药水剂,包含上述农药乳化剂,具体组成如下表所示:
表16一种农药水剂的组成表
原料 | 质量百分比(%) |
农药乳化剂 | 8 |
噻虫嗪 | 2 |
去离子水 | 余量 |
对比例4:
一种农药水剂,其组成如下表所示:
表17一种农药水剂的组成表
原料 | 质量百分比(%) |
支链型C<sub>13</sub>H<sub>27</sub>-O-(EO)<sub>3</sub>-[(EO)<sub>4</sub>-(PO)<sub>4</sub>]-H | 8 |
氟虫腈 | 5 |
去离子水 | 余量 |
对比例5:
一种农药水剂,其组成如下表所示:
表18一种农药水剂的组成表
原料 | 质量百分比(%) |
脂肪酸甲酯磺酸盐 | 8 |
氟虫腈 | 5 |
去离子水 | 余量 |
注:
实施例1~5和对比例4中的EO为-CH2CH2O-单元,PO为-CH2CH2CH2O-单元。
测试例:
1)对实施例1~5和对比例1~5的农药水剂进行分散性和稳定性测试,测试结果如下表所示:
表19实施例1~5和对比例1~5的农药水剂的分散性和稳定性测试结果
注:
分散性测试方法:取1mL农药水剂倒入250mL的烧杯中,再用浓度342mg/L的标准硬水稀释200倍,并用玻璃棒不断搅拌,再将烧杯放入恒温水浴中,在30±2℃的条件下静置1h,并根据以下标准进行评级:
一级:自动云雾状均匀分散,无可见油珠,试样澄清透明;
二级:自动云雾状均匀分散,无可见油珠,试样呈澄清半透明;
三级:自动云雾状分散,无可见油珠,试样澄清呈白色;
四级:部分自动分散,乳化颗粒粗,试样呈白色;
五级:不会自动分散,入水呈油珠状,摇动后可乳化,放置则很快分层。
稳定性测试方法:参照GB/T 1603-2001进行测试。在250mL烧杯中加入99.5mL标准硬水,用移液管吸取0.5mL农药水剂,在不断搅拌的情况下慢慢加入硬水中,将其配成100mL乳状液。加完乳剂后,继续用2~3r/s的速度搅拌30s,立即将乳状液移至清洁、干燥的100mL量筒中,并将量筒置于恒温水浴内,在30±2℃的条件下静置1h,取出,观察乳状液分离情况,如在量筒中无浮油、沉油和沉淀析出,则判定乳液稳定性合格。
低温析出率测试方法:参考GB/T 19137-2003农药低温稳定性测定方法进行测试。移取100mL的农药水剂置于离心管中,在制冷器中冷却至0±2℃,让离心管及内容物在0±2℃保持1h,并每间隔15min搅拌一次,每次15s,检查并记录有无固体物或油状物析出。将离心管放回制冷器,在0±2℃继续放置7d,7d后,将离心管取出,在室温下静止3h,离心分离15min(管子顶部相对离心力为500~600g,g为重力加速度),记录管子底部离析物的体积(精确至0.05mL),计算析出率。
热贮析出率测试方法:参考GB/T 19136-2003农药热贮稳定性测试方法进行测试。用注射器将约30mL农药水剂注入洁净的安瓿瓶中,置此安瓿瓶于冰盐浴中制冷,用高温火焰封口,冷却至室温称重。将封好的安瓿瓶置于金属容器内,再将金属容器在54±2℃的恒温箱中放置14d,取出,将安瓿瓶外面拭净后称量,质量未发生变化的试样,计算析出率。
由表19可知:
1)实施例1~5的环保型农药乳化剂具有良好的乳化分散性,兑水稀释时具备良好的乳化效果,都可得到澄清的农药水剂;
2)实施例1~5的农药水剂具有良好的乳液稳定性,在正常的运输搬运过程中不会分层,而对比例1~5的农药水剂在测试条件下已经出现分层;
3)实施例1~5的农药水剂在低温条件下性能稳定,依然能保持稳定均一的溶液体系,而对比例1~5的农药水剂则出现不同程度的物质析出;
4)在高温条件下所有农药水剂均未出现析出分层,但实施例1~5的农药水剂的析出率远远小于对比例1~5的农药水剂,说明其高温稳定性更好;
5)脂肪醇聚氧烷基醚和阴离子表面活性剂两者都是必备组分,具有优异的协同作用,双组分的总体效果优于单一组分。
2)对实施例1~5和对比例1~5的农药水剂进行乳液粒径和粒径分布测试,测试结果如下表所示:
表20实施例1~5和对比例1~5的农药水剂的乳液粒径和粒径分布测试结果
实验组 | 乳液粒径(nm) | 粒径分布 |
实施例1 | 58 | 0.055 |
实施例2 | 55 | 0.098 |
实施例3 | 60 | 0.075 |
实施例4 | 85 | 0.068 |
实施例5 | 80 | 0.096 |
对比例1 | 110 | 0.135 |
对比例2 | 120 | 0.165 |
对比例3 | 280 | 0.203 |
对比例4 | 130 | 0.180 |
对比例5 | 430 | 0.290 |
注:
乳液粒径和粒径分布使用动态粒径测试仪进行测试。
乳液粒径越小,越不易沉降,分散效果越好,且粒径小也有利于有效成分穿透植物或昆虫的表皮,更好的发挥药效。
粒径分布值越小,说明粒径大小分布越窄,当PDI≤0.1时,说明分布均一,当PDI≥0.2时,说明分布不均。
由表20可知:
1)实施例1~5的农药水剂的乳液粒径均小于100nm,粒径分布值均小于0.1,而对比例1~5的乳液粒径均大于100nm,粒径分布值均大于0.1,说明实施例1~5的农药水剂的更稳定,不易分层沉降,粒径分布均一;
2)脂肪醇聚氧烷基醚和阴离子表面活性剂两者都是必备组分,具有优异的协同作用,双组分的总体效果优于单一组分。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (8)
1.一种环保型农药乳化剂,其特征在于:由以下质量百分比的组分组成:
脂肪醇聚氧烷基醚:40%~50%;
阴离子表面活性剂:10%~20%;
防冻剂:5%~15%;
消泡剂:1%~2%;
水:余量;
所述脂肪醇聚氧烷基醚为支链型C12H25-O-(EO)4-[(EO)3-(PO)3]-H、直链型C14H29-O-[(EO)2-(PO)4]-(EO)4-H、直链型C12H25-O-(EO)3-[(EO)2-(PO)3]-H、支链型C13H27-O-[(EO)2-(PO)4]-(EO)4-H、支链型C13H27-O-(EO)3-[(EO)4-(PO)4]-H中的一种;
所述阴离子表面活性剂为十二烷基苯磺酸钠、乙氧基化烷基硫酸钠、脂肪酸甲酯磺酸盐、α-烯基磺酸盐、仲烷基磺酸钠中的至少一种。
2.根据权利要求1所述的环保型农药乳化剂,其特征在于:所述防冻剂为乙二醇、丙二醇、丙三醇、聚乙二醇、山梨醇中的至少一种。
3.根据权利要求2所述的环保型农药乳化剂,其特征在于:所述聚乙二醇的数均分子量为200~600g/mol。
4.根据权利要求1所述的环保型农药乳化剂,其特征在于:所述消泡剂为有机硅消泡剂、高碳醇消泡剂中的至少一种。
5.一种农药水剂,其特征在于:包含权利要求1~4中任意一项所述的环保型农药乳化剂。
6.根据权利要求5所述的农药水剂,其特征在于:所述环保型农药乳化剂的质量百分含量为5%~15%。
7.根据权利要求5或6所述的农药水剂,其特征在于:农药活性成分为啶虫脒、氯虫苯甲酰胺、噻虫嗪、氰氟草酯、氟虫腈、莠去津、硝磺草酮中的至少一种。
8.根据权利要求7所述的农药水剂,其特征在于:所述农药活性成分的质量百分含量为1%~15%。
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