基于绿色表面活性剂的农药环境友好型制剂的研究
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摘要
近年来,随着人们环保意识的增强,对表面活性剂的开发和应用提出了更高的要求,绿色表面活性剂的制备和应用已成为研究的热点。与常规表面活性剂相比,绿色表面活性剂是指由天然或再生资源加工的,对人体刺激性小和易于生物降解的表面活性剂。在表面活性剂行业中,农用表面活性剂是一个重要的领域。本文以常见绿色表面活性剂脂肪酸甲酯磺酸盐(MES)、烷基糖苷(APG)、脂肪醇聚氧乙烯醚(AEO)、醇醚羧酸盐(AEC)、单烷基磷酸酯钾盐(MAPK)、α-烯基磺酸盐(AOS)等为材料研究在其制备常见农药制剂的可能性,结果表明,绿色表面活性剂单独使用或者与常规表面活性剂复配使用可以制备出质量技术指标符合要求的5%联苯菊酯水乳剂、5%联苯菊酯微乳剂、3%甲维盐微乳剂、5%甲维盐水分散粒剂、1OOOOIU/mg苏云金杆菌(BT)悬浮剂、10000IU/mg苏云金杆菌(BT)水分散粒剂。
分别在成功筛选出制备5%联苯菊酯水乳剂的绿色表面活性剂和常规表面活性剂最佳复配比例和用量的基础上,比较了两类表面活性剂对制剂稳定性的影响,同时探讨水乳剂不稳定机理及水乳剂稳定性快速判断的方法,结果表明,1)通过筛选表面活性剂组合最佳复配比例和用量可以制备粒剂大小为纳米级的水乳剂,当绿色表面活性剂组合MAPK:AEO=6:4时,乳化剂用量10%时,制备的水乳剂最稳定,水乳剂的初始粒径为200.7nm；当常规表面活性剂组合NP-1OP:EL-60=5:5时,乳化剂用量10%时,制备的水乳剂最稳定,水乳剂的初始粒径为288.9nm；2)两种乳化剂复配体系可以制备出较稳定的水乳剂是因为在最佳比例时,两种表面活性剂间有一定的协同作用,当MAP:AEO=6:4时,水乳剂的粒径变化最小,试验发现在此比例时,表面活性剂复配后有最小的临界胶束浓度(cmc)、临界胶束浓度时的表面张力(γcmc)和表面吸附层被吸附分子的平均截面积(Acmc)；3)水乳剂的粒径的立方随时间变化呈较好的线性关系,表明奥氏熟化是水乳剂不稳定的重要原因之一；4)可以用稳定性分析仪的短期描替代动态光散射技术的测试,来对水乳剂的粒径变化进行快速判断；5)绿色表面活性剂组合MAPK-AEO制备的水乳剂粒径增加速率小于常规表面活性剂NP-10P-EL-60组合,绿色表面活性剂制备的水乳剂更加稳定。
分别在用拟三元相图法筛选出制备3%甲维盐微乳剂的绿色表面活性剂和常规表面活性剂最佳复配比例的基础上,比较了两类表面活性剂复配体系对甲维盐原药的增溶能力。结果表明,绿色表面活性剂组合MAPK:APG=2:1和常规表面活性剂组合NP-10P：OP-10=1：2时有利于甲维盐微乳剂的形成,在最佳复配比例下绿色表面活性剂复配体系对甲维盐的增溶能力低于常规表面活性剂复配体系。
室内生物活性表明,分别用绿色表面活性剂和常规表面活性剂制备的5%联苯菊酯水乳剂对黏虫、3%甲维盐微乳剂对小菜蛾的生物活性没有显著差异。
生物降解试验表明,绿色表面活性剂的生物降解性较常规表面活性剂好；斑马鱼安全性评价测试结果显示,除常规表面活性剂OP-10对斑马鱼为中毒外,其余表面活性剂对斑马鱼均为低毒,绿色与常规表面活性剂对斑马鱼LC50值大小存在差异；大型溞安全性评价测试结果显示,除常规表面活性剂OP-10、MOA9PK、T-2700、NNO对大型溞为中毒外,其余表面活性剂对大型溞均为低毒,绿色与常规表面活性剂对大型溞LC50值大小存在差异。
在乳化剂总量10%情况下,通过调节阴、非离子乳化剂的复配比例来调节体系的HLB值,通过Turbuscan稳定性分析仪的短期扫描确定了制备5%联苯菊酯、高效氯氟氰菊酯和氯菊酯水乳剂的最佳HLB值分别为10.82、9.48、10.15,而且在相同表面活性剂用量、最佳比例制备的水乳剂质量技术指标均符合要求,MAPK和AEO-3可以复配作为制备菊酯类农药水乳剂的专用乳化剂。运用绿色表面活性剂MAPK和APG复配,运用拟三元相图分别筛选出制备3%阿维菌素、甲维盐和伊维菌素ME的最佳比例分别为2：1、2：1、1：1,在乳化剂总量10%含量下,分别制备了技术指标符合要求的微乳剂,MAPK和APG可以复配作为制备大环内酯类农药微乳剂的专用乳化剂。
In recent years, as people's consciousness of environmental protection get much stronger, the development and application of surfactants have been put forward higher request, the preparation and application of green surfactants have become the research focus. Compared with the traditional surfactant, green surfactant is refers to by natural or processing of renewable resources, to human body excitant small and easy to biodegradation of surfactants, green surfactant is produced by natural or renewable resources, mild to human body and easy to biodegradation. In surfactant industry, agricultural surfactant is an important field. The possibility of preparing the common pesticides formulation using the green surfactant, such as MES, APG, AEO, AEC, MAPK, AOS was studied. The results showed that using green surfactants alone or mixed system with traditional surfactants, bifenthrin50EW, bifenthrin50ME, emamectin benzoate30ME, emamectin benzoate50WDG,10000IU/mg Bacillus thuringiensis SC and10000IU/mg Bacillus thuringiensis WDG were prepared and their quality and technical indexes meet the requirements.
Based on choosing the best mixing ratio and dosage of green surfactant and traditional surfactant respectively to prepare the bifenthrin50EW, comparison of the effect of the two types of surfactant on the effect on the stability was made and also, the emulsion instability mechanism and fast judgment method of stability of the emulsion were discussion, the results showed that,1) the stable nano-emulsions could be prepared by choosing the best mixing ratio and dosage of the two surfactants, when the mixing ratio of MAPK and AEO was6:4and the dosage was10%, the emulsion prepared with green surfactants was more stable and the original droplet size was200.7nm, while the mixing ratio of NP-10P and EL-60was5:5and the dosage was10%, the emulsion prepared with traditional surfactants was more stable and the original droplet size was288.9nm.2) The reason of why the emulsion showed the most stable was the mixed system of MAPK and AEO has the smallest cmc, ycmc, Acmc when the mixing ratio was6:4and the two emulsifiers have a synergistic effect.3) A good correlation of r3and time was obtained with good regression coefficient for all emulsions, indicating that Ostwald ripening was the driving force for instability.4) The dynamic light scattering technique can be replaced by short-term scan of stability analyzer to judge the stability of the emulsion.5) The increasement rate of droplet size of emulsion prepared with MAPK-AEO was smaller than that of NP-10P-EL-60, the emulsion prepared with green surfactant showed more stable.
Based on choosing the best mixing ratio of green surfactants mixture and traditional surfactants mixture respectively using pseudo-ternary phase diagram to prepare the emamectin benzoate30ME, comparison of solubilising power on emamectin benzoate with two kinds of surfactants was made. The results showed that the micro-emulsion of emamectin benzoate was much easier to form when the MAPK: APG=2:1and NP-10P:OP-10=1:2, the solubilising power on emamectin benzoate of green surfactants mixture was low than that of traditional surfactants mixture.
The bioassay in the room showed that the bioactivity on Mythimna seperata of bifenthrin50EW prepared with green surfactants had no marked difference with the emamectin benzoate30ME prepared with traditional surfactants. The bioactivity on Plutella xylostella of emamectin benzoate30'ME has the same result.
The biodegradation experiment showed that the green surfactants have better bio degradation rate than traditional surfactants. Safety estimation of the two kinds of surfactants on zebra fish showed that the surfactants for test were all low toxic to zebra fish except the OP-10was moderate toxic and there was a difference of LC50value on zebra fish between green and traditional surfactants. Safety estimation of the two kinds of surfactants on Daphnia magna showed that the surfactants for test were all low toxic to Daphnia magna except the OP-10, MOA9PK, T-2700, NNO were moderate toxic and there was a difference of LC50value on Daphnia magna between green and traditional surfactants.
Make certain the optimal HLB value to prepare bifenthrin50EW, lambda-cyhalothrin50EW and permethrin50EW by adjusting the mixing ratios of anion-nonionic surfactants with a constant total concentration (10%) using short-term scan of turbiscan lab stability analyzer. The optimal HLB value to prepare bifenthrin50EW, lambda-cyhalothrin50EW and permethrin50EW was10.82、9.48、10.15respectively. The quality and technical indexes all the formulation prepare with the best mixing ratio and the same surfactant concentration meet the requirements. The mixture of MAPK and AEO-3could be used for prepare pyrethroid pesticide emulsions. The best mixing ratio of MAPK and APG mixture to prepare avermectins30ME, emamectin benzoate30ME and ivermectin30ME was2:1,2:1,1:1using pseudo-ternary phase diagram to study. The quality and technical indexes all the formulation prepare with the best mixing ratio and the same surfactant concentration meet the requirements. The mixture of MAPK and APG could be used for prepare macrolides antibiotics pesticide micro emulsions.
分别在成功筛选出制备5%联苯菊酯水乳剂的绿色表面活性剂和常规表面活性剂最佳复配比例和用量的基础上,比较了两类表面活性剂对制剂稳定性的影响,同时探讨水乳剂不稳定机理及水乳剂稳定性快速判断的方法,结果表明,1)通过筛选表面活性剂组合最佳复配比例和用量可以制备粒剂大小为纳米级的水乳剂,当绿色表面活性剂组合MAPK:AEO=6:4时,乳化剂用量10%时,制备的水乳剂最稳定,水乳剂的初始粒径为200.7nm；当常规表面活性剂组合NP-1OP:EL-60=5:5时,乳化剂用量10%时,制备的水乳剂最稳定,水乳剂的初始粒径为288.9nm；2)两种乳化剂复配体系可以制备出较稳定的水乳剂是因为在最佳比例时,两种表面活性剂间有一定的协同作用,当MAP:AEO=6:4时,水乳剂的粒径变化最小,试验发现在此比例时,表面活性剂复配后有最小的临界胶束浓度(cmc)、临界胶束浓度时的表面张力(γcmc)和表面吸附层被吸附分子的平均截面积(Acmc)；3)水乳剂的粒径的立方随时间变化呈较好的线性关系,表明奥氏熟化是水乳剂不稳定的重要原因之一；4)可以用稳定性分析仪的短期描替代动态光散射技术的测试,来对水乳剂的粒径变化进行快速判断；5)绿色表面活性剂组合MAPK-AEO制备的水乳剂粒径增加速率小于常规表面活性剂NP-10P-EL-60组合,绿色表面活性剂制备的水乳剂更加稳定。
分别在用拟三元相图法筛选出制备3%甲维盐微乳剂的绿色表面活性剂和常规表面活性剂最佳复配比例的基础上,比较了两类表面活性剂复配体系对甲维盐原药的增溶能力。结果表明,绿色表面活性剂组合MAPK:APG=2:1和常规表面活性剂组合NP-10P：OP-10=1：2时有利于甲维盐微乳剂的形成,在最佳复配比例下绿色表面活性剂复配体系对甲维盐的增溶能力低于常规表面活性剂复配体系。
室内生物活性表明,分别用绿色表面活性剂和常规表面活性剂制备的5%联苯菊酯水乳剂对黏虫、3%甲维盐微乳剂对小菜蛾的生物活性没有显著差异。
生物降解试验表明,绿色表面活性剂的生物降解性较常规表面活性剂好；斑马鱼安全性评价测试结果显示,除常规表面活性剂OP-10对斑马鱼为中毒外,其余表面活性剂对斑马鱼均为低毒,绿色与常规表面活性剂对斑马鱼LC50值大小存在差异；大型溞安全性评价测试结果显示,除常规表面活性剂OP-10、MOA9PK、T-2700、NNO对大型溞为中毒外,其余表面活性剂对大型溞均为低毒,绿色与常规表面活性剂对大型溞LC50值大小存在差异。
在乳化剂总量10%情况下,通过调节阴、非离子乳化剂的复配比例来调节体系的HLB值,通过Turbuscan稳定性分析仪的短期扫描确定了制备5%联苯菊酯、高效氯氟氰菊酯和氯菊酯水乳剂的最佳HLB值分别为10.82、9.48、10.15,而且在相同表面活性剂用量、最佳比例制备的水乳剂质量技术指标均符合要求,MAPK和AEO-3可以复配作为制备菊酯类农药水乳剂的专用乳化剂。运用绿色表面活性剂MAPK和APG复配,运用拟三元相图分别筛选出制备3%阿维菌素、甲维盐和伊维菌素ME的最佳比例分别为2：1、2：1、1：1,在乳化剂总量10%含量下,分别制备了技术指标符合要求的微乳剂,MAPK和APG可以复配作为制备大环内酯类农药微乳剂的专用乳化剂。
In recent years, as people's consciousness of environmental protection get much stronger, the development and application of surfactants have been put forward higher request, the preparation and application of green surfactants have become the research focus. Compared with the traditional surfactant, green surfactant is refers to by natural or processing of renewable resources, to human body excitant small and easy to biodegradation of surfactants, green surfactant is produced by natural or renewable resources, mild to human body and easy to biodegradation. In surfactant industry, agricultural surfactant is an important field. The possibility of preparing the common pesticides formulation using the green surfactant, such as MES, APG, AEO, AEC, MAPK, AOS was studied. The results showed that using green surfactants alone or mixed system with traditional surfactants, bifenthrin50EW, bifenthrin50ME, emamectin benzoate30ME, emamectin benzoate50WDG,10000IU/mg Bacillus thuringiensis SC and10000IU/mg Bacillus thuringiensis WDG were prepared and their quality and technical indexes meet the requirements.
Based on choosing the best mixing ratio and dosage of green surfactant and traditional surfactant respectively to prepare the bifenthrin50EW, comparison of the effect of the two types of surfactant on the effect on the stability was made and also, the emulsion instability mechanism and fast judgment method of stability of the emulsion were discussion, the results showed that,1) the stable nano-emulsions could be prepared by choosing the best mixing ratio and dosage of the two surfactants, when the mixing ratio of MAPK and AEO was6:4and the dosage was10%, the emulsion prepared with green surfactants was more stable and the original droplet size was200.7nm, while the mixing ratio of NP-10P and EL-60was5:5and the dosage was10%, the emulsion prepared with traditional surfactants was more stable and the original droplet size was288.9nm.2) The reason of why the emulsion showed the most stable was the mixed system of MAPK and AEO has the smallest cmc, ycmc, Acmc when the mixing ratio was6:4and the two emulsifiers have a synergistic effect.3) A good correlation of r3and time was obtained with good regression coefficient for all emulsions, indicating that Ostwald ripening was the driving force for instability.4) The dynamic light scattering technique can be replaced by short-term scan of stability analyzer to judge the stability of the emulsion.5) The increasement rate of droplet size of emulsion prepared with MAPK-AEO was smaller than that of NP-10P-EL-60, the emulsion prepared with green surfactant showed more stable.
Based on choosing the best mixing ratio of green surfactants mixture and traditional surfactants mixture respectively using pseudo-ternary phase diagram to prepare the emamectin benzoate30ME, comparison of solubilising power on emamectin benzoate with two kinds of surfactants was made. The results showed that the micro-emulsion of emamectin benzoate was much easier to form when the MAPK: APG=2:1and NP-10P:OP-10=1:2, the solubilising power on emamectin benzoate of green surfactants mixture was low than that of traditional surfactants mixture.
The bioassay in the room showed that the bioactivity on Mythimna seperata of bifenthrin50EW prepared with green surfactants had no marked difference with the emamectin benzoate30ME prepared with traditional surfactants. The bioactivity on Plutella xylostella of emamectin benzoate30'ME has the same result.
The biodegradation experiment showed that the green surfactants have better bio degradation rate than traditional surfactants. Safety estimation of the two kinds of surfactants on zebra fish showed that the surfactants for test were all low toxic to zebra fish except the OP-10was moderate toxic and there was a difference of LC50value on zebra fish between green and traditional surfactants. Safety estimation of the two kinds of surfactants on Daphnia magna showed that the surfactants for test were all low toxic to Daphnia magna except the OP-10, MOA9PK, T-2700, NNO were moderate toxic and there was a difference of LC50value on Daphnia magna between green and traditional surfactants.
Make certain the optimal HLB value to prepare bifenthrin50EW, lambda-cyhalothrin50EW and permethrin50EW by adjusting the mixing ratios of anion-nonionic surfactants with a constant total concentration (10%) using short-term scan of turbiscan lab stability analyzer. The optimal HLB value to prepare bifenthrin50EW, lambda-cyhalothrin50EW and permethrin50EW was10.82、9.48、10.15respectively. The quality and technical indexes all the formulation prepare with the best mixing ratio and the same surfactant concentration meet the requirements. The mixture of MAPK and AEO-3could be used for prepare pyrethroid pesticide emulsions. The best mixing ratio of MAPK and APG mixture to prepare avermectins30ME, emamectin benzoate30ME and ivermectin30ME was2:1,2:1,1:1using pseudo-ternary phase diagram to study. The quality and technical indexes all the formulation prepare with the best mixing ratio and the same surfactant concentration meet the requirements. The mixture of MAPK and APG could be used for prepare macrolides antibiotics pesticide micro emulsions.
引文
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