CN109221114A - 一种二甲戊灵悬浮剂用梳型分散剂的制备方法 - Google Patents
一种二甲戊灵悬浮剂用梳型分散剂的制备方法 Download PDFInfo
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
-
- 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
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Abstract
本发明公开了一种二甲戊灵悬浮剂用梳型分散剂的制备方法。该方法为将配方量溶剂、配方量甲基烯丙醇聚氧乙烯醚和对苯乙烯磺酸钠加入到250ml四口烧瓶中,温度升至90℃时,滴加配方量甲基丙烯酸羟乙酯和50ml过硫酸铵溶液,控制滴定速度,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用NaOH水溶液中和,使PH在7‑8左右。反应产物用透析袋纯化后经冷冻干燥,得到淡黄色聚羧酸盐分散剂。本发明工艺简单,耗能低,可以大规模生产,基于该分散剂制备的二甲戊灵悬浮剂性能优异。
Description
技术领域
本发明涉及一种二甲戊灵悬浮剂用梳型分散剂的制备方法。
背景技术
二甲戊灵是一种杀草谱广,持续药效长的苯胺类选择性除草剂,但是在实际应用中发现高浓度二甲戊灵悬浮剂在贮存过程中稳定性差,容易出现稠化、沉积、结块、析水等问题,影响悬浮剂的药效,而合理运用性能优良的分散剂是改善高含量二甲戊灵悬浮剂稳定性的有效方法。
传统的小分子分散剂可以使二甲戊灵固体颗粒分散,但对颗粒表面的吸附不牢固,容易从颗粒表面解吸而导致颗粒重新聚集或沉淀,很难满足悬浮剂加工需求。聚羧酸盐分散剂是阴离子型分散剂,可以与固体颗粒表面的部分官能团形成氢键等作用力,依靠空间位阻及静电斥力对固体颗粒的分散可以有效弥补小分子分散剂的不足,提高悬浮稳定性。聚羧酸盐分散剂具有特殊的梳状碳骨架结构,对晶体表面具有强烈的亲和性,被吸附到晶体表面后能够起到抑制晶体长大的作用,这种特殊的结构保证了其良好的分散性能。通过改变侧链的种类和长度,可以很容易地对聚羧酸盐分散剂的分子结构进行修改,改进的分子结构有助于最大限度地提高目标性能,满足不同应用的具体要求。目前,有很多学者研究了聚羧酸盐分散剂的结构与性能的关系,并广泛应用于水泥、陶瓷、农药悬浮剂体系等领域。
发明内容
本发明的目的是克服现有二甲戊灵悬浮剂所用分散剂技术不足,提供一种二甲戊灵悬浮剂用梳型分散剂的制备方法。
本发明的目的是通过以下技术方案实现的:一种二甲戊灵悬浮剂用梳型分散剂的制备方法,该方法为:将溶剂、甲基烯丙醇聚氧乙烯醚和对苯乙烯磺酸钠混合后,温度升至90℃时,滴加甲基丙烯酸羟乙酯和过硫酸铵溶液,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用NaOH水溶液中和,使PH在7‐8左右。反应产物用透析袋纯化后经冷冻干燥,得到聚羧酸盐分散剂。其中,甲基烯丙醇聚氧乙烯醚HPEG:对苯乙烯磺酸钠SSS:甲基丙烯酸羟乙酯HEMA质量比例10:1~5:2~10,引发剂的质量占单体总量的4%。
进一步地,所述溶剂为乙醇和水按照体积比1:3组成的混合溶剂。
进一步地,所述过硫酸铵溶液为8wt%过硫酸铵的水溶液。
进一步地,所述NaOH水溶液的浓度为30wt%。
进一步地,所述透析袋的规格为3000分子量。
进一步地,甲基烯丙醇聚氧乙烯醚HPEG:对苯乙烯磺酸钠SSS:甲基丙烯酸羟乙酯HEMA质量比例10:1:4,过硫酸铵的质量占单体总量的4%。
本发明的有益效果在于:
本发明根据自由基聚合及分散机理,采用甲基烯丙醇聚氧乙烯醚、甲基丙烯酸羟乙酯和对苯乙烯磺酸钠为单体合成一种水溶性良好的梳状分散剂,引入酯基、羟基、磺酸基多种锚固基团和聚醚高分子溶剂化链,该聚羧酸盐还具有良好的润湿性能,能有效地在亲水和疏水叶片上铺展,这一特性有利于二甲戊灵药效的有效发挥;该分散剂的磺酸基为分散提供静电作用,-OH、-C=O极性基团提供氢键作用,PEO侧链形成亲水性溶剂层,提供了空间障碍效应。该分散剂是制备二甲戊灵悬浮剂的优良选择。
经过大量实验,在反应溶剂乙醇和水比例为1:3、HPEG:SSS:HEMA质量比例10:1:4、引发剂用量占单体总量4%时溶剂化链和锚固基团之间达到平衡,二甲戊灵颗粒表面的聚羧酸盐分散剂吸附密度和吸附层厚度达到最优,筛选后的聚羧酸盐分散剂制备成高浓度二甲戊灵悬浮剂具有良好的分散性能和润湿性能。
本发明制备工艺简单,制备的分散剂对二甲戊灵的分散性能优异,适用于大规模生产,可以用于二甲戊灵悬浮剂的制备,同时可以为其他类农药、兽药、人药悬浮剂的制备提供参考。
附图说明
图1:不同浓度的聚羧酸盐分散剂分散二甲戊灵后粒径分布图;
图2:聚羧酸盐分散剂分散的二甲戊灵在加热处理后的粒径分布图;
图3:聚羧酸盐分散剂分散的二甲戊灵在紫甘蓝和黄瓜叶面铺展情况。
具体实施方式
以下结合实例进一步说明本发明内容。
实施例1:将30ml乙醇、90ml水、10克甲基烯丙醇聚氧乙烯醚和1克对苯乙烯磺酸钠加入到250ml四口烧瓶中,温度升至90℃时,滴加4克甲基丙烯酸羟乙酯和7.5ml 8%过硫酸铵水溶液,控制滴定速度,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用30wt%的NaOH水溶液中和,使PH在7‐8左右。反应产物用3000分子量的透析袋纯化后经冷冻干燥,得到淡黄色聚羧酸盐分散剂。
向25ml具塞量筒加入1.00g聚羧酸盐分散剂,加入约10ml去离子水,使聚合物溶解,再加入2.50g二甲戊灵细粉末,加水至25.00ml,混匀,制得二甲戊灵悬浮液。测定二甲戊灵悬浮液的悬浮性能为96.16%。
取12克二甲戊灵,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水16.01克,获得聚羧酸盐分散剂含量为0%二甲戊灵悬浮体系。取12克二甲戊灵,1.65克分散剂,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水14.36克,获得聚羧酸盐分散剂含量为5%二甲戊灵悬浮体系。取12克二甲戊灵,3.30克分散剂,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水12.71克,获得聚羧酸盐分散剂含量为10%二甲戊灵悬浮体系。分散剂含量对粒径的影响如图1所示。
取12克二甲戊灵,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水16.01克,获得聚羧酸盐分散剂含量为0%二甲戊灵悬浮体系。取12克二甲戊灵,3.30克分散剂,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水12.71克,获得聚羧酸盐分散剂含量为10%二甲戊灵悬浮体系。取约30mL二甲戊灵悬浮剂于安瓿瓶中,用高温火焰封口,于(54±2)℃恒温箱中放置14天。取出冷却至室温,稀释后,测定热贮前后的粒径如图2所示。
取12克二甲戊灵,3.30克分散剂,0.07克黄原胶,0.07克消泡剂,硅酸镁铝0.25克,丙三醇1.6克,去离子水12.71克,获得聚羧酸盐分散剂含量为10%二甲戊灵悬浮体系。该体系在在植物叶片上的铺展性能如图3所示。
实施例2:将30ml乙醇、90ml水、10克甲基烯丙醇聚氧乙烯醚和5克对苯乙烯磺酸钠加入到250ml四口烧瓶中,温度升至90℃时,滴加2克甲基丙烯酸羟乙酯和7.5ml 8%过硫酸铵水溶液,控制滴定速度,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用30wt%的NaOH水溶液中和,使PH在7‐8左右。反应产物用3000分子量的透析袋纯化后经冷冻干燥,得到淡黄色聚羧酸盐分散剂。
按照实施例1所述的方法对本实施例制备得到的聚羧酸盐分散剂进行效果验证,结果表明,本实施例制备得到的聚羧酸盐分散剂对二甲戊灵具有良好的分散性能和润湿性能,可用于高浓度二甲戊灵悬浮剂的制备。
实施例3:将30ml乙醇、90ml水、10克甲基烯丙醇聚氧乙烯醚和3克对苯乙烯磺酸钠加入到250ml四口烧瓶中,温度升至90℃时,滴加10克甲基丙烯酸羟乙酯和7.5ml 8%过硫酸铵水溶液,控制滴定速度,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用30wt%的NaOH水溶液中和,使PH在7‐8左右。反应产物用3000分子量的透析袋纯化后经冷冻干燥,得到淡黄色聚羧酸盐分散剂。
按照实施例1所述的方法对本实施例制备得到的聚羧酸盐分散剂进行效果验证,结果表明,本实施例制备得到的聚羧酸盐分散剂对二甲戊灵具有良好的分散性能和润湿性能,可用于高浓度二甲戊灵悬浮剂的制备。
Claims (6)
1.一种二甲戊灵悬浮剂用梳型分散剂的制备方法,其特征在于,该方法为:将溶剂、甲基烯丙醇聚氧乙烯醚和对苯乙烯磺酸钠混合后,温度升至90℃时,滴加甲基丙烯酸羟乙酯和过硫酸铵溶液,反应过程中氮气保护,反应3小时,停止加热,继续搅拌冷却至室温后用NaOH水溶液中和,使PH在7‐8左右。反应产物用透析袋纯化后经冷冻干燥,得到聚羧酸盐分散剂。其中,甲基烯丙醇聚氧乙烯醚HPEG:对苯乙烯磺酸钠SSS:甲基丙烯酸羟乙酯HEMA质量比例10:1~5:2~10,引发剂的质量占单体总量的4%。
2.根据权利要求1所述的方法,其特征在于,所述溶剂为乙醇和水按照体积比1:3组成的混合溶剂。
3.根据权利要求1所述的方法,其特征在于,所述过硫酸铵溶液为8wt%过硫酸铵的水溶液。
4.根据权利要求1所述的方法,其特征在于,所述NaOH水溶液的浓度为30wt%。
5.根据权利要求1所述的方法,其特征在于,所述透析袋的规格为3000分子量。
6.根据权利要求1所述的方法,其特征在于,甲基烯丙醇聚氧乙烯醚HPEG:对苯乙烯磺酸钠SSS:甲基丙烯酸羟乙酯HEMA质量比例10:1:4,过硫酸铵的质量占单体总量的4%。
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