CN106614549A - 一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 - Google Patents
一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 Download PDFInfo
- Publication number
- CN106614549A CN106614549A CN201611230296.1A CN201611230296A CN106614549A CN 106614549 A CN106614549 A CN 106614549A CN 201611230296 A CN201611230296 A CN 201611230296A CN 106614549 A CN106614549 A CN 106614549A
- Authority
- CN
- China
- Prior art keywords
- ivermectin
- compounded
- adds
- dissolved
- chlorpyrifos
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
本发明公开了一种伊维菌素复配的毒死蜱微囊悬浮剂,及其制备工艺,其特征在于,以毒死蜱、聚碳酸亚丙酯、聚乙烯醇、聚乳酸、明胶、乳化硅油、海藻酸钠、有机膨润土、MCM‑41分子筛、KH550、聚丙烯酸、水滑石、伊维菌素、聚醚L‑64、尿素、N,N‑二甲基甲酰胺、乙二醇等为原料。本发明中有机膨润土与海藻酸钠共混改性,实现插层,提高疏水性及吸附效果,与生物可降解材料聚乳酸复合为壁材,制得药物缓释微胶囊。用KH550对MCM‑41分子筛进行改性作为载体,以带负电荷的聚丙烯酸为功能分子,通过静电吸附作用制备了缓释体系。以层状水滑石为主体,以微胶囊化的毒死蜱为客体分子,得到插层材料,制得一种毒死蜱微囊悬浮剂。
Description
技术领域
本发明涉及农药领域,具体涉及一种伊维菌素复配的毒死蜱微囊悬浮剂,及其制备工艺。
背景技术
毒死蜱是广泛使用的有机磷杀虫剂,可作为高毒农药的替代品,可应用于卫生及农业害虫的防治,可有效防治粮食、蔬菜、果树等多种作物上的百余种害虫。毒死蜱异味大、相对易光解、对敏感作物易产生药害,为提高其安全性与持效期、降低对环境的污染,将其进行微囊化。
孟锐在其研究论文《可降解聚碳酸亚丙酯-毒死蜱微胶囊的制备及缓释性能评价》一文中,以聚碳酸亚丙酯(PPC)为壁材,聚乙烯醇(PVA)为连续相稳定剂,采用乳化溶剂挥发法制备了包裹毒死蜱的可降解微胶囊,微胶囊对毒死蜱具有明显的缓释效应。取毒死蜱原药,将PPC溶于二氯甲烷中作为有机相,以PVA作为连续相,将连续相与有机相混合后在高剪切乳化分散机下乳化分散,使之形成稳定的O/W型乳液,室温下搅拌4h,直至二氯甲烷完全挥发,使微胶囊固化,将微胶囊悬浊液离心分离,用蒸馏水洗涤数次后冷冻干燥,收集微胶囊干样。但是存在缓释性能不足。
本发明中聚乳酸是一种高分子聚合物,具有优良的生物相容性、可降解性,无毒害;海藻酸钠具有无毒、低成本、可生物降解、生物相容性好的特点,有机膨润土与海藻酸钠共混改性,实现插层,提高疏水性及吸附效果,与生物可降解材料聚乳酸复合为壁材,加入消泡剂乳化硅油,制得药物的缓释微胶囊。介孔硅材料具有规则孔道、高比表面积等特点,用KH550对MCM-41分子筛进行改性作为载体,以带负电荷的聚丙烯酸为功能分子,通过静电吸附作用制备了缓释体系。以层状水滑石为主体,以微胶囊化的毒死蜱为客体分子,以乙醇为溶剂,制备得到插层材料;以聚甲基丙烯酸甲酯为壁材,以聚乙烯醇为连续相,制得了毒死蜱微囊悬浮剂。
发明内容
本发明主要解决的技术问题是提供一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备工艺,依照该工艺制作的微囊悬浮剂低毒、成本低、防效稳定、缓释性能好,可生物降解。
本发明所要解决的技术问题采用以下的技术方案来实现:
毒死蜱5-8,聚碳酸亚丙酯25-30,聚乙烯醇14-18,聚乳酸8-14,明胶5-10,乳化硅油0.1-0.3,海藻酸钠3-6,有机膨润土4-9,MCM-41分子筛4-8,KH550 1-3,聚丙烯酸3-6,水滑石4-7,伊维菌素1-2,聚醚L-64 3-7,尿素2-4,二氯甲烷、乙醇、甲苯、N,N-二甲基甲酰胺、乙二醇、蒸馏水适量。
一种伊维菌素复配的毒死蜱微囊悬浮剂的制备方法,其特征在于,按以下步骤进行:
a. 将聚乳酸1:5-10溶于二氯甲烷,聚乙烯醇、明胶1:1:50-100溶于蒸馏水,两者混合高速分散乳化30-50s,加入乳化硅油,磁力搅拌2-3h,得A液;向海藻酸钠中1:20-30加入蒸馏水,搅拌溶解,1:10-15加入有机膨润土、乙醇,超声分散1-2h,得B液;将A、B液均匀混合待用;
b. 向MCM-41分子筛中1:20-30加入甲苯,搅拌下滴加KH550,在氮气保护下,加热回流、搅拌反应2-4h,冷却至室温后,1:30-40加入聚丙烯酸、蒸馏水,磁力搅拌2-3h,过滤,醇洗水洗3-5次,干燥;
c. 在氮气保护下,将水滑石1:20-30溶于乙醇中形成透明溶液,与a、b中所得物料混合,调pH为6-7,在60-80℃下反应4-8h,产物经过滤、水洗醇洗3-5次,在烘箱中于80-90℃干燥2-3h;
d. 将伊维菌素1:20-30溶解于N,N-二甲基甲酰胺中,加入聚醚L-64,搅拌均匀,得到透明液;向尿素中1:5-10:15-20加入抗冻剂乙二醇、蒸馏水,磁力搅拌下,将其滴入透明液中,得到均匀溶液;
e. 将聚碳酸亚丙酯1:5-10溶于二氯甲烷中,加入毒死蜱,60-70℃振荡摇匀,与c、d中所得物料混合乳化分散5-10min,使之形成稳定的O/W型乳液,恒温水浴搅拌2-4h,即得到一种微囊悬浮剂。
本发明的反应机理如下:
(1)聚乳酸是一种高分子聚合物,具有优良的生物相容性、可降解性,无毒害;海藻酸钠具有无毒、低成本、可生物降解、生物相容性好的特点,有机膨润土与海藻酸钠共混改性,实现插层,提高疏水性及吸附效果,与生物可降解材料聚乳酸复合为壁材,加入消泡剂乳化硅油,制得药物的缓释微胶囊。
(2)介孔硅材料具有规则孔道、高比表面积等特点,用KH550对MCM-41分子筛进行改性作为载体,以带负电荷的聚丙烯酸为功能分子,通过静电吸附作用制备了缓释体系。
(3)以层状水滑石为主体,以微胶囊化的毒死蜱为客体分子,以乙醇为溶剂,制备得到插层材料;以聚甲基丙烯酸甲酯为壁材,以聚乙烯醇为连续相,制得了毒死蜱微囊悬浮剂。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例
一种伊维菌素复配的毒死蜱微囊悬浮剂,由下述重量份(g)的原料制得:
毒死蜱8,聚碳酸亚丙30,聚乙烯醇18,聚乳酸14,明胶10,乳化硅油0.3,海藻酸钠6,有机膨润土9,MCM-41分子筛8,KH550 3,聚丙烯酸6,水滑石7,伊维菌素2,聚醚L-64 7,尿素4,二氯甲烷、乙醇、甲苯、N,N-二甲基甲酰胺、乙二醇、蒸馏水适量。
一种伊维菌素复配的毒死蜱微囊悬浮剂的制备方法,其特征在于,按以下步骤进行:
a. 将聚乳酸1:10溶于二氯甲烷,聚乙烯醇、明胶1:1:50溶于蒸馏水,两者混合高速分散乳化40s,加入乳化硅油,磁力搅拌2h,得A液;向海藻酸钠中1:20加入蒸馏水,搅拌溶解,1:15加入有机膨润土、乙醇,超声分散2h,得B液;将A、B液均匀混合待用;
b. 向MCM-41分子筛中1:20加入甲苯,搅拌下滴加KH550,在氮气保护下,加热回流、搅拌反应2h,冷却至室温后,1:30加入聚丙烯酸、蒸馏水,磁力搅拌3h,过滤,醇洗水洗3次,干燥;
c. 在氮气保护下,将水滑石1:25溶于乙醇中形成透明溶液,与a、b中所得物料混合,调pH为6-7,在70-80℃下反应4h,产物经过滤、水洗醇洗3次,在烘箱中于80-90℃干燥3h;
d. 将伊维菌素1:20溶解于N,N-二甲基甲酰胺中,加入聚醚L-64,搅拌均匀,得到透明液;向尿素中1:10:20加入抗冻剂乙二醇、蒸馏水,磁力搅拌下,将其滴入透明液中,得到均匀溶液;
e. 将聚碳酸亚丙酯1:10溶于二氯甲烷中,加入毒死蜱,60-70℃振荡摇匀,与c、d中所得物料混合乳化分散10min,使之形成稳定的O/W型乳液,恒温水浴搅拌3h,即得到一种微囊悬浮剂。
上述实施例制备的一种伊维菌素复配的毒死蜱微囊悬浮剂的性能检测结果如下所示:
对农田中的害虫杀灭效果好,10h害虫死亡率为100%;缓释效果好,自然条件下50d的累积释药率≥80%;持效性好,用药后100d的杀灭率≥98%。
Claims (2)
1.一种伊维菌素复配的毒死蜱微囊悬浮剂,其特征在于,由下述重量份的原料制得:
毒死蜱5-8,聚碳酸亚丙酯25-30,聚乙烯醇14-18,聚乳酸8-14,明胶5-10,乳化硅油0.1-0.3,海藻酸钠3-6,有机膨润土4-9,MCM-41分子筛4-8,KH550 1-3,聚丙烯酸3-6,水滑石4-7,伊维菌素1-2,聚醚L-64 3-7,尿素2-4,二氯甲烷、乙醇、甲苯、N,N-二甲基甲酰胺、乙二醇、蒸馏水适量。
2.根据权利要求1所述的一种伊维菌素复配的毒死蜱微囊悬浮剂的制备方法,其特征在于,按以下步骤进行:
a. 将聚乳酸1:5-10溶于二氯甲烷,聚乙烯醇、明胶1:1:50-100溶于蒸馏水,两者混合高速分散乳化30-50s,加入乳化硅油,磁力搅拌2-3h,得A液;向海藻酸钠中1:20-30加入蒸馏水,搅拌溶解,1:10-15加入有机膨润土、乙醇,超声分散1-2h,得B液;将A、B液均匀混合待用;
b. 向MCM-41分子筛中1:20-30加入甲苯,搅拌下滴加KH550,在氮气保护下,加热回流、搅拌反应2-4h,冷却至室温后,1:30-40加入聚丙烯酸、蒸馏水,磁力搅拌2-3h,过滤,醇洗水洗3-5次,干燥;
c. 在氮气保护下,将水滑石1:20-30溶于乙醇中形成透明溶液,与a、b中所得物料混合,调pH为6-7,在60-80℃下反应4-8h,产物经过滤、水洗醇洗3-5次,在烘箱中于80-90℃干燥2-3h;
d. 将伊维菌素1:20-30溶解于N,N-二甲基甲酰胺中,加入聚醚L-64,搅拌均匀,得到透明液;向尿素中1:5-10:15-20加入抗冻剂乙二醇、蒸馏水,磁力搅拌下,将其滴入透明液中,得到均匀溶液;
e.将聚碳酸亚丙酯1:5-10溶于二氯甲烷中,加入毒死蜱,60-70℃振荡摇匀,与c、d中所得物料混合乳化分散5-10min,使之形成稳定的O/W型乳液,恒温水浴搅拌2-4h,即得到一种微囊悬浮剂。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611230296.1A CN106614549A (zh) | 2016-12-28 | 2016-12-28 | 一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611230296.1A CN106614549A (zh) | 2016-12-28 | 2016-12-28 | 一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN106614549A true CN106614549A (zh) | 2017-05-10 |
Family
ID=58831646
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201611230296.1A Withdrawn CN106614549A (zh) | 2016-12-28 | 2016-12-28 | 一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106614549A (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113846518A (zh) * | 2021-09-20 | 2021-12-28 | 河南中烟工业有限责任公司 | 一种提升卷烟感官品质的卷烟纸及其制备方法 |
-
2016
- 2016-12-28 CN CN201611230296.1A patent/CN106614549A/zh not_active Withdrawn
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113846518A (zh) * | 2021-09-20 | 2021-12-28 | 河南中烟工业有限责任公司 | 一种提升卷烟感官品质的卷烟纸及其制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR101969156B1 (ko) | 안정화된 화학 조성물 | |
CN102933523B (zh) | 稳定的农用化学组合物 | |
CN104970013B (zh) | 一种缓控释农药颗粒剂及其制备方法 | |
CN105494327A (zh) | 一种具有缓释效果的微囊悬浮剂组合物及其制备方法 | |
CN107517960A (zh) | 一种微球悬浮种衣剂及其制备方法 | |
CN106577736A (zh) | 一种介孔硅分子筛为载体的毒死蜱微囊悬浮剂及其制备方法 | |
CN106614567A (zh) | 一种聚合物交联微球负载的毒死蜱微囊悬浮剂及其制备方法 | |
CN103651346B (zh) | 丙硫克百威缓释颗粒剂及制备方法 | |
CN103070166A (zh) | 一种微囊悬浮-水乳剂zw及其制备方法 | |
CN106614566A (zh) | 一种含丙环唑的杀菌型毒死蜱微囊悬浮剂及其制备方法 | |
CN106614549A (zh) | 一种伊维菌素复配的毒死蜱微囊悬浮剂及其制备方法 | |
CN102334478B (zh) | 一种含螺螨酯的悬乳剂及制备方法 | |
CN107412193A (zh) | 以麦羟硅钠石为乳化剂的Pickering乳液模板法制备的纳米杂化药物载体及其制法 | |
CN102204529A (zh) | 一种噻唑磷微胶囊悬浮剂及其制备方法 | |
CN105746509B (zh) | 一种杀线虫剂微胶囊及其制备方法 | |
CN100490647C (zh) | 一种杀虫剂组合物 | |
CN101703069B (zh) | 毒死蜱水分散组合物及其制备方法 | |
CN105409944A (zh) | 除虫菊酯微胶囊的制备方法 | |
CN103517757A (zh) | 自组装聚合物颗粒释放系统 | |
CN106376561A (zh) | 一种微囊剂型的农药组合物 | |
CN105494333A (zh) | 灭幼脲微胶囊的制备方法 | |
CN107333759A (zh) | 光控缓释农药制剂及其制备方法 | |
CN102972401B (zh) | 防治绿盲蝽的2,5-二苯基噻吩的纳米微胶囊制剂及其制备方法 | |
CN109769853A (zh) | 一种含有机磷类杀虫剂与几丁质合成抑制剂的复配组合物及其应用 | |
CN105494332A (zh) | 辛硫磷微胶囊的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170510 |
|
WW01 | Invention patent application withdrawn after publication |