CN108623724A - 用于信息素缓释的高分子微球的制备方法 - Google Patents

用于信息素缓释的高分子微球的制备方法 Download PDF

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CN108623724A
CN108623724A CN201710159465.5A CN201710159465A CN108623724A CN 108623724 A CN108623724 A CN 108623724A CN 201710159465 A CN201710159465 A CN 201710159465A CN 108623724 A CN108623724 A CN 108623724A
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pheromones
polymer microsphere
deionized water
sustained release
solution
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韩国志
李俊
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Jiangsu Huachang Yarns And Fabrics Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F112/02—Monomers containing only one unsaturated aliphatic radical
    • C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F112/06—Hydrocarbons
    • C08F112/08—Styrene
    • 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
    • A01N25/08—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 solids as carriers or diluents
    • A01N25/10—Macromolecular 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
    • A01N25/26—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
    • 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
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    • A01N63/10—Animals; Substances produced thereby or obtained therefrom
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    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

本发明涉及用于信息素缓释的高分子微球的制备方法，按比例称取苯乙烯、十六烷和信息素；称取一定量的SDS溶于去离子水中，得到SDS水溶液；将上述化合物混溶，超声10min，得到乳白色溶液；然后转移到圆底烧瓶中，搅拌氮气除氧30min；称取一定量的过硫酸钾溶于去离子水中，得到过硫酸钾水溶液，然后加热升温至70‑75℃；将除氧后的混合液加入至过硫酸钾水溶液中，反应4h，然后离心处理，用去离子水重新分散，即得高分子微球。用此方法制得的用于信息素缓释的高分子微球粒径均一；价格低，非常容易大批量工业化生产；缓释周期长，40天以上效果依旧好。

Description

用于信息素缓释的高分子微球的制备方法
技术领域
本发明涉及一种用于信息素缓释的高分子微球的制备方法。
背景技术
昆虫性信息素是成虫性成熟后分泌于体外，作为求偶通讯联系的一种化学物质。应用昆虫性信息素防治害虫是当前农作物害虫绿色防控的技术措施之一，它具有专一性强、操作简便、高效、无残毒、不伤害天敌、不污染环境、不会引起害虫产生抗药性、对人畜安全等优点，用于农业害虫防治，可减少用药次数，降低农药污染，保护生态环境。其中迷向法是主要的手段。迷向法是在一定范围内大量释放性信息素,使雄成虫的触角一直处于高浓度的性信息素包围之中,或大量释放性信息素的同系物、抑制剂,用以干扰雌雄成虫间正常的化学通讯,使之无法定向找到雌虫交尾而达到控制其交配繁殖的目的。
国外对迷向法研究较多,目前已直接用于防治的有棉红铃虫、舞毒蛾、桃透翅蛾、西方松斑螟等数十种制剂，例如棉红铃虫的迷向防治法已得到较大面积的推广应用,可减少1/3-2/3的用药量,效果明显。但国内的研究尚处于起步阶段。具体的产品有迷向丝，诱芯与微胶囊。但是大部分属于国外进口产品，价格不菲。另一方面，大部分的产品工业化程度较低，缓释周期较短，也导致成本增加。
发明内容
本发明的目的在于：为解决以上问题提供一种价格低，适合工业化生产、缓释周期长的用于信息素缓释的高分子微球的制备方法。
本发明所采用的技术方案是这样的：
用于信息素缓释的高分子微球的制备方法，包括如下步骤：
(1)、按质量比300-500:20-25:1分别称取苯乙烯、十六烷和信息素；
(2)、称取一定量的乳化剂溶于去离子水中，其中信息素、SDS、和去离子水的质量比为1：3：1500；
(3)、将步骤(1)中所得混合物与步骤(2)中乳化剂水溶液混溶，超声10min，得到乳白色溶液；
(4)、将上述所得溶液转移到圆底烧瓶中，搅拌氮气除氧30min；
(5)、称取一定量的引发剂溶于去离子水中，其中信息素、引发剂和去离子水的质量比为1：5：300，然后加热升温至70-75℃；
(6)、将步骤(4)处理后的溶液加入至步骤(5)中引发剂水溶液中，反应4h；
(7)、将上述反应所得溶液离心处理，用去离子水重新分散，即得高分子微球。
进一步地，所述乳化剂为SDS。
进一步地，所述引发剂为过硫酸钾。
综上所述，由于采用上述技术方案，本发明的有益效果是：
本发明利用乳液聚合的方法，将信息素包埋于聚苯乙烯纳米微球之中，利用微球纳米级的天然孔洞通道控制释放信息素，具有缓释周期长，成本低廉，容易工业化的优点。
附图说明
图1为本发明方法原理图；
图2为本发明制得的高分子微球扫描电镜图；
图3为本发明制得的高分子微球扫描电镜图；
图4为本发明制得的高分子微球扫描电镜图；
图5为本发明制得的高分子微球缓释效果图。
具体实施方式
本发明以苹果小卷蛾信息素为目标分子，采用乳液聚合的方法，将信息素分子包埋于聚苯乙烯分子中，制备信息素缓释的高分子微球。
如图1所示，用于信息素缓释的高分子微球的制备方法，包括如下步骤：
(1)、称取苯乙烯4.0g、十六烷0.23g和信息素0.01g；
(2)、称取0.03g的SDS溶于15g去离子水中；
(3)、将步骤(1)中所得混合物与步骤(2)中SDS水溶液混溶，超声10min，得到乳白色溶液；
(4)、将上述所得溶液转移到圆底烧瓶中，搅拌氮气除氧30min；
(5)、称取0.05g的过硫酸钾溶于3g去离子水中，然后加热升温至70℃；
(6)、将步骤(4)处理后的溶液加入至步骤(5)中过硫酸钾水溶液中，反应4h；
(7)、将上述反应所得溶液离心处理，用去离子水重新分散，即得高分子微球。
苯乙烯含量的增加，高分子微球粒径随之增加；如图2-4所示，苯乙烯含量分别为3g、4g、5g，微球粒径分别为200nm、215nm、260nm，颗粒粒径均一。
本发明采用气相色谱检测信息素的缓释，实验结果显示(详见图5)，40天之后，微球依然具有较好的缓释作用。

Claims (3)

1.用于信息素缓释的高分子微球的制备方法，其特征在于：包括如下步骤：
(1)、按质量比300-500：20-25：1分别称取苯乙烯、十六烷和信息素；
(2)、称取一定量的乳化剂溶于去离子水中，其中信息素、乳化剂和去离子水的质量比为1：3：1500；
(3)、将步骤(1)中所得混合物与步骤(2)中乳化剂水溶液混溶，超声10min，得到乳白色溶液；
(4)、将上述所得溶液转移到圆底烧瓶中，搅拌氮气除氧30min；
(5)、称取一定量的引发剂溶于去离子水中，其中信息素、引发剂和去离子水的质量比为1：5：300，然后加热升温至70-75℃；
(6)、将步骤(4)处理后的溶液加入至步骤(5)中引发剂水溶液中，反应4h；
(7)、将上述反应所得溶液离心处理，用去离子水重新分散，即得高分子微球。
2.根据权利要求1所述的用于信息素缓释的高分子微球的制备方法，其特征在于：所述乳化剂为SDS。
3.根据权利要求1所述的用于信息素缓释的高分子微球的制备方法，其特征在于：所述引发剂为过硫酸钾。
CN201710159465.5A 2017-03-17 2017-03-17 用于信息素缓释的高分子微球的制备方法 Pending CN108623724A (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1135175A (zh) * 1994-08-03 1996-11-06 萨伊泰克公司 制备活性组分控释的固体剂型的装置和方法
CN102427721A (zh) * 2009-05-19 2012-04-25 科派克有限公司 包含活性物质的缓释微囊和微球
CN103665226A (zh) * 2012-09-20 2014-03-26 大连理工常熟研究院有限公司 一种光引发原位乳液聚合制备高分子微球的方法
WO2016061482A1 (en) * 2014-10-17 2016-04-21 Sergeant's Pet Care Products, Inc. Animal litter containing a pheromone composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1135175A (zh) * 1994-08-03 1996-11-06 萨伊泰克公司 制备活性组分控释的固体剂型的装置和方法
CN102427721A (zh) * 2009-05-19 2012-04-25 科派克有限公司 包含活性物质的缓释微囊和微球
CN103665226A (zh) * 2012-09-20 2014-03-26 大连理工常熟研究院有限公司 一种光引发原位乳液聚合制备高分子微球的方法
WO2016061482A1 (en) * 2014-10-17 2016-04-21 Sergeant's Pet Care Products, Inc. Animal litter containing a pheromone composition

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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Application publication date: 20181009