CN115152753A - 一种长效型电热蚊香片的制备方法 - Google Patents
一种长效型电热蚊香片的制备方法 Download PDFInfo
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Abstract
本发明公开了一种长效型电热蚊香片的制备方法,按重量百分比计,将50‑80%的驱蚊精油,15‑35%增溶剂及5‑15%二茂铁羧酸衍生物混合均匀后得到驱蚊增效液,再加入拟除虫菊酯并负载于载体片上得到;所述电蚊香片具有缓释性,能够在较长时间内均匀释放灭蚊成分,挥发量较为稳定,具备长效灭蚊的效果。
Description
技术领域
本发明涉及电热蚊香片技术领域,更具体地说,本发明涉及一种长效型电热蚊香片的制备方法。
背景技术
菊酯类药液对于驱蚊灭蚊已经成熟应用于各类灭蚊产品,但随之而来的是蚊虫对菊酯类药液的抗性逐渐增强,且菊酯类药液的含量要求必须限定在一定的范围内,因此,对于菊酯类药液而言,驱蚊效果会随着时间的推移而降低。
市面上常见的增效剂包括增效胺(MGK-264)、增效醚(S1)、八氯二丙醚、胡椒基丁醚等,但这些增效剂目前常用于触杀类杀虫气雾剂产品上,且多为化学合成成分,对环境并不友好。一些植物源成分的使用对现有菊酯类药液表现出了一定的增效活性,且对环境友好,如中国专利文献CN101558770A公开了一种以植物提取物桉叶油和肉桂油为有效物质的蚊香增效剂,能够与农药品种组成增效农药组合物,配置成蚊香液并涂于蚊香胚上,制成蚊香。通过增效试验判断其使用效果,通过活性系数表示,活性系数均大于1,表明使用该增效剂的蚊香具有增效作用。中国专利文献CN104938530A公开了的一种以植物提取物冬青油、蓝桉油、丁香油、薄荷油和松节油为有效物质的蚊香片增效剂,通过活性测定试验数据证实,该蚊香片增效剂对多种除虫菊酯类农药具有增效作用。但实际应用时发现药剂的挥发存在明显的衰减,前期挥发量较大,后期挥发量小,对于多次使用时后期效果并不理想,主要是因为上述增效剂与药剂负载于载体片上难以起到均匀释放的效果。
因此,有必要提出一种长效型电热蚊香片的制备方法,在保证驱蚊效果的基础上,控制释放均匀性进而提高驱蚊的持续性。
发明内容
鉴于此,本发明提供了一种电热蚊香片安全无毒增效剂及其电热蚊香片,在保证驱蚊效果的基础上,控制释放均匀性进而提高驱蚊的持续性。
本发明的技术方案如下:
一种长效型电热蚊香片的制备方法,按重量百分比计,将50-80%的驱蚊精油,15-35%增溶剂及5-15%二茂铁羧酸衍生物混合均匀后,再加入拟除虫菊酯得到驱蚊液,将驱蚊液负载于载体片上得到。
本发明中,所述驱蚊液按110-190mg/片的量负载于载体片。
本发明中,所述增溶剂包括挥发性硅油及挥发性酯类。
进一步地,所述挥发性硅油与挥发性酯类的体积比为1:(0.5-2)。
进一步地,所述挥发性酯类为甲酸乙酯、甲酸丙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯及乙酸丁酯中的至少一种。优选地,所述挥发性酯类为乙酸乙酯。
本发明中,所述二茂铁羧酸衍生物为二茂铁一元酸、二茂铁二元酸,及其衍生物中的至少一种。
本发明中,所述驱蚊精油包括柠檬草精油、薰衣草精油、薄荷精油、丁香精油及天竺葵精油中的至少一种。
本发明中,所述拟除虫菊酯选自四氟甲醚菊酯、四氟苯菊酯、氯氟醚菊酯、炔丙菊酯、Es-生物烯丙菊酯中至少一种;作为优选,所述蚊香片中拟除虫菊酯的量为13mg。
相比现有技术,本发明的有益效果在于:
1.本发明所述制备方法得到的电蚊香片具有缓释性,能够在较长时间内均匀释放灭蚊成分,挥发量较为稳定,具备长效灭蚊的效果。
2.本发明所述制备方法得到的电蚊香片中采用了环保型成分,添加的二茂铁羧酸衍生物本身具备樟脑气味,可增强驱蚊效果。
具体实施方式
为了解决现有技术中植物源增效剂仅具备增效作用,但增效持续性不佳,增效剂与药剂负载于载体片上不能稳定的释放,导致挥发量呈衰减趋势的缺陷,本发明通过引入新型增效成分,具备一定的缓释作用,使得植物增效成分及药剂发生协同作用,具备持续均匀的驱蚊效果。
本发明提出的一种长效型电热蚊香片的制备方法,具体步骤包括:
1.按重量百分比计,将50-80%的驱蚊精油,15-35%增溶剂及5-15%二茂铁羧酸衍生物混合均匀得到增效液;
驱蚊精油包括柠檬草精油、薰衣草精油、薄荷精油、丁香精油及天竺葵精油中的至少一种。增溶剂包括挥发性硅油与挥发性酯类,两者的体积比为1:(0.5-2);挥发性酯类为甲酸乙酯、甲酸丙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯及乙酸丁酯中的至少一种。优选地,所述挥发性酯类为乙酸乙酯。
二茂铁羧酸衍生物选择分子量较小的二茂铁羧酸及衍生物,优选二茂铁一元酸、二茂铁二元酸,及其衍生物中的至少一种。
2.增效液中再加入拟除虫菊酯得到驱蚊液;拟除虫菊酯选自四氟甲醚菊酯、四氟苯菊酯、氯氟醚菊酯、炔丙菊酯、Es-生物烯丙菊酯中至少一种。
3.将驱蚊液按110-190mg/片的量负载于载体片上得到电蚊香片,其中,根据灭蚊驱蚊效果及产品标准,所述拟除虫菊酯的加入量为13mg。
本发明的设计构思在于,驱蚊精油对于拟除虫菊酯类有增效作用,而选择二茂铁羧酸衍生物的目的在于,一方面在增溶剂体系下,可以与驱蚊精油中含有羟基的成分进行键合,随着增溶剂的持续挥发,仍然能够形成一定的网状体系,从而形成缓释效应;另一方面二茂铁羧酸衍生物本身独特的樟脑气味具备驱蚊作用,且属于环保型成分,属于较佳的选择。
以下是本发明具体实施实验例,作为本发明的较佳选择和详细说明。应当理解的是,本说明书中描述的具体实施方式仅仅是为了解释本发明,并不是为了限定本发明。
实施例1
取35g增溶剂(挥发性硅油与乙酸乙酯体积比1:2)加入15g二茂铁一元酸溶解,加入柠檬草精油50g混匀后,再加入氯氟醚菊酯6.5g、炔丙菊酯7g混匀,按照110mg/片的量负载于载体片上得到电蚊香片。
实施例2
取15g增溶剂(挥发性硅油与乙酸乙酯体积比1:0.5)加入5g二茂铁二元酸溶解,加入薰衣草精油、薄荷精油共计80g混匀后,再加入氯氟醚菊酯7.5g混匀,按照190mg/片的量负载于载体片上得到电蚊香片。
实施例3
取25g增溶剂(挥发性硅油与甲酸乙酯、乙酸丁酯体积比1:0.5:0.5)加入5g二茂铁一元酸、5g二茂铁二元酸溶解,加入柠檬草精油、薰衣草精油、薄荷精油共计65g混匀后,再加入氯氟醚菊酯3g、炔丙菊酯3.5g、Es-生物烯丙菊酯4.5g混匀,按照130mg/片的量负载于载体片上得到电蚊香片。
实施例4
取20g增溶剂(挥发性硅油与乙酸乙酯、乙酸丁酯体积比1:1:0.5)加入5g二茂铁一元酸、3g二茂铁二元酸溶解,加入丁香精油及天竺葵精油共计72g混匀后,再加入四氟甲醚菊酯2g、氯氟醚菊酯3g、炔丙菊酯3g、Es-生物烯丙菊酯3g混匀,按照130mg/片的量负载于载体片上得到电蚊香片。
对比例1
取35g增溶剂(挥发性硅油与乙酸乙酯体积比1:2)加入柠檬草精油50g混匀后,再加入氯氟醚菊酯6.5g、炔丙菊酯7g混匀,按照110mg/片的量负载于载体片上得到电蚊香片。
对比例2
取15g增溶剂(挥发性硅油与乙酸乙酯体积比1:0.5)加入薰衣草精油、薄荷精油共计80g混匀后,再加入氯氟醚菊酯7.5g混匀,按照190mg/片的量负载于载体片上得到电蚊香片。
对比例3
取25g增溶剂(挥发性硅油与甲酸乙酯、乙酸丁酯体积比1:0.5:0.5)加入5g二茂铁一元酸、5g二茂铁二元酸溶解,再加入氯氟醚菊酯3g、炔丙菊酯3.5g、Es-生物烯丙菊酯4.5g混匀,按照130mg/片的量负载于载体片上得到电蚊香片。
对比例4
取20g增溶剂(挥发性硅油与乙酸乙酯、乙酸丁酯体积比1:1:0.5)加入5g二茂铁一元酸、3g二茂铁二元酸溶解,再加入四氟甲醚菊酯2g、氯氟醚菊酯3g、炔丙菊酯3g、Es-生物烯丙菊酯3g混匀,按照130mg/片的量负载于载体片上得到电蚊香片。
对比例5
取20g增溶剂(挥发性硅油与乙酸乙酯、乙酸丁酯体积比1:1:0.5)加入四氟甲醚菊酯2g、氯氟醚菊酯3g、炔丙菊酯3g、Es-生物烯丙菊酯3g混匀,按照130mg/片的量负载于载体片上得到电蚊香片。
以下是本发明的实验例,对上述实施例1-4及对比例1-5所得电蚊香片进行效果性验证。
实验例
1.试验条件:温度(26±1)℃,相对湿度65±10%。
2.供试昆虫:按照CB/T 13917-2009的有关要求提供致倦库蚊(Culex fatigans)。
3.试验设备及器材:
方箱装置:透明无色有机玻璃制,长、宽、高内径均为700mm,在方箱一侧面的一下角有一小门,此侧面的上方还有一放虫孔,可用胶塞塞紧,另有一侧面整个为一大门,测试时密封。
4.试验方法:按照GB/T 13917.6-2009《农药登记用卫生杀虫剂室内药效试验及评价第5部分:电热蚊香片》的有关规定执行。采用方箱法,通电时间分为1h、3h、6h、9h、12h进行药效测试。将致倦库蚊50只自放虫孔放入,塞紧胶塞。待试虫恢复正常活动后,由小门将连续通电预燃至相应时段点的载有待测电热蚊香片的加热器一起放入方箱的中央,立即封闭整个方箱装置,并计时。每隔一定时间记录被击倒的试虫数。每次试验结束后,清洗试验装置。运用直线回归编程计算其KT50值。
5.检测结果:
任意选取上述实施例1-4及其对应的对比例1-5所述电热蚊香片,对致倦库蚊室内药效进行测定,结果参见下表1。
表1:
从表1中不难看出,相对于对比例1-5,实施例1-4中电蚊香片随通电时间的延长,其KT50值变化幅度不大,基本维持在5.0-5.8之间,可以有效对驱蚊成分进行缓释,挥发量较为稳定,并且整体驱蚊灭蚊效果较好。对比例1-2因未添加二茂铁羧酸或其衍生物的情况下,其KT50初始值较实施例1-4更低,但在通电6h之后出现明显大幅波动,但在12h后达到8min以上,可能的原因在于,在缺少二茂铁羧酸的情况下,不能与驱蚊精油中存在的羟基形成结合,不能形成释放阻力,导致释放量先高后低;对比例3-4在缺少驱蚊精油的情况下,同样也不能形成缓释体系,仍然会出现释放量先高后低;对比例5未添加驱蚊精油和二茂铁羧酸(接近市售样),相比对比例4的KT50值更大,可能的原因在于实施例4中未发生结合的二茂铁羧酸在加热过程中发生升华,呈现较微弱的协同驱蚊作用,导致KT50值变小。
最后应说明的几点是,虽然上文中已经用一般性说明及具体实施例对本发明作了详尽的描述,但在本发明的基础上,以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种长效型电热蚊香片的制备方法,其特征在于,按重量百分比计,将50-80%的驱蚊精油,15-35%增溶剂及5-15%二茂铁羧酸衍生物混合均匀后,再加入拟除虫菊酯得到驱蚊液,将驱蚊液负载于载体片上得到。
2.根据权利要求1所述的制备方法,其特征在于,所述驱蚊液按110-190mg/片的量负载于载体片。
3.根据权利要求1所述的制备方法,其特征在于,所述增溶剂包括挥发性硅油及挥发性酯类。
4.根据权利要求3所述的制备方法,其特征在于,所述挥发性硅油与挥发性酯类的体积比为1:(0.5-2)。
5.根据权利要求3所述的制备方法,其特征在于,所述挥发性酯类为甲酸乙酯、甲酸丙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯及乙酸丁酯中的至少一种。
6.根据权利要求3所述的制备方法,其特征在于,所述挥发性酯类为乙酸乙酯。
7.根据权利要求1所述的制备方法,其特征在于,所述二茂铁羧酸衍生物为二茂铁一元酸、二茂铁二元酸,及其衍生物中的至少一种。
8.根据权利要求1所述的制备方法,其特征在于,所述驱蚊精油包括柠檬草精油、薰衣草精油、薄荷精油、丁香精油及天竺葵精油中的至少一种。
9.根据权利要求1所述的制备方法,其特征在于,所述拟除虫菊酯为四氟甲醚菊酯、四氟苯菊酯、氯氟醚菊酯、炔丙菊酯、Es-生物烯丙菊酯中至少一种。
10.根据权利要求1所述的制备方法,其特征在于,所述蚊香片中拟除虫菊酯的量为13mg。
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