CN110292052B - 一种液体蚊香及其制备方法 - Google Patents
一种液体蚊香及其制备方法 Download PDFInfo
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- CN110292052B CN110292052B CN201910685624.4A CN201910685624A CN110292052B CN 110292052 B CN110292052 B CN 110292052B CN 201910685624 A CN201910685624 A CN 201910685624A CN 110292052 B CN110292052 B CN 110292052B
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Classifications
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- A—HUMAN NECESSITIES
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- 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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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
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- A—HUMAN NECESSITIES
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- 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
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
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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
- 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
- A01N25/30—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 characterised by the surfactants
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
本发明公开了一种液体蚊香及其制备方法。所述的液体蚊香包含以下质量百分比计的组分：右旋七氟甲醚菊酯0.01～0.03％、对‑聚伞花素0.2～0.5％、欧白芷根精油0.5～2％、月桂酰肌氨酸钠1～3％、混合醇50～65％，余量为去离子水。本发明的液体蚊香是一种热力学稳定的O/W型水基微乳液体系，性质稳定，乳液的粒径较小，不易堵塞芯棒，可持续发挥驱蚊杀蚊的效果，具有长效性，并且还具有消除焦虑、舒缓压力的功效，VOC含量低，是健康家居生活的理想选择。
Description
技术领域
本发明涉及卫生用品技术领域，具体涉及一种液体蚊香及其制备方法。
背景技术
目前市面上大部分的电热液体蚊香均为油基产品，即以煤油或其它挥发性烷烃作为溶剂，成本较高，不符合现在低碳经济、节能减排的环保理念。并且油基类的电热液体蚊香中使用的低碳链烷烃易形成有机挥发物即VOC，在消费者日常家居生活中，会通过电热液体蚊香的加热使用和自然挥发造成家居环境的污染，给消费者健康带来一定影响。
水基电热液体蚊香具有体系低VOC化和常温常压下的难燃的优点，是目前液体蚊香研究的热点。现有的水基电热液体蚊香大部分含有拟除虫菊酯类成分，如四氟苯菊酯、氯氟醚菊酯、炔丙菊酯、胺菊酯等，具有击倒快、杀虫力强、广谱、低毒、低残留等特点，但是长期使用除虫菊酯类杀虫剂容易产生抗药性，影响了蚊香液的药效，并且液体蚊香中拟除虫菊酯类成分的含量普遍达到0.1％以上，甚至高达2～5％，长期使用对人体健康影响较大。另一方面，为了降低拟除虫菊酯的用量，降低抗药性，以天然植物提取物或植物精油为杀虫活性剂的液体蚊香是近年来研究的热点，但是天然植物提取物的制备工艺复杂，成本较高，而植物精油在水基产品中难以溶解，需要加入表面活性剂促进乳化，而这些表面活性剂分子量一般较大，多数为聚合物，配套挥发的芯棒正常会因这类聚合物而堵塞，造成后期挥发越来越慢，有明显的挥发不均匀现象。
公开号为CN 102232379 A的中国专利申请公开了一种水基型电热蚊香液及其制备方法，该水基蚊香液含有拟除虫菊酯类驱蚊药物、防腐剂、抗氧化剂、乙醇、水等成分，并以吐温-80或脂肪醇聚氧乙烯醚作为表面活性剂，驱蚊药物的含量较高，存在使用安全隐患，并且所使用的表面活性剂分子量均较大，粘度较高，容易堵塞芯棒。
公开号为CN 107136133 A的中国专利申请公开了一种水基型植物电蚊香液的制备方法，该水基蚊香液含有四氟甲醚菊酯、植物提取物、非离子表面活性剂、防腐剂、乙醇、水等成分，其中植物提取物的原料包括柠檬香茅、鼠尾草、野菊花、芦荟、黄滕根、烟草、艾叶、丁香、薄荷、藿香、龙胆草，制备工艺较为复杂，成本较高。
发明内容
本发明的目的是提供一种液体蚊香及其制备方法。所述的液体蚊香是一种热力学稳定的O/W型水基微乳液体系，性质稳定，乳液的粒径较小，不易堵塞芯棒，可持续发挥驱蚊杀蚊的效果，具有长效性。
本发明是通过以下技术方案予以实现的：
一种液体蚊香，包含以下质量百分比计的组分：
所述的混合醇为1-己醇、1-辛醇和二丙二醇以(0.5～2):(1～3):(3～4)的质量比组成。
优选，所述的混合醇为1-己醇、1-辛醇和二丙二醇以1:2:3.5的质量比组成。
所述的液体蚊香还包含0.05～0.1％的稳定剂。
所述的稳定剂为2,6-二叔丁基-4-甲基苯酚、丁基羟基茴香醚或叔丁基对苯二酚。
优选，所述的稳定剂为叔丁基对苯二酚。
优选，所述的液体蚊香，包含以下质量百分比计的组分：
本发明还提供上述的液体蚊香的制备方法，其包括以下步骤：
将右旋七氟甲醚菊酯、对-聚伞花素、欧白芷根精油、叔丁基对苯二酚、月桂酰肌氨酸钠、混合醇和去离子水混合，充分搅拌溶解调匀，得到液体蚊香半成品，将液体蚊香半成品灌装于包装瓶内，配合以内塞、芯棒制成成品。
本发明在试验中发现，使用吐温-80、脂肪醇聚氧乙烯醚硫酸钠等表面活性剂制备的液体蚊香持效期较短，小于300h，推测这是由于所使用的表面活性剂分子量较大，粘度较高，容易堵塞芯棒，造成后期挥发越来越慢所致。为了克服上述的缺陷，本发明尝试使用分子量较小的氨基酸型表面活性剂月桂酰肌氨酸钠，结果发现液体蚊香的持效期有所延长，但效果仍不是很理想，并且体系泡沫较多。出乎意料之外，本发明人发现加入由1-己醇、1-辛醇和二丙二醇按一定比例组成的混合醇，不仅显著延长液体蚊香的持效期，使其长达750h，还能抑制泡沫的形成，使液体蚊香形成稳定的O/W型水基微乳液体系。所述的混合醇在一定程度上抑制月桂酰肌氨酸钠的增稠、发泡作用，促使液体蚊香持续稳定发挥驱蚊灭蚊效果。混合醇中的1-己醇具有水果芬芳香气，兼具防腐效果，可延长液体蚊香的有效期；1-辛醇具有柠檬气味，兼具消泡作用，可抑制液体蚊香泡沫的形成；二丙二醇具有很好的水分，油分和碳氢化合物共溶能力，是理想的溶剂，有助于溶解右旋七氟甲醚菊酯、对-聚伞花素和欧白芷根精油，促使液体蚊香形成稳定的乳液体系，并且挥发较慢，可调整液体蚊香的挥发速度。1-己醇、1-辛醇和二丙二醇三者合用，除了发挥助乳化剂的作用外，还兼具防腐剂、消泡剂、溶剂、挥发调整剂的效果，使液体蚊香无需额外添加其它助剂，显著降低成本，取得了意料不到的技术效果。应当注意的是，所述的混合醇并非是简单醇类的组合，其成分之间的改变或配比的调整，对液体蚊香的持效期、驱蚊灭蚊的效果均有影响，优选，所述的混合醇为1-己醇、1-辛醇和二丙二醇以1:2:3.5的质量比组成，取得的效果最佳。
在本发明中，右旋七氟甲醚菊酯是一种新型的拟除虫菊酯类卫生杀虫剂，具有高效、高蒸气压的特点，其基础毒力活性显著高于其它的拟除虫菊酯类药物，仅需少量即可获得高效的驱蚊灭蚊效果。本发明人在前期的试验中发现，对-聚伞花素与右旋七氟甲醚菊酯合用，具有显著的增效作用，以对-聚伞花素和右旋七氟甲醚菊酯作为驱蚊药物，可降低右旋七氟甲醚菊酯的用量，并保证高效的驱蚊灭蚊效果。不仅对蚊子有效，对蝇科、虻科、蠓科、蚋科等双翅目害虫同样具有驱逐杀灭效果。
所述的欧白芷根精油内含一种具有麝香般野性芳香气味的十五内酯(巨环内酯类)，有助于调整忧郁情绪、激发勇气与信念，消除焦虑、提振精神。同时兼具杀菌效果。
与现有技术相比，本发明具有以下有益效果：
(1)本发明的液体蚊香是一种热力学稳定的O/W型水基微乳液体系，性质稳定，乳液的粒径较小，不易堵塞芯棒，可持续发挥驱蚊杀蚊的效果，具有长效性，不仅对蚊子有效，对蝇科、虻科、蠓科、蚋科等双翅目害虫同样具有驱逐杀灭效果。此外还具有消除焦虑、舒缓压力的功效，VOC含量低，是健康家居生活的理想选择。
(2)本发明的液体蚊香制备工艺简单，成本较低，绿色环保，易于大规模生产。
具体实施方式
以下实施例是对本发明的进一步说明，而不是对本发明的限制。下述实施例中配方的组分，若无特别说明，均为常规市售产品。
实施例1
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.4％、欧白芷根精油1.5％、月桂酰肌氨酸钠2％、叔丁基对苯二酚0.1％、1-己醇9.2％、1-辛醇18.5％、二丙二醇32.3％和去离子水35.99％。
制备步骤：将右旋七氟甲醚菊酯、对-聚伞花素、欧白芷根精油、叔丁基对苯二酚、月桂酰肌氨酸钠、1-己醇、1-辛醇、二丙二醇和去离子水混合，充分搅拌溶解调匀，得到液体蚊香半成品，将液体蚊香半成品灌装于包装瓶内，配合以内塞、芯棒制成成品。
实施例2
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.5％、欧白芷根精油0.5％、月桂酰肌氨酸钠1％、叔丁基对苯二酚0.1％、1-己醇7.7％、1-辛醇15.4％、二丙二醇26.9％和去离子水47.89％。
制备步骤参考实施例1。
实施例3
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.2％、欧白芷根精油2％、月桂酰肌氨酸钠3％、叔丁基对苯二酚0.1％、1-己醇10％、1-辛醇20％、二丙二醇35％和去离子水29.69％。
制备步骤参考实施例1。
实施例4
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.02％、对-聚伞花素0.3％、欧白芷根精油1％、月桂酰肌氨酸钠1.5％、丁基羟基茴香醚0.05％、1-己醇12.2％、1-辛醇18.3％、二丙二醇24.5％和去离子水42.13％。
制备步骤参考实施例1。
实施例5
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.03％、对-聚伞花素0.2％、欧白芷根精油0.5％、月桂酰肌氨酸钠1％、2,6-二叔丁基-4-甲基苯酚0.05％、1-己醇6.7％、1-辛醇13.3％、二丙二醇40％和去离子水38.22％。
制备步骤参考实施例1。
对比例1
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、欧白芷根精油1.5％、月桂酰肌氨酸钠2％、叔丁基对苯二酚0.1％、1-己醇9.2％、1-辛醇18.5％、二丙二醇32.3％和去离子水36.39％。
制备步骤参考实施例1。
对比例1的液体蚊香与实施例1比较，区别在于不含对-聚伞花素，相应增加去离子水的含量，其余的组分及配比不变。
对比例2
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.4％、欧白芷根精油1.5％、吐温-802％、叔丁基对苯二酚0.1％、乙醇60％和去离子水35.99％。
制备步骤参考实施例1。
对比例2的液体蚊香与实施例1比较，区别在于，以吐温-80替换月桂酰肌氨酸钠，以乙醇替换本发明的混合醇，其余的组分及配比不变。
对比例3
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.4％、欧白芷根精油1.5％、脂肪醇聚氧乙烯醚硫酸钠2％、叔丁基对苯二酚0.1％、乙醇60％和去离子水35.99％。
制备步骤参考实施例1。
对比例3的液体蚊香与实施例1比较，区别在于，以脂肪醇聚氧乙烯醚硫酸钠替换月桂酰肌氨酸钠，以乙醇替换本发明的混合醇，其余的组分及配比不变。
对比例4
一种液体蚊香，包含以下质量百分比计的组分：
右旋七氟甲醚菊酯0.01％、对-聚伞花素0.4％、欧白芷根精油1.5％、月桂酰肌氨酸钠2％、叔丁基对苯二酚0.1％、乙醇60％和去离子水35.99％。
制备步骤参考实施例1。
对比例4的液体蚊香与实施例1比较，区别在于，以乙醇替换本发明的混合醇，其余的组分及配比不变。
试验例一、安全性检测
1、皮肤斑贴试验：分别对实施例1-5和对比例1-4制得的液体蚊香进行人体皮肤斑贴试验，结果显示，志愿受试者的受试部位的皮肤均没有出现红斑、水肿等现象，说明本发明提供的液体蚊香对皮肤无刺激作用。
2、眼刺激试验：分别对实施例1-5和对比例1-4制得的液体蚊香进行人体眼部刺激试验，结果显示，志愿受试者的急性眼刺激积分指数为0，说明本发明提供的液体蚊香对眼部粘膜无刺激作用。
3、急性吸入毒性试验：分别对实施例1-5和对比例1-4制得的液体蚊香进行大鼠急性吸入毒性试验，结果显示，染毒后的大鼠饮食活动未见异常，观察期无死亡，LD50大于10克/立方米，属于实际无毒。
4、急性经口毒性试验：分别对实施例1-5和对比例1-4制得的液体蚊香进行大鼠急性经口毒性试验，结果显示，染毒后的大鼠活动正常，饮食正常，观察期无死亡，LD50大于5000毫克/公斤，属于实际无毒。
以上结果表明，本发明实施例1-5和对比例1-4制得的液体蚊香，安全性高，属于低毒、无毒范畴，是健康家居生活的理想选择。
试验例二、室内药效检测
按照GB 13917.6-2009《农药登记用卫生杀虫剂室内药效试验及评价第6部分：电热液体蚊香》的试验方法对实施例1-5和对比例1-4制得的液体蚊香进行药效检测，在该标准中，KT50值(密闭圆筒法)≤4分钟为A级标准。测试结果如下表1所示。
表1液体蚊香室内药效
| 组别 | KT50(min) |
| 实施例1 | 2.74 |
| 实施例2 | 2.60 |
| 实施例3 | 2.92 |
| 实施例4 | 2.25 |
| 实施例5 | 1.73 |
| 对比例1 | 4.08 |
| 对比例2 | 3.20 |
| 对比例3 | 3.27 |
| 对比例4 | 2.98 |
结果显示，本发明实施例1-5制得的液体蚊香的室内药效优于对比例1-4制得的液体蚊香。由实施例1、4、5可知，随着右旋七氟甲醚菊酯用量的增加，液体蚊香的驱蚊效果更为明显。由对比例1可知，对-聚伞花素对提高右旋七氟甲醚菊酯的灭蚊效果具有重要作用。由对比例2-3可知，分别以吐温-80、脂肪醇聚氧乙烯醚硫酸钠替换月桂酰肌氨酸钠，并以乙醇替换混合醇，会降低液体蚊香的驱蚊效果，由对比例4可知，使月桂酰肌氨酸钠作为乳化剂，并以乙醇替换混合醇，略影响液体蚊香的驱蚊效果。
试验例三、持效时间检测
1、混合醇不同配比及组成对液体蚊香持效时间的影响
参比实施例1的配方组成，混合醇用量保持60％不变，调整混合醇的组成，检测不同1-己醇、1-辛醇和二丙二醇的配比，以及不同的混合醇的组成(具体见表2)对液体蚊香持效时间的影响，结果见表3所示。
表2混合醇不同配比及组成
| 序号 | 具体组成(质量比) |
| 1 | 1-己醇：1-辛醇：二丙二醇＝1:2:3.5 |
| 2 | 1-己醇：1-辛醇：二丙二醇＝2:3:4 |
| 3 | 1-己醇：1-辛醇：二丙二醇＝0.5:1:3 |
| 4 | 1-己醇：1-辛醇：二丙二醇＝1:1:1 |
| 5 | 1-己醇：1-辛醇：二丙二醇＝2:1:1 |
| 6 | 1-己醇：1-辛醇：二丙二醇＝1:2:1 |
| 7 | 1-己醇：1-辛醇＝1:2 |
| 8 | 1-己醇：二丙二醇＝1:3.5 |
| 9 | 1-辛醇：二丙二醇＝2:3.5 |
表3混合醇不同配比及组成对液体蚊香持效时间的影响
由表2和表3可知，1-己醇：1-辛醇：二丙二醇的质量比在(0.5～2):(1～3):(3～4)的范围内，液体蚊香的持效时间长，加热750h，KT50＜4分钟，仍保持A级标准。调整1-己醇：1-辛醇：二丙二醇三者的比例，或调整混合醇的组成均会影响液体蚊香持效时间。尤其当混合醇为1-己醇：1-辛醇以1:2的质量比组成时，加热600h，KT50＞10分钟，为不合格产品。
2、不同表面活性剂和乙醇的组合对液体蚊香持效时间的影响
对实施例1、对比例2-4制得的液体蚊香的持效时间进行检测，结果见表4所示。
表4不同表面活性剂和乙醇的组合对液体蚊香持效时间的影响
由表4可知，以月桂酰肌氨酸钠作为乳化剂，并结合混合醇，制得的液体蚊香加热750h，KT50＜4分钟，仍保持A级标准。以吐温-80或脂肪醇聚氧乙烯醚硫酸钠替换月桂酰肌氨酸钠，并以乙醇替换混合醇，会降低液体蚊香的驱蚊效果，使液体蚊香加热300h，KT50＞10分钟，变为不合格产品，并且随着加热时间的延长，KT50越大，这是由于液体蚊香使用后期发生芯棒堵塞现象，导致活性明显降低。以月桂酰肌氨酸钠作为乳化剂，并结合乙醇，制得的液体蚊香加热360h后就挥发完全，使用时间短，表明单独使用小分子的月桂酰肌氨酸钠作为乳化剂，虽可改善芯棒堵塞现象，但是并不能延长液体蚊香的有效使用时间。
以上仅是本发明的优选实施方式，应当指出的是，上述优选实施方式不应视为对本发明的限制，本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说，在不脱离本发明的精神和范围内，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (6)
1.一种液体蚊香，其特征在于，包含以下质量百分比计的组分：
所述的混合醇为1-己醇、1-辛醇和二丙二醇以(0.5～2):(1～3):(3～4)的质量比组成。
2.根据权利要求1所述的液体蚊香，其特征在于，所述的混合醇为1-己醇、1-辛醇和二丙二醇以1:2:3.5的质量比组成。
3.根据权利要求1所述的液体蚊香，其特征在于，所述的液体蚊香还包含0.05～0.1％的稳定剂。
4.根据权利要求3所述的液体蚊香，其特征在于，所述的稳定剂为2,6-二叔丁基-4-甲基苯酚、丁基羟基茴香醚或叔丁基对苯二酚。
5.根据权利要求1-4任一所述的液体蚊香，其特征在于，包含以下质量百分比计的组分：
6.一种制备权利要求5所述的液体蚊香的方法，其特征在于，包括以下步骤：
将右旋七氟甲醚菊酯、对-聚伞花素、欧白芷根精油、叔丁基对苯二酚、月桂酰肌氨酸钠、混合醇和去离子水混合，充分搅拌溶解调匀，得到液体蚊香半成品，将液体蚊香半成品灌装于包装瓶内，配合以内塞、芯棒制成成品。
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