CN117617262A - Quick-burning mosquito-repellent incense and preparation method thereof - Google Patents
Quick-burning mosquito-repellent incense and preparation method thereof Download PDFInfo
- Publication number
- CN117617262A CN117617262A CN202210953608.0A CN202210953608A CN117617262A CN 117617262 A CN117617262 A CN 117617262A CN 202210953608 A CN202210953608 A CN 202210953608A CN 117617262 A CN117617262 A CN 117617262A
- Authority
- CN
- China
- Prior art keywords
- powder
- repellent incense
- component
- cyano
- tetrafluorobenzyl
- 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.)
- Pending
Links
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- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
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- KVSRWNPBUMDYOQ-UHFFFAOYSA-N methyl 3-formyl-2,2-dimethylcyclopropane-1-carboxylate Chemical compound COC(=O)C1C(C=O)C1(C)C KVSRWNPBUMDYOQ-UHFFFAOYSA-N 0.000 description 2
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- MSQKMFXJFBXZNQ-UHFFFAOYSA-N dipropan-2-yl pentanedioate Chemical compound CC(C)OC(=O)CCCC(=O)OC(C)C MSQKMFXJFBXZNQ-UHFFFAOYSA-N 0.000 description 1
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 1
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- 229910052700 potassium Chemical group 0.000 description 1
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- CZYGEVQQOCNIML-UHFFFAOYSA-N propan-2-yl tridecanoate Chemical compound CCCCCCCCCCCCC(=O)OC(C)C CZYGEVQQOCNIML-UHFFFAOYSA-N 0.000 description 1
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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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
Description
技术领域Technical field
本发明涉及一种蚊香,具体涉及一种速燃驱蚊熏香及其制备方法,仅需要10~30分钟即可完成整个燃烧过程,可形成长达24小时驱蚊效果。The invention relates to a mosquito repellent incense, specifically to a quick-burning mosquito repellent incense and a preparation method thereof. It only takes 10 to 30 minutes to complete the entire burning process and can achieve a mosquito repellent effect of up to 24 hours.
背景技术Background technique
式I所示的拟除虫菊酯化合物是一种新颖的卫生杀虫剂,有很好的防治卫生害虫的基础活性;式I所示的拟除虫菊酯化合物可按如下反应路线制备:The pyrethroid compound represented by formula I is a novel sanitary insecticide with good basic activity in preventing and controlling sanitary pests; the pyrethroid compound represented by formula I can be prepared according to the following reaction route:
其中R为甲基或乙基,M为钠或钾R1为氢。Where R is methyl or ethyl, M is sodium or potassium and R1 is hydrogen.
例如,以3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号62138-41-4)为起始原料,和乙腈在60℃,乙醇钠作用下发生缩合反应4小时,加烯盐酸中和pH到8,加入乙酸乙酯及水分液,油层脱溶得到中间体3-(2-氰基-1-乙烯基)-2,2-二甲基环丙烷羧酸甲酯。For example, 3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 62138-41-4) is used as the starting material, and acetonitrile undergoes a condensation reaction under the action of sodium ethoxide at 60°C for 4 hours. , add enene hydrochloric acid to neutralize the pH to 8, add ethyl acetate and water to separate, and desolubilize the oil layer to obtain the intermediate 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester.
在得到的3-(2-氰基-1-乙烯基)-2,2-二甲基环丙烷羧酸甲酯中加入2,3,5,6-四氟苄醇(CAS号4084-38-2)、催化量钛酸四异丙酯及甲苯溶剂,缓慢升温至回流采出副产甲醇,气相中控,待原料转化完全后,降温至0-5℃,滴加少量的水,分液,脱溶,得到式I的拟除虫菊酯化合物。Add 2,3,5,6-tetrafluorobenzyl alcohol (CAS No. 4084-38) to the obtained methyl 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylate. -2), use catalytic amounts of tetraisopropyl titanate and toluene solvent, slowly heat up to reflux to extract the by-product methanol, and control the gas phase. After the raw materials are completely converted, cool down to 0-5°C, add a small amount of water dropwise, and separate. liquid and desolvated to obtain the pyrethroid compound of formula I.
以不同单一构型的环丙烷羧酸酯为起始原料,可以得到相应构型的式I的拟除虫菊酯化合物,例如以(1R,3R)-3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号27335-33-7)为起始原料合成,得到的是菊酸部分1R,3R的产物,再进行分布结晶,分离双键CN基Z,E异构体,可得到单一的2,3,4,5-四氟苄基-(1R,3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R,3R)-3-[(1E)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。以(1R,3S)-3-甲酰基-2,2-二甲基环丙烷羧酸甲酯(CAS号55701-02-5),可得到2,3,4,5-四氟苄基-(1R,3S)-3-(-2-氰基-1-乙烯基)-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯或2,3,4,5-四氟苄基-(1R,3S)-3-[(1E)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。Using cyclopropanecarboxylic acid esters of different single configurations as starting materials, pyrethroid compounds of formula I with corresponding configurations can be obtained, for example, (1R,3R)-3-formyl-2,2-dimethyl Methyl cyclopropanecarboxylate (CAS No. 27335-33-7) is used as the starting raw material for synthesis. What is obtained is the 1R and 3R products of the chrysanthemic acid part. Distribution crystallization is then carried out to separate the double bond CN group Z and E isomers. A single 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropane can be obtained carboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclo Propyl carboxylate. Using (1R,3S)-3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 55701-02-5), 2,3,4,5-tetrafluorobenzyl- (1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R , 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-( 1R,3S)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.
目前市场上的盘式蚊香需要燃烧8小时左右,长时间燃烧会出现较大的烟雾和气味,不仅给人们带来了不愉快的产品使用体验,而且也存在长时间的火灾隐患。为了改善传统蚊香剂型的缺点,提高使用体验感,本发明提供了一种速燃驱蚊熏香,短时间内将活性成分释放出来,达到驱蚊效果。这就对活性成分的安全性提高了要求,所以本产品优选式I化合物,式I化合物急性经口毒性评级为微毒,安全性优于市面上四氟甲醚菊酯、富右旋反式烯丙菊酯等为有效成分的产品,更适合用于速燃驱蚊熏香的配制。且本产品克重小、燃烧快,同时大量减少了溶剂的使用,减碳效果明显,持效时间长。The disc-type mosquito coils currently on the market need to burn for about 8 hours. If burned for a long time, larger smoke and odor will appear, which not only brings people an unpleasant product use experience, but also creates long-term fire hazards. In order to improve the shortcomings of traditional mosquito repellent incense and improve the user experience, the present invention provides a quick-burning mosquito repellent incense that releases active ingredients in a short time to achieve a mosquito repellent effect. This raises the requirements for the safety of active ingredients, so this product prefers the compound of formula I. The acute oral toxicity of the compound of formula I is rated as slightly toxic, and its safety is better than that of perfluthrin and dextrotrans-rich on the market. Products with active ingredients such as allethrin are more suitable for the preparation of fast-burning mosquito repellent incense. In addition, this product has a small weight and fast burning. At the same time, it greatly reduces the use of solvents. It has obvious carbon reduction effect and long lasting effect.
发明内容Contents of the invention
本发明所要解决的技术问题是针对现有技术中存在的不足,而提供一种速燃驱蚊熏香及其制备方法,本发明的蚊香可以在短时间燃烧完全。The technical problem to be solved by the present invention is to provide a quick-burning mosquito repellent incense and a preparation method thereof in view of the deficiencies in the prior art. The mosquito repellent incense of the present invention can burn completely in a short time.
为了实现上述目的,本发明采用如下技术方案:In order to achieve the above objects, the present invention adopts the following technical solutions:
一种速燃驱蚊熏香,按重量计,包含0.03%-0.5%组分A、0.5%-8%组分B、50%-95%助燃剂、2%-35%粘合剂、0.01%~10%的其他助剂;A quick-burning mosquito repellent incense, by weight, contains 0.03%-0.5% component A, 0.5%-8% component B, 50%-95% combustion accelerant, 2%-35% binder, 0.01 %~10% other additives;
所述的组分A为式(I)所示的化合物,即2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯;The component A is a compound represented by formula (I), namely 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate;
所述的组分B为溶剂;The component B is a solvent;
上述技术方案中,所示的组分A,优选自2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1S,3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1R,3R)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯、2,3,4,5-四氟苄基-(1S,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯四个异构体中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the component A shown is preferably from 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl] -2,2-Dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1S,3R)-3-[(1Z)-2-cyano-1-vinyl ]-2,2-Dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1R,3R)-3-[(1Z)-2-cyano-1-ethylene [(1Z)-2-cyano-1- A mixture of any one or two or more of the four isomers of vinyl]-2,2-dimethylcyclopropylcarboxylate in any proportion.
上述技术方案中,所述的组分A,进一步优选为2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯。In the above technical solution, the component A is further preferably 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl ]-2,2-dimethylcyclopropylcarboxylate.
上述技术方案中,所述组分B,选自酰胺类溶剂、一元羧酸酯类溶剂、三元羧酸酯类溶剂、醇醚类溶剂、C8-20的烷烃类溶剂;水;十二烷基苯、十烷基苯;C2-8的醇类溶剂;碳酸丙烯酯、碳酸丁烯酯、山梨醇酐单油酸酯、脂肪醇与环氧乙烷缩合物、γ-丁内酯、乙烷基乙氧基酯、二丙二醇甲醚乙酸酯、式(II)所示化合物、式(III)所示化合物、式(IV)所示化合物中的任意一种或两种及以上以任意比例混合而成的混合物;In the above technical solution, the component B is selected from the group consisting of amide solvents, monocarboxylic acid ester solvents, tricarboxylic acid ester solvents, alcohol ether solvents, C8-20 alkane solvents; water; dodecane Benzene, dedecylbenzene; C2-8 alcohol solvents; propylene carbonate, butylene carbonate, sorbitan monooleate, fatty alcohol and ethylene oxide condensate, γ-butyrolactone, ethyl Any one or two or more of alkyl ethoxy esters, dipropylene glycol methyl ether acetate, compounds represented by formula (II), compounds represented by formula (III), compounds represented by formula (IV), and any A mixture of proportions;
其中R1、R2和R3均为C1-C10的烷基。Wherein R 1 , R 2 and R 3 are all C1-C10 alkyl groups.
上述技术方案中,所述的酰胺类溶剂优选为N,N-二甲基葵酰胺。In the above technical solution, the amide solvent is preferably N,N-dimethylsulfonamide.
上述技术方案中,所述的一元羧酸酯类溶剂,优选自油酸甲酯、十三酸异丙酯、十四酸异丙酯、十六酸异丙酯、苯乙酸异丙酯、苯乙酸乙酯、十四酸正丁酯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the monocarboxylic acid ester solvent is preferably selected from the group consisting of methyl oleate, isopropyl tridecanoate, isopropyl myristate, isopropyl hexadecanoate, isopropyl phenylacetate, and benzene. Any one or a mixture of two or more of ethyl acetate and n-butyl myristate in any proportion.
上述技术方案中,所述的三元羧酸酯类溶剂,优选自戊二酸二异丙酯、己二酸二异丙酯、己二酸二异丁酯等二元羧酸酯类溶剂;柠檬酸三丁酯、乙酰柠檬酸三丁酯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the tricarboxylic acid ester solvent is preferably a dicarboxylic acid ester solvent such as diisopropyl glutarate, diisopropyl adipate, diisobutyl adipate; Any one of tributyl citrate and acetyl tributyl citrate or a mixture of two or more in any proportion.
上述技术方案中,所述的醇醚类溶剂,优选自三乙二醇单丁醚、二乙二醇单丁醚、丙二醇甲醚中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the alcohol ether solvent is preferably made from any one or two or more of triethylene glycol monobutyl ether, diethylene glycol monobutyl ether, and propylene glycol methyl ether in any proportion. mixture.
上述技术方案中,所述的C8-20的烷烃类溶剂,优选为D60(埃克森美孚石油化工公司)、D80(埃克森美孚石油化工公司)、D100(埃克森美孚石油化工公司)、D110(埃克森美孚石油化工公司)、D130(埃克森美孚石油化工公司)、Isopar-E(埃克森美孚石油化工公司)、Isopar-G(埃克森美孚石油化工公司)、Isopar-H(埃克森美孚石油化工公司)、Isopar-L(埃克森美孚石油化工公司)、Isopar-M(埃克森美孚石油化工公司)、辛烷、壬烷、奎烷、十一碳烷、十二碳烷、十三碳烷、十四碳烷、十五碳烷、十六碳烷中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the C8-20 alkane solvent is preferably D60 (ExxonMobil Petrochemical Company), D80 (ExxonMobil Petrochemical Company), or D100 (ExxonMobil Petrochemical Company) , D110 (ExxonMobil Petrochemical Company), D130 (ExxonMobil Petrochemical Company), Isopar-E (ExxonMobil Petrochemical Company), Isopar-G (ExxonMobil Petrochemical Company), Isopar -H (ExxonMobil Petrochemical Company), Isopar-L (ExxonMobil Petrochemical Company), Isopar-M (ExxonMobil Petrochemical Company), octane, nonane, quinane, undecane A mixture of any one, two or more of alkane, dodecane, tridecane, tetradecane, pentadecane and hexadecane in any proportion.
上述技术方案中,所述的C2-8的醇类溶剂,优选为乙醇、异丙醇、正丙醇、正丁醇、仲丁醇、叔丁醇、正戊醇及其异构体、正己醇及其异构体、正庚醇及其异构体、正辛醇及其异构体中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the C2-8 alcohol solvent is preferably ethanol, isopropanol, n-propanol, n-butanol, sec-butanol, tert-butanol, n-amyl alcohol and its isomers, n-hexyl alcohol. A mixture of any one, two or more of alcohol and its isomers, n-heptanol and its isomers, n-octanol and its isomers in any proportion.
上述技术方案中,所述的助燃剂,选自植物干燥粉末和/或炭粉末;所述的植物干燥粉末优选自木粉、菊科植物粉末、芹科植物粉末、桑科植物粉末、木犀科植物粉末、紫苏科植物粉末、忍冬科植物粉末、稻科植物粉末中的任意一种或两种及以上以任意比例混合而成的混合物;所述的炭粉末优选自木炭、活性炭、煤、炭黑中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the combustion accelerant is selected from dry plant powder and/or charcoal powder; the dry plant powder is preferably selected from wood powder, Asteraceae plant powder, Apiaceae plant powder, Moraceae plant powder, Oleaceae plant powder. Any one or a mixture of two or more plant powders, Perillaceae plant powders, Lonicerae plant powders, Oryzae plant powders in any proportion; the carbon powder is preferably selected from charcoal, activated carbon, coal, Any one or a mixture of two or more carbon blacks in any proportion.
上述技术方案中,所述的粘合剂,优选自羧甲基纤维素钠、羟乙基纤维素、羟丙基纤维素、阿拉伯树胶、海藻酸钠、玉米淀粉、塔布粉、聚丙烯酰胺、聚丙烯酸钠、聚氧化乙烯中的任意一种或两种及以上以任意比例混合而成的混合物。In the above technical solution, the adhesive is preferably selected from the group consisting of sodium carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, gum arabic, sodium alginate, corn starch, tarcloth flour, and polyacrylamide , sodium polyacrylate, polyethylene oxide, or a mixture of two or more in any proportion.
上述技术方案中,所述的其他助剂,包括香料、染料、防腐剂。In the above technical solution, the other auxiliaries include spices, dyes and preservatives.
上述技术方案中,所述的香料,选自精油和/或植物浸膏;所述的精油优选自玫瑰油、薰衣草油、甜橙油中的任意一种、两种及以上以任意比例混合而成的混合物;所述的植物浸膏优选自桂花浸膏、茉莉浸膏、晚香玉浸膏中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the fragrance is selected from essential oils and/or plant extracts; the essential oil is preferably selected from any one of rose oil, lavender oil, and sweet orange oil, or two or more are mixed in any proportion. The plant extract is preferably a mixture of any one, two or more of osmanthus extract, jasmine extract, and tuberose extract in any proportion.
上述技术方案中,所述的染料选自不同色系中的任意一种。In the above technical solution, the dye is selected from any one of different color systems.
上述技术方案中,所述的防腐剂选自苯甲酸钠、脱氢乙酸钠、山梨酸钾、尼铂金甲酯或卡松中的任意一种、两种及以上以任意比例混合而成的混合物。In the above technical solution, the preservative is selected from any one of sodium benzoate, sodium dehydroacetate, potassium sorbate, niplatin methyl ester or kason, or a mixture of two or more in any proportion.
本发明还提供一种上述的速燃驱蚊熏香的制备方法,将助燃剂、粘合剂、其他助剂按所述比例混合均匀后加水并捏合成形,然后烘干形成熏香基材,再将所述比例的组分A、组分B在室温(或加热至溶剂沸点以下)的条件下混合至澄清,最后喷涂到熏香基材上制得所述的速燃驱蚊熏香。The present invention also provides a method for preparing the above-mentioned quick-burning mosquito repellent incense. The combustion accelerant, adhesive and other auxiliaries are mixed evenly according to the stated proportion, then water is added and kneaded into shape, and then dried to form an incense base material. Then, Component A and Component B in the stated ratio are mixed at room temperature (or heated to below the boiling point of the solvent) until clarified, and finally sprayed onto the incense base material to prepare the quick-burning mosquito repellent incense.
上述技术方案中,所述的熏香基材,重量为1-10g,形状为扇形、菱形、三角形、椭圆形、不规则形状等。In the above technical solution, the weight of the incense base material is 1-10g, and the shape is fan-shaped, rhombus, triangle, oval, irregular shape, etc.
与现有技术相比,具有以下特点:Compared with existing technology, it has the following characteristics:
本发明的速燃驱蚊熏香,仅需10~30分钟即可完成整个燃烧过程,燃烧后可形成长达24小时驱蚊效果。The quick-burning mosquito repellent incense of the present invention can complete the entire burning process in only 10 to 30 minutes, and can achieve a mosquito repelling effect of up to 24 hours after burning.
具体实施方式Detailed ways
以下对本发明技术方案的具体实施方式详细描述,但本发明并不限于以下描述内容:Specific embodiments of the technical solution of the present invention are described in detail below, but the present invention is not limited to the following description:
本发明各实施例中的速燃驱蚊熏香制备方法如下:将助燃剂、粘合剂、其他助剂按比例混合均匀后加水并捏合成形,然后烘干形成熏香基材,将所述比例的组分A、B在室温(或加热至溶剂沸点以下)混合至澄清后喷涂到上述基材上制得速燃驱蚊熏香。The preparation method of the quick-burning mosquito repellent incense in each embodiment of the present invention is as follows: mix the combustion accelerant, adhesive, and other auxiliaries in proportion, add water and knead them into shape, and then dry them to form the incense base material. The proportions of components A and B are mixed at room temperature (or heated below the boiling point of the solvent) until clarified, and then sprayed onto the above substrate to prepare a quick-burning mosquito repellent incense.
下面结合具体的实施例,对本发明进行阐述:The present invention is described below in conjunction with specific examples:
制剂实施例1:(0.03%式I化合物驱蚊熏香,总重10g)Preparation Example 1: (0.03% mosquito repellent incense with compound of formula I, total weight 10g)
1.5g2,3,4,5-四氟苄基-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯((1R,3S)、(1S,3R)、(1R,3R)、(1S,3S)四种异构体各占25%),十四酸异丙酯补足至100g,得到1.5%母液;1.5g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R,3S ), (1S, 3R), (1R, 3R), (1S, 3S) four isomers each account for 25%), isopropyl myristate is added to 100g to obtain 1.5% mother liquor;
向1.5g玉米淀粉、3.5g活性炭粉、4.5g桑科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 1.5g corn starch, 3.5g activated carbon powder, 4.5g moraceae plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base material ;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例2:(0.05%式I化合物驱蚊熏香,总重6g)Preparation Example 2: (0.05% mosquito repellent incense with compound of formula I, total weight 6g)
1.5g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到1.5%母液;1.5g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 1.5% mother liquor;
向0.5g塔布粉、2g木炭粉、3g菊科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g tabu powder, 2g charcoal powder, 3g Asteraceae plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例3:(0.06%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重4g)Formulation Example 3: (0.06% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 4g)
1.2g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到1.2%母液;1.2g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 1.2% mother liquor;
向0.3g羧甲基纤维素钠、1.4g木炭粉、1.8g稻科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g绿色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.3g sodium carboxymethylcellulose, 1.4g charcoal powder, 1.8g rice plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g green dye, knead it into shape, and then dry it to form a smoked mixture. Fragrance base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例4:(0.08%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 4: (0.08% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
2g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到2%母液;2g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , make up isopropyl myristate to 100g to obtain 2% mother liquor;
向0.5g塔布粉、1.5g炭黑粉、2.5g芹科植物粉末、0.1g薰衣草油、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g tabu powder, 1.5g carbon black powder, 2.5g apiaceae plant powder, 0.1g lavender oil, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base. material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例5:(0.09%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 5: (0.09% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
2.25g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到2.25%母液;2.25g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 2.25% mother liquor;
向0.5g阿拉伯树胶、2g木炭粉、2g菊科植物粉末、0.1g薰衣草油、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g gum arabic, 2g charcoal powder, 2g Asteraceae plant powder, 0.1g lavender oil, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例6:(0.1%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 6: (0.1% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
2.5g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到2.5%母液;2.5g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 2.5% mother liquor;
向0.5g阿拉伯树胶、1.5g炭黑粉、2.5g稻科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g绿色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g gum arabic, 1.5g carbon black powder, 2.5g rice plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g green dye, knead it into shape, and then dry it to form an incense base material ;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例7:(0.15%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 7: (0.15% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
3.75g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到3.75%母液;3.75g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 3.75% mother liquor;
向0.5g阿拉伯树胶、2g木炭粉、2g菊科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g gum arabic, 2g charcoal powder, 2g Asteraceae plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例8:(0.2%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 8: (0.2% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
5g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到5%母液;5g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , make up isopropyl myristate to 100g to obtain 5% mother liquor;
向0.5g玉米淀粉、1.5g活性炭粉、2.5g稻科植物粉末、0.1g茉莉浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g corn starch, 1.5g activated carbon powder, 2.5g rice plant powder, 0.1g jasmine extract, 0.1g sodium benzoate, and 0.1g blue dye, knead it into shape, and then dry it to form an incense base material ;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例9:(0.4%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 9: (0.4% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
10g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到10%母液;10g 2,3,4,5-Tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate , make up isopropyl myristate to 100g to obtain 10% mother liquor;
向0.5g玉米淀粉、1.5g活性炭粉、2.5g稻科植物粉末、0.1g茉莉浸膏、0.1g苯甲酸钠、0.1g棕色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g corn starch, 1.5g activated carbon powder, 2.5g rice plant powder, 0.1g jasmine extract, 0.1g sodium benzoate, and 0.1g brown dye, knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例10:(0.5%2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 10: (0.5% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-di Methylcyclopropylcarboxylate mosquito repellent incense, total weight 5g)
12.5g2,3,4,5-四氟苄基-(1R,3S)-3-[(1Z)-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到12.5%母液;12.5g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylic acid Ester, isopropyl myristate was added to 100g to obtain 12.5% mother liquor;
向0.5g阿拉伯树胶、2g木碳粉、2g芹科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g gum arabic, 2g wood charcoal powder, 2g celery plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g blue dye and knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
制剂实施例11:(0.5%2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯驱蚊熏香,总重5g)Formulation Example 11: (0.5% 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate flooding Mosquito Incense, total weight 5g)
12.5g2,3,4,5-四氟苄基-3-[-2-氰基-1-乙烯基]-2,2-二甲基环丙基羧酸酯,十四酸异丙酯补足至100g,得到12.5%母液;12.5g 2,3,4,5-Tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, supplemented by isopropyl myristate to 100g to obtain 12.5% mother liquor;
向0.5g阿拉伯树胶、2g木碳粉、2g芹科植物粉末、0.1g桂花浸膏、0.1g苯甲酸钠、0.1g蓝色染料的混合物中加水并捏合成形,然后烘干形成熏香基材;Add water to a mixture of 0.5g gum arabic, 2g wood charcoal powder, 2g celery plant powder, 0.1g osmanthus extract, 0.1g sodium benzoate, and 0.1g blue dye and knead it into shape, and then dry it to form an incense base material;
取上述母液0.2g喷涂到上述熏香基材上。Take 0.2g of the above mother liquor and spray it onto the above incense base material.
对比实施例1:市售0.03%四氟甲醚菊酯盘式蚊香Comparative Example 1: Commercially available 0.03% permethrin disc mosquito coil
测试实施例1:Test Example 1:
将快燃蚊香按照《GBT 13917.4-2009农药登记用卫生杀虫剂室内药效试验及评价第4部分:蚊香》进行药效对比。采用圆筒装置。吸取试蚊30只,自筒下方原板(F)的中央圆孔处放入,塞紧胶塞(H)。待试蚊恢复正常活动后,随机取待测蚊香一段,水平状架在蚊香架上,在另处预点燃5min后,移至圆筒内熏烟1min,立即将蚊香移去,塞上胶塞(H),并计时,每隔一定时间记录被击倒的试虫数。观察时限为20min。测试应设三次及以上重复,且重复试验用蚊香应随机采取。每次试验结束后,应清洗试验装置。试验结果如下表所示:The effectiveness of fast-burning mosquito coils was compared in accordance with "GBT 13917.4-2009 Indoor Efficacy Test and Evaluation of Sanitary Insecticides for Pesticide Registration Part 4: Mosquito Repellents". Use cylinder device. Take 30 test mosquitoes, put them into the central round hole of the original plate (F) at the bottom of the tube, and tighten the rubber stopper (H). After the test mosquito returns to normal activities, randomly take a section of the mosquito coil to be tested, place it horizontally on the mosquito coil rack, pre-light it in another place for 5 minutes, then move it to the cylinder to smoke for 1 minute, immediately remove the mosquito coil and put a rubber stopper on it. (H), and time, and record the number of test insects knocked down at certain intervals. The observation time limit is 20 minutes. The test should be repeated three or more times, and the mosquito coils used for repeated tests should be randomly selected. After each test, the test device should be cleaned. The test results are shown in the table below:
测试实施例2:Test Example 2:
参考《GB/T 13917.10-2009农药登记用卫生杀虫剂室内药效试验及评价第10部分:模拟现场》,将蚊香样品放置于模拟房地面中央,分别在点燃后的第8h、16h、24h放入试蚊各100只,并计时,每隔一定时间记录被击倒的试虫数。观察时限为1h。测试应设三次及以上重复,且重复试验用蚊香应随机采取。每次试验结束后,应清洗试验装置。试验结果如下表所示:Referring to "GB/T 13917.10-2009 Indoor Efficacy Test and Evaluation of Sanitary Pesticides for Pesticide Registration Part 10: Simulation Site", place the mosquito coil samples in the center of the floor of the simulation room, and place them at 8h, 16h, and 24h after ignition. Put in 100 test mosquitoes each and time it. Record the number of test mosquitoes knocked down at certain intervals. The observation time limit is 1h. The test should be repeated three or more times, and the mosquito coils used for repeated tests should be randomly selected. After each test, the test device should be cleaned. The test results are shown in the table below:
上述实例只是为说明本发明的技术构思以及技术特点,并不能以此限制本发明的保护范围。凡根据本发明的实质所做的等效变换或修饰,都应该涵盖在本发明的保护范围之内。The above examples are only for illustrating the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent transformations or modifications made based on the essence of the present invention should be included in the protection scope of the present invention.
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