CN105211115A - A kind of natural liquid and preparation method thereof and application - Google Patents
A kind of natural liquid and preparation method thereof and application Download PDFInfo
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- CN105211115A CN105211115A CN201510746478.3A CN201510746478A CN105211115A CN 105211115 A CN105211115 A CN 105211115A CN 201510746478 A CN201510746478 A CN 201510746478A CN 105211115 A CN105211115 A CN 105211115A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- 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
A kind of natural liquid and preparation method thereof and application, relate to mosquito killing liquid.The raw material of described natural liquid consists of terpane-3,8-glycol, eucalyptus citriodora oil or citronellal, catalyzer, described to terpane-3, the mass ratio of 8-glycol and eucalyptus citriodora oil or citronellal is 1: (0.5 ~ 2), the addition of catalyzer is to terpane-3,8-glycol 0.1% ~ 2% by mass percentage.In to terpane-3,8-glycol, add eucalyptus citriodora oil or citronellal, then add catalyzer, after dehydration, by reactant liquor purifying, obtain natural liquid.Described natural liquid can be applied preparing in mosquito-repellent incense liquid, and in mosquito-repellent incense liquid, the content of natural liquid is 2% ~ 10% by mass percentage, and surplus is solvent; Mosquito rate of knockdown more than 95% during 30min, walk quickly and keep away rate less than 5%, overall mosquito-proof rate reaches 100%.Directly separation and Extraction from eucalyptus citriodora essential oil, can avoid eucalyptus citriodora raw material to waste in a large number, reduce costs, and promotes production capacity.
Description
Technical field
The present invention relates to mosquito killing liquid, especially relate to a kind of natural liquid and preparation method thereof and application.
Background technology
What in summer, drone mosquito vocal cords came is not only worry, and bite by mosquitos more may bring the deadly infectious diseases such as encephalitis B, malaria, dengue fever, yellow fever, filariosis, West Nile fever, kala-azar.People are except carrying out environmental renovation and physical isolation, and hygienic insecticide and culicifuge are last line of defenses of mosquito control.Because hygienic insecticide and environment for human survival close contact, its high insecticidal activity and hypotoxicity require to limit the mosquitocide that most of insecticides tested becomes practicality.Although have mosquito-repellent incense, electric mat, mosquito liquid etc. multi-form at the kill mosquito product of indoor use, its inherent desinsection composition all contains natural pyrethrin or pyrethroid.These pyrethrins insecticide mechanism of action are similar to DDT, it is aixs cylinder toxic agent, there is features such as knocking down fast, insecticidal power strong, wide spectrum, low toxicity, low-residual, but Long-Time Service is with after insecticides, makes mosquito create very strong pesticide resistance to pyrethrins insecticide.If continue to use pyrethrins insecticide kill mosquito always, only make small variations or only escalated dose to its structure, how long have more than is needed, pyrethrins insecticide thoroughly will take leave of the stage of kill mosquito product.Exploitation brand new kill mosquito culicifuge become mosquito control invade and harass, protection people ' s health in the urgent need to.
Chinese patent CN1806550 discloses a kind of ultrasonic fly eradication kill mosquito and to go out cockroach bactericidal liquid and the ultrasonic vaporising device using method for Pesticidal and sterilizing.By pure natural pyrethrin 0.25-2.5%, natural synergic agent lemon oil 10.0-20.0%, plant essence 1-5.0%, natural stabiliser rosemary, Xue MingRosma rinus officinalis 0.1-0.4%, use containing adding in ultrasonic vaporising device after the solvent 62.1-88.65% mixing of plant extracts nopinene; Or after pure natural pyrethrin 2.5-10%, natural synergic agent lemon oil 10-20%, plant essence 5-10%, natural stabiliser rosemary, Xue MingRosma rinus officinalis 1.0-4.0%, emulsifier 10-20%, plant extracts nopinene 36-71.9% mix, dilute with water 1-40 doubly, joins in ultrasonic vaporising device and use.
Chinese patent CN104381290A provides a kind of mosquito liquid, by the heating absorbability plug be immersed in insecticidal solution, active ingredient is volatilized to prevent and treat the insecticidal solution of mosquito, described mosquito liquid comprises formula (1) pyrethroid compound of 0.05-0.20% weight, and solvent is a kind of or its several mixture in ester class, alkanes or alcohol compound.
Chinese patent CN103704279A discloses a kind of mosquito liquid, comprises the composition of following part by weight: mosquito repellent working substance: 0.2-2%, solvent 20-70%, synergist 10-20%, surfactant 5-15%.
Although have mosquito-repellent incense, electric mat, mosquito liquid etc. multi-form at the kill mosquito product of indoor use, its inherent desinsection composition all contains natural pyrethrin or pyrethroid.These pyrethrins insecticide mechanism of action are similar to DDT, it is aixs cylinder toxic agent, have knock down fast, insecticidal power strong, the feature of wide spectrum, low toxicity, low-residual, but Long-Time Service is with after insecticides, makes mosquito create very strong pesticide resistance to pyrethrins insecticide.If continue to use pyrethrins insecticide kill mosquito always, only make small variations or only escalated dose to its structure, how long have more than is needed, pyrethrins insecticide thoroughly will take leave of the stage of kill mosquito product.Therefore, develop that the kill mosquito culicifuge of brand new has become that mosquito control is invaded and harassed, protection people ' s health in the urgent need to.
Summary of the invention
The object of the present invention is to provide a kind of natural liquid and preparation method thereof.
Another object of the present invention is to provide the application of described natural liquid in preparation kill mosquito product.
The raw material of described natural liquid consists of terpane-3,8-glycol, eucalyptus citriodora oil or citronellal, catalyzer, described to terpane-3, the mass ratio of 8-glycol and eucalyptus citriodora oil or citronellal is 1: (0.5 ~ 2), the addition of described catalyzer is to terpane-3,8-glycol 0.1% ~ 2% by mass percentage.
Described catalyzer can be selected from least one in lewis acid, Bronsted acid etc., and described lewis acid can be selected from least one in zinc chloride, zinc bromide, aluminium chloride etc.; Described Bronsted acid can be selected from least one in p-methyl benzenesulfonic acid, methanesulfonic acid, sulfuric acid, nitric acid etc.
The preparation method of described natural liquid is as follows:
In to terpane-3,8-glycol, add eucalyptus citriodora oil or citronellal, then add catalyzer, after dehydration, by reactant liquor purifying, obtain natural liquid.
Described when adding eucalyptus citriodora oil or citronellal in terpane-3,8-glycol, can solvent be added; The optional at least one in deodorized kerosine, ethanol, butyl butyrate etc. of described solvent.
The temperature of described dehydration can be 50 ~ 100 DEG C, and the time of dehydration can be more than 1h, the temperature of described dehydration preferably 60 DEG C, the time preferably 2 ~ 6h of described dehydration.
The method of described purifying can be: it is 7 ~ 9 that reactant liquor sodium carbonate liquor is neutralized to water layer pH, is washed to neutrality, and leave standstill separatory, get upper liquid and carry out fractionation in fractionation still, steam low-boiling point material, in fractionation still, residue is natural liquid.
The mass percentage concentration of described sodium carbonate liquor can be 0.5% ~ 5%.
The described preparation method to terpane-3,8-glycol is as follows:
Eucalyptus citriodora oil or citronellal and sulfuric acid solution are stirred at 20 ~ 40 DEG C, stratification, upper liquid is terpane-3,8-glycol.
The time of described stirring can be more than 5h, preferably 10 ~ 24h; The mass percentage concentration of described sulfuric acid solution can be 0.5% ~ 5%.
Described natural liquid can be applied preparing in mosquito-repellent incense liquid, and in described mosquito-repellent incense liquid, the content of natural liquid is 2% ~ 10% by mass percentage, and surplus is solvent.
Described solvent can be selected from least one in cyclohexane, n-hexane, toluene etc.
Through test, described mosquito-repellent incense liquid when 30min mosquito rate of knockdown more than 95%, walk quickly and keep away rate less than 5%, overall mosquito-proof rate reaches 100%.
The present invention is separation and Extraction from eucalyptus citriodora essential oil directly, eucalyptus citriodora raw material can be avoided to waste in a large number, greatly reduce costs, and promotes production capacity.
The mosquito repellent plant that the present invention extensively plants China---isolate the multiple composition with mosquito repellent function in eucalyptus citriodora, as citronellal, citronellol, to terpane-3, the materials such as 8-glycol, wherein one group of isomer mixing composition do not paid close attention to for people shows significant kill mosquito effect.
By analysis, the Main Ingredients and Appearance in described natural liquid is 2-[2,6-dimethyl-5-heptenyl]-4,4,8-trimethyl-1,3-hexahydrobenzenes and dioxanes, and molecular formula is C
20h
36o
2, chemical structural formula is as follows:
Accompanying drawing explanation
Fig. 1 is the gas-chromatography spectrum of the natural liquid that embodiment 2 obtains.
Fig. 2 is the mass spectrogram of the natural liquid that embodiment 2 obtains.Mass spectrogram is the mass spectrogram of appearance time 35.726min material.
Embodiment
The preparation of the natural liquid of embodiment 1
A, get 200g citronellal, 220g to terpane-3,8-glycol, 2.5g p-methyl benzenesulfonic acid, 100g cyclohexane reflux dewatering, 90 ~ 100 DEG C of reaction 4h, obtain natural liquid crude product a;
B, the natural liquid crude product a 400g1% sodium carbonate liquor neutralization obtained by A, be washed to neutrality, leave standstill separatory, obtain natural liquid crude product b;
C, the natural liquid crude product b obtained by B are placed in fractionation still, 1kPa vacuum topping, capital vapor (steam) temperature 54 ~ 130 DEG C, fluid temperature 88 ~ 144 DEG C in fractionation still, steam low-boiling point material 50g, in fractionation still, residue is the natural liquid of final products, weight 340g, adopt gas chromatography-mass spectrometry analysis, wherein 2-[2,6-dimethyl-5-heptenyl]-4,4,8-trimethyl-1,3-hexahydrobenzene the content of dioxanes is 75.7%.
The preparation of the natural liquid of embodiment 2
A, by 500g eucalyptus citriodora oil, add 1283g2.5% sulfuric acid solution, stirring reaction 19h at 30 DEG C, point disacidify liquid obtains terpane-3,8-glycol crude product;
B, get that A obtains to terpane-3,8-glycol crude product 50g, add 50g eucalyptus citriodora oil, 0.5g p-methyl benzenesulfonic acid, vacuum dehydration at 60 DEG C, reaction 4h, obtains natural liquid crude product a;
C, the natural liquid crude product a 100g2% sodium carbonate liquor neutralization that B is obtained, be washed to neutrality, leave standstill separatory, obtain natural liquid crude product b, crude product weight 95g;
D, the natural liquid crude product b obtained by C are placed in fractionation still, vacuum topping under 1kPa, capital vapor (steam) temperature 54 ~ 130 DEG C, fluid temperature 88 ~ 144 DEG C in fractionation still, steam low-boiling point material 28g, in fractionation still, residue is the natural liquid of final products, weight 60g, adopt gas chromatography-mass spectrometry analysis, wherein 2-[2,6-dimethyl-5-heptenyl]-4,4,8-trimethyl-1,3-hexahydrobenzene the content of dioxanes is 86.815%.
The Performance Detection of the natural liquid of embodiment 3
By the final products of embodiment 1, embodiment 2 by 4% addition add in deodorized kerosine, make mosquito liquid sample, sample entrusts Prevention & Control Station of Parasitic Disease, China Diseases Prevention & C to carry out effect exterminating mosquito test, and test result is as shown in table 1.
Table 1
Test result shows, the natural liquid of gained of the present invention has good mosquito-proof effect.
Claims (10)
1. a natural liquid, it is characterized in that its raw material consists of terpane-3,8-glycol, eucalyptus citriodora oil or citronellal, catalyzer, described to terpane-3, the mass ratio of 8-glycol and eucalyptus citriodora oil or citronellal is 1: (0.5 ~ 2), the addition of described catalyzer is to terpane-3,8-glycol 0.1% ~ 2% by mass percentage.
2. a kind of natural liquid as claimed in claim 1, is characterized in that described catalyzer is selected from least one in lewis acid, Bronsted acid; Described lewis acid can be selected from least one in zinc chloride, zinc bromide, aluminium chloride; Described Bronsted acid can be selected from least one in p-methyl benzenesulfonic acid, methanesulfonic acid, sulfuric acid, nitric acid.
3. the preparation method of natural liquid as claimed in claim 1, is characterized in that its concrete steps are as follows:
In to terpane-3,8-glycol, add eucalyptus citriodora oil or citronellal, then add catalyzer, after dehydration, by reactant liquor purifying, obtain natural liquid.
4. the preparation method of natural liquid as claimed in claim 3, is characterized in that described when adding eucalyptus citriodora oil or citronellal in terpane-3,8-glycol, adds solvent; The optional at least one in deodorized kerosine, ethanol, butyl butyrate of described solvent.
5. the preparation method of natural liquid as claimed in claim 3, it is characterized in that the temperature of described dehydration is 50 ~ 100 DEG C, the time of dehydration is more than 1h; The temperature of described dehydration preferably 60 DEG C, the time preferably 2 ~ 6h of described dehydration.
6. the preparation method of natural liquid as claimed in claim 3, it is characterized in that the method for described purifying is: reactant liquor sodium carbonate liquor being neutralized to water layer pH is 7 ~ 9, be washed to neutrality, leave standstill separatory, get upper liquid and carry out fractionation in fractionation still, steam low-boiling point material, in fractionation still, residue is natural liquid.
7. the preparation method of natural liquid as claimed in claim 6, is characterized in that the mass percentage concentration of described sodium carbonate liquor is 0.5% ~ 5%.
8. the preparation method of natural liquid as claimed in claim 3, is characterized in that the described preparation method to terpane-3,8-glycol is as follows:
Eucalyptus citriodora oil or citronellal and sulfuric acid solution are stirred at 20 ~ 40 DEG C, stratification, upper liquid is terpane-3,8-glycol.
9. the preparation method of natural liquid as claimed in claim 8, is characterized in that the time of described stirring is more than 5h, preferably 10 ~ 24h; The mass percentage concentration of described sulfuric acid solution can be 0.5% ~ 5%.
10. natural liquid is applied preparing in mosquito-repellent incense liquid as claimed in claim 1, and in described mosquito-repellent incense liquid, the content of natural liquid is 2% ~ 10% by mass percentage, and surplus is solvent;
Described solvent can be selected from least one in cyclohexane, n-hexane, toluene.
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| CN201510746478.3A CN105211115B (en) | 2015-11-05 | 2015-11-05 | A kind of natural liquid and the preparation method and application thereof |
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| CN201510746478.3A CN105211115B (en) | 2015-11-05 | 2015-11-05 | A kind of natural liquid and the preparation method and application thereof |
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| CN105211115B CN105211115B (en) | 2019-04-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108477243A (en) * | 2018-02-07 | 2018-09-04 | 黄珊珊 | A kind of pest repellant, insecticides |
| CN111264570A (en) * | 2020-03-10 | 2020-06-12 | 中山榄菊日化实业有限公司 | Plant mosquito-repellent incense and preparation method thereof |
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| US5959161A (en) * | 1997-10-28 | 1999-09-28 | Takasago International Corporation | Method for producing para-menthane-3,8-diol |
| CN1731931A (en) * | 2002-10-31 | 2006-02-08 | 弗朗茨·本契奇 | Acetals as insect repellant agents |
| WO2009034352A1 (en) * | 2007-09-13 | 2009-03-19 | Ian Thomas Dell | Composition containing p-menthane-3, 8-diol and its use as insect repellent |
| CN103193598A (en) * | 2013-03-15 | 2013-07-10 | 彭学东 | Oriented synthesis preparation process of cis-form p-menthane-3,8-diol |
| CN103570501A (en) * | 2013-11-19 | 2014-02-12 | 南宁辰康生物科技有限公司 | Preparation method of bis-terpane-3,8-diol |
-
2015
- 2015-11-05 CN CN201510746478.3A patent/CN105211115B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5959161A (en) * | 1997-10-28 | 1999-09-28 | Takasago International Corporation | Method for producing para-menthane-3,8-diol |
| CN1731931A (en) * | 2002-10-31 | 2006-02-08 | 弗朗茨·本契奇 | Acetals as insect repellant agents |
| WO2009034352A1 (en) * | 2007-09-13 | 2009-03-19 | Ian Thomas Dell | Composition containing p-menthane-3, 8-diol and its use as insect repellent |
| CN103193598A (en) * | 2013-03-15 | 2013-07-10 | 彭学东 | Oriented synthesis preparation process of cis-form p-menthane-3,8-diol |
| CN103570501A (en) * | 2013-11-19 | 2014-02-12 | 南宁辰康生物科技有限公司 | Preparation method of bis-terpane-3,8-diol |
Non-Patent Citations (1)
| Title |
|---|
| HAIYANG CHENG: "Cyclization of citronellal to p-menthane-3,8-diols in water and carbon dioxide", 《GREEN CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108477243A (en) * | 2018-02-07 | 2018-09-04 | 黄珊珊 | A kind of pest repellant, insecticides |
| CN111264570A (en) * | 2020-03-10 | 2020-06-12 | 中山榄菊日化实业有限公司 | Plant mosquito-repellent incense and preparation method thereof |
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| CN105211115B (en) | 2019-04-26 |
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Address after: No. 308, Tong'an Park, Tong'an Industrial Concentration Zone, Xiamen City, Fujian Province, 361100 Patentee after: Xiamen Amber Flavor Co.,Ltd. Address before: No. 308, Tong'an Park, Tong'an Industrial Concentration Zone, Xiamen City, Fujian Province, 361100 Patentee before: XIAMEN AMBER DAILY CHEMICAL TECHNOLOGY CO.,LTD. |
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