CN105211115B - A kind of natural liquid and the preparation method and application thereof - Google Patents
A kind of natural liquid and the preparation method and application thereof Download PDFInfo
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- CN105211115B CN105211115B CN201510746478.3A CN201510746478A CN105211115B CN 105211115 B CN105211115 B CN 105211115B CN 201510746478 A CN201510746478 A CN 201510746478A CN 105211115 B CN105211115 B CN 105211115B
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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 the preparation method and application thereof, is related to mosquito killing liquid.The raw material group of the natural liquid becomes to terpane -3,8- glycol, eucalyptus citriodora oil or citronellal, catalyst, it is described to terpane -3, the mass ratio of 8- glycol and eucalyptus citriodora oil or citronellal is 1: (0.5~2), the additive amount of catalyst is 0.1%~2% to terpane -3,8- glycol by mass percentage.It to eucalyptus citriodora oil or citronellal are added in terpane -3,8- glycol, is adding catalyst, after dehydration, reaction solution is being purified to get natural liquid.The natural liquid can be applied in preparing mosquito-repellent incense liquid, and the content of natural liquid is 2%~10% by mass percentage in mosquito-repellent incense liquid, and surplus is solvent；95% or more mosquito rate of knockdown when 30min walks quickly and keeps away rate 5% hereinafter, overall mosquito-proof rate reaches 100%.The separation and Extraction directly from eucalyptus citriodora essential oil can avoid eucalyptus citriodora raw material and largely waste, reduce cost, promotes production capacity.
Description
Technical field
The present invention relates to mosquito killing liquids, more particularly, to a kind of natural liquid and the preparation method and application thereof.
Background technique
Drone mosquito sound bring is not only worry in summer, and bite by mosquitos is more likely to that encephalitis B can be brought, malaria, steps on
Remove from office the deadly infectious diseases such as heat, yellow fever, filariasis, West Nile fever, kala-azar.People are in addition to carrying out environmental renovation and physical isolation
Outside, hygienic insecticide and culicifuge are last line of defense of mosquito control.Because hygienic insecticide connects closely with environment for human survival
Touching, high insecticidal activity and hypotoxicity require to limit most of insecticides tested as practical mosquitocide.Although using indoors
Mosquito eradication product have a different forms such as mosquito-repellent incense, electric mat, mosquito liquid, but all contain natural deinsectization in desinsection composition in it
Pyrethroids or pyrethroid.These pyrethrins insecticide mechanism of action are similar to DDT, are aixs cylinder toxic agents, have knock down it is fast,
The features such as insecticidal power is strong, wide spectrum, low toxicity, low-residual, but after being used for a long time with insecticides, make mosquito to cinerins desinsection
Agent produces very strong drug resistance.If continuing to use pyrethrins insecticide mosquito eradication always, only to its structure make small variations or
How long only escalated dose has more than is needed, and pyrethrins insecticide will thoroughly take leave of the stage of mosquito eradication product.The completely new knot of exploitation
The mosquito eradication culicifuge of structure have become mosquito control invade and harass, protection people's health there is an urgent need to.
Chinese patent CN1806550 discloses that cockroach bactericidal liquid is gone out in a kind of ultrasonic wave fly eradication mosquito eradication and ultrasonic wave vaporising device is used
In the application method of Pesticidal and sterilizing.By pure natural pyrethrin 0.25-2.5%, natural synergic agent lemon oil 10.0-
20.0%, the solvent of plant essence 1-5.0%, natural stabiliser rosemary 0.1-0.4%, the nopinene containing plant extracts
It is added in ultrasonic wave vaporising device and uses after 62.1-88.65% mixing；Or it is pure natural pyrethrin 2.5-10%, natural
Synergist lemon oil 10-20%, plant essence 5-10%, natural stabiliser rosemary 1.0-4.0%, emulsifier 10-
20%, it is diluted with water 1-40 times after plant extracts nopinene 36-71.9% mixing, be added in ultrasonic wave vaporising device
It uses.
Chinese patent CN104381290A provides a kind of mosquito liquid, is by heating the absorbability being immersed in insecticidal solution
Plug makes effective component volatilization to prevent and treat the insecticidal solution of mosquito, and the mosquito liquid includes the formula (1) of 0.05-0.20% weight
Pyrethroid compound, solvent are one of esters, alkanes or alcohol compound or its several mixture.
Chinese patent CN103704279A discloses a kind of mosquito liquid, and the ingredient including following weight ratio: mosquito repellent has
Imitate object: 0.2-2%, solvent 20-70%, synergist 10-20%, surfactant 5-15%.
Although the mosquito eradication product used indoors has the different forms such as mosquito-repellent incense, electric mat, mosquito liquid, in
Desinsection composition all contains natural pyrethrin or pyrethroid.These pyrethrins insecticide mechanism of action are similar to DDT,
It is aixs cylinder toxic agent, has the characteristics that knock down that fast, insecticidal power is strong, wide spectrum, low toxicity, low-residual, but after is used for a long time with insecticides,
Mosquito is set to produce very strong drug resistance to pyrethrins insecticide.If continuing to use pyrethrins insecticide mosquito eradication always,
Small variations or only escalated dose only are made to its structure, how long are had more than is needed, pyrethrins insecticide, which will thoroughly take leave of, to go out
The stage of mosquito product.Therefore, the mosquito eradication culicifuge for developing brand new has become mosquito control and invades and harasses, protects compeling for people's health
It is essential and wants.
Summary of the invention
The purpose 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 application of the natural liquid in preparation mosquito eradication product.
The raw material group of the natural liquid becomes to terpane -3,8- glycol, eucalyptus citriodora oil or citronellal, catalyst, described
Mass ratio to terpane -3,8- glycol and eucalyptus citriodora oil or citronellal is 1: the additive amount of (0.5~2), the catalyst is pressed
Mass percent is to the 0.1%~2% of terpane -3,8- glycol.
The catalyst can be selected from least one of lewis acid, Bronsted acid etc., and the lewis acid can be selected from chlorination
At least one of zinc, zinc bromide, aluminium chloride etc.；The Bronsted acid can be selected from p-methyl benzenesulfonic acid, methanesulfonic acid, sulfuric acid, nitric acid etc.
At least one of.
The natural liquid the preparation method is as follows:
To eucalyptus citriodora oil or citronellal are added in terpane -3,8- glycol, catalyst added, it, will after dehydration
Reaction solution purifies to get natural liquid.
It is described to eucalyptus citriodora oil is added in terpane -3,8- glycol or when citronellal, solvent can be added；The solvent can
Selected from least one of deodorized kerosine, ethyl alcohol, butyl butyrate etc..
The temperature of the dehydration can be 50~100 DEG C, and the time of dehydration can be 1h or more, the dehydration
Preferably 60 DEG C of temperature, the time of the dehydration preferably 2~6h.
The method of the purifying can are as follows: and it is 7~9 that reaction solution, which is neutralized to water layer pH with sodium carbonate liquor, is washed to neutrality,
Liquid separation is stood, takes upper liquid to be fractionated in fractionation kettle, steams low-boiling point material, being fractionated residue in kettle is natural liquid.
The mass percentage concentration of the sodium carbonate liquor can be 0.5%~5%.
It is described to terpane -3,8- glycol the preparation method is as follows:
Eucalyptus citriodora oil or citronellal and sulfuric acid solution are stirred at 20~40 DEG C, stratification, upper liquid is to thin
Lotus alkane -3,8- glycol.
The time of the stirring can be 5h or more, preferably 10~for 24 hours；The mass percentage concentration of the sulfuric acid solution can be
0.5%~5%.
The natural liquid can be applied in preparing mosquito-repellent incense liquid, and the content of natural liquid is by mass percentage in the mosquito-repellent incense liquid
2%~10%, surplus is solvent.
The solvent can be selected from least one of hexamethylene, n-hexane, toluene etc..
Through testing, the mosquito-repellent incense liquid in 30min 95% or more mosquito rate of knockdown, walk quickly and keep away rate 5% hereinafter, overall mosquito-proof rate
Reach 100%.
The present invention can largely waste, pole compared to the separation and Extraction directly from eucalyptus citriodora essential oil to avoid eucalyptus citriodora raw material
The earth reduces cost, promotes production capacity.
Mosquito repellent plant that the present invention plants China extensively --- isolated in eucalyptus citriodora it is a variety of with mosquito repellent function at
Part, such as citronellal, citronellol, to substances such as terpane -3,8- glycol, wherein one group of not concerned isomers mixing
Composition shows significant mosquito eradication effect.
Through analyzing, the main ingredient in the natural liquid is 2- [2,6- dimethyl -5- heptenyl] -4,4,8- trimethyls -
1,3- hexahydro benzdioxan, molecular formula C20H36O2, chemical structural formula is as follows:
Detailed description of the invention
Fig. 1 is the gas-chromatography spectrum of natural liquid made from embodiment 2.
Fig. 2 is the mass spectrogram of natural liquid made from embodiment 2.Mass spectrogram is the matter of appearance time 35.726min substance
Spectrogram.
Specific embodiment
The preparation of the natural liquid of embodiment 1
A, 200g citronellal is taken, 220g takes off terpane -3,8- glycol, 2.5g p-methyl benzenesulfonic acid, the reflux of 100g hexamethylene
Water, 90~100 DEG C of reaction 4h, obtains natural liquid crude product a；
B, the natural liquid crude product a for obtaining A is neutralized with 1% sodium carbonate liquor of 400g, is washed to neutrality, is stood liquid separation, is obtained
To natural liquid crude product b；
C, the natural liquid crude product b for obtaining B is placed in fractionation kettle, 1kPa vacuum topping, capital vapor (steam) temperature 54~130
DEG C, 88~144 DEG C of fluid temperature are fractionated in kettle, low-boiling point material 50g is steamed, being fractionated residue in kettle is that final products are natural
Liquid, weight 340g, using gas chromatography-mass spectrometry analysis, wherein 2- [2,6- dimethyl -5- heptenyl] -4,4,8- trimethyl -1,
The content of 3- hexahydro benzdioxan is 75.7%.
The preparation of the natural liquid of embodiment 2
A, by 500g eucalyptus citriodora oil, 2.5% sulfuric acid solution of 1283g is added, is stirred to react 19h at 30 DEG C, divides and acid solution is gone to obtain
To terpane -3,8- glycol crude product；
B, take that A obtains to terpane -3,8- glycol crude product 50g, 50g eucalyptus citriodora oil, 0.5g p-methyl benzenesulfonic acid is added, in
Vacuum dehydration at 60 DEG C reacts 4h, obtains natural liquid crude product a；
C, the natural liquid crude product a that B is obtained is neutralized with 2% sodium carbonate liquor of 100g, is washed to neutrality, is stood liquid separation, is obtained
To natural liquid crude product b, crude product weight 95g；
D, the natural liquid crude product b for obtaining C is placed in fractionation kettle, vacuum topping under 1kPa, capital vapor (steam) temperature 54~130
DEG C, 88~144 DEG C of fluid temperature are fractionated in kettle, low-boiling point material 28g is steamed, being fractionated residue in kettle is that final products are natural
Liquid, weight 60g, using gas chromatography-mass spectrometry analysis, wherein 2- [2,6- dimethyl -5- heptenyl] -4,4,8- trimethyl -1,
The content of 3- hexahydro benzdioxan is 86.815%.
The performance detection of the natural liquid of embodiment 3
The final products of embodiment 1, embodiment 2 are added in deodorized kerosine by 4% additive amount, electric mosquito repellent is made
Liquid sample, sample entrust Prevention & Control Station of Parasitic Disease, China Diseases Prevention & C to carry out effect exterminating mosquito test, test knot
Fruit is as shown in table 1.
Table 1
Test result shows that the natural liquid of gained of the invention has good mosquito-proof effect.
Claims (5)
1. a kind of application of natural liquid in mosquito eradication, it is characterised in that its raw material group becomes to terpane -3,8- glycol, eucalyptus citriodora
Oil and catalyst；Or its raw material group becomes to terpane -3,8- glycol, citronellal and catalyst, it is described to terpane -3,8- bis-
The mass ratio of alcohol and eucalyptus citriodora oil or citronellal is 1: (0.5~2), the additive amount of the catalyst are to thin by mass percentage
The 0.1%~2% of lotus alkane -3,8- glycol；The catalyst is selected from least one of lewis acid, Bronsted acid；The Louis
This acid is selected from least one of zinc chloride, zinc bromide, aluminium chloride；The Bronsted acid is selected from p-methyl benzenesulfonic acid, methanesulfonic acid, sulphur
At least one of acid, nitric acid；
The natural liquid is prepared using following methods:
It to eucalyptus citriodora oil or citronellal are added in terpane -3,8- glycol, is adding catalyst, after dehydration, will react
Liquid purifies to get natural liquid；It is described to terpane -3,8- glycol the preparation method is as follows: by eucalyptus citriodora oil or citronellal and sulphur
Acid solution stirs at 20~40 DEG C, stratification, and upper liquid is to terpane -3,8- glycol；The time of the stirring is
5h or more；The mass percentage concentration of the sulfuric acid solution is 0.5%~5%；
The method of the purifying are as follows: it is 7~9 that reaction solution, which is neutralized to water layer pH with sodium carbonate liquor, is washed to neutrality, stands and divide
Liquid takes upper liquid to be fractionated in fractionation kettle, steams low-boiling point material, and being fractionated residue in kettle is natural liquid；The carbon
The mass percentage concentration of acid sodium solution is 0.5%~5%.
2. application of a kind of natural liquid in mosquito eradication as described in claim 1, it is characterised in that described to terpane -3,8- bis-
When eucalyptus citriodora oil or citronellal being added in alcohol, solvent is added；The solvent in deodorized kerosine, ethyl alcohol, butyl butyrate extremely
Few one kind.
3. the application of a kind of natural liquid in mosquito eradication as described in claim 1, it is characterised in that the temperature of the dehydration is
50~100 DEG C, the time of dehydration is 1h or more.
4. the application of a kind of natural liquid in mosquito eradication as claimed in claim 3, it is characterised in that the temperature of the dehydration is
60 DEG C, the time of the dehydration is 2~6h.
5. the application of a kind of natural liquid in mosquito eradication as described in claim 1, it is characterised in that the time of the stirring is 10~
24h。
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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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| CN105211115A CN105211115A (en) | 2016-01-06 |
| CN105211115B true CN105211115B (en) | 2019-04-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108477243A (en) * | 2018-02-07 | 2018-09-04 | 黄珊珊 | A kind of pest repellant, insecticides |
| CN111264570B (en) * | 2020-03-10 | 2022-01-04 | 中山榄菊日化实业有限公司 | Plant mosquito repellent incense and preparation method thereof |
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 Repellents |
| 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 Repellents |
| 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 |
|---|
| Cyclization of citronellal to p-menthane-3,8-diols in water and carbon dioxide;Haiyang Cheng;《Green Chemistry》;20091231;第1227–1231页 |
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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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