CN102860303A - Method for utilizing citriodora oil to extract waste liquid to prepare mosquito repellent - Google Patents
Method for utilizing citriodora oil to extract waste liquid to prepare mosquito repellent Download PDFInfo
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- CN102860303A CN102860303A CN2012103886320A CN201210388632A CN102860303A CN 102860303 A CN102860303 A CN 102860303A CN 2012103886320 A CN2012103886320 A CN 2012103886320A CN 201210388632 A CN201210388632 A CN 201210388632A CN 102860303 A CN102860303 A CN 102860303A
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Abstract
The invention provides a method for utilizing citriodora oil to extract waste liquid to prepare a mosquito repellent and relates to a method for preparing the mosquito repellent. The method comprises utilizing aqueous phase distillate flowing out of an oil-water separator of a citriodora oil extractor, enabling p-menthane-3, 8-diol in the aqueous phase distillate to be dissolved out by adding sodium chloride or potassium chloride, adding an organic solvent to perform extraction, then performing pressure-reducing distillation on the organic solvent to obtain light yellow oily liquid, freezing the light yellow oily liquid, dissolving out and crystallizing, filtering to obtain p-menthane-3, 8-diol, finally evenly mixing and dissolving 10%-50% of p-menthane-3, 8-diol, 5%-20% of propylene glycol, 10%-50% of 75% ethanol, 2%-10% of glycerol and 2%-10% of 1,3-butanediol according to mass ratio, and obtaining the mosquito repellent. The method is simple to operate, reduces environmental pollution and harm caused to the humans, and is low in cost and convenient to popularize and use.
Description
Technical field
The present invention relates to a kind of method for preparing the mosquito repellant, particularly a kind of lemon eucalyptus oil that utilizes extracts the method that waste liquid prepares the mosquito repellant.
Background technology
The production of domestic lemon eucalyptus oil all is to adopt traditional steam distillation technique.The cardinal principle of steam distillation: under water and be heated to and boil (such as water distillation) or when passing into the bed of material (such as water and steam distillation and live (open) steam distillation) of aromatic raw material with steam when the vegetalitas aromatic raw material, because boiling water or steam at first produce such effect to raw material, namely the fragrant oil content on the raw tissue surface directly contacts with boiling water, thereby two partial vapour pressures of water and oil have been produced, and the stagnation pressure of this mixed vapour equals the interior pressure that adopts of boiler all the time, as adopting air-distillation in the pot, then the mixed vapour temperature is always below 100 ℃, mixed vapour enters condenser by wireway and carries out condensing cooling, and then after water-oil separating, namely get essential oil.When boiling water or steam when dividing the generation effect to the raw tissue surface oil, its boiling water or steam permeate, spread to the plant material organization internal simultaneously, thereby make the essential oil of organization internal, take water as carrier, constantly be diffused into again step by step tissue surface, because surperficial oil content constantly gasifies, this diffusion process just can continue to carry out, until fragrant oil content almost all diffuses to the surface till being distilled out of.
In steam distillation technique, generally only collect in the distillate oil phase part as essential oil product, then do not receive publicity for the water soluble ingredient in the essential oil.Water soluble ingredient in the essential oil mainly is present in the extraction waste liquid of isolating behind the essential oil, these compositions mainly are the containing oxygen derivatives of terpenoid, although content is not high, but give off a strong fragrance, represented the distinctive fragrance of volatile oil, it is the part of most worthy in the essential oil, these components are slightly soluble in water, they fully can not be separated by simple mechanics means, and be slightly soluble in this part essential oil of water, because the oil-water ratio of distillate is little, to distillate ratio shared in the essential oil be appreciable whole.
The killing propagation disease is endangering human health.For a long time, people use number of chemical insecticide control mosquito, but chemical insecticide is when killing mosquito, not only contaminated environment, and infringement health.These factors impel people attempt to seek a kind of environmentally friendly, to the insecticide of people's low toxicity.Studies show that some plants essential oils have certain poisoning and repellent action to mosquito, mosquito is had food refusal, repellent, lures, directly kills and suppresses growth, compare with traditional synthetic pesticide have low toxicity, low-residual, to advantages such as environmental influence are little.
Summary of the invention
The purpose of this invention is to provide the method for preparing the mosquito repellant that a kind of environmental protection, cost product low, that be convenient to promote the use of, make can be effectively mosquito-proof.
The technical scheme that solves the problems of the technologies described above is: a kind of lemon eucalyptus oil that utilizes extracts the method that waste liquid prepares the mosquito repellant, comprises the steps:
A. extract from lemon eucalyptus oil and extract the anophelifuge activity composition the waste liquid
p-menthane-3,8-diol:
(1) collects the water distillate, the water distillate of described water distillate for from the oil water separator of lemon eucalyptus leaf oil extractor, flowing out;
(2) in above-mentioned obtained water distillate, add sodium chloride or potassium chloride, make in the water distillate
p-menthane-3,8-diol separates out;
(3) to extracting through adding organic solvent in the water distillate after the step (2), get the organic solvent phase after the extraction;
(4) above-mentioned obtained organic solvent is carried out decompression distillation mutually, obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed carry out freezingly in the refrigerating chamber, treat crystallization, filter and namely obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepare the mosquito repellant:
In mass ratio with 10%～50%
p-menthane-3,8-diol, 5%～20% propane diols, 10%～50% 75% ethanol, 2%～10% glycerine, 2%～10% 1,3-BDO mix, stir evenly, are dissolved into finished product, namely are prepared into the mosquito repellant.
Its further technical scheme is: the water distillate that flows out in the oil water separator of the lemon eucalyptus leaf oil extractor described in the step (1) is colourless transparent liquid, for isolating the remaining distilled water behind the lemon eucalyptus oil, be dissolved with the volatile ingredient of part lemon eucalyptus leaf in this water, its main component is
p-menthane-3,8-diol.
Its further technical scheme is: the amount that adds sodium chloride or potassium chloride in the described step (2) is: sodium chloride or Klorvess Liquid concentration are reached capacity.
Its further technical scheme is: the organic solvent that adds in the described step (3) is ether, benzinum or ethyl acetate, and organic solvent is 1/5 with the water distillate volume ratio of taking.
Its further technical scheme is: the decompression distillation in the described step (4) is: be to carry out decompression distillation by Rotary Evaporators under 48 ℃ ~ 52 ℃ the condition in temperature.
Its further technical scheme is: the temperature in the refrigerating chamber in the described step (5) is-10 ℃ ~-20 ℃, and cooling time is 6～12 hours.
Its further technical scheme is: also can add 2%～5% hyaluronic acid in step b during preparation mosquito repellant.
Owing to adopt technique scheme, the present invention's the method for utilizing lemon eucalyptus oil extraction waste liquid to prepare the mosquito repellant is compared with the existing method for preparing the mosquito repellant, has following beneficial effect:
1. environmental contamination reduction:
Because the present invention extracts the waste liquid from lemon eucalyptus oil to extract p-menthane-3,8-diol, its refining purification is rear for the preparation of the mosquito repellant, and lemon eucalyptus oil to extract waste liquid be uncared-for in the production process of lemon eucalyptus oil, it generally all is used as waste liquid and discharges, and the present invention recycles this lemon eucalyptus oil extraction waste liquid, has not only increased the value of lemon eucalyptus oil extraction waste liquid, has also greatly reduced it and has discharged pollution on the environment.
2. effectively prevented the killing propagation disease:
It is to extract the anophelifuge activity composition p-menthane-3 that extracts the waste liquid from lemon eucalyptus oil that the present invention uses raw material, 8-diol, have certain fragrance and anophelifuge activity, it is dissolved in propane diols, 75% ethanol, glycerine and 1, the mosquito repellant that is prepared in the 3-butanediol, can prevent for a long time biting of mosquito, effectively prevent the killing propagation disease, smear and rear skin is also had the effect of moistening of certain water conservation.
3. reduced the harm that culicifuge causes the mankind and environment:
Using at present maximum mosquito repellent modes is to burn mosquito-repellent incense and spray the atomizing chemical insecticide, mosquito-repellent incense and chemical insecticide are when killing mosquito, contaminated environment not only, and infringement health, and the mosquito repellant that adopts the present invention to prepare belongs to plants essential oil class culicifuge, this culicifuge can not only effectively be driven mosquito, has also reduced the pollution to environment, has also reduced the harm to human health.
4. reduced cost, be convenient to promote the use of:
Although also released plants essential oil class culicifuge on the market now, but compare with mosquito-repellent incense and atomizing chemical insecticide, its price comparison is expensive, so be difficult to extensively be used, and main material used in the present invention is to extract from lemon eucalyptus oil to extract p-menthane-3,8-diol the waste liquid, greatly reduce the cost of raw material, thereby also reduced the price of finished product, improved the market competitiveness of finished product, used so that the mosquito repellant that adopts the inventive method to prepare is easy to large-scale popularization.
5. method is simple, easy to operate:
Main material used in the present invention is not only the colourless transparent liquid water distillate that flows out from the oil water separator of lemon eucalyptus leaf oil extractor, namely isolate the remaining distilled water behind the lemon eucalyptus oil, it can also be the muddy vinasse of brownish black of collecting in the lemon eucalyptus leaf oil extractor, again with this vinasse re-distillation, collect distillate, other raw material also are existing materials on the market, and the key step that the present invention adopts is separated out for dissolving, extraction, decompression distillation, some simple chemical methodes such as low temperature crystallization and mixed dissolution, method is simple, easy to operate, be convenient to promote the use of.
Embodiment
The present invention utilizes lemon eucalyptus oil to extract the method that waste liquid prepares the mosquito repellant, comprises the steps:
A. extract from lemon eucalyptus oil and extract the anophelifuge activity composition the waste liquid
p-menthane-3, the 8-diol(Chinese translation is: to alkane-3 in the Meng, 8-glycol; Be called for short: the Meng glycol):
(1) collects the water distillate, the water distillate of described water distillate for from the oil water separator of lemon eucalyptus leaf oil extractor, flowing out; This water distillate is colourless transparent liquid, for isolating the remaining distilled water behind the lemon eucalyptus oil, is dissolved with the volatile ingredient of part lemon eucalyptus leaf in this water, and its main component is
p-menthane-3,8-diol;
(2) in above-mentioned obtained water distillate, add sodium chloride or potassium chloride, make in the water distillate
p-menthane-3,8-diol separates out; The amount that adds sodium chloride or potassium chloride is: sodium chloride or Klorvess Liquid concentration are reached capacity;
(3) to extracting through adding organic solvent in the water distillate after the step (2), get the organic solvent phase after the extraction; The organic solvent that adds in the present embodiment is ether, benzinum or ethyl acetate, and organic solvent is 1/5 with the water distillate volume ratio of taking;
(4) organic solvent with above-mentioned gained carries out decompression distillation mutually, and decompression distillation is: be to carry out decompression distillation by Rotary Evaporators under 48 ℃ ~ 52 ℃ the condition in temperature; After obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed carry out freezingly in the refrigerating chamber, the temperature in the refrigerating chamber is controlled to be-10 ℃ ~-20 ℃, and freezing 6～12 hours, treat crystallization, filter and namely obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepare the mosquito repellant:
In mass ratio with 10%～50%
p-menthane-3,8-diol, 5%～20% propane diols, 10%～50% 75% ethanol, 2%～10% glycerine, 2%～10% 1,3-BDO mix, stir evenly, are dissolved into finished product, namely are prepared into the mosquito repellant.
In the present embodiment, also can add 2%～5% hyaluronic acid during preparation mosquito repellant, add hyaluronic acid so that the mosquito repellant has better moistening effect.
The concrete prescription one of preparation mosquito repellant is: will
p-menthane-3,8-diol 2g, propane diols 1g, 75% ethanol 5g, glycerine 1g, 1,3-BDO 1g mix, stir evenly, are dissolved into finished product, namely are prepared into the mosquito repellant.
Preparation mosquito repellent formula two to prescription eight each required constituent content see table:
| Component (g) | Prescription two | Prescription three | Prescription four | Prescription five | Prescription six | Prescription seven | Prescription eight |
| p-menthane-3,8-diol | 3 | 3.5 | 5 | 1 | 5 | 4 | 5 |
| Propane diols | 1 | 1 | 2 | 1 | 0.5 | 0.8 | 1.5 |
| 75% ethanol | 4.5 | 4 | 2.6 | 5 | 2.5 | 3 | 1 |
| Glycerine | 0.5 | 1 | 0.2 | 1 | 0.7 | 1 | 1 |
| 1,3-BDO | 1 | 0.5 | 0.2 | 1 | 0.8 | 1 | 1 |
| Hyaluronic acid | 0 | 0 | 0 | 1 | 0.5 | 0.2 | 0.5 |
By fill a prescription two in the above-mentioned table～consumption of prescription eight described each material is prepared into the mosquito repellant by mixing, stir evenly, dissolving.
As a kind of conversion of the present invention: each required constituent content of preparation mosquito repellant is not limited to above-mentioned prescription one listed content to the prescription eight, as long as the conversion of doing within the scope of the invention all belongs to category of the present invention.
In the laboratory, adopt prescription one to test to the prescription eight mosquito repellants of preparing, experimentation and result are as follows:
1. attack experiment:
(the female culex pipiens fatigans adult (being provided by professional unit) of not sucking blood in 3～5 days after 200 emergence is provided for 200mm * 300mm * 200mm) in the mosquito cage.Experimenter's the back of the hand exposes 4cm * 4cm baring skin, and the back of the hand remainder tightly covers with white gauze gloves.During experiment, hand is stretched into ready mosquito cage the inside, close observation 2min, if when finding that mosquito lights on the baring skin face of the back of the hand, the shake arm drives it and leaves before mosquito inserts skin with its mouthpart, and is designated as 1 mosquito and stops falling.The mosquito that comes to stop falling is that attack is qualified more than 20 experimenter and test mosquito, and this person and this cage mosquito can carry out repellency test.
2. repellent experiment:
After the experimenter is qualified by the attack experiment with the experiment mosquito, carry out the mosquito repelling experiment.Respectively draw the skin area of 5cm * 5cm at the qualified experimenter's of 2 attacks both hands back, wherein a hand is blank, the another hand evenly is applied in the back of the hand by the mosquito repellant that the dosage of 1.5 μ L/cm2 adopts the inventive method to be prepared into, expose wherein 4cm * 4cm skin, tightly cover remainder.After smearing repellant, immediately hand is stretched into 2min in the cage that is placed with the qualified mosquito of attack, observe and to have or not mosquito to come to suck blood, later per test half an hour is once made repellant and was lost efficacy as long as have 1 mosquito to come to suck blood namely to declare.The effective protecting time (h) of record repellant.Effective protecting time with experimenter A is as the criterion, and experimenter B is reference, surpasses one hour if experimenter A and experimenter B two people's effective protecting times differ, and then again does the repellent experiment of this sample.
3. experimental result:
The result shows by many experiments, adopt mosquito repellant that the inventive method prepares to the effective protecting time of human body all above 4 hours.
Claims (7)
1. one kind is utilized lemon eucalyptus oil to extract the method that waste liquid prepares the mosquito repellant, it is characterized in that: comprise the steps:
A. extract from lemon eucalyptus oil and extract the anophelifuge activity composition the waste liquid
p-menthane-3,8-diol:
(1) collects the water distillate, the water distillate of described water distillate for from the oil water separator of lemon eucalyptus leaf oil extractor, flowing out;
(2) in above-mentioned obtained water distillate, add sodium chloride or potassium chloride, make in the water distillate
p-menthane-3,8-diol separates out;
(3) to extracting through adding organic solvent in the water distillate after the step (2), get the organic solvent phase after the extraction;
(4) above-mentioned obtained organic solvent is carried out decompression distillation mutually, obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed carry out freezingly in the refrigerating chamber, treat crystallization, filter and namely obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepare the mosquito repellant:
In mass ratio with 10%～50%
p-menthane-3,8-diol, 5%～20% propane diols, 10%～50% 75% ethanol, 2%～10% glycerine, 2%～10% 1,3-BDO mix, stir evenly, are dissolved into finished product, namely are prepared into the mosquito repellant.
2. the lemon eucalyptus oil that utilizes according to claim 1 extracts the method that waste liquid prepares the mosquito repellant, it is characterized in that: the water distillate that flows out in the oil water separator of the lemon eucalyptus leaf oil extractor described in the step (1) is colourless transparent liquid, for isolating the remaining distilled water behind the lemon eucalyptus oil, be dissolved with the volatile ingredient of part lemon eucalyptus leaf in this water, its main component is
p-menthane-3,8-diol.
3. the lemon eucalyptus oil that utilizes according to claim 1 extracts the method that waste liquid prepares the mosquito repellant, it is characterized in that: the amount that adds sodium chloride or potassium chloride in the described step (2) is: sodium chloride or Klorvess Liquid concentration are reached capacity.
4. the lemon eucalyptus oil that utilizes according to claim 1 extracts the method that waste liquid prepares the mosquito repellant, it is characterized in that: the organic solvent that adds in the described step (3) is ether, benzinum or ethyl acetate, and organic solvent is 1/5 with the water distillate volume ratio of taking.
5. the lemon eucalyptus oil that utilizes according to claim 1 extracts the method that waste liquid prepares the mosquito repellant, and it is characterized in that: the decompression distillation in the described step (4) is: be to carry out decompression distillation by Rotary Evaporators under 48 ℃ ~ 52 ℃ the condition in temperature.
6. the lemon eucalyptus oil that utilizes according to claim 1 extracts the method that waste liquid prepares the mosquito repellant, and it is characterized in that: the temperature in the refrigerating chamber in the described step (5) is-10 ℃ ~-20 ℃, and cooling time is 6～12 hours.
7. the described lemon eucalyptus oil that utilizes of arbitrary claim extracts the method that waste liquid prepares the mosquito repellant according to claim 1 ~ 6, it is characterized in that: also can add 2%～5% hyaluronic acid in step b during preparation mosquito repellant.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108697077A (en) * | 2015-09-25 | 2018-10-23 | 组合块公司 | Polyalcohol, carbohydrate, nucleobase and nucleotide composition and application thereof |
| CN108902199A (en) * | 2018-08-20 | 2018-11-30 | 湖南省园艺研究所 | Eucalyptus oil is luring the application in citrus fruit fly |
| CN110326618A (en) * | 2019-07-16 | 2019-10-15 | 广西科技大学 | Utilize the method for Chinese anise oil extract waste liquid preparation mosquito repellant |
| CN110330431A (en) * | 2019-07-16 | 2019-10-15 | 广西科技大学 | Utilize the method for husky ginger oil extract waste liquid preparation mosquito repellant |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108697077A (en) * | 2015-09-25 | 2018-10-23 | 组合块公司 | Polyalcohol, carbohydrate, nucleobase and nucleotide composition and application thereof |
| CN108697077B (en) * | 2015-09-25 | 2022-04-19 | 组合块公司 | Polyol, carbohydrate, nucleobase and nucleoside compositions and uses thereof |
| US11553713B2 (en) | 2015-09-25 | 2023-01-17 | Chunbo Zhang | Polyalcohol, carbohydrate, nucleobase and nucleotide compositions and uses thereof |
| CN108902199A (en) * | 2018-08-20 | 2018-11-30 | 湖南省园艺研究所 | Eucalyptus oil is luring the application in citrus fruit fly |
| CN108902199B (en) * | 2018-08-20 | 2020-12-04 | 湖南省园艺研究所 | Application of eucalyptus essential oil in attracting bactrocera minax |
| CN110326618A (en) * | 2019-07-16 | 2019-10-15 | 广西科技大学 | Utilize the method for Chinese anise oil extract waste liquid preparation mosquito repellant |
| CN110330431A (en) * | 2019-07-16 | 2019-10-15 | 广西科技大学 | Utilize the method for husky ginger oil extract waste liquid preparation mosquito repellant |
| CN110330431B (en) * | 2019-07-16 | 2022-04-15 | 广西科技大学 | Method for preparing mosquito repellent by using sand ginger oil extraction waste liquid |
| 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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