CN102860303B - 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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- CN102860303B CN102860303B CN 201210388632 CN201210388632A CN102860303B CN 102860303 B CN102860303 B CN 102860303B CN 201210388632 CN201210388632 CN 201210388632 CN 201210388632 A CN201210388632 A CN 201210388632A CN 102860303 B CN102860303 B CN 102860303B
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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 is all to adopt traditional steam distillation technique.The cardinal principle of steam distillation: when the vegetalitas aromatic raw material is soaked in water and be heated to boil (as water distillation) or pass into the bed of material (as water and steam distillation and live (open) steam distillation) of aromatic raw material with steam, because at first boiling water or steam produce such effect to raw material, 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 pressure adopted in boiler all the time, as adopted air-distillation in pot, 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, obtain essential oil.When boiling water or steam when to the raw tissue surface oil, dividing the generation effect, its boiling water or steam are permeated, are 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 surface and is distilled out of.
Generally only collect distillate in steam distillation technique in, the oil phase part, as essential oil product, does not receive publicity for the water soluble ingredient in essential oil.Water soluble ingredient in essential oil mainly is present in the extraction waste liquid of isolating after essential oil, these compositions are mainly 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 essential oil, these components are slightly soluble in water, by simple mechanics means, they fully can not be separated, and be slightly soluble in this part essential oil of water, because the oil-water ratio of distillate is little, whole distillate essential oil in shared ratio be appreciable.
The killing propagation disease, the health that is endangering the mankind.For a long time, people use the number of chemical insecticide to 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.Research shows that some plants essential oils have certain poisoning and repellent action to mosquito, mosquito is had to food refusal, repellent, lures, directly kills and suppresses growth, with traditional synthetic pesticide, compare there is low toxicity, low-residual, to advantages such as environmental influence are little.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the mosquito repellant that environmental protection, cost product low, that be convenient to promote the use of, make can be effectively mosquito-proof.
The technical scheme solved 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 waste liquid and extract the anophelifuge activity composition from lemon eucalyptus oil
p-menthane-3,8-diol:
(1) collect the water distillate, the water distillate of described water distillate for flowing out from the oil water separator of lemon eucalyptus leaf oil extractor;
(2) add sodium chloride or potassium chloride in above-mentioned obtained water distillate, make in the water distillate
p-menthane-3,8-diol separates out;
(3) in the water distillate after step (2), add organic solvent to be extracted, get the organic solvent phase after extraction;
(4) above-mentioned obtained organic solvent is carried out to decompression distillation mutually, obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed in and carries out freezingly in refrigerating chamber, treat crystallization, filter and obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepares the mosquito repellant:
In mass ratio by 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, are prepared into the mosquito repellant.
Its further technical scheme is: the water distillate flowed out in the oil water separator of the lemon eucalyptus leaf oil extractor described in step (1) is colourless transparent liquid, for isolating the remaining distilled water after 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: in described step (2), add the amount of sodium chloride or potassium chloride to be: sodium chloride or Klorvess Liquid concentration are reached capacity.
Its further technical scheme is: the organic solvent added in 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 described step (4) is: under the condition that is 48 ℃ ~ 52 ℃ in temperature, by Rotary Evaporators, carry out decompression distillation.
Its further technical scheme is: the temperature in the refrigerating chamber in 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 adopting 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 waste liquid and extracts p-menthane-3 from lemon eucalyptus oil, 8-diol, by after its refining purification 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, not only increased the value of lemon eucalyptus oil extraction waste liquid, also greatly reduce it and discharged pollution on the environment.
2. effectively prevented the killing propagation disease:
It is to extract from lemon eucalyptus oil the anophelifuge activity composition p-menthane-3 extracted waste liquid that the present invention uses raw material, 8-diol, there is certain fragrance and anophelifuge activity, it is dissolved in to propane diols, 75% ethanol, glycerine and 1, the mosquito repellant be 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 to 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 on market, also released plants essential oil class culicifuge now, but compare with mosquito-repellent incense and atomizing chemical insecticide, its price comparison costliness, so be difficult to extensively be used, and main material used in the present invention is to extract waste liquid from lemon eucalyptus oil to extract p-menthane-3,8-diol, greatly reduce the cost of raw material, thereby also reduced the price of finished product, improved the market competitiveness of finished product, made the mosquito repellant that adopts the inventive method to prepare be easy to large-scale popularization and use.
5. method is simple, easy to operate:
Main material used in the present invention is not only the colourless transparent liquid water distillate flowed out from the oil water separator of lemon eucalyptus leaf oil extractor, isolate the remaining distilled water after lemon eucalyptus oil, it can also be the muddy vinasse of brownish black of collecting in the lemon eucalyptus leaf oil extractor, again by this vinasse re-distillation, collect distillate, other raw material are also existing materials on 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 waste liquid and extract the anophelifuge activity composition from lemon eucalyptus oil
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) collect the water distillate, the water distillate of described water distillate for flowing out from the oil water separator of lemon eucalyptus leaf oil extractor; This water distillate is colourless transparent liquid, for isolating the remaining distilled water after 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) add sodium chloride or potassium chloride in above-mentioned obtained water distillate, make in the water distillate
p-menthane-3,8-diol separates out; Add the amount of sodium chloride or potassium chloride to be: sodium chloride or Klorvess Liquid concentration are reached capacity;
(3) in the water distillate after step (2), add organic solvent to be extracted, get the organic solvent phase after extraction; The organic solvent added 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 of above-mentioned gained is carried out to decompression distillation mutually, decompression distillation is: under the condition that is 48 ℃ ~ 52 ℃ in temperature, by Rotary Evaporators, carry out decompression distillation; After obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed in and carries out freezingly in refrigerating chamber, the temperature in refrigerating chamber is controlled as-10 ℃ ~-20 ℃, and freezing 6～12 hours, treat crystallization, filter and obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepares the mosquito repellant:
In mass ratio by 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, are prepared into the mosquito repellant.
In the present embodiment, also can add 2%～5% hyaluronic acid during preparation mosquito repellant, add hyaluronic acid to make the mosquito repellant there is better moistening effect.
The concrete formula 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, are prepared into the mosquito repellant.
Preparation mosquito repellent formula two to formula eight each required constituent contents see table:
| Component (g) | Formula two | Formula three | Formula four | Formula five | Formula six | Formula seven | Formula 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 |
Be prepared into the mosquito repellant by the consumption of two～eight described each materials of filling a prescription of filling a prescription in above-mentioned table 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 formula one to listed content in formula eight, as long as the conversion done within the scope of the invention all belongs to category of the present invention.
In laboratory, adopt formula one to be tested to the formula eight mosquito repellants of preparing, experimentation and result are as follows:
1. attack experiment:
In the mosquito cage, the female culex pipiens fatigans adult (being provided by professional unit) of not sucking blood in 3～5 days after 200 emergence is provided (200mm * 300mm * 200mm).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 to ready mosquito cage the inside, close observation 2min, when if find, mosquito lights on the baring skin face of the back of the hand, before mosquito inserts skin by its mouthpart, the shake arm drives it and leaves, and is designated as 1 mosquito and stops falling.The mosquito that comes to stop falling is that attack is qualified more than experimenter and the test mosquito of 20, and this person and this cage mosquito can carry out repellency test.
2. repellent experiment:
The experimenter and the experiment mosquito by attack, test qualified after, carry out the mosquito repelling experiment.At 2 attacks, qualified experimenter's both hands back respectively draws the skin area of 5cm * 5cm, wherein a hand is blank, the mosquito repellant that the another hand adopts the inventive method to be prepared into by the dosage of 1.5 μ L/cm2 evenly is applied in the back of the hand, expose 4cm wherein * 4cm skin, tightly cover remainder.After smearing repellant, immediately hand is stretched into to 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 once, is made repellant and was lost efficacy as long as have 1 mosquito to come to suck blood to sentence.Record the effective protecting time (h) of repellant.Effective protecting time with experimenter A is as the criterion, and experimenter B is reference, if experimenter A and experimenter B two people's effective protecting times differ, surpasses one hour, again does the repellent experiment of this sample.
3. experimental result:
By the many experiments result, show, the mosquito repellant that adopts the inventive method to prepare to the effective protecting time of human body all over 4 hours.
Claims (3)
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 waste liquid and extract the anophelifuge activity composition from lemon eucalyptus oil
p-menthane-3,8-diol:
(1) collect the water distillate, the water distillate of described water distillate for flowing out from the oil water separator of lemon eucalyptus leaf oil extractor, the water distillate flowed out in the oil water separator of described lemon eucalyptus leaf oil extractor is colourless transparent liquid, for isolating the remaining distilled water after 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;
(2) add sodium chloride or potassium chloride in above-mentioned obtained water distillate, add the amount of sodium chloride or potassium chloride to be: sodium chloride or Klorvess Liquid concentration are reached capacity; Make in the water distillate
p-menthane-3,8-diol separates out;
(3) in the water distillate after step (2), add organic solvent to be extracted, get the organic solvent phase after extraction, the organic solvent added in this step is benzinum or ethyl acetate, and organic solvent is 1/5 with the water distillate volume ratio of taking;
(4) above-mentioned obtained organic solvent is carried out to decompression distillation mutually, obtain the pale yellow oily liquid body;
(5) the pale yellow oily liquid body of above-mentioned gained is placed in and carries out freezingly in refrigerating chamber, treat crystallization, filter and obtain
p-menthane-3,8-diol;
B. use above-mentioned steps a prepared
p-menthane-3,8-diol prepares the mosquito repellant:
In mass ratio by 10%～50%
p-menthane-3,8-diol, 5%～20% propane diols, 10%～50% 75% ethanol, 2%～10% glycerine, 2%～10% 1,3-BDO, 2%～5% hyaluronic acid mix, stir evenly, are dissolved into finished product, 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, and it is characterized in that: the decompression distillation in described step (4) is: under the condition that is 48 ℃ ~ 52 ℃ in temperature, by Rotary Evaporators, carry out decompression distillation.
3. 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 described step (5) is-10 ℃ ~-20 ℃, and cooling time is 6～12 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11553713B2 (en) | 2015-09-25 | 2023-01-17 | Chunbo Zhang | Polyalcohol, carbohydrate, nucleobase and nucleotide compositions and uses thereof |
| 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 |
| 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 |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072314A (en) * | 1991-10-07 | 1993-05-26 | 贝克卡明斯皮肤病药品有限公司 | insect repellent |
| CN101880600A (en) * | 2010-08-17 | 2010-11-10 | 厦门百度科技开发有限公司 | Method for extracting eucalyptus citriodra volatile oil and 3,8-diol |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072314A (en) * | 1991-10-07 | 1993-05-26 | 贝克卡明斯皮肤病药品有限公司 | insect repellent |
| CN101880600A (en) * | 2010-08-17 | 2010-11-10 | 厦门百度科技开发有限公司 | Method for extracting eucalyptus citriodra volatile oil and 3,8-diol |
Non-Patent Citations (2)
| Title |
|---|
| 柠檬桉叶挥发性成分的提取及成分分析;田玉红等;《色谱》;20051130;第23卷(第6期);第651-654页 * |
| 田玉红等.柠檬桉叶挥发性成分的提取及成分分析.《色谱》.2005,第23卷(第6期), |
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