CN110330431A - Utilize the method for husky ginger oil extract waste liquid preparation mosquito repellant - Google Patents
Utilize the method for husky ginger oil extract waste liquid preparation mosquito repellant Download PDFInfo
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- CN110330431A CN110330431A CN201910642436.3A CN201910642436A CN110330431A CN 110330431 A CN110330431 A CN 110330431A CN 201910642436 A CN201910642436 A CN 201910642436A CN 110330431 A CN110330431 A CN 110330431A
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- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
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- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The method that the present invention prepares mosquito repellant using husky ginger oil extract waste liquid, trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate mixture are first extracted from husky ginger oil extract waste liquid, later in mass ratio by 30~50 parts of trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate mixture, 10~20 parts of glycerol, 1~5 part of Eucalyptus urophylla-grandis leaf oil, 2~20 parts of propylene glycol, 3~5 parts of polyoxyethylene 20 sorbitan monooleate, 1~3 part of sorbitan monopalmitate, 20~40 parts of lemon eucalyptus leaf hydrosol, mosquito repellant is made in 0.5~1 part of pyrrolidone-5-carboxylic acid sodium mixing and emulsifying at 75 DEG C.This method is easy to operate, the product being prepared can effectively it is mosquito-proof, environmentally friendly, at low cost, convenient for promote the use of.
Description
Technical field
The present invention relates to a kind of methods for preparing mosquito repellant, especially a kind of to prepare mosquito using husky ginger oil extract waste liquid
The method of sub- repellant.
Background technique
Husky ginger (Kaempferia galangal LIt is) that the dry rhizome of zingiberaceous plant mountain naphthalene mainly originates in Guangdong, Guangxi
Equal provinces and regions, are important medical and edible dual purpose plant, have promoting the circulation of qi middle benefit gas, and help digestion the effect of relieving pain, and can also treat rheumatism, roar
Asthma, cough and skin disease.Since husky ginger has special aromatic odor, acrid flavour is peppery, in addition to medicinal, is also largely used as non-staple foodstuff and tune
Taste agent.The rhizome of husky ginger is rich in essential oil, is widely used in medicine, cosmetics and food service industry.The production of husky ginger essential oil mostly uses greatly
Traditional steam distillation technique is generally only collected oil phase part in distillate in steam distillation technique and is allocated as essential oil production
Product, main component be trans- Ethyl p-methoxy-silicate (14.3%~51.6%) and ethyl cinnamate (13.3~31.2%), from
The brown color waste liquid usually quilt in water phase distillate and husky ginger oil extract tank flowed out in the oil water separator of husky ginger oil extractor
It is expelled directly out.
It keeps contacting for a long time with vapor in distillation process due to essential oil molecule in the production process of essential oil, so
Polarity and hydrophilic composition in essential oil are partly dissolved in water, as the water-soluble volatile ingredient of essential oil.This part is slightly soluble in
The volatile component of water, the mainly containing oxygen derivative of terpene substances, these substances give off a strong fragrance, and represent the distinctive perfume (or spice) of essential oil
Gas is the part of most worthy in essential oil, and since the oil-water ratio of distillate is small, this Some essential oils is entirely distillating institute in essential oil
The ratio accounted for is considerable.
As people gradually deepen the understanding of water-soluble volatile ingredient, find water-soluble volatile ingredient due to rich in oxygen-containing
Not only there is terpenoid aromatic odor can be applied to cosmetics and food additives, but also have antibacterial, antiviral etc. raw
Object active function, has broad application prospects.The water-soluble volatile ingredient in spice berry is usually with vinasse at present
And discarded, cause huge waste.Therefore extraction and research for application and development in relation to volatile ingredient water-soluble in spice berry
Increasingly by attention both domestic and external.
Killing propagation disease endangers the health of the mankind.For a long time, people are to burn mosquito-repellent incense with most mosquito repellent modes
And sprinkling atomizing chemical insecticide controls mosquito, mosquito-repellent incense and chemical insecticide not only pollute environment while mosquitocide, but also
Damage human health.These factors promote to be attempted to seek culicifuge environmentally friendly, to people's low toxicity.Research shows that some
Plants essential oil has certain poisoning and repellent action to mosquito, has food refusal to mosquito, repellent, lures, directly kills and press down
Growth processed has many advantages, such as that low toxicity, low-residual, effect on environment are small compared with traditional synthetic pesticide.
Summary of the invention
The purpose of the present invention is in view of the above-mentioned drawbacks of the prior art, providing a kind of utilization husky ginger oil extract waste liquid system
The method of standby mosquito repellant, this method is nontoxic to the human body, it is environmentally friendly, at low cost, convenient for promoting the use of, product obtained can be effective
It is mosquito-proof.
The present invention to achieve the above object the technical solution adopted is that: it is a kind of using husky ginger oil extract waste liquid preparation mosquito drive
The method for keeping away agent, includes the following steps:
A. trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are extracted from husky ginger oil extract waste liquid
Mixture, comprising the following steps:
(1) water phase distillate is collected, water phase distillate is that the water phase flowed out from the oil water separator of husky ginger oil extract tank distillates
Liquid；Or the water phase distillate that will be collected after the brown color muddiness waste liquid re-distillation in husky ginger oil extract tank；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), make in water phase distillate it is trans--
Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is dichloro
Methane or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are 1/ with the water phase distillate volume ratio taken
10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, obtains brown yellow oil liquid；
(5) cryogenic freezing is carried out to brown yellow oil liquid acquired by step (4), wait which crystallization is precipitated, rapid filtration under suction is obtained
Trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate mixture, trans- in mixture-to methoxyl group
The content of ethyl cinnamate is that the content of 83 ~ 92%, cis--Ethyl p-methoxy-silicate is 3 ~ 13%；
B. the preparation-obtained trans--Ethyl p-methoxy-silicate of above-mentioned steps a and cis--p-methoxycinnamic acid are used
Ethyl ester mixture prepares mosquito repellant:
30~50 parts of trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are mixed in mass ratio
Object, 10~20 parts of glycerol, 1~5 part of Eucalyptus urophylla-grandis leaf oil, 2~20 parts of propylene glycol, 3~5 parts of polyoxyethylene sorbitan
Alcohol monoleate, 1~3 part of sorbitan monopalmitate, 20~40 parts of lemon eucalyptus leaf hydrosol, 0.5~1 part of pyrroles
Mosquito repellant is made in alkanone -5- carboxylic acid sodium mixing and emulsifying at 75 DEG C.
A further technical solution of the present invention is: the amount of sodium chloride or potassium chloride is added in the step (2) are as follows: make chlorination
The 30~70% of concentration when sodium or Klorvess Liquid concentration are saturation solubility.
A further technical solution of the present invention is: the vacuum distillation in the step (4) are as follows: in temperature be 55 DEG C ~ 85 DEG C
Under conditions of be evaporated under reduced pressure by Rotary Evaporators.
A further technical solution of the present invention is: the cryogenic freezing temperature in the step (5) is 0 DEG C ~ -10 DEG C, freezing
Time is 1 ~ 5 hour.
A further technical solution of the present invention is: lemon eucalyptus leaf hydrosol used in the step b is from lemon eucalyptus oil
The water phase distillate flowed out in the oil water separator of extractor is the by-product of generation during lemon eucalyptus leaf extraction of essential oil.
Due to the adoption of the above technical scheme, the present invention using husky ginger oil extract waste liquid preparation mosquito repellant method with
The method of existing preparation mosquito repellant is compared, and is had the advantages that
1. effectively preventing killing propagation disease:
The raw material that the present invention uses is the trans--Ethyl p-methoxy-silicate extracted from husky ginger oil extract waste liquid and cis--
Ethyl p-methoxy-silicate mixture has certain fragrance and anophelifuge activity, by it with glycerol, Eucalyptus urophylla-grandis leaf oil, the third two
Alcohol, polyoxyethylene 20 sorbitan monooleate, sorbitan monopalmitate, lemon eucalyptus leaf hydrosol, pyrrolidones -5- carboxylic
Mosquito repellant is made after the ingredients mixing and emulsifying such as sour sodium, biting for mosquito can be prevented for a long time, effectively prevent killing propagation
Disease.
2. product has good anti-sunlight function:
The ultraviolet light in 280 ~ 320 regions nm easily makes skin sunburn, " solar dermatitises " such as erythema, bubbles is generated, to methoxyl group meat
Ethyl cinnamate has wide and strong absorption in the region 280 ~ 320nm, and non-stimulated to skin, safety is good, is a kind of ideal anti-
Shine agent；The raw material that the present invention uses is the trans--Ethyl p-methoxy-silicate extracted from husky ginger oil extract waste liquid and cis--
The mosquito repellant of Ethyl p-methoxy-silicate mixture, preparation has good sun-proof result.
3. reducing culicifuge harm caused by the mankind and environment:
Plants essential oil class culicifuge is belonged to using the mosquito repellant for preparing of the present invention, this culicifuge can not only to mosquito into
Row is effectively driven, and also reduces the pollution to environment, also reduces the harm to human health.
4. reducing costs, convenient for popularization and use:
Although being also proposed plants essential oil class culicifuge currently on the market, compared with mosquito-repellent incense and atomizing chemical insecticide,
Price is more expensive, so be difficult to be used extensively, and anophelifuge activity ingredient used in the present invention is useless from husky ginger oil extract
On the one hand trans--the Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate mixture extracted in liquid drops significantly
The low cost of raw material improves the market competitiveness of finished product to also reduce the price of finished product, so that using the method for the present invention
The mosquito repellant being prepared is easy to large-scale popularization use；Another aspect husky ginger oil extract waste liquid is typically all by as discarded
Liquid is discharged into environment, and the present invention recycles the husky ginger oil extract waste liquid, increases the comprehensive utilization of husky ginger
Value.
5. method is simple and convenient to operate:
Main material used in the present invention is not only the colorless and transparent water flowed out from the oil water separator of husky ginger oil extract tank
Phase distillate, that is, the remaining distilled water after isolating husky ginger oil, can also be that the brown color collected in husky ginger oil extract tank is muddy
Turbid vinasse, then by this vinasse re-distillation, collects distillate, and other raw material are also existing material in the market,
And the present invention use mainly comprise the following steps some simple chemical methodes such as solution modeling, extraction, vacuum distillation and mixing and emulsifying,
Method is simple and convenient to operate, convenient for popularization and use.
The present invention is made using the method for husky ginger oil extract waste liquid preparation mosquito repellant below by specific embodiment
Further instruction.
Specific embodiment
The present invention is included the following steps: using the method for husky ginger oil extract waste liquid preparation mosquito repellant
A. trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are extracted from husky ginger oil extract waste liquid
Mixture includes the following steps:
(1) water phase distillate is collected, water phase distillate is that the water phase flowed out from the oil water separator of husky ginger oil extract tank distillates
Liquid；Or the water phase distillate that will be collected after the brown color muddiness waste liquid re-distillation in husky ginger oil extract tank；Wherein husky ginger oil
The water phase distillate flowed out in the oil water separator of extractor is colourless transparent liquid, to isolate the remaining steaming after husky ginger oil
Distilled water, is dissolved with the volatile component of part husky ginger in this water, and main component is trans--Ethyl p-methoxy-silicate and suitable
Formula-Ethyl p-methoxy-silicate；The water phase wherein collected after the brown color muddiness waste liquid re-distillation in husky ginger oil extract tank
Distillate is colourless or micro-strip sundown liquid, is dissolved with the volatile component of husky ginger in this water, main component be it is trans--
Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), wherein sodium chloride or potassium chloride is added
Amount are as follows: the 60% of concentration when making the concentration saturation solubility of sodium chloride or Klorvess Liquid；Make anti-in water phase distillate
Formula-Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is dichloro
Methane or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are 1/ with the water phase distillate volume ratio taken
10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, be evaporated under reduced pressure specifically: in temperature be 55 DEG C ~ 85
It is evaporated under reduced pressure under conditions of DEG C by Rotary Evaporators；Brown yellow oil liquid is obtained after vacuum distillation；
(5) cryogenic freezing is carried out to brown yellow oil liquid acquired by step (4), cryogenic freezing temperature is controlled 0 DEG C ~ -10
DEG C, cooling time is 3 hours, and wait which crystallization is precipitated after cryogenic freezing, rapid filtration under suction obtains trans--Ethyl p-methoxy-silicate
With cis--Ethyl p-methoxy-silicate mixture, in mixture trans--Ethyl p-methoxy-silicate content be 83 ~ 92%,
The content of cis--Ethyl p-methoxy-silicate is 3 ~ 13%.
B. using the preparation-obtained trans--Ethyl p-methoxy-silicate of above-mentioned steps a and cis--to methoxyl group meat
Ethyl cinnamate mixture prepares mosquito repellant:
30~50 parts of trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are mixed in mass ratio
Object, 10~20 parts of glycerol, 1~5 part of Eucalyptus urophylla-grandis leaf oil, 2~20 parts of propylene glycol, 3~5 parts of polyoxyethylene sorbitan
Alcohol monoleate, 1~3 part of sorbitan monopalmitate, 20~40 parts of lemon eucalyptus leaf hydrosol, 0.5~1 part of pyrroles
Mosquito repellant is made in alkanone -5- carboxylic acid sodium mixing and emulsifying at 75 DEG C.
Lemon eucalyptus leaf hydrosol used is the oil from lemon eucalyptus oil extractor when preparing mosquito repellant in the step b
The water phase distillate flowed out in separator is the by-product of generation during lemon eucalyptus leaf extraction of essential oil, with pleasant virtue
Fragrance taste.
Prepare the specific formula of mosquito repellant first is that: trans--Ethyl p-methoxy-silicate and cis--is to methoxyl group meat
Ethyl cinnamate mixture 38g, glycerol 18g, Eucalyptus urophylla-grandis leaf oil 4g, propylene glycol 12g, polyoxyethylene 20 sorbitan monooleate
4g, 2 g of sorbitan monopalmitate, lemon eucalyptus leaf hydrosol 21g, 1 g of pyrrolidone-5-carboxylic acid sodium mix cream at 75 DEG C
Mosquito repellant is made in change.
Each component content needed for preparing mosquito repellent formula two to formula seven is referring to following table:
| Component (g) | Formula two | Formula three | Formula four | Formula five | Formula six | Formula seven |
| Trans--Ethyl p-methoxy-silicate and cis--p-methoxycinnamic acid second Ester admixture | 41 | 35 | 46 | 30 | 50 | 40 |
| Glycerol | 15 | 20 | 10 | 10 | 20 | 19 |
| Eucalyptus urophylla-grandis leaf oil | 3 | 4 | 2 | 5 | 3.5 | 1 |
| Propylene glycol | 10 | 2 | 5 | 14 | 20 | 5 |
| Polyoxyethylene 20 sorbitan monooleate | 5 | 3.5 | 3 | 3.2 | 4 | 3 |
| Sorbitan monopalmitate | 1.4 | 1 | 1.3 | 2 | 3 | 1.5 |
| Lemon eucalyptus leaf hydrosol | 20 | 26 | 32 | 35 | 40 | 30 |
| Pyrrolidone-5-carboxylic acid sodium | 0.6 | 0.5 | 0.7 | 1 | 0.5 | 0.5 |
By the dosage of each substance described in formula two to formula seven in above-mentioned table, mosquito repellant is made in mixing and emulsifying at 75 DEG C.
As a kind of transformation of the invention: each component content needed for preparation mosquito repellant is not limited to above-mentioned formula
One content listed into formula seven, as long as transformation made by within the scope of the invention belongs to scope of the invention.
In the lab, it is tested using formula one to the mosquito repellant that formula seven is prepared, experimentation and knot
Fruit is as follows:
1. attack is tested:
In mosquito cage (400mm × 300mm × 400mm) be put into 300 sprout wings after the female culex pipiens fatigans do not sucked blood for 3~5 days at
Worm (is provided) by professional unit.Experimenter's the back of the hand exposes 40mm × 40mm baring skin, the back of the hand rest part white yarn cloth hand
The tight masking of set.When experiment, hand is protruded into inside ready mosquito cage, close observation 2min, if discovery mosquito stops falling, in mosquito
Shake arm before its mouthpart insertion skin is driven it to leave, 1 mosquito is denoted as and stops falling.The mosquito for stopping falling that comes is more than 30 realities
The person of testing and test worm are that attack is qualified, and this person and this cage mosquito can carry out repellency test.
2. repellent is tested:
The tester (men and women is fifty-fifty) of selection 4 and above attack qualification, respectively draws 50mm × 50mm in its both hands back
Skin area, wherein hand is blank control, another hand presses 1.5 μ L/cm2Dosage be prepared into using the method for the present invention
Mosquito repellant be uniformly applied to the back of the hand, exposure 40mm × 40mm skin therein tightly covers rest part.Smear repellent
After agent 2h, hand is protruded into 2min in the cage for being placed with attack qualification mosquito, whether there is or not mosquitoes to come to suck blood for observation, later at interval of 1h
Test is primary, as long as there is 1 mosquito to come to suck blood to sentence and make repellant failure.Record the effective protecting time (h) of repellant.
3. experimental result:
By many experiments the result shows that, when being prepared into effective protection of the standby mosquito repellant to human body using the method for the present invention
Between more than 3 hours.
Claims (5)
1. utilizing the method for husky ginger oil extract waste liquid preparation mosquito repellant, it is characterised in that: include the following steps:
A. trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are extracted from husky ginger oil extract waste liquid
Mixture, comprising the following steps:
(1) water phase distillate is collected, water phase distillate is that the water phase flowed out from the oil water separator of husky ginger oil extract tank distillates
Liquid；Or the water phase distillate that will be collected after the brown color muddiness waste liquid re-distillation in husky ginger oil extract tank；
(2) sodium chloride or potassium chloride are added into water phase distillate acquired by step (1), make in water phase distillate it is trans--
Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are precipitated；
(3) organic solvent is added into the water phase distillate after step (2) to be extracted, the organic solvent of addition is dichloro
Methane or petroleum ether or n-hexane or acetone or ethyl acetate, organic solvent are 1/ with the water phase distillate volume ratio taken
10, organic solvent phase is taken after extraction；
(4) organic solvent acquired by step (3) is mutually evaporated under reduced pressure, obtains brown yellow oil liquid；
(5) cryogenic freezing is carried out to brown yellow oil liquid acquired by step (4), wait which crystallization is precipitated, rapid filtration under suction is obtained
Trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate mixture, trans- in mixture-to methoxyl group
The content of ethyl cinnamate is that the content of 83 ~ 92%, cis--Ethyl p-methoxy-silicate is 3 ~ 13%；
B. the preparation-obtained trans--Ethyl p-methoxy-silicate of above-mentioned steps a and cis--p-methoxycinnamic acid are used
Ethyl ester mixture prepares mosquito repellant:
30~50 parts of trans--Ethyl p-methoxy-silicate and cis--Ethyl p-methoxy-silicate are mixed in mass ratio
Object, 10~20 parts of glycerol, 1~5 part of Eucalyptus urophylla-grandis leaf oil, 2~20 parts of propylene glycol, 3~5 parts of polyoxyethylene sorbitan
Alcohol monoleate, 1~3 part of sorbitan monopalmitate, 20~40 parts of lemon eucalyptus leaf hydrosol, 0.5~1 part of pyrroles
Mosquito repellant is made in alkanone -5- carboxylic acid sodium mixing and emulsifying at 75 DEG C.
2. the method according to claim 1 using husky ginger oil extract waste liquid preparation mosquito repellant, it is characterised in that: institute
State the amount that sodium chloride or potassium chloride are added in step (2) are as follows: dense when making sodium chloride or Klorvess Liquid concentration saturation solubility
The 30~70% of degree.
3. the method according to claim 1 using husky ginger oil extract waste liquid preparation mosquito repellant, it is characterised in that: institute
State the vacuum distillation in step (4) are as follows: be evaporated under reduced pressure under conditions of being 55 DEG C ~ 85 DEG C in temperature by Rotary Evaporators.
4. the method according to claim 1 using husky ginger oil extract waste liquid preparation mosquito repellant, it is characterised in that:
Cryogenic freezing temperature in the step (5) is 0 DEG C ~ -10 DEG C, and cooling time is 1 ~ 5 hour.
5. the side of husky ginger oil extract waste liquid preparation mosquito repellant is utilized described in any claim according to claim 1 ~ 4
Method, it is characterised in that: lemon eucalyptus leaf hydrosol used in the step b is from the oil water separator of lemon eucalyptus oil extractor
The water phase distillate of outflow is the by-product of generation during lemon eucalyptus leaf extraction of essential oil.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022136067A1 (en) * | 2020-12-23 | 2022-06-30 | Workforce Biologics Ltd | Formulation comprising p-menthane-3,8-diol |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101919534A (en) * | 2010-06-08 | 2010-12-22 | 华南农业大学 | Sand ginger paste and preparation method thereof |
| CN102860303A (en) * | 2012-10-15 | 2013-01-09 | 广西工学院 | Method for utilizing citriodora oil to extract waste liquid to prepare mosquito repellent |
| CN104434687A (en) * | 2014-12-12 | 2015-03-25 | 广西科技大学 | Guanglin No.9 eucalyptus leaf essential oil mosquito repellent and preparation method thereof |
| CN105010337A (en) * | 2015-07-23 | 2015-11-04 | 广西科技大学 | Method of preparing mosquito repellant by utilizing cassia oil extraction waste liquid |
| TW201600115A (en) * | 2014-06-30 | 2016-01-01 | Univ Vanung | Mosquito repelling and sun protection composition |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101919534A (en) * | 2010-06-08 | 2010-12-22 | 华南农业大学 | Sand ginger paste and preparation method thereof |
| CN102860303A (en) * | 2012-10-15 | 2013-01-09 | 广西工学院 | Method for utilizing citriodora oil to extract waste liquid to prepare mosquito repellent |
| TW201600115A (en) * | 2014-06-30 | 2016-01-01 | Univ Vanung | Mosquito repelling and sun protection composition |
| CN104434687A (en) * | 2014-12-12 | 2015-03-25 | 广西科技大学 | Guanglin No.9 eucalyptus leaf essential oil mosquito repellent and preparation method thereof |
| CN105010337A (en) * | 2015-07-23 | 2015-11-04 | 广西科技大学 | Method of preparing mosquito repellant by utilizing cassia oil extraction waste liquid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022136067A1 (en) * | 2020-12-23 | 2022-06-30 | Workforce Biologics Ltd | Formulation comprising p-menthane-3,8-diol |
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