CN106497678A - A kind of method that molecular sieve extractant extracts Rosa Damascana - Google Patents
A kind of method that molecular sieve extractant extracts Rosa Damascana Download PDFInfo
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- CN106497678A CN106497678A CN201611014351.3A CN201611014351A CN106497678A CN 106497678 A CN106497678 A CN 106497678A CN 201611014351 A CN201611014351 A CN 201611014351A CN 106497678 A CN106497678 A CN 106497678A
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- Prior art keywords
- molecular sieve
- extractant
- essential oil
- water
- rosa damascana
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention belongs to flower class extraction of essential oil technical field, the method that more particularly to a kind of molecular sieve extractant extracts Rosa Damascana.Using the selection suction-operated of molecular sieve, improve extractant and ability is impregnated with and emulsification and solubilization to essential oil in rose to rose, increase dispersion amount of the essential oil in rose in extractant.The not wide-open fresh roseleaf for cutting off holder is preprocessed, extraction, filtration under diminished pressure, steam distillation, water-oil separating, the product of gained is strong without pigment, pure bright, fragrant, yield is 0.020%～0.025%, and the recovery rate of more industrial traditional extraction method essential oil is high by 11%.Organic solvent is replaced disposably to extract Rosa Damascana with the adsorbing molecular sieve extractant of selection in aqueous, the problem of environmental pollution is not only overcome, solve the problems, such as that traditional extraction process high energy consumption, oil yield are low, but also have molecular sieve extractant can be recycled, safe operation, low production cost.
Description
Technical field
The invention belongs to flower class extraction of essential oil technical field, more particularly to a kind of molecular sieve extractant extraction Rosa Damascana
Method.
Background technology
Rosa Damascana is most expensive in essential oil in the world, has the laudatory title of " after essential oil ".Rosa Damascana to women more
Term discomfort, Gong Han, frigidity, dysmenorrhoea and endocrinopathy have adjustment or alleviate effect, and in terms of beauty and skin care
Effect is even more important.Rosa Damascana, is by within to support outer principle, promotes melanin to decompose, so as to desalinate color spot, makes skin
Recovery elasticity, water are tender, women can be allowed to have again the fair skin of health, be a cosmetic for being well suited for women beauty and skin care
Product.Rosa Damascana is the important source material for manufacturing highclass perfumes, and price is high, is the essence in the famous and precious senior concentration essence in the world
Product.Rosa Damascana can be used not only for the cosmetic fields such as beauty, skin care, hair care, can be also used for medicine and field of food.Than
Such as, Rosa Damascana is used as medicinal, nervous system, stagnation of liver qi, suffer from indiestion, the aspect such as gynecological disease and cardiovascular and cerebrovascular disease
All there is preventive and therapeutic effect；Often drink or edible rose essential oil, also have the effect of beautifying face and moistering lotion, disease preventing and treating.
At present, extracting the conventional method of essential oil from rose has：Milling process, solvent extraction, supercritical extraction and
Steam distillation.Steam distillation vapo(u)rizing temperature height, time length, high energy consumption, easily cause the conversion of fragrance active ingredient rotten；
Solvent extraction is with substantial amounts of virose organic solvent, serious to product and environmental pollution；Supercritical methanol technology, equipment are complicated,
Operation difficulty is big, and production cost is high；Milling process, essential oil output capacity are low.In conjunction with have been disclosed for from rose extract essential oil
Domestic and international patent, have mostly process complicated, using the organic solvent for having pollution to environment, repeatedly extraction, steam repeatedly
The temperature for evaporating, extracting essential oil is high, easily causes the bad reactions such as essential oil oxidation, polymerization, so as to affect the quality of product or fuel-displaced
The not high shortcoming of rate.
Content of the invention
In sum, in order to overcome the shortcomings of existing extraction essential oil technology from rose, the invention provides a kind of behaviour
Make simple, safe and environment-friendly and can be more thoroughly the method that essential oil is extracted from rose.The present invention adopt mesoporous molecular sieve for
Adsorbent, neopelex are extractant, realize the essential oil dispersion in rose in extract, further process
Extract obtains essential oil.Molecular sieve has uniform pore structure, and its hole diameter is adjustable, and these holes can be more straight than which
Inside of the little Molecular Adsorption in footpath to vestibule, and there is the selectivity of Preferential adsorption to polar molecule and unsaturated molecule, thus
Polarity degree difference, the molecule that degree of saturation is different, molecular size is different and boiling point is different can be separated.Detergent alkylate
There is hydrophily, non-polar group there is lipophile for simultaneously polarized group and non-polar group in sodium sulfonate, polar group, it
One end hydrophilic, one end oleophylic so as to reduce the interfacial tension of essential oil and water surface, reduces absorption affinity of the rose to essential oil, increases
Plus solubility of the essential oil in water；Neopelex can improve rose wettability of the surface energy, make rose surface have parent
Aqueous, be conducive to the essential oil in rose to be cemented out by water；Neopelex has very strong permeance property, and it can soak
Enter the inside to rose, by essential oil dispersion in extract.
The technical solution used in the present invention is as follows：
A kind of method that molecular sieve extractant extracts Rosa Damascana, comprises the steps：
1. rose pretreatment：The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, so
4min is stirred in mixer, flower sauce is made；
2. extract：The flower sauce that makes, the molecular sieve extractant aqueous solution are mixed with 1: 1～1.5 mass ratio, at 40～50 DEG C
At a temperature of, stir 1h；
3. filtration under diminished pressure：Filtrate and filter residue is collected, is contaminated with spending the molecular sieve filter residue drying of slag, roasting, be can be recycled；
4. steam distillation：Distillation filtrate, distillate are the mixture of essential oil and water；
5. water-oil separating：The mixture that essential oil and water are separated with oil water separator, separates water outlet, obtains essential oil product, isolate
Water can be recycled.
Further, described molecular sieve extractant is made up of adsorbent and extractant, and its mass ratio is：1: 2～3.
Further, described adsorbent is mesoporous molecular sieve, and extractant is neopelex.
Further, the mass percent of the described molecular sieve extractant aqueous solution is 1.5～2%.
Using technical solution of the present invention, the essential oil in rose is extracted, effect is very notable.Products obtained therefrom non-pigment is remained,
Color is pure bright, and fragrant is strong.
Beneficial effect：
1st, the purity of essential oil is high, makees adsorbent using mesoporous molecular sieve, and Selective adsorption is strong, hydrothermal stability is high；And use 12
Extractant made by sodium alkyl benzene sulfonate, and boiling point is high, not volatile, is difficult to be distilled off being mixed in essential oil, so as to improve essential oil
Purity.
2nd, the low production cost of essential oil, the molecular sieve extractant of the present invention can be recycled, thus reduce production cost.
3rd, the quality of essential oil is high, and with molecular sieve as extractant, extraction temperature is low（At a temperature of 40～50 DEG C）, effectively
Original natural component in Rosa Damascana is protected, therefore the product aroma of pure of gained, quality is high-end.
4th, the high income of essential oil, is measured by gas-chromatography, and the yield of the present invention is 0.020%～0.025%（Raw material is
Fresh wet petal）, higher by 11% than now industrial traditional extracting method, also above the level 0.02% that reports both at home and abroad～
0.04%（Raw material is dry petal）.Using mesoporous molecular sieve and surfactant as extractant, as both significantly cooperate with
Effect, selective absorption, infiltration, emulsification, solubilization, significantly reduce remaining quantity of the essential oil in rose, increase essence
Dispersion amount of the oil in extract.By contrast experiment, i.e., under same experiment condition, adsorbent mesoporous molecular sieve is individually adopted
（Yield is 0.010%～0.015%）With individually using extractant neopelex（Yield be 0.012%～
0.015%）Yield all well below yield associated with both.
5th, using the extracting method of the present invention, process is simple, safe operation, and production process is pollution-free.
6th, using the extracting method of the present invention, during extraction, liquid-solid ratio is little, can so shorten distillation time, can reduce energy again
Consumption, moreover it is possible to improve the concentration of essential oil in distillate, so as to be conducive to water-oil separating.
Specific embodiment
Embodiment 1
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min weighs 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5% into flower sauce
Than 1: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.40 DEG C are heated to, 1h is stirred, filtration under diminished pressure collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water, with profit point
Water is removed from device separation, the oily liquids product 0.21g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 2
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5%
Than 1: the aqueous solution 2.5), it is added in the three-necked bottle of 5000ml.40 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.20g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 3
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5%
Than 1: the aqueous solution 3), it is added in the three-necked bottle of 5000ml.40 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.20g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 4
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two mass ratio 1 of 1000g 2%
: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.40 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filtrate, will
Which is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With oil water separator point
Leave away water, obtain the oily liquids product 0.21g of colourless, limpid transparent, aroma of pure.
Embodiment 5
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5%
Than 1: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.50 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.22g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 6
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min weighs 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5% into flower sauce
Than 1: the aqueous solution 2.5), it is added in the three-necked bottle of 5000ml.50 DEG C are heated to, 1h is stirred, filtration under diminished pressure collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water, with profit point
Water is removed from device separation, the oily liquids product 0.22g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 7
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1000g 1.5%
Than 1: the aqueous solution 3), it is added in the three-necked bottle of 5000ml.50 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.22g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 8
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1500g 1.5%
Than 1: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.40 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.22g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 9
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1500g 1.5%
Than 1: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.45 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.23g of colourless, limpid transparent, aroma of pure is obtained.
Embodiment 10
A kind of method that molecular sieve extractant extracts Rosa Damascana, is obtained through the following steps：
The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, stirred in mixer
4min is into flower sauce.Weigh 1000g flower sauces, mesoporous molecular sieve and neopelex (the two quality of 1500g 1.5%
Than 1: the aqueous solution 2), it is added in the three-necked bottle of 5000ml.50 DEG C are heated to, 1h is stirred.Filtration under diminished pressure, collects filter
Liquid, is transferred in the distilling flask of 5000ml, steam distillation, and distillate is the mixture of essential oil and water.With profit point
Water is removed from device separation, the oily liquids product 0.25g of colourless, limpid transparent, aroma of pure is obtained.
It is noted that above-described embodiment is to the illustrative and not limiting of technical solution of the present invention, art is general
The equivalent of logical technical staff or other modifications that is made according to existing technology, as long as no beyond the technology of the present invention side
The thinking and scope of case, should be included within interest field of the presently claimed invention.
Claims (4)
1. a kind of method that molecular sieve extractant extracts Rosa Damascana, it is characterised in that comprise the following steps：
1.. rose pre-processes：The not wide-open fresh roseleaf for cutting off holder is cleaned up, is dried naturally, so
4min is stirred in mixer, flower sauce is made；
2.. extraction：The flower sauce that makes, the molecular sieve extractant aqueous solution are mixed with 1: 1～1.5 mass ratio, at 40～50 DEG C
At a temperature of, stir 1h；
3.. filtration under diminished pressure：Filtrate and filter residue is collected, is contaminated with spending the molecular sieve filter residue drying of slag, roasting, be can be recycled；
4.. steam distillation：Distillation filtrate, distillate are the mixture of essential oil and water；
5.. water-oil separating：The mixture that essential oil and water are separated with oil water separator, separates water outlet, obtains essential oil product, isolate
Water can be recycled.
2. the method that a kind of molecular sieve extractant according to claim 1 extracts Rosa Damascana, it is characterised in that：Described
Molecular sieve extractant is made up of adsorbent and extractant, and its mass ratio is：1: 2～3.
3. the method that a kind of molecular sieve extractant according to claim 2 extracts Rosa Damascana, it is characterised in that：Described
Adsorbent is mesoporous molecular sieve, and extractant is neopelex.
4. a kind of method that molecular sieve extractant extracts Rosa Damascana according to claim 1, it is characterised in that：Described divides
The mass percent of the son sieve extractant aqueous solution is 1.5～2%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294739A (en) * | 2017-07-25 | 2019-02-01 | 丘健 | The extracting mode of rose extracting solution |
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Application publication date: 20170315 |