CN108342252A - A kind of method of high efficiency extraction agilawood essential oil - Google Patents
A kind of method of high efficiency extraction agilawood essential oil Download PDFInfo
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- CN108342252A CN108342252A CN201810053668.0A CN201810053668A CN108342252A CN 108342252 A CN108342252 A CN 108342252A CN 201810053668 A CN201810053668 A CN 201810053668A CN 108342252 A CN108342252 A CN 108342252A
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 60
- 238000000605 extraction Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910021647 smectite Inorganic materials 0.000 claims abstract description 54
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 53
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 52
- 239000012452 mother liquor Substances 0.000 claims abstract description 38
- 239000012065 filter cake Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 78
- 239000003921 oil Substances 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 32
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 21
- 239000011734 sodium Substances 0.000 claims description 21
- 229910052708 sodium Inorganic materials 0.000 claims description 21
- 241000271309 Aquilaria crassna Species 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 6
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 6
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 5
- 229910000271 hectorite Inorganic materials 0.000 claims description 5
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims description 3
- 229910052923 celestite Inorganic materials 0.000 claims description 3
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 3
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 3
- 239000000344 soap Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- BOXVSFHSLKQLNZ-UHFFFAOYSA-K dysprosium(iii) chloride Chemical compound Cl[Dy](Cl)Cl BOXVSFHSLKQLNZ-UHFFFAOYSA-K 0.000 claims description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000002023 wood Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 24
- 239000011229 interlayer Substances 0.000 description 6
- 241000549556 Nanos Species 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- -1 alkane quaternary ammonium salt Chemical class 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 241001533085 Aquilaria sinensis Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 244000292411 Excoecaria agallocha Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 235000005324 Typha latifolia Nutrition 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 244000118869 coast club rush Species 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 208000003243 intestinal obstruction Diseases 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000275 saponite Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000004114 suspension culture Methods 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to extraction of essential oil technical fields, and in particular to a kind of method of high efficiency extraction agilawood essential oil.The method of the high efficiency extraction agilawood essential oil includes：Step 1: preparing the organic smectite of rare earth modified nano；Step 2: agallochum wood powder is broken and boil；Step 3: mother liquor reacts with the organic smectite of rare earth modified nano and collects filter cake；Step 4: absolute ethyl alcohol is added in filter cake and collects mother liquor；Step 5: high-purity agilawood essential oil is made.The method of the high efficiency extraction agilawood essential oil is simple and efficient with abstraction process, and technical process is environmentally protective, energy Substantial evaluation, and the advantage that production cost is quite cheap.And the refined agilawood essential oil purity obtained is up to 95% or more (using current existing extracting method, the purity of agilawood essential oil can only be close to 90%), therefore the method for the high efficiency extraction agilawood essential oil of the present invention has very strong practicability, and industrial prospect is extremely bright.
Description
Technical field
The present invention relates to extraction of essential oil technical fields, and in particular to a kind of method of high efficiency extraction agilawood essential oil.
Background technology
Agalloch eaglewood be the resiniferous timber of Thymelaeceae eaglewood suspension culture of Aquilaria sinensis (also known as " buta-buta ", " tabernaemontanus bulrush fragrant ", " Hainan is heavy
It is fragrant " etc.), all it is the extremely rare traditional Chinese medicine of the fragrance of most expensive and China in the world all the time.Agalloch eaglewood not only has
There is very strong unique perfume, the beautiful impressions such as pleasant, the comfortable, tranquilizing the mind to continue for ever, beauty treatment is brought to people, and related
Research confirms that agalloch eaglewood has the plurality of medical function such as analgesic, spasmolysis, Zhichuan, decompression, is especially also clinically widely used in treatment
It is cold to have a stomach-ache, alleviate senile intestinal obstruction, inhibit the diseases such as growth of bacillus tubercle.As main production country implements agalloch eaglewood woods in succession in recent years
The wooden protection of resources, supply falls short of demand for international market lignum aquilariae, and price is constantly soaring.According to statistics, the valence of international market lignum aquilariae timber
Lattice have reached 0.6~10,000 dollars/kg, 2014 be only Malaysia, Vietnam, the outlet of three state of Singapore agalloch eaglewood timber the output value
Reach more than 10 hundred million dollars.
Wherein, agilawood essential oil is the application form of most significant end in all products of agalloch eaglewood, is that domestic and international research and development are burnt all the time
Point.But agilawood essential oil extraction difficulty is very big at present, not only operating procedure is complicated, but also recovery rate is extremely low, and it is heavy seriously to hinder
The industrialization of essence oil extract and its scale application.Therefore, it is highly desirable to develop a kind of environmentally friendly, efficient, safe, sustainable
The agilawood essential oil extraction process that property utilizes.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to a kind of method of high efficiency extraction agilawood essential oil is provided, it should
The method of high efficiency extraction agilawood essential oil has simple for process, safety, environmental protection, energy Substantial evaluation, and extraction cost is cheap
The advantages of.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of method of high efficiency extraction agilawood essential oil is provided, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After water is warming up to certain temperature, adds sodium base and cover soap
Stone simultaneously stirs certain time with certain rotating speed, and rare-earth substance is then added and continues to stir certain time with certain rotating speed,
Then quaternary ammonium salt is added and certain time is stirred with certain rotating speed, finally filters and is fully washed with water, then by filter cake one
Determine fully to dry to constant weight at temperature, obtains the organic smectite of the rare earth modified nano；
Step 2: crushing agalloch eaglewood trees to powder, then powder is added to the water and is boiled, kept certain and boil
The time is boiled, then filters and collects mother liquor；
Step 3: the organic smectite of rare earth modified nano made from step 1 is added in the mother liquor that step 2 obtains, and
Certain time is stirred with certain rotating speed, then filters and collects filter cake；
Step 4: absolute ethyl alcohol is added in the obtained filter cake of step 3, and certain time is stirred with certain rotating speed,
Then it filters and collects mother liquor；
Step 5: water is added in the obtained mother liquor of step 4, and certain time is stirred with certain rotating speed, stands one
After fixing time, removes the water phase of lower layer and collect the oil phase on upper layer；Then water is added in oil phase, and continues with certain rotating speed
Certain time is stirred, is stood after a certain period of time, lower layer's water phase is removed and collects upper oil phase；It so operates repeatedly several times, most
The oil phase collected afterwards is high-purity agilawood essential oil.
In above-mentioned technical proposal, in the step 1, the sodium base smectite is one kind in na-montmorillonite, hectorite
Or two kinds of compositions in any proportion.
In above-mentioned technical proposal, in the step 1, the rare-earth substance is Ce (NO3)3、Ce2(SO4)3、CeCl3、Dy
(NO3)3、Dy2(SO4)3、DyCl3、Sr(NO3)2、SrSO4Or SrCl2In one kind or arbitrary two or more groups in any proportion
Close object.
In above-mentioned technical proposal, in the step 1, the quaternary ammonium salt is cetyl trimethylammonium bromide, cetyl
One or more of trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide or dodecyl trimethyl ammonium chloride, which are pressed, appoints
The combination of meaning ratio.
In above-mentioned technical proposal, in the step 1, the organic smectite of rare earth modified nano is prepared：By 200~400 parts of water
After being warming up to 60~85 DEG C, adds 100 parts of sodium base smectites and 30~60min is stirred with the rotating speed of 50~150rpm, then
5~10 parts of rare-earth substances are added and continue to stir 15~30min with the rotating speed of 50~150rpm, 20~50 parts of quaternary ammoniums are then added
Salt simultaneously stirs 1~3h with the rotating speed of 150~300rpm, finally filters and is fully washed with water, then by filter cake at 50~60 DEG C
It is fully dry to constant weight, obtain the organic smectite of the rare earth modified nano.
In above-mentioned technical proposal, in the step 2, it is the mesh of 1 mesh~10 that 100 parts of agalloch eaglewood trees, which are crushed to granularity,
Powder, then by powder be added 100~500 parts of water in and boil, holdings boiling time be 6~10h, then filter and collect
Mother liquor.
In above-mentioned technical proposal, in the step 3, it is added made from step 1 in the mother liquor that 100 parts of step 2 obtain
20~50 parts of organic smectites of rare earth modified nano, and 3~5h is stirred with the rotating speed of 150~300rpm, it then filters and collects
Filter cake.
In above-mentioned technical proposal, in the step 4,100~200 parts are added in 100 parts of obtained filter cakes of step 3
Absolute ethyl alcohol, and 1~2h is stirred with the rotating speed of 150~300rpm, it then filters and collects mother liquor.
In above-mentioned technical proposal, in the step 5,100~300 parts of water are added in the obtained mother liquor of step 4, and
15~20min is stirred with the rotating speed of 50~150rpm, after standing 30~60min, the water phase of lower layer is removed and collects the oil on upper layer
Phase；Then 100~300 parts of water are added in oil phase, and continue to stir 15~20min with the rotating speed of 50~150rpm, stand 30
After~60min, removes lower layer's water phase and collect upper oil phase；It so operates 3~6 times repeatedly, the oil phase finally collected is height
Purity agilawood essential oil.
It is described Step 1: the water in step 2 and step 5 is pure water in above-mentioned technical proposal.
Compared with prior art, advantageous effect is the present invention：
(1) method of a kind of high efficiency extraction agilawood essential oil provided by the invention, the rare earth modified nano prepared in step 1
Organic smectite to agilawood essential oil can efficient selective absorb, wherein na-montmorillonite and lithium included by sodium base smectite
There are layer structures for saponite, have the layer-shaped area of certain space, when sodium base smectite and cetyl trimethylammonium bromide etc.
After long chain alkane quaternary ammonium salt reacts, quaternary ammonium salt forms organic smectite between entering sodium base smectite, at this point, organic illiteracy soap
Stone does not have agilawood essential oil the function of any selective absorbing.But as addition Ce (NO3)3Equal rare-earth substances and sodium base smectite
Or organic smectite is when reacting, Ce3+Equal rare earth ions can enter the Si-O tetrahedrons of sodium base smectite or organic smectite
In lattice.When drying, Ce3+/ Si-O octahedron lattices are distorted, the layer of the organic smectite of the rare earth modified nano generated
Between region to agilawood essential oil can efficient selective absorb, and at the same time do not absorb any other liquid organic material.Therefore,
After the organic smectite of rare earth modified nano is mixed with agallochum water boiling liquid, the interlayer of the organic smectite of rare earth modified nano
Region can slowly attract agilawood essential oil molecule to enter interlayer.Later, absolute ethyl alcohol is added and carries out dipping extracting.Due to absolute ethyl alcohol
Molecular volume very little is not limited by the steric hindrance of interlayer region, therefore is largely entered interlayer region and dissolved agilawood essential oil.Quilt
The agilawood essential oil molecule of anhydrous ethanol solvent constantly expands, until breaking through the organic smectite interlayer region of rare earth modified nano
It limits (i.e. interlayer region is caved in, and layer structure is delaminated completely)；At this point, the organic smectite of the rare earth modified nano delaminated and
Agilawood essential oil detaches each other, that is, has separated agilawood essential oil.Absolute ethyl alcohol molecule is removed using the means of washing later,
Obtain high-purity agilawood essential oil (purity is up to 95% or more).
(2) method of a kind of high efficiency extraction agilawood essential oil provided by the invention, is simple and efficient, technique mistake with abstraction process
Journey is environmentally protective, energy Substantial evaluation, and the advantage that production cost is quite cheap.Extraction process of the present invention is mainly in aqueous solution
Operation system extracts, and does not need cumbersome organic solvent method multistep extraction process, and required production equipment is all routinely
Conventional equipment, need not the institute such as supercritical carbon dioxide extracting must prohibitively expensive large scale equipment, what is obtained refines
Agilawood essential oil purity be up to 95% or more (using current existing extracting method, the purity of agilawood essential oil can only close to 90%),
Therefore the method for the high efficiency extraction agilawood essential oil of the present invention has very strong practicability, and industrial prospect is extremely bright.
Specific implementation mode
In order to make the technical problems, technical solutions and beneficial effects solved by the present invention be more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
Embodiment 1.
A kind of method of high efficiency extraction agilawood essential oil, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After 300 parts of water are warming up to 70 DEG C, 100 parts of sodium are added
Base smectite simultaneously stirs 45min with the rotating speed of 100rpm, and 7 parts of rare-earth substances are then added and continue to stir with the rotating speed of 100rpm
Then 20min is added 35 parts of quaternary ammonium salts and stirs 1~3h with the rotating speed of 200rpm, finally filters and fully washed with water, then will
Filter cake is fully dried to constant weight at 55 DEG C, obtains the organic smectite of the rare earth modified nano；
In the present embodiment, sodium base smectite is na-montmorillonite；
In the present embodiment, rare-earth substance is Ce (NO3)3；
In the present embodiment, quaternary ammonium salt is cetyl trimethylammonium bromide；
Step 2: it is 5 mesh powders that 100 parts of agalloch eaglewood trees, which are crushed to granularity, 300 parts of water then are added in powder
In and boil, holding boiling time be 8h, then filter and collect mother liquor；
Step 3: it is organic that 35 parts of rare earth modified nanos made from step 1 are added in the mother liquor that 100 parts of step 2 obtain
Smectite, and 4h is stirred with the rotating speed of 200rpm, it then filters and collects filter cake；
Step 4: 150 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and with the rotating speed of 200rpm
1.5h is stirred, then filters and collects mother liquor；
Step 5: 200 parts of water are added in the obtained mother liquor of step 4, and 18min is stirred with the rotating speed of 100rpm, it is quiet
After setting 45min, removes the water phase of lower layer and collect the oil phase on upper layer；Then in oil phase be added 200 parts of water, and continue with
The rotating speed of 100rpm stirs 18min, after standing 45min, removes lower layer's water phase and collects upper oil phase；It so operates 5 times repeatedly,
The oil phase finally collected is high-purity agilawood essential oil.
Wherein, Step 1: the water in step 2 and step 5 is pure water.
Embodiment 2.
A kind of method of high efficiency extraction agilawood essential oil, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After 200 parts of water are warming up to 60 DEG C, 100 parts of sodium are added
Base smectite simultaneously stirs 60min with the rotating speed of 50rpm, and 5 parts of rare-earth substances are then added and continue to stir with the rotating speed of 50rpm
Then 30min is added 20 parts of quaternary ammonium salts and stirs 3h with the rotating speed of 150rpm, finally filters and fully washed with water, then will filter
Cake is fully dried to constant weight at 50 DEG C, obtains the organic smectite of the rare earth modified nano；
In the present embodiment, sodium base smectite is hectorite；
In the present embodiment, rare-earth substance Ce2(SO4)3；
In the present embodiment, quaternary ammonium salt is hexadecyltrimethylammonium chloride；
Step 2: it is 1 mesh powder that 100 parts of agalloch eaglewood trees, which are crushed to granularity, 100 parts of water then are added in powder
In and boil, holding boiling time be 6h, then filter and collect mother liquor；
Step 3: it is organic that 20 parts of rare earth modified nanos made from step 1 are added in the mother liquor that 100 parts of step 2 obtain
Smectite, and 5h is stirred with the rotating speed of 150rpm, it then filters and collects filter cake；
Step 4: 100 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and with the rotating speed of 150rpm
2h is stirred, then filters and collects mother liquor；
Step 5: 100 parts of water are added in the obtained mother liquor of step 4, and 20min is stirred with the rotating speed of 50rpm, it is quiet
After setting 30min, removes the water phase of lower layer and collect the oil phase on upper layer；Then in oil phase be added 100 parts of water, and continue with
The rotating speed of 50rpm stirs 20min, after standing 30min, removes lower layer's water phase and collects upper oil phase；It so operates 3 times repeatedly,
The oil phase finally collected is high-purity agilawood essential oil.
Wherein, Step 1: the water in step 2 and step 5 is pure water.
Embodiment 3.
A kind of method of high efficiency extraction agilawood essential oil, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After 400 parts of water are warming up to 85 DEG C, 100 parts of sodium are added
Base smectite simultaneously stirs 30min with the rotating speed of 150rpm, and 10 parts of rare-earth substances are then added and continue to stir with the rotating speed of 150rpm
15min is mixed, 50 parts of quaternary ammonium salts are then added and 1h is stirred with the rotating speed of 300rpm, finally filters and is fully washed with water, then will
Filter cake is fully dried to constant weight at 60 DEG C, obtains the organic smectite of the rare earth modified nano；
In the present embodiment, sodium base smectite is the composition of na-montmorillonite and hectorite in any proportion；
In the present embodiment, rare-earth substance CeCl3With Dy (NO3)3Composition in any proportion；
In the present embodiment, quaternary ammonium salt is dodecyl trimethyl ammonium bromide；
Step 2: it is 10 mesh powders that 100 parts of agalloch eaglewood trees, which are crushed to granularity, powder is then added 500 parts
It in water and boils, holding boiling time is 10h, then filters and collects mother liquor；
Step 3: it is organic that 50 parts of rare earth modified nanos made from step 1 are added in the mother liquor that 100 parts of step 2 obtain
Smectite, and 3h is stirred with the rotating speed of 300rpm, it then filters and collects filter cake；
Step 4: 200 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and with the rotating speed of 300rpm
1h is stirred, then filters and collects mother liquor；
Step 5: 300 parts of water are added in the obtained mother liquor of step 4, and 15min is stirred with the rotating speed of 150rpm, it is quiet
After setting 60min, removes the water phase of lower layer and collect the oil phase on upper layer；Then in oil phase be added 300 parts of water, and continue with
The rotating speed of 150rpm stirs 15min, after standing 60min, removes lower layer's water phase and collects upper oil phase；It so operates 6 times repeatedly,
The oil phase finally collected is high-purity agilawood essential oil.
Wherein, Step 1: the water in step 2 and step 5 is pure water.
Embodiment 4.
A kind of method of high efficiency extraction agilawood essential oil, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After 250 parts of water are warming up to 65 DEG C, 100 parts of sodium are added
Base smectite simultaneously stirs 50min with the rotating speed of 80rpm, and 6 parts of rare-earth substances are then added and continue to stir with the rotating speed of 80rpm
Then 25min is added 25 parts of quaternary ammonium salts and stirs 2.5h with the rotating speed of 250rpm, finally filters and fully washed with water, then will
Filter cake is fully dried to constant weight at 53 DEG C, obtains the organic smectite of the rare earth modified nano；
In the present embodiment, sodium base smectite is na-montmorillonite；
In the present embodiment, rare-earth substance Dy2(SO4)3、DyCl3With Sr (NO3)2Composition in any proportion；
In the present embodiment, quaternary ammonium salt is that dodecyl trimethyl ammonium bromide and dodecyl trimethyl ammonium chloride press arbitrary ratio
The combination of example；
Step 2: it is 3 mesh powders that 100 parts of agalloch eaglewood trees, which are crushed to granularity, 200 parts of water then are added in powder
In and boil, holding boiling time be 7h, then filter and collect mother liquor；
Step 3: 20~50 parts of rare earth modified nanos made from step 1 are added in the mother liquor that 100 parts of step 2 obtain
Organic smectite, and 4.5h is stirred with the rotating speed of 180rpm, it then filters and collects filter cake；
Step 4: 120 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and with the rotating speed of 180rpm
1.8h is stirred, then filters and collects mother liquor；
Step 5: 150 parts of water are added in the obtained mother liquor of step 4, and 18min is stirred with the rotating speed of 80rpm, it is quiet
After setting 50min, removes the water phase of lower layer and collect the oil phase on upper layer；Then in oil phase be added 150 parts of water, and continue with
The rotating speed of 80rpm stirs 18min, after standing 50min, removes lower layer's water phase and collects upper oil phase；It so operates 4 times repeatedly,
The oil phase finally collected is high-purity agilawood essential oil.
Wherein, Step 1: the water in step 2 and step 5 is pure water.
Embodiment 5.
A kind of method of high efficiency extraction agilawood essential oil, it includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After 350 parts of water are warming up to 75 DEG C, 100 parts of sodium are added
Base smectite simultaneously stirs 35min with the rotating speed of 120rpm, and 9 parts of rare-earth substances are then added and continue to stir with the rotating speed of 120rpm
Then 18min is added 45 parts of quaternary ammonium salts and stirs 1.5h with the rotating speed of 250rpm, finally filters and fully washed with water, then will
Filter cake is fully dried to constant weight at 58 DEG C, obtains the organic smectite of the rare earth modified nano；
In the present embodiment, sodium base smectite is hectorite；
In the present embodiment, rare-earth substance SrSO4And SrCl2Composition in any proportion；
In the present embodiment, quaternary ammonium salt is hexadecyltrimethylammonium chloride, dodecyl trimethyl ammonium bromide and dodecane
The combination of base trimethyl ammonium chloride in any proportion；
Step 2: it is 8 mesh powders that 100 parts of agalloch eaglewood trees, which are crushed to granularity, 400 parts of water then are added in powder
In and boil, holding boiling time be 9h, then filter and collect mother liquor；
Step 3: 20~50 parts of rare earth modified nanos made from step 1 are added in the mother liquor that 100 parts of step 2 obtain
Organic smectite, and 3.5h is stirred with the rotating speed of 250rpm, it then filters and collects filter cake；
Step 4: 180 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and with the rotating speed of 250rpm
1.2h is stirred, then filters and collects mother liquor；
Step 5: 250 parts of water are added in the obtained mother liquor of step 4, and 18min is stirred with the rotating speed of 120rpm, it is quiet
After setting 35min, removes the water phase of lower layer and collect the oil phase on upper layer；Then in oil phase be added 250 parts of water, and continue with
The rotating speed of 120rpm stirs 18min, after standing 50min, removes lower layer's water phase and collects upper oil phase；It so operates 5 times repeatedly,
The oil phase finally collected is high-purity agilawood essential oil.
Wherein, Step 1: the water in step 2 and step 5 is pure water.
Experiment：
Above-described embodiment 1 to 4 is extracted into obtained high-purity agilawood essential oil A~D, market existing product (model：GL-T,
Level-one agilawood essential oil, the production of Guo Lin agalloch eaglewood bio tech ltd of Zhongshan city) various contrast tests are carried out, as a result such as the following table 1
It is shown.
1 agilawood essential oil finished product contrast test result of table
As shown in Table 1, the performance indicators such as purity, color, storage stability of agilawood essential oil of the application extraction are excellent,
Significantly better than existing product at present on the market.Therefore, the application preparation process industrial prospect is bright, can create huge
Economic benefit.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than limiting the scope of the invention, although
The present invention is explained in detail with reference to preferred embodiment, it will be understood by those of ordinary skill in the art that, it can be to this hair
Bright technical solution is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention.
Claims (10)
1. a kind of method of high efficiency extraction agilawood essential oil, it is characterised in that：It includes the following steps：
Step 1: preparing the organic smectite of rare earth modified nano：After water is warming up to certain temperature, sodium base smectite is added simultaneously
Certain time is stirred with certain rotating speed, rare-earth substance is then added and continues to stir certain time with certain rotating speed, then
Quaternary ammonium salt is added and certain time is stirred with certain rotating speed, finally filters and is fully washed with water, then by filter cake in a constant temperature
Degree is lower fully dry to constant weight, obtains the organic smectite of the rare earth modified nano；
Step 2: crushing agalloch eaglewood trees to powder, then powder is added to the water and is boiled, keeps certain when boiling
Between, it then filters and collects mother liquor；
Step 3: the organic smectite of rare earth modified nano made from step 1 is added in the mother liquor that step 2 obtains, and with one
Fixed rotating speed stirs certain time, then filters and collects filter cake；
Step 4: absolute ethyl alcohol is added in the obtained filter cake of step 3, and certain time is stirred with certain rotating speed, then
It filters and collects mother liquor；
Step 5: water is added in the obtained mother liquor of step 4, and certain time is stirred with certain rotating speed, stands a timing
Between after, remove the water phase of lower layer and collect the oil phase on upper layer；Then water is added in oil phase, and continues to stir with certain rotating speed
Certain time stands after a certain period of time, removes lower layer's water phase and collects upper oil phase；So operation several times, is finally received repeatedly
The oil phase of collection is high-purity agilawood essential oil.
2. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 1,
The sodium base smectite is the composition of one or both of na-montmorillonite, hectorite in any proportion.
3. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 1,
The rare-earth substance is Ce (NO3)3、Ce2(SO4)3、CeCl3、Dy(NO3)3、Dy2(SO4)3、DyCl3、Sr(NO3)2、SrSO4Or
SrCl2In one kind or arbitrary two or more compositions in any proportion.
4. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 1,
The quaternary ammonium salt be cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, dodecyl trimethyl ammonium bromide or
The combination of one or more of dodecyl trimethyl ammonium chloride in any proportion.
5. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 1,
Prepare the organic smectite of rare earth modified nano：After 200~400 parts of water are warming up to 60~85 DEG C, add 100 parts of sodium bases and cover soap
Stone simultaneously stirs 30~60min with the rotating speed of 50~150rpm, 5~10 parts of rare-earth substances are then added and continue with 50~150rpm
Rotating speed stir 15~30min, then be added 20~50 parts of quaternary ammonium salts and with the rotating speed of 150~300rpm stir 1~3h, finally
It filters and is fully washed with water, then filter cake is fully dried to constant weight at 50~60 DEG C, obtain the rare earth modified nano
Organic smectite.
6. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 2,
It is the mesh powder of 1 mesh~10 that 100 parts of agalloch eaglewood trees, which are crushed to granularity, and then powder is added in 100~500 parts of water simultaneously
It boils, holding boiling time is 6~10h, then filters and collects mother liquor.
7. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 3,
20~50 parts of organic smectites of rare earth modified nano made from addition step 1 in the mother liquor that 100 parts of step 2 obtain, and with
The rotating speed of 150~300rpm stirs 3~5h, then filters and collects filter cake.
8. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：In the step 4,
100~200 parts of absolute ethyl alcohols are added in 100 parts of obtained filter cakes of step 3, and 1 is stirred with the rotating speed of 150~300rpm
~2h, then filters and collects mother liquor.
9. a kind of method of high efficiency extraction agilawood essential oil according to claim 8, it is characterised in that：In the step 5,
100~300 parts of water are added in the obtained mother liquor of step 4, and 15~20min is stirred with the rotating speed of 50~150rpm, stand
After 30~60min, removes the water phase of lower layer and collect the oil phase on upper layer；Then 100~300 parts of water of addition in oil phase, and after
The continuous rotating speed with 50~150rpm stirs 15~20min, after standing 30~60min, removes lower layer's water phase and collects upper oil phase；
It so operates 3~6 times repeatedly, the oil phase finally collected is high-purity agilawood essential oil.
10. a kind of method of high efficiency extraction agilawood essential oil according to claim 1, it is characterised in that：It is described Step 1: step
Rapid two and step 5 in water be pure water.
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