CN108342252B - Method for efficiently extracting agilawood essential oil - Google Patents
Method for efficiently extracting agilawood essential oil Download PDFInfo
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- CN108342252B CN108342252B CN201810053668.0A CN201810053668A CN108342252B CN 108342252 B CN108342252 B CN 108342252B CN 201810053668 A CN201810053668 A CN 201810053668A CN 108342252 B CN108342252 B CN 108342252B
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910021647 smectite Inorganic materials 0.000 claims abstract description 63
- 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 42
- 239000012065 filter cake Substances 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 77
- 238000003756 stirring Methods 0.000 claims description 58
- 239000003921 oil Substances 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 31
- 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 27
- 229910052708 sodium Inorganic materials 0.000 claims description 27
- 239000011734 sodium Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 18
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 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 6
- 229910000271 hectorite 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
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 4
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-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
- 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
- 239000008236 heating water Substances 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
- 238000000605 extraction Methods 0.000 abstract description 15
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 29
- 239000011229 interlayer Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 241001533085 Aquilaria sinensis Species 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 241000984061 Aquilaria Species 0.000 description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 3
- 229910052901 montmorillonite Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 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
- 239000002023 wood Substances 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 241000187479 Mycobacterium tuberculosis Species 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 241001534930 Thymelaeaceae Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 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
- 238000007654 immersion Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 208000003243 intestinal obstruction Diseases 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
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- 238000003815 supercritical carbon dioxide extraction 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
Abstract
The invention relates to the technical field of essential oil extraction, and particularly relates to a method for efficiently extracting agilawood essential oil. The method for efficiently extracting the agilawood essential oil comprises the following steps: step one, preparing rare earth modified nano organic smectite; step two, crushing and boiling the agilawood trees; step three, reacting the mother liquor with the rare earth modified nano organic smectite and collecting a filter cake; adding absolute ethyl alcohol into the filter cake and collecting mother liquor; and step five, preparing the high-purity agilawood essential oil. The method for efficiently extracting the agilawood essential oil has the advantages of simple and efficient extraction process, green and environment-friendly process, sustainable utilization and quite low production cost. And the purity of the obtained refined agilawood essential oil is as high as 95% or more (the purity of the agilawood essential oil can only approach 90% by adopting the existing extraction method), so the method for efficiently extracting the agilawood essential oil has strong practicability and extremely bright industrial prospect.
Description
Technical Field
The invention relates to the technical field of essential oil extraction, and particularly relates to a method for efficiently extracting agilawood essential oil.
Background
The aquilaria sinensis is a resin-containing wood (also known as 'native aquilaria sinensis', 'Aquilaria sinensis', 'Hainan aquilaria sinensis' and the like) of aquilaria plant belonging to Aquilaria of Thymelaeaceae, is the most expensive perfume in the world all the time, and is also an extremely rare traditional Chinese medicinal material in China. The agilawood has very strong unique fragrance, brings wonderful feelings of delightful feeling, comforting, soothing the nerves, beautifying and the like to people, and related researches prove that the agilawood has multiple medical functions of relieving pain, relieving spasm, relieving asthma, reducing blood pressure and the like, and is particularly widely used for treating cold stomachache, relieving senile intestinal obstruction, inhibiting the growth of mycobacterium tuberculosis and the like in clinic. Along with the successive implementation of agilawood forest resource protection in recent years by the leading country, the agilawood supply is not in demand in the international market, and the selling price is continuously increased. According to statistics, the price of the agilawood in the international market reaches 0.6-1 ten thousand dollars/kg, and the yield value of the agilawood exported only in three countries of Malaysia, Vietnam and Singapore in 2014 reaches more than 10 hundred million dollars.
The agilawood essential oil is the highest application form of all agilawood products, and is always the focus of research and development at home and abroad. However, the extraction difficulty of the agilawood essential oil is very high at present, the operation process is complex, the extraction rate is very low, and the industrialization and the large-scale application of the agilawood essential oil extraction are seriously hindered. Therefore, there is a great need to develop an environment-friendly, efficient, safe and sustainable extraction process of agilawood essential oil.
Disclosure of Invention
The invention aims to provide a method for efficiently extracting agilawood essential oil aiming at the defects of the prior art, and the method for efficiently extracting agilawood essential oil has the advantages of simple process, safety, environmental protection, sustainable utilization and low extraction cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for efficiently extracting the agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating water to a certain temperature, adding sodium-based smectite, stirring for a certain time at a certain rotating speed, adding a rare earth substance, continuing stirring for a certain time at a certain rotating speed, adding quaternary ammonium salt, stirring for a certain time at a certain rotating speed, filtering, fully washing with water, fully drying a filter cake at a certain temperature to constant weight, and thus obtaining the rare earth modified nano organic smectite;
step two, crushing the agilawood trees into powder, adding the powder into water, boiling, keeping for a certain boiling time, filtering, and collecting mother liquor;
step three, adding the rare earth modified nano organic smectite prepared in the step one into the mother liquor obtained in the step two, stirring for a certain time at a certain rotating speed, filtering and collecting a filter cake;
step four, adding absolute ethyl alcohol into the filter cake obtained in the step three, stirring for a certain time at a certain rotating speed, and then filtering and collecting mother liquor;
step five, adding water into the mother liquor obtained in the step four, stirring for a certain time at a certain rotating speed, standing for a certain time, removing the water phase at the lower layer and collecting the oil phase at the upper layer; then adding water into the oil phase, continuously stirring for a certain time at a certain rotating speed, standing for a certain time, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for several times, and collecting the oil phase as high-purity agilawood essential oil.
In the above technical scheme, in the first step, the sodium-based smectite is one or a combination of two of sodium-based smectite and hectorite according to any proportion.
In the above technical solution, in the step one, the rare earth material is Ce (NO)3)3、Ce2(SO4)3、CeCl3、Dy(NO3)3、Dy2(SO4)3、DyCl3、Sr(NO3)2、SrSO4Or SrCl2One or any two or more of the compositions according to any proportion.
In the above technical solution, in the first step, the quaternary ammonium salt is one or a combination of two or more of cetyltrimethyl ammonium bromide, cetyltrimethyl ammonium chloride, dodecyltrimethyl ammonium bromide or dodecyltrimethyl ammonium chloride in any proportion.
In the above technical scheme, in the first step, preparing rare earth modified nano organic smectite: heating 200-400 parts of water to 60-85 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 50-150 rpm for 30-60 min, adding 5-10 parts of rare earth substances, continuing to stir at the rotating speed of 50-150 rpm for 15-30 min, adding 20-50 parts of quaternary ammonium salt, stirring at the rotating speed of 150-300 rpm for 1-3 h, filtering, fully washing with water, and fully drying a filter cake at the temperature of 50-60 ℃ to constant weight to obtain the rare earth modified nano organic smectite.
In the technical scheme, in the second step, 100 parts of agilawood trees are crushed into powder with the granularity of 1-10 meshes, then the powder is added into 100-500 parts of water and boiled, the boiling time is kept for 6-10 hours, and then the mother liquor is filtered and collected.
In the technical scheme, in the third step, 20-50 parts of rare earth modified nano organic smectite prepared in the first step is added into 100 parts of mother liquor obtained in the second step, the mother liquor is stirred at the rotating speed of 150-300 rpm for 3-5 hours, and then the mother liquor is filtered and a filter cake is collected.
In the technical scheme, in the fourth step, 100-200 parts of absolute ethyl alcohol are added into 100 parts of the filter cake obtained in the third step, the mixture is stirred at the rotating speed of 150-300 rpm for 1-2 hours, and then the mother liquor is filtered and collected.
In the technical scheme, in the fifth step, 100-300 parts of water are added into the mother liquor obtained in the fourth step, the mother liquor is stirred for 15-20 min at a rotating speed of 50-150 rpm, and after standing for 30-60 min, the water phase at the lower layer is removed and the oil phase at the upper layer is collected; then adding 100-300 parts of water into the oil phase, continuously stirring at the rotating speed of 50-150 rpm for 15-20 min, standing for 30-60 min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the operation for 3-6 times, and finally collecting the oil phase which is the high-purity agilawood essential oil.
In the above technical scheme, the water in the first step, the second step and the fifth step is pure water.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method for efficiently extracting the agilawood essential oil, the rare earth modified nano organic smectite prepared in the step one can efficiently and selectively absorb the agilawood essential oil, wherein sodium-based smectite and hectorite contained in the sodium-based smectite have layered structures and have layered regions in certain spaces, and after the sodium-based smectite reacts with long-chain paraffin quaternary ammonium salts such as hexadecyl trimethyl ammonium bromide and the like, the quaternary ammonium salts enter the sodium-based smectite layers to form the organic smectite, and at the moment, the organic smectite does not have any selective absorption function on the agilawood essential oil. However, when Ce (NO) is added3)3When the rare earth material reacts with sodium-based smectite or organic smectite, Ce3+The rare earth ions enter the Si-O tetrahedral lattice of the sodium-based smectite or organic smectite. When dry, Ce3+the/Si-O octahedral lattice is distorted, and the interlayer region of the generated rare earth modified nano organic smectite can be highly selectively used for the agilawood essential oilAbsorbing while at the same time not absorbing any other liquid organic substances. Therefore, when the rare earth modified nano organic smectite is mixed with aquilaria sinensis water boiling liquid, the interlayer region of the rare earth modified nano organic smectite can slowly attract agilawood essential oil molecules to enter the interlayer. Then, absolute ethyl alcohol is added for immersion extraction. The absolute ethyl alcohol has small molecular volume and is not limited by the steric hindrance of an interlayer region, so that a large amount of the absolute ethyl alcohol enters the interlayer region and dissolves the agilawood essential oil. Continuously expanding agilawood essential oil molecules solvated by absolute ethyl alcohol until the limit of the interlayer region of the rare earth modified nano organic smectite is broken through (namely the interlayer region collapses and the laminated structure is completely peeled); at the moment, the peeled rare earth modified nano organic smectite and the agilawood essential oil are separated from each other, namely the agilawood essential oil is separated. Then, absolute ethyl alcohol molecules are removed by a water washing method, and the high-purity agilawood essential oil (the purity is as high as 95 percent or more) is prepared.
(2) The method for efficiently extracting the agilawood essential oil provided by the invention has the advantages of simple and efficient extraction process, green and environment-friendly process flow, sustainable utilization and quite low production cost. The extraction process is mainly used for extraction in an aqueous solution operation system, complicated organic solvent method multi-step extraction procedures are not needed, required production equipment is conventional equipment, expensive large-scale equipment such as supercritical carbon dioxide extraction and the like is not needed, the purity of the obtained refined agilawood essential oil is as high as 95% or more (the purity of the agilawood essential oil can only be close to 90% by adopting the existing extraction method), and therefore, the method for efficiently extracting the agilawood essential oil has strong practicability and has extremely bright industrial prospect.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1.
A method for efficiently extracting agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating 300 parts of water to 70 ℃, adding 100 parts of sodium-based smectite, stirring for 45min at the rotating speed of 100rpm, adding 7 parts of rare earth substances, continuing to stir for 20min at the rotating speed of 100rpm, adding 35 parts of quaternary ammonium salt, stirring for 1-3 h at the rotating speed of 200rpm, filtering, fully washing with water, and fully drying a filter cake at 55 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
in this embodiment, the sodium-based smectite is sodium-based montmorillonite;
in this example, the rare earth material is Ce (NO)3)3；
In this example, the quaternary ammonium salt is cetyltrimethylammonium bromide;
step two, crushing 100 parts of agilawood trees into powder with the granularity of 5 meshes, adding the powder into 300 parts of water, boiling for 8 hours, filtering and collecting mother liquor;
step three, adding 35 parts of rare earth modified nano organic smectite prepared in the step one into 100 parts of mother liquor obtained in the step two, stirring for 4 hours at the rotating speed of 200rpm, filtering and collecting a filter cake;
step four, adding 150 parts of absolute ethyl alcohol into 100 parts of the filter cake obtained in the step three, stirring at the rotating speed of 200rpm for 1.5 hours, and then filtering and collecting mother liquor;
step five, adding 200 parts of water into the mother liquor obtained in the step four, stirring for 18min at the rotating speed of 100rpm, standing for 45min, removing the water phase at the lower layer and collecting the oil phase at the upper layer; then adding 200 parts of water into the oil phase, continuously stirring at the rotating speed of 100rpm for 18min, standing for 45min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for 5 times, and collecting the oil phase as high-purity agilawood essential oil.
Wherein, the water in the first step, the second step and the fifth step is pure water.
Example 2.
A method for efficiently extracting agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating 200 parts of water to 60 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 50rpm for 60min, adding 5 parts of rare earth substances, continuing to stir at the rotating speed of 50rpm for 30min, adding 20 parts of quaternary ammonium salt, stirring at the rotating speed of 150rpm for 3h, filtering, fully washing with water, and fully drying a filter cake at 50 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
in this embodiment, the sodium-based smectite is hectorite;
in this example, the rare earth material is Ce2(SO4)3；
In this example, the quaternary ammonium salt is cetyltrimethylammonium chloride;
step two, crushing 100 parts of agilawood trees into powder with the granularity of 1 mesh, adding the powder into 100 parts of water, boiling for 6 hours, filtering and collecting mother liquor;
step three, adding 20 parts of rare earth modified nano organic smectite prepared in the step one into 100 parts of mother liquor obtained in the step two, stirring at the rotating speed of 150rpm for 5 hours, filtering and collecting a filter cake;
step four, adding 100 parts of absolute ethyl alcohol into 100 parts of the filter cake obtained in the step three, stirring for 2 hours at the rotating speed of 150rpm, and then filtering and collecting mother liquor;
step five, adding 100 parts of water into the mother liquor obtained in the step four, stirring at the rotating speed of 50rpm for 20min, standing for 30min, removing the water phase at the lower layer and collecting the oil phase at the upper layer; then adding 100 parts of water into the oil phase, continuously stirring at the rotating speed of 50rpm for 20min, standing for 30min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for 3 times, and collecting the oil phase as high-purity agilawood essential oil.
Wherein, the water in the first step, the second step and the fifth step is pure water.
Example 3.
A method for efficiently extracting agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating 400 parts of water to 85 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 150rpm for 30min, adding 10 parts of rare earth substances, continuing to stir at the rotating speed of 150rpm for 15min, adding 50 parts of quaternary ammonium salt, stirring at the rotating speed of 300rpm for 1h, filtering, fully washing with water, and fully drying a filter cake at 60 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
in the embodiment, the sodium-based smectite is a composition of sodium-based montmorillonite and hectorite according to any proportion;
in this example, the rare earth substance is CeCl3And Dy (NO)3)3The composition in any proportion;
in this example, the quaternary ammonium salt is dodecyl trimethyl ammonium bromide;
step two, crushing 100 parts of agilawood trees into powder with the granularity of 10 meshes, adding the powder into 500 parts of water, boiling for 10 hours, filtering and collecting mother liquor;
step three, adding 50 parts of rare earth modified nano organic smectite prepared in the step one into 100 parts of mother liquor obtained in the step two, stirring for 3 hours at the rotating speed of 300rpm, filtering and collecting a filter cake;
step four, adding 200 parts of absolute ethyl alcohol into 100 parts of the filter cake obtained in the step three, stirring at the rotating speed of 300rpm for 1 hour, and then filtering and collecting mother liquor;
step five, adding 300 parts of water into the mother liquor obtained in the step four, stirring for 15min at the rotating speed of 150rpm, standing for 60min, removing the lower-layer water phase and collecting the upper-layer oil phase; then adding 300 parts of water into the oil phase, continuously stirring at the rotating speed of 150rpm for 15min, standing for 60min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for 6 times, and collecting the oil phase as high-purity agilawood essential oil.
Wherein, the water in the first step, the second step and the fifth step is pure water.
Example 4.
A method for efficiently extracting agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating 250 parts of water to 65 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 80rpm for 50min, adding 6 parts of rare earth substances, continuing to stir at the rotating speed of 80rpm for 25min, adding 25 parts of quaternary ammonium salt, stirring at the rotating speed of 250rpm for 2.5h, filtering, fully washing with water, and fully drying a filter cake at 53 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
in this embodiment, the sodium-based smectite is sodium-based montmorillonite;
in this example, Dy is the rare earth element2(SO4)3、DyCl3And Sr (NO)3)2The composition in any proportion;
in the embodiment, the quaternary ammonium salt is the combination of dodecyl trimethyl ammonium bromide and dodecyl trimethyl ammonium chloride according to any proportion;
step two, crushing 100 parts of agilawood trees into powder with the granularity of 3 meshes, adding the powder into 200 parts of water, boiling for 7 hours, filtering and collecting mother liquor;
step three, adding 20-50 parts of rare earth modified nano organic smectite prepared in the step one into 100 parts of mother liquor obtained in the step two, stirring at the rotating speed of 180rpm for 4.5 hours, filtering and collecting a filter cake;
step four, adding 120 parts of absolute ethyl alcohol into 100 parts of the filter cake obtained in the step three, stirring at the rotating speed of 180rpm for 1.8h, and then filtering and collecting mother liquor;
step five, adding 150 parts of water into the mother liquor obtained in the step four, stirring for 18min at the rotating speed of 80rpm, standing for 50min, removing the lower-layer water phase and collecting the upper-layer oil phase; then adding 150 parts of water into the oil phase, continuously stirring at the rotating speed of 80rpm for 18min, standing for 50min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for 4 times, and collecting the oil phase as high-purity agilawood essential oil.
Wherein, the water in the first step, the second step and the fifth step is pure water.
Example 5.
A method for efficiently extracting agilawood essential oil comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating 350 parts of water to 75 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 120rpm for 35min, adding 9 parts of rare earth substances, continuing to stir at the rotating speed of 120rpm for 18min, adding 45 parts of quaternary ammonium salt, stirring at the rotating speed of 250rpm for 1.5h, filtering, fully washing with water, and fully drying a filter cake at 58 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
in this embodiment, the sodium-based smectite is hectorite;
in this embodiment, the rare earth material is SrSO4And SrCl2The composition in any proportion;
in the embodiment, the quaternary ammonium salt is the combination of hexadecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide and dodecyl trimethyl ammonium chloride according to any proportion;
step two, crushing 100 parts of agilawood trees into powder with the granularity of 8 meshes, adding the powder into 400 parts of water, boiling for 9 hours, filtering and collecting mother liquor;
step three, adding 20-50 parts of rare earth modified nano organic smectite prepared in the step one into 100 parts of mother liquor obtained in the step two, stirring at the rotating speed of 250rpm for 3.5 hours, filtering and collecting a filter cake;
step four, adding 180 parts of absolute ethyl alcohol into 100 parts of the filter cake obtained in the step three, stirring at the rotating speed of 250rpm for 1.2h, and then filtering and collecting mother liquor;
step five, adding 250 parts of water into the mother liquor obtained in the step four, stirring for 18min at the rotating speed of 120rpm, standing for 35min, removing the water phase at the lower layer and collecting the oil phase at the upper layer; then adding 250 parts of water into the oil phase, continuously stirring at the rotating speed of 120rpm for 18min, standing for 50min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the above operation for 5 times, and collecting the oil phase as high-purity agilawood essential oil.
Wherein, the water in the first step, the second step and the fifth step is pure water.
Experiment:
various comparative tests were carried out on the high-purity agilawood essential oils a to D extracted in the above examples 1 to 4 and the commercially available products (model: GL-T, first-grade agilawood essential oil, manufactured by national aquilaria wood biotechnology limited, zhongshan city), and the results are shown in table 1 below.
Table 1 agilawood essential oil product comparative test results
As can be seen from table 1, the agilawood essential oil extracted by the method has excellent performance indexes such as purity, color degree and storage stability, and is obviously better than the existing products on the market. Therefore, the preparation process has bright industrial prospect and can create huge economic benefit.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. The method for efficiently extracting the agilawood essential oil is characterized by comprising the following steps of: it comprises the following steps:
step one, preparing rare earth modified nano organic smectite: heating water to 60-85 ℃, adding sodium-based smectite, stirring at the rotating speed of 50-150 rpm for 30-60 min, adding rare earth substances, continuing to stir at the rotating speed of 50-150 rpm for 15-30 min, adding quaternary ammonium salt, stirring at the rotating speed of 150-300 rpm for 1-3 h, filtering, fully washing with water, and fully drying a filter cake at 50-60 ℃ to constant weight to obtain the rare earth modified nano organic smectite;
step two, crushing the agilawood trees into powder, adding the powder into water, boiling for 6-10 hours, filtering, and collecting mother liquor;
step three, adding the rare earth modified nano organic smectite prepared in the step one into the mother liquor obtained in the step two, stirring for 3-5 hours at the rotating speed of 150-300 rpm, filtering and collecting a filter cake;
step four, adding absolute ethyl alcohol into the filter cake obtained in the step three, stirring at the rotating speed of 150-300 rpm for 1-2 hours, filtering and collecting mother liquor;
step five, adding water into the mother liquor obtained in the step four, stirring for 15-20 min at a rotating speed of 50-150 rpm, standing for 30-60 min, removing the water phase at the lower layer and collecting the oil phase at the upper layer; adding water into the oil phase, continuously stirring at the rotating speed of 50-150 rpm for 15-20 min, standing for 30-60 min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the operation for 3-6 times, and finally collecting the oil phase which is the high-purity agilawood essential oil.
2. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the first step, the sodium-based smectite is one or a composition of two of sodium-based smectite and hectorite according to any proportion.
3. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the first step, the rare earth substance is Ce (NO)3)3、Ce2(SO4)3、CeCl3、Dy(NO3)3、Dy2(SO4)3、DyCl3、Sr(NO3)2、SrSO4Or SrCl2One or any two or more of the compositions according to any proportion.
4. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the first step, the quaternary ammonium salt is one or a combination of more than two of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide or dodecyl trimethyl ammonium chloride according to any proportion.
5. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the first step, preparing rare earth modified nano organic smectite: heating 200-400 parts of water to 60-85 ℃, adding 100 parts of sodium-based smectite, stirring at the rotating speed of 50-150 rpm for 30-60 min, adding 5-10 parts of rare earth substances, continuing to stir at the rotating speed of 50-150 rpm for 15-30 min, adding 20-50 parts of quaternary ammonium salt, stirring at the rotating speed of 150-300 rpm for 1-3 h, filtering, fully washing with water, and fully drying a filter cake at the temperature of 50-60 ℃ to constant weight to obtain the rare earth modified nano organic smectite.
6. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the second step, 100 parts of agilawood trees are crushed into powder with the granularity of 1-10 meshes, then the powder is added into 100-500 parts of water and boiled, the boiling time is kept for 6-10 hours, and then the mother liquor is filtered and collected.
7. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: and in the third step, adding 20-50 parts of rare earth modified nano organic smectite prepared in the first step into 100 parts of the mother liquor obtained in the second step, stirring at the rotating speed of 150-300 rpm for 3-5 hours, filtering and collecting a filter cake.
8. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: in the fourth step, 100-200 parts of absolute ethyl alcohol is added into 100 parts of the filter cake obtained in the third step, the mixture is stirred for 1-2 hours at the rotating speed of 150-300 rpm, and then the mother liquor is filtered and collected.
9. The method for efficiently extracting agilawood essential oil according to claim 8, characterized by comprising the following steps: in the fifth step, 100-300 parts of water is added into the mother liquor obtained in the fourth step, the mother liquor is stirred for 15-20 min at a rotating speed of 50-150 rpm, and after standing for 30-60 min, the water phase at the lower layer is removed and the oil phase at the upper layer is collected; then adding 100-300 parts of water into the oil phase, continuously stirring at the rotating speed of 50-150 rpm for 15-20 min, standing for 30-60 min, removing the lower-layer water phase and collecting the upper-layer oil phase; repeating the operation for 3-6 times, and finally collecting the oil phase which is the high-purity agilawood essential oil.
10. The method for efficiently extracting agilawood essential oil according to claim 1, which is characterized in that: and water in the first step, the second step and the fifth step is pure water.
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