CN111135795A - Preparation method and application of adsorption material for gardenia essential oil head fragrance extraction - Google Patents
Preparation method and application of adsorption material for gardenia essential oil head fragrance extraction Download PDFInfo
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Abstract
The invention provides a preparation method and application of a high-efficiency adsorption material for extracting gardenia essential oil top note, wherein the preparation method comprises the following steps: putting lignin, montmorillonite and deionized water into a reaction kettle, adding 0.1mol/L dilute acid, stirring and reacting at 80-250 ℃, separating after full reaction, and washing to obtain the biochar and clay composite material. And roasting the biochar and montmorillonite composite material for 1-10 hours at the temperature of 250-700 ℃ under the protection of nitrogen to obtain the lignin biochar and montmorillonite composite material.
Description
Technical Field
The invention relates to the technical field of gardenia essential oil extraction, and particularly relates to a manufacturing method and application of a high-efficiency adsorption material for extracting the fragrance of gardenia essential oil.
Background
Gardenia jasminoides is known as Gardenia jasminoides, Gardenia jasminoides Ellis and Gardenia jasminoides Ellis belonging to Rubiaceae of the order Longdaniales. Belongs to the family of Rubiaceae and is evergreen shrub with luxuriant branches and leaves, evergreen leaves and fragrant flowers. The Chinese herbal medicine can be planted in most areas, the flowering period is generally 5-7 months, the Chinese herbal medicine is also named as sparrow tongue flower, wild sweet osmanthus flower, yellow gardenia and the like, and one of the eight Chinese herbal medicine fragrant flowers is cold in nature and sweet and bitter in taste and can clear lung heat, relieve cough, cool blood and stop bleeding. The flowers have different sizes and colors, and the small flowers have heavier fresh fragrance compared with the large flowers, better white flower fragrance, fresh fruit fragrance and sweet and fresh fragrance.
At present, gardenia is used for aromatizing products which are industrially processed, mainly extractum or absolute oil, and the products are mostly used in high-grade perfume, perfumed soap and cosmetic essence. In recent years, with the gradual rise of the domestic aromatherapy industry, the extractum and the absolute oil cannot be used for human bodies due to the organic solvent, so that the application of the traditional gardenia fragrant product form has certain limitation.
Steam distillation is one of the most commonly used techniques in the production of natural botanical flavors. The method has the advantages of simple equipment, easy operation, low cost, high yield and the like. Except for plant materials whose main fragrance components are easily dissolved, hydrolyzed or decomposed in boiling water, most of aromatic plants can be used for producing essential oil by steam distillation. However, the conventional distillation of the spice plants, especially flowers, has problems of serious loss of top note, residual cooking gas and the like, and finally results in that the extracted fragrance is far from the natural fragrance and the fragrance of the natural flowers does not exist. Therefore, how to extract the top note of the essential oil is important in order to keep the natural fragrance of the essential oil from disappearing.
Montmorillonite (MMT) is an aqueous aluminosilicate clay having a unique layered structure, and the main components of montmorillonite are: SiO2, Al2O3, MgO, CaO, Na2O, Fe2O3, FeO, K2O, TiO2 and H2O, belonging to 2:1 type three-layer mineral clay. The unit cell of montmorillonite contains two layers of silicon-oxygen tetrahedron and one layer of aluminum-oxygen octahedron, wherein the silicon-oxygen tetrahedron sheet is formed by sharing three oxygen atoms in the same plane with adjacent silicon-oxygen tetrahedron provided by three vertexes of silicon-oxygen tetrahedron; the aluminum (magnesium) oxygen (oxyhydrogen) octahedron sheet is a hexa-coordinated aluminum (magnesium) oxygen (hydroxyl) octahedron formed by oxygen atoms provided by four vertexes of silicon-oxygen tetrahedron opposite to each other and oxygen atoms provided by two hydroxyl groups in the same plane, and takes metal aluminum (magnesium) as a center, the tetrahedron and the octahedron are connected through shared oxygen atoms, and unit cells are stacked in parallel. In the structure of montmorillonite, Al3+ and Si4+ are easily replaced by other low-valence ions, so that the crystal layer is negatively charged and the charge balance is maintained by the action of interlayer isoelectric cations. The middle of the sheet is filled with free water molecules and exchangeable cations, as well as some soluble species, in order to balance the charge. The montmorillonite is a unique layered structure, so that the montmorillonite has good adsorption performance, expansibility and ion exchange performance.
Research shows that the activated carbon, the molecular sieve, the resin and the like can be used for adsorbing gardenia head fragrance (which balance, aged rock ice, Yanjiaying, Wanjia. supercritical CO2 extracts gardenia head fragrance oil and analytical application thereof [ J ]. fragrance and essence cosmetics, 2011, 1: 17-20; sympodial, kaempfery, Liuyi. resin adsorption method extracts gardenia flower oil and component analytical research thereof [ J ]. fragrance and essence cosmetics, 2018, 3: 11-13). In recent years, bio-porous carbon materials have been widely used in the field of adsorption (Yener J, Kopac T, dog G, dynamic analysis of reflection of methyl Blue on granular and powdered activated carbon [ J ]. Chemical Engineering Journal,2008,144(3): 400-) -406; Albadarin A B, Collins M N, Mu N. activated carbon-ceramic expanded radiation for adsorption of methyl Blue [ J ]. Chemical Engineering Journal,2016,307: 264-. Recently, it has been shown that cellulose biochar, montmorillonite composite material for methylene blue and the like show good adsorption performance (Dong Shen Tong, Cheng Wen Wu, Moses O. Adebajo, Gui Chen Jin, Wei Hua Yu, Sheng Fu Ji, Chun Hui Zhou. adsorption of methyl blue from aqueous solution on to porous cellulose derivative carbon, mineral carbon and minerals adsorption [ J ] Applied Clay Science,2018,161: 256. 264; arianlong, Zhang, Liping. activated carbon coated palladium synthesis reaction and adsorption of carbon adsorption for methyl J [ J ] blue of Journal of 33. Journal of molecular synthesis of Journal of 33. the present invention is a new research. The lignin portion of biomass is an amorphous aromatic polymer widely present in plants whose molecular structure is composed of structural units of oxyphenbutamol or its derivatives, such as coniferyl alcohol, sinapyl alcohol and coumaryl alcohol. The lignin molecular formula can be expressed as (C6H10O2) n, and the chemical composition of the lignin shows that the lignin contains carbon (60% -66%) and low hydrogen (5% -5.5%). With the research and utilization of renewable resources, people have increasingly studied lignin. According to the research, in order to improve the adsorption performance of materials such as activated carbon and the like, the lignin biochar and montmorillonite composite adsorption material is prepared and applied to the extraction of gardenia essential oil, and the application of the materials in the field of gardenia essential oil extraction is rarely reported.
Disclosure of Invention
Aiming at the problems pointed out in the background technology, the invention provides a preparation method and application of a high-efficiency adsorption material for extracting the gardenia essential oil head fragrance; the invention provides a lignin-based biochar and montmorillonite composite adsorbing material with a porous structure characteristic and application of the lignin-based biochar and montmorillonite composite adsorbing material to adsorption and extraction of gardenia headings.
The technical scheme of the invention is realized as follows:
a preparation method of a high-efficiency adsorption material for extracting gardenia essential oil head fragrance is prepared by the following steps: putting lignin, montmorillonite and deionized water into a reaction kettle, adding 0.1mol/L dilute acid, stirring and reacting at 80-250 ℃, separating after full reaction, and washing to obtain the biochar and clay composite material. And roasting the biochar and montmorillonite composite material for 1-10 hours at the temperature of 250-700 ℃ under the protection of nitrogen to obtain the lignin biochar and montmorillonite composite material.
The invention is further set that the dilute acid is obtained by modifying sulfuric acid, phosphoric acid, hydrochloric acid, p-toluenesulfonic acid or nitric acid.
The invention is further set that the dosage of the distilled water is 10-100ml/g by the mass of the bentonite.
The invention is further provided that in the dilute acid solution, the mass percentage of the acid is preferably 0.5-5%, and the volume dosage of the acid solution is preferably 1-3mL/g calculated by the mass of the bentonite.
The invention is further set that the mass ratio of the lignin, the montmorillonite and the deionized water is 0.1-10: 1: 1-20, preferably 1-3:1: 10-20.
The invention is further provided that the reaction time is 2 to 8 hours, preferably 4 hours.
The invention is further provided that the temperature of the hydrothermal carbonization reaction is 170-230 ℃, and preferably 200 ℃.
The invention is further provided that the roasting carbonization reaction temperature is 500 ℃ at 300-.
An application of high-efficiency adsorption material for extracting the head fragrance of gardenia essential oil is to deoxidize the biological carbon and montmorillonite composite material for 2-10 hours under 0.01 MPa. And then transferring the biochar and montmorillonite composite material into a drying oven with a certain amount of fresh gardenia, enabling the mass ratio of the biochar and montmorillonite composite material to the gardenia to be 0.5-2, sealing, adsorbing at room temperature for 5-20 hours, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain an eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drop, thus obtaining the gardenia flower head essential oil.
The obtained essential oil was analyzed by GC-MS. GC conditions were as follows: a chromatographic column: HP-5(30 m.times.0.25 mm.times.0.25 μm); starting the column temperature at 90 ℃, keeping for 1min, heating to 130 ℃ at 10 ℃/min, keeping for 10min, heating to 250 ℃ at 5 ℃/min, keeping for 10min, heating to 280 ℃ at 10 ℃/min, keeping for 10 min; sample inlet temperature: 250 ℃; carrier gas: high purity helium gas; flow rate of carrier gas: 1.2 mL/min; sample introduction amount: 1 μ L (gardenia oil diluted with n-hexane); the split ratio is 50: 1.
MS conditions: an ion source: an EI source; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; solvent delay time: 4.0 min; the mass scanning range m/z is 35-500.
Compared with the prior art, the invention has the beneficial effects that:
(1) the biological carbon and montmorillonite composite material has the characteristic of mesoporous structure.
(2) The preparation method of the biochar and montmorillonite composite material is simple and has low cost.
(3) The composite material has excellent gardenia head fragrance adsorption performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1: XRD patterns of the biochar and montmorillonite composite material (b) prepared from pure montmorillonite (a) (Zhejiang Renzhen science and technology, Inc.) and example 2 (b);
FIG. 2: BET results for biochar, montmorillonite composite (b) prepared from pure montmorillonite (a) and example 2 (b);
FIG. 3: GC-MS analysis results of gardenia fragrance adsorbed by the biochar and montmorillonite composite material prepared by the activated carbon (a) (science and technology limited in Zhikang carbon of Jiangsu) and the example 2 (b);
FIG. 4: examples 1-6 yield of gardenia fragrance adsorbed by biochar, montmorillonite composite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention is described below with reference to fig. 1-4:
example 1
Weighing 3g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 30g of the biochar and montmorillonite composite material are weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The amount of adsorption of essential oil by the composite is shown in fig. 4.
Example 2
Weighing 3g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 50g of the biochar and montmorillonite composite material are weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The XRD and BET results of the material are shown in fig. 1 and 2. The results of GC-MS for adsorbing essential oils and the amounts of adsorbed essential oils are shown in FIGS. 3 and 4.
Example 3
Weighing 3g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 70g of the biochar and montmorillonite composite material are weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The amount of adsorption of essential oil by the composite is shown in fig. 4.
Example 4
Weighing 3g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 90g of the biochar and montmorillonite composite material is weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The amount of adsorption of essential oil by the composite is shown in fig. 4.
Example 5
Weighing 5g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 50g of the biochar and montmorillonite composite material are weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The amount of adsorption of essential oil by the composite is shown in fig. 4.
Example 6
Weighing 10g of lignin, 5g of montmorillonite and 7ml of deionized water, placing the materials in a reaction kettle, adding 0.1mol/L H3PO43ml, stirring the materials at 200 ℃ for reaction, separating the materials after full reaction, and washing the materials with water to obtain the biochar/clay composite material. Roasting the biochar and montmorillonite composite material for 3 hours at 400 ℃ under the protection of nitrogen atmosphere to obtain the lignin biochar and montmorillonite composite material.
Before use, 50g of the biochar and montmorillonite composite material are weighed and desorbed for 3 hours under 0.01 MPa. Then the biochar and montmorillonite composite material is transferred into an oven with 50g of fresh gardenia. After sealing, the mixture was adsorbed at room temperature for 10 hours. And then, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drip off to obtain the gardenia flower head essential oil. The amount of adsorption of essential oil by the composite is shown in fig. 4.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a high-efficiency adsorption material for extracting gardenia essential oil head fragrance is prepared by the following steps: putting lignin, montmorillonite and deionized water into a reaction kettle, adding 0.1mol/L dilute acid, stirring and reacting at 80-250 ℃, separating after full reaction, and washing to obtain the biochar and clay composite material. And roasting the biochar and montmorillonite composite material for 1-10 hours at the temperature of 250-700 ℃ under the protection of nitrogen to obtain the lignin biochar and montmorillonite composite material.
2. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the dilute acid is obtained by modifying sulfuric acid, phosphoric acid, hydrochloric acid, p-toluenesulfonic acid or nitric acid.
3. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the dosage of the distilled water is 10-100ml/g based on the mass of the bentonite.
4. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: in the dilute acid solution, the mass percentage of the acid is preferably 0.5-5%, and the volume consumption of the acid solution is preferably 1-3mL/g calculated by the mass of the bentonite.
5. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the mass ratio of the lignin to the montmorillonite to the deionized water is 0.1-10: 1: 1-20, preferably 1-3:1: 10-20.
6. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the reaction time is 2 to 8 hours, preferably 4 hours.
7. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the temperature of the hydrothermal carbonization reaction is 170-230 ℃, and preferably 200 ℃.
8. The method for preparing the efficient adsorbing material for extracting the gardenia essential oil head fragrance according to claim 1, which is characterized by comprising the following steps of: the roasting carbonization reaction temperature is 300-500 ℃, and preferably 350-450 ℃.
9. The application of the efficient adsorption material for extracting the gardenia essential oil head fragrance is characterized in that: deoxidizing the composite material of biochar and montmorillonite for 2-10 hours under 0.01 MPa. And then transferring the biochar and montmorillonite composite material into a drying oven with a certain amount of fresh gardenia, enabling the mass ratio of the biochar and montmorillonite composite material to the gardenia to be 0.5-2, sealing, adsorbing at room temperature for 5-20 hours, eluting the adsorbed biochar and montmorillonite composite material by using absolute ethyl alcohol and n-hexane to obtain an eluent, and evaporating the eluent by using a rotary evaporator until no liquid drops drop, thus obtaining the gardenia flower head essential oil.
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| CN112892482A (en) * | 2021-01-26 | 2021-06-04 | 中国热带农业科学院海口实验站 | Preparation method of halloysite-biochar composite material |
| CN118059005A (en) * | 2024-04-22 | 2024-05-24 | 广州巴宝莉化妆品有限公司 | Method for keeping fragrance of fresh flower fragrance extract |
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