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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- CN111135795A CN111135795A CN202010072521.3A CN202010072521A CN111135795A CN 111135795 A CN111135795 A CN 111135795A CN 202010072521 A CN202010072521 A CN 202010072521A CN 111135795 A CN111135795 A CN 111135795A
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 239000000341 volatile oil Substances 0.000 title claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000003205 fragrance Substances 0.000 title claims description 31
- 240000001972 Gardenia jasminoides Species 0.000 title abstract description 6
- 238000000605 extraction Methods 0.000 title description 6
- 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 claims abstract description 74
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 74
- 239000002131 composite material Substances 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 229920005610 lignin Polymers 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004927 clay Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 241000157835 Gardenia Species 0.000 claims description 46
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003480 eluent Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
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- 238000001704 evaporation Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
- 229910001868 water Inorganic materials 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 235000018958 Gardenia augusta Nutrition 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002537 cosmetic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
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- 241000411851 herbal medicine Species 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 241001107098 Rubiaceae Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- -1 aluminum (magnesium) oxygen Chemical compound 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- JMFRWRFFLBVWSI-NSCUHMNNSA-N coniferol Chemical compound COC1=CC(\C=C\CO)=CC=C1O JMFRWRFFLBVWSI-NSCUHMNNSA-N 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LZFOPEXOUVTGJS-ONEGZZNKSA-N trans-sinapyl alcohol Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O LZFOPEXOUVTGJS-ONEGZZNKSA-N 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 244000242564 Osmanthus fragrans Species 0.000 description 1
- 235000019083 Osmanthus fragrans Nutrition 0.000 description 1
- 241000287127 Passeridae Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000222 aromatherapy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- LZFOPEXOUVTGJS-UHFFFAOYSA-N cis-sinapyl alcohol Natural products COC1=CC(C=CCO)=CC(OC)=C1O LZFOPEXOUVTGJS-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229940119526 coniferyl alcohol Drugs 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- NOTVAPJNGZMVSD-UHFFFAOYSA-N potassium monoxide Inorganic materials [K]O[K] NOTVAPJNGZMVSD-UHFFFAOYSA-N 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- Inorganic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
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- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Cosmetics (AREA)
- Fats And Perfumes (AREA)
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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