CN104830528B - A kind of preparation method and application method of agalloch eaglewood fragrance - Google Patents

A kind of preparation method and application method of agalloch eaglewood fragrance Download PDF

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Publication number
CN104830528B
CN104830528B CN201510196176.3A CN201510196176A CN104830528B CN 104830528 B CN104830528 B CN 104830528B CN 201510196176 A CN201510196176 A CN 201510196176A CN 104830528 B CN104830528 B CN 104830528B
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agalloch eaglewood
fragrance
glass container
preparation
sawdust
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CN104830528A (en
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吴新星
余汉谋
姜兴涛
李剑政
肖海鸿
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Botton Spices Co ltd
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Dongguan Bowden Spices Co Ltd
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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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Seasonings (AREA)
  • Cosmetics (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present invention relates to fragrance technical fields, and in particular to a kind of preparation method and application method of agalloch eaglewood fragrance, its preparation method are：Agalloch eaglewood sawdust is positioned in the glass container of a upper end opening, adds in stainless steel Dixon ring filler；The external condensation reflux unit in glass container upper end；To being mounted with the glass container bottom-heated of agalloch eaglewood sawdust, the aromatic compound distilled is collected using the external condensation reflux unit in glass container upper end；Obtained aromatic compound addition absolute ethyl alcohol dissolving will be collected, after freezing processing, filtering is concentrated under reduced pressure, obtains a kind of agalloch eaglewood fragrance dissolved matter.Obtained fragrance is consistent with the fragrance of agalloch eaglewood champignon, and preparation method is easily operated, and productivity is high, is suitable for industrialized production, is a kind of more economic and practical agalloch eaglewood fragrance, can be applied to daily use chemicals blending and champignon field.Agalloch eaglewood fragrance obtained can be positioned over interior, be evaporated by means such as ultrasonic atomizations, it is calm so as to achieve the effect that calm the nerves.

Description

A kind of preparation method and application method of agalloch eaglewood fragrance
Technical field
The present invention relates to fragrance technical field more particularly to a kind of preparation methods and application method of agalloch eaglewood fragrance.
Background technology
Agalloch eaglewood is the resiniferous timber of Thymelaeceae eaglewood suspension culture of Aquilaria sinensis Aquilaria sinensis, is《Middle traditional Chinese medicines Allusion quotation》The kind recorded is clinically common qi-regulating drug.Agalloch eaglewood is a kind of traditional rare medicinal herbs and natural perfume material, has drop Gas, middle benefit gas, the function that warm kidney is supporing yang.Cure mainly the swollen bored pain of chest and abdomen, gastrofrigid vomiting hiccup, the asthma of the kidney deficiency circulation of vital energy in the wrong direction suddenly.Agalloch eaglewood is containing volatilization The amount of oil is higher, has strong fragrance, is the main component of agalloch eaglewood volatility drug effect, the amount containing volatile oil is directly and medicinal material Quality it is related.
The preparation method of agalloch eaglewood fragrance includes steam distillation, supercritical fluid extraction, solvent extraction, Asia at present Critical extraction etc., but these methods the agalloch eaglewood fragrance prepared and fragrance difference that agalloch eaglewood champignon generates are very big.And it directly fires It burns agalloch eaglewood and generates open fire, easily trigger security incident.How to prepare the agalloch eaglewood fragrance consistent with fragrance during agalloch eaglewood champignon is this hair Bright central point.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method and application method of agalloch eaglewood fragrance, have Preparation method is simple, is conducive to industrialized production, and the fragrance fragrance of preparation is pure.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of agalloch eaglewood fragrance, comprises the following steps：
A. agalloch eaglewood sawdust and stainless steel Dixon ring filler are mixed, are positioned in the glass container of a upper end opening；
B. the external condensation reflux unit in glass container upper end；
C. to being mounted with the glass container bottom-heated of agalloch eaglewood sawdust, the external condensing reflux in glass container upper end is utilized The aromatic compound that device collection distills；
D. obtained aromatic compound addition absolute ethyl alcohol dissolving being collected, dissolved matter is after freezing processing, filtering, It is concentrated under reduced pressure, obtains a kind of agalloch eaglewood fragrance.
Preferably, agalloch eaglewood sawdust granularity described in step a is 3~8mm.Agalloch eaglewood sawdust granularity should not be too large, agalloch eaglewood sawdust heap Product granularity is too big, is unfavorable for agalloch eaglewood and carries out aerobic cracking, generate aromatic compound, adds in stainless steel Dixon ring filler, can be into one Step ensures the gap between agalloch eaglewood sawdust, so as to promote aerobic cracking, while also ensures the thermally equivalent of agalloch eaglewood sawdust, avoids coke Change.
Preferably, stainless steel Dixon ring filler additive amount described in step a is 2~5 times of agalloch eaglewood sawdust weight, and is loaded Total height is no more than 2/5ths of glass container.Stainless steel Dixon ring filler is also known as Dixon（Dixon）Filler is a kind of small High efficiency particulate filler, is made of woven wire, and the diameter of filler is equal with height.Due to the capillarity of woven wire, liquid It can disperse film forming well, two carry out abundant mass transfer, heat transfer beneficial to gas-liquid, can substantially eliminate the wild effects such as channel.
Preferably, mode of heating described in step c is common electrical heating or microwave heating, and the rate of heat addition is 5 DEG C/min, is added During heat to predetermined temperature, 20~40min is kept.Slow heating is conducive to the progressively aerobic cracking of agalloch eaglewood sawdust.
Preferably, the maximum temperature of the predetermined temperature is 250 DEG C~280 DEG C.Distillation collects target at a temperature of this Substance is distilled, and ensure that agalloch eaglewood sawdust does not generate pyrogenetic reaction, influences the quality of final fragrance.
Preferably, absolute ethyl alcohol amount is added in described in step d to collect 3~5 times of obtained aromatic compound weight.Such as This, it is ensured that aromatic compound is completely dissolved in absolute ethyl alcohol, and has enough amount of solution Xun Huan distillations, is ensureing to obtain target While distilling substance, yield is improved.
Preferably, the freezing processing time described in step d is for 24 hours~36h.After freezing processing, filtering removal aromatization The insoluble wax and impurity component in object are closed, ensure that the fragrance component of final fragrance product.
Preferably, the temperature being concentrated under reduced pressure described in step d is 45 DEG C~55 DEG C, and pressure is -0.08~-0.09MPa.
Preferably, the glass container is glass round bottom container.Glass round bottom container is heated evenly when heating, heating surface area Greatly, convenient for the reflux and volatilization of steam, be conducive to improve production efficiency.
A kind of application method of above-mentioned agalloch eaglewood fragrance is：The agalloch eaglewood fragrance being prepared is placed in ultrasonic ultrasonic delay line memory and is led to It crosses steaming mode to evaporate, ultrasonic frequency is 1.7MHz ± 0.17MHz.The fragrance that need not burn generates champignon, avoids bright The possibility of fire safety accident.
The beneficial effects of the present invention are：Agalloch eaglewood fragrance prepared by the present invention is consistent with the fragrance of agalloch eaglewood champignon, and makes Preparation Method is easily operated, and productivity is high, is suitable for industrialized production, is a kind of more economic and practical agalloch eaglewood fragrance, can apply In daily use chemicals blending and champignon field.Agalloch eaglewood fragrance obtained is positioned over interior, is evaporated by means such as ultrasonic atomizations, It is calm so as to achieve the effect that calm the nerves.
Description of the drawings
Invention is described further using attached drawing, but the embodiment in attached drawing does not form any limitation of the invention, For those of ordinary skill in the art, without creative efforts, can also it be obtained according to the following drawings Its attached drawing.
Fig. 1 is the gas chromatogram of agalloch eaglewood fragrance produced by the present invention.
Specific embodiment
Embodiment 1
A kind of preparation method of agalloch eaglewood fragrance of the present embodiment, comprises the following steps：
A. 100g eaglewood powders are broken to the agalloch eaglewood sawdust that granularity is 5mm, mix, put with 200g stainless steel Dixon ring fillers It is placed in the glass round bottom container of a upper end opening；
B. the external condensation reflux unit in glass container upper end；
C. the glass round bottom container bottom for being mounted with agalloch eaglewood sawdust is heated, is heated with the speed of 5 DEG C/min, work as heating When temperature reaches 250 DEG C, 30min is kept, is distilled using the external condensation reflux unit collection of glass round bottom container upper end Aromatic compound, 0.85g；
D. obtained aromatic compound addition 3.4g absolute ethyl alcohol dissolvings being collected, dissolved matter passes through freezing processing 36h, Filtering, at 50 DEG C, is concentrated under reduced pressure under the conditions of -0.09MPa, obtains 0.6g oily agalloch eaglewood fragrance.
Yield=0.6g/100g × 100%=6 ‰ of agalloch eaglewood fragrance.
Embodiment 2-4
The preparation process of embodiment 2-4 is same as Example 1, and preparation parameter is as shown in table 1.
Table 1
The agalloch eaglewood fragrance obtained by embodiment 1 to 4 is placed in ultrasonic ultrasonic delay line memory respectively and is volatilized by steaming mode Come, ultrasonic frequency is 1.7MHz ± 0.17MHz.The fragrance distributed is consistent with the fragrance of agalloch eaglewood champignon, and it is calm to play tranquilizing the mind Effect, and need not burn fragrance generate champignon, it is safe to use.
The volatile and semi-volatile compounds of obtained agalloch eaglewood fragrance are detected by gas chromatography-mass spectrum, The chemical composition and mass fractions relative identified are as shown in table 2, and gas chromatogram is as shown in Figure 1.GC conditions：Chromatography Column：Agilent 19091S-105（50.0m×0.2mm×0.33μm）；Temperature programming：50 DEG C of initial temperature, 2 DEG C/min programs 150 DEG C are warming up to, 4 DEG C/min temperature programmings retain 10min to 270 DEG C；Injector temperature：250℃；Carrier gas is helium（Quality Component）；Carrier gas flux：Constant 1.0mL/min；Split ratio：40:1, sample size：0.6uL；Using area normalization standard measure.
Table 2
No. Retention time/min Compound Mass fractions relative/%
1 3.570 Formic acid 0.591
2 4.105 Acetic acid 4.285
3 4.220 Propionic acid 0.360
4 4.701 Hydroxypropanone- 0.163
5 4.932 Acrylic acid 0.194
6 5.272 Hydroxy methyl acetate 0.101
7 5.816 Pyridine 0.128
8 6.446 Acetamide 0.280
9 6.541 Diacetamide 0.472
10 7.916 2- butenoic acids 0.191
11 9.055 Furfural 0.265
12 9.669 3-methyl-3-butenoic acid 0.225
13 9.832 Furfuryl alcohol 0.088
14 10.302 3- methyl-2-butenoic acids 0.259
15 10.512 Lactic acid 0.259
16 10.901 2- methyl-2-butenoic acids 0.025
17 11.059 Butyl cellosolve 0.086
18 11.525 2 (5H)-furanones 0.831
19 11.820 3- hydracrylic acids 0.261
20 11.982 2- hydroxyl -2- cyclopentene-1-ones 0.217
21 12.966 β-angelica lactone 0.105
22 13.790 5 methyl furfural 0.015
23 14.819 Phenol 0.175
24 15.124 3- furancarboxylic acids 0.300
25 15.536 2- hydroxy-gamma-butyrolactones 0.346
26 16.028 3-Methoxy Pyridine 0.078
27 16.576 N- formylpyrroles 0.054
28 16.709 Methyl cyclopentenyl ketone 1.007
29 16.967 4- methyl -2 (5H) furanone 0.110
30 17.557 Benzyl alcohol 0.119
31 17.769 Levulic acid 0.227
32 20.127 Furanone 0.329
33 20.416 Methylfuroate 0.065
34 20.966 Furancarboxylic acid 1.225
35 21.240 Guaiacol 0.177
36 22.844 Maltol 0.860
37 23.105 3- pyridones 0.550
38 24.176 Benzoic acid 1.228
39 24.824 It is hydrated maltol 0.249
40 25.393 Single-ethyl succinate 0.172
41 27.504 Hydroxyl maltol 0.482
42 28.055 Catechol 0.577
43 28.470 To methyl guaiacol and 4 0.128
44 29.918 P methoxy phenol 0.407
45 30.619 5 hydroxymethyl furfural 4.240
46 30.835 Phenylacetic acid 0.404
47 31.686 Glucopyranose acetic acid esters 3.918
48 31.909 Anisic aldehyde 0.761
49 32.425 3- methoxyl group catechols 0.368
50 33.057 Anisyl alcohol 0.049
51 33.456 2- acetyl group hydroquinones 0.109
52 33.935 Hydroquinone 0.526
53 35.308 Salicylaldhyde 0.100
54 35.475 5 hydroxymethyl furfural acetic acid esters 0.520
55 36.024 To vinyl guaiacol 0.100
56 37.102 Phthalic anhydride 0.050
57 37.465 Benzenpropanoic acid 2.442
58 38.067 2,6- syringol 2.378
59 38.422 Acetanisole 0.095
60 38.597 Isoeugenol 0.091
61 39.194 Parahydroxyben-zaldehyde 0.728
62 41.187 Ortho-methylthio phenol 0.839
63 41.798 Cinnamic acid 0.088
64 42.428 Anisic acid 0.698
65 43.828 Different vanillic acid 1.134
66 44.516 To propyl guaiacol 0.291
67 46.051 To acetyl group guaiacol 0.941
68 46.779 Anisylacetone 0.690
69 47.870 Vanillic acid methyl esters 0.332
70 49.592 3- acetyl group guaiacol 0.192
71 50.262 To propiono guaiacol 0.071
72 51.671 4-Methoxyhydrocinnamic acid 0.846
73 52.697 3,4- dihydroxy -5- methoxybenzaldehydes 0.135
74 53.921 6- methoxyl group eugenols 0.134
75 55.872 Syringaldehyde 11.297
76 56.181 3- hydroxyl -4- methoxyl group cinnamic acids 0.044
77 55.368 Zingiberone 0.822
78 56.870 2,5- dimethoxy -3,4- 4-dihydroxy benzaldehydes 0.129
79 59.455 4- hydroxyl -2- methoxyl group cinnamic aldehydes 2.501
80 59.566 To acetyl group syringone 1.137
81 60.753 4- hydroxy 3-methoxybenzene propionic acid 0.371
82 61.522 NSC 611398 0.912
83 63.914 3,5- dimethoxy-4 's-hydroxybenzoic acid 0.710
84 71.469 3,5- dimethoxy-4 's-hydroxyl cinnamic aldehyde 1.923
Agalloch eaglewood fragrance prepared by the present invention, volatility and half volatile material composition identify 84 kinds of compounds altogether, mainly For substances such as the organic acid of low carbon chain, alcohols, esters, phenols, ketones, what wherein content was higher has syringaldehyde（11.297%）, second Acid（4.285%）, 5 hydroxymethyl furfural（4.24%）, glucopyranose acetic acid esters（3.918%）, 4- hydroxyl -2- methoxyl group cinnamic aldehydes （2.501%）, the agalloch eaglewood fragrance being prepared has stayed the original fragrance component of agalloch eaglewood, logical including furanone, furfural, benzoic acid etc. It is consistent with fragrance during agalloch eaglewood champignon to cross the fragrance that ultrasonic ultrasonic delay line memory steaming mode evaporates.
Preparation method of the present invention is easily operated, and productivity is high, up to 4.2 ‰ ~ 6.7 ‰, is suitable for industrialized production, is one The more economic and practical agalloch eaglewood fragrance of kind, can be applied to daily use chemicals blending and champignon field.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, those of ordinary skill in the art should Work as understanding, technical scheme can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention Matter and scope.

Claims (3)

1. a kind of preparation method of agalloch eaglewood fragrance, it is characterised in that：Comprise the following steps：
Step a. mixes agalloch eaglewood sawdust and stainless steel Dixon ring filler, is positioned in the glass container of a upper end opening；
The external condensation reflux unit in step b. glass containers upper end；
Step c. utilizes the condensing reflux dress that glass container upper end is external to being mounted with the glass container bottom-heated of agalloch eaglewood sawdust Put the aromatic compound collected and distilled；
Step d. will collect obtained aromatic compound addition absolute ethyl alcohol dissolving, and after freezing processing, filtering subtracts dissolved matter Pressure concentration, obtains a kind of agalloch eaglewood fragrance；
Wherein, agalloch eaglewood sawdust granularity described in step a is 3~8mm, and the stainless steel Dixon ring filler additive amount is agalloch eaglewood sawdust weight 2~5 times of amount, and load total height is no more than glass container 2/5ths；Mode of heating described in step c adds for common electricity Heat or microwave heating, the rate of heat addition are 5 DEG C/min, are heated to predetermined temperature, the maximum temperature of the predetermined temperature is 250 DEG C ~280 DEG C, keep 20~40min；Absolute ethyl alcohol amount is added in described in step d to collect the 3~5 of obtained aromatic compound weight Times, the freezing processing time is for 24 hours~36h, and the temperature being concentrated under reduced pressure is 45 DEG C~55 DEG C, pressure for -0.08~- 0.09MPa。
2. a kind of preparation method of agalloch eaglewood fragrance according to claim 1, it is characterised in that：The glass container is round bottom Glass container.
3. a kind of application method of agalloch eaglewood fragrance, it is characterised in that：A kind of agalloch eaglewood described in by any one in claim 1-2 Agalloch eaglewood fragrance made from the preparation method of fragrance is placed in ultrasonic ultrasonic delay line memory to be evaporated by steaming mode, ultrasonic frequency For 1.7MHz ± 0.17MHz.
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EP1127101B1 (en) * 2000-05-31 2006-08-09 Shiseido Co., Ltd. Method of collection of fragrance ingredient, perfume composition and cosmetics containing same
CN1205160C (en) * 2003-01-24 2005-06-08 华宝香化科技发展（上海）有限公司 Method for producing perfume using ionol ester as raw material by thermo-wacking rectifying
CN101988026A (en) * 2009-08-06 2011-03-23 林韦志 Method and device for extracting essential oil by biomass wastes
CN101871922B (en) * 2010-06-18 2012-07-04 云南烟草科学研究院 Method for pyrolyzing tobacco additive and trapping and analyzing pyrolysis product
CN102423739B (en) * 2011-10-27 2014-07-30 佛山市南海科日超声电子有限公司 Ultrasonic atomizer
CN103184102A (en) * 2013-01-14 2013-07-03 中山市国林沉香科学研究所 Extraction method and application of agilawood essential oil
CN203244621U (en) * 2013-05-02 2013-10-23 邹进山 Aromatherapy machine
CN103315060B (en) * 2013-05-23 2014-12-03 暨南大学 Ultrasonic fumigating atomization method for insect-expelling and anti-mildew for storage agricultural products by utilizing composite essential oil
CN103789094A (en) * 2014-01-21 2014-05-14 广州大学 Method for extracting agilawood essential oil from agilawood chips
CN104140889B (en) * 2014-04-29 2016-05-25 江苏悦禧玫瑰科技有限公司 A kind of preparation method of rose absolute

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