CN104178346B - A kind of preparation method of high-purity chrysanthemum essential oil - Google Patents
A kind of preparation method of high-purity chrysanthemum essential oil Download PDFInfo
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- CN104178346B CN104178346B CN201410246462.1A CN201410246462A CN104178346B CN 104178346 B CN104178346 B CN 104178346B CN 201410246462 A CN201410246462 A CN 201410246462A CN 104178346 B CN104178346 B CN 104178346B
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 18
- 235000007516 Chrysanthemum Nutrition 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 244000189548 Chrysanthemum x morifolium Species 0.000 title 1
- 241000628997 Flos Species 0.000 claims abstract description 49
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000004821 distillation Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005507 spraying Methods 0.000 claims abstract description 17
- 241000723353 Chrysanthemum Species 0.000 claims abstract description 16
- 239000010779 crude oil Substances 0.000 claims abstract description 12
- 238000004108 freeze drying Methods 0.000 claims abstract description 12
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 12
- 239000012530 fluid Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 238000002061 vacuum sublimation Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 5
- 238000000199 molecular distillation Methods 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 abstract description 5
- 241000196324 Embryophyta Species 0.000 abstract description 4
- 230000007812 deficiency Effects 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000000859 sublimation Methods 0.000 description 4
- 230000008022 sublimation Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of high-purity chrysanthemum essential oil, it comprises the steps：(1) spraying treatment is carried out to Flos Chrysanthemi raw material with water；(2) Flos Chrysanthemi for crossing spraying treatment carries out pre-freeze, and vacuum sublimation is dried；(3) Flos Chrysanthemi after lyophilization is carried out into pulverization process；(4) fluid of Flos Chrysanthemi raw material and supercriticality after crushing is loaded in extraction kettle and is extracted, obtain the crude oil of Flos Chrysanthemi supercritical fluid extraction；(5) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, highly purified chrysanthemum essential oil can be collected.The deficiency of traditional extraction process is this method avoid, protects effective ingredients in plant to keep from heat destruction to greatest extent；Quick, efficient, abundant, completely extraction requirement is not only reached, and easy to operate, separating rate is fast, substantially increases work efficiency.
Description
Technical field
The present invention relates to the technical field of natural plant essential oils is extracted, more particularly to a kind of system of high-purity chrysanthemum essential oil
Preparation Method.
Background technology
China possesses abundant vegetal natural perfume resource, but due to extraction process backwardness, only part Flavour resources
It is exploited.Many vegetal natural perfumes tentatively can only be extracted, and extract yield and purity is relatively low, aroma quality
The problems such as destroying serious, easy residual harmful solvent, causes the serious waste of resource.
Supercritical fluid extraction and molecular distillation technique are all new generation extractive techniques in recent years.Supercritical fluid extraction is
There is special dissolution to some special natural products using the fluid of supercriticality, room temperature and supercritical can be close to
The fluid of state is extracted under shrouding, and effectively prevents the oxidation and loss of heat-sensitive substance, and the extracting method without having
Machine solvent.Molecular distillation technique is to realize separating using the difference of different material molecular tools, the technological merit
It is that vapo(u)rizing temperature is low, speed fast, can separates and conventional be difficult separate material.
The supercritical fluid extraction and molecular distillation technique effective ingredient suitable for low boiling, heat sensitive material is carried
Take, the original local flavor of natural product can be preserved and effective ingredient is not suffered a loss；And both are pure physical method, protect well
Shield separated object matter does not receive solvent contamination.
The content of the invention
Present invention aims to the deficiency of existing traditional extraction and separation technology, there is provided a kind of rapid extraction and separation
The method of highly purified chrysanthemum essential oil.The present invention is achieved through the following technical solutions：
For achieving the above object, the preparation method of the high-purity chrysanthemum essential oil that the present invention is provided, it comprises the following steps：
(1) spraying treatment is carried out to Flos Chrysanthemi raw material with water；
(2) Flos Chrysanthemi for crossing spraying treatment carries out pre-freeze, and vacuum sublimation is dried；
(3) Flos Chrysanthemi after lyophilization is carried out into pulverization process；
(4) fluid of Flos Chrysanthemi raw material and supercriticality after crushing is loaded in extraction kettle, extracting pressure 20～
50MPa, extracts 2～6h, obtains the crude oil of Flos Chrysanthemi supercritical fluid extraction under conditions of 30～60 DEG C of extraction temperature；
(5) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, can
Collect highly purified chrysanthemum essential oil.
Preferably, in the step (5), the working condition of molecular distillation is：Distillation vacuum is 0.1～
1MPa, knifing rotating speed are 100～300r/min, and chilling temperature is -10～-20 DEG C, and one-level distillation heating-up temperature is 50～70 DEG C,
Secondary distillation heating-up temperature is 80～100 DEG C, can collect highly purified chrysanthemum essential oil.
Further, in the step (1), the material of Flos Chrysanthemi raw material Flos Chrysanthemi raw material sprayed with water and water
Mass ratio is 1:100.
Further, in the step (1), the retention time sprayed to Flos Chrysanthemi raw material is 5～10 hours.
Further, in rapid (2), the Flos Chrysanthemi raw material crossed to spraying treatment carries out lyophilization, wherein pre-freeze
Temperature is -25～-35 DEG C, keeps 0.5～2h.
Further, in the step (2), the Flos Chrysanthemi raw material crossed to spraying treatment carries out lyophilization, wherein passing through
It is -15～-25 DEG C that evacuation carries out the temperature of sublimation drying, keeps 1～3h.
Further, in the step (3), the Flos Chrysanthemi degree of grinding after lyophilization is 80～120 mesh.
Further, in the step (4), supercritical fluid is CO2Or NO2；Its flow velocity is 5kkg/h～10kkg/h.
It is an advantage of the current invention that：
1st, this extraction and separation method method are pure physical method, it is not necessary to organic solvent, protect separated object well
Matter does not receive solvent contamination；
2nd, this extracting method, Flos Chrysanthemi was carried out spraying treatment originally, is contributed to the spilling of fragrance component, effectively can be carried
Rise yield；
3rd, this prepares quintessence oil method and can complete at low temperature, effectively prevents the oxidation and loss of heat-sensitive substance, maximum
Protection effective ingredients in plant in limit ground keeps from heat destruction, makes the flavouring essence quality of quintessence oil better than other traditional methods.
4th, the deficiency of traditional extraction process is this method avoid, protects effective ingredients in plant to keep from heat brokenly to greatest extent
It is bad；Quick, efficient, abundant, completely extraction requirement is not only reached, and easy to operate, separating rate is fast, substantially increases
Work efficiency.
Specific embodiment
Make further Detailed Description to the present invention below by way of specific embodiment.
Embodiment one：
The preparation method of high-purity chrysanthemum essential oil of the present invention, its step are as follows：
(1) Flos Chrysanthemi raw material 3kg is taken, spraying treatment is carried out to which with water 300kg, kept for 5 hours under room temperature；At spraying
The Flos Chrysanthemi managed is placed in vacuum freeze drier carries out pre-freeze, and design temperature is -25 DEG C, keeps 0.5h；By evacuation
The temperature for carrying out sublimation drying is -15 DEG C, keeps 1h；The Flos Chrysanthemi after lyophilization is carried out into pulverization process to 80 with pulverizer
Mesh；
(2) the Flos Chrysanthemi raw material after crushing is loaded in extraction kettle, then by the CO of the supercriticality of 5kg/h flow velocitys2Note
Enter in extraction kettle, 2h is extracted under conditions of extracting pressure 20MPa, 30 DEG C of extraction temperature, Flos Chrysanthemi supercritical fluid is obtained
The crude oil of extraction.
(3) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, point
The working condition of sub- distilling apparatus is：Distillation vacuum is 0.1MPa, knifing rotating speed 100r/min, -10 DEG C of chilling temperature, one-level
Distillation heating-up temperature is 50 DEG C, and secondary distillation heating-up temperature is 80 DEG C, can collect highly purified chrysanthemum essential oil.
Embodiment two：
The preparation method of high-purity chrysanthemum essential oil of the present invention, its step are as follows：
(1) Flos Chrysanthemi raw material 5kg is taken, spraying treatment is carried out to which with 500kg water, kept for 8 hours under room temperature；At spraying
The Flos Chrysanthemi managed is placed in vacuum freeze drier carries out pre-freeze, and design temperature is -30 DEG C, keeps 1h；Entered by evacuation
The temperature of row sublimation drying is -20 DEG C, keeps 2h；The Flos Chrysanthemi after lyophilization is carried out into pulverization process to 100 with pulverizer
Mesh；
(2) the Flos Chrysanthemi raw material after crushing is loaded in extraction kettle, then by the NO of the supercriticality of 8kg/h flow velocitys2Note
Enter in extraction kettle, 4h is extracted under conditions of extracting pressure 30MPa, 40 DEG C of extraction temperature, Flos Chrysanthemi supercritical fluid is obtained
The crude oil of extraction.
(3) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, point
The working condition of sub- distilling apparatus is：Distillation vacuum is 0.5MPa, knifing rotating speed 200r/min, -15 DEG C of chilling temperature, one-level
Distillation heating-up temperature is 60 DEG C, and secondary distillation heating-up temperature is 90 DEG C, can collect highly purified chrysanthemum essential oil.
Embodiment three：
The preparation method of high-purity chrysanthemum essential oil of the present invention, its step are as follows：
(1) Flos Chrysanthemi raw material 8kg is taken, spraying treatment is carried out to which with 800kg water, kept for 10 hours under room temperature；Will spraying
The Flos Chrysanthemi for processing is placed in vacuum freeze drier carries out pre-freeze, and design temperature is -35 DEG C, keeps 2h；By evacuation
The temperature for carrying out sublimation drying is -25 DEG C, keeps 3h；The Flos Chrysanthemi after lyophilization is carried out into pulverization process extremely with pulverizer
120 mesh；
(2) the Flos Chrysanthemi raw material after crushing is loaded in extraction kettle, then by the CO of the supercriticality of 10kg/h flow velocitys2Note
Enter in extraction kettle, 6h is extracted under conditions of extracting pressure 50MPa, 60 DEG C of extraction temperature, Flos Chrysanthemi supercritical fluid is obtained
The crude oil of extraction.
(3) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, point
The working condition of sub- distilling apparatus is：Distillation vacuum is 1MPa, and knifing rotating speed 300r/min, -20 DEG C of chilling temperature, one-level are steamed
Heating-up temperature is evaporated for 70 DEG C, secondary distillation heating-up temperature is 100 DEG C, can collect highly purified chrysanthemum essential oil.
Claims (1)
1. a kind of preparation method of high-purity chrysanthemum essential oil, it comprises the steps：
(1) spraying treatment is carried out to Flos Chrysanthemi raw material with water；
(2) Flos Chrysanthemi for crossing spraying treatment carries out pre-freeze, and vacuum sublimation is dried；
(3) Flos Chrysanthemi after lyophilization is carried out into pulverization process；
(4) fluid of Flos Chrysanthemi raw material and supercriticality after crushing is loaded in extraction kettle, extracting pressure 20～
50MPa, extracts 2～6h, obtains the crude oil of Flos Chrysanthemi supercritical fluid extraction under conditions of 30～60 DEG C of extraction temperature；
(5) crude oil of the Flos Chrysanthemi supercritical fluid extraction for obtaining is carried out into purifies and separates by quadratic component distillation, can be collected
To highly purified chrysanthemum essential oil；
In the step (5), the working condition of molecular distillation is：Distillation vacuum is 0.1～1MPa, knifing rotating speed is 100～
300r/min, chilling temperature are -10～-20 DEG C, and one-level distillation heating-up temperature is 50～70 DEG C, and secondary distillation heating-up temperature is 80
～100 DEG C；
In the step (1), the Flos Chrysanthemi raw material sprayed to Flos Chrysanthemi raw material with water is 1 with the quality of material ratio of water:
100；
In the step (1), the retention time sprayed to Flos Chrysanthemi raw material is 5～10 hours；
In rapid (2), the Flos Chrysanthemi raw material crossed to spraying treatment carries out lyophilization, and the wherein temperature of pre-freeze is -25～-35
DEG C, keep 0.5～2h；
In the step (2), the Flos Chrysanthemi raw material crossed to spraying treatment carries out lyophilization, wherein being distilled by evacuation
Dry temperature is -15～-25 DEG C, keeps 1～3h；
In the step (3), the Flos Chrysanthemi degree of grinding after lyophilization is 80～120 mesh；
In the step (4), supercritical fluid is CO2Or NO2；Its flow velocity is 5kg/h～10kg/h.
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| CN201410246462.1A CN104178346B (en) | 2014-06-05 | 2014-06-05 | A kind of preparation method of high-purity chrysanthemum essential oil |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104498192A (en) * | 2014-12-15 | 2015-04-08 | 云南中烟工业有限责任公司 | Preparation method and application of florists chrysanthemum extract |
| CN105273846A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. leaf essential oil |
| CN105273833A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. flower essential oil |
| CN106811304A (en) * | 2016-09-14 | 2017-06-09 | 湖北中烟工业有限责任公司 | A kind of preparation method of high-quality cigarette apricot kernel oil |
| CN106635418A (en) * | 2016-11-01 | 2017-05-10 | 湖北中烟工业有限责任公司 | Preparation method of high-purity citrus aurantium flower essential oil and flavor addition essence used for cigarettes and blended with high-purity citrus aurantium flower essential oil |
| CN106551418A (en) * | 2016-12-07 | 2017-04-05 | 湖北中烟工业有限责任公司 | A kind of method for preparing cigarette Radix Angelicae Pubescentiss extractum |
| CN106978258A (en) * | 2017-05-24 | 2017-07-25 | 湖北中烟工业有限责任公司 | Enzymatic flavouring improves the preparation method and application of the FLOS CHRYSANTHEMI ALBA from Haizhou of China volatile oil of flavouring essence quality |
| CN111040880A (en) * | 2020-01-08 | 2020-04-21 | 湖北中烟工业有限责任公司 | Preparation method of high-purity lemongrass essential oil |
| CN112353726A (en) * | 2020-11-23 | 2021-02-12 | 象鼻山香(杭州)生物科技有限公司 | Effective mosquito-repelling part in chrysanthemum indicum leaf and application |
| CN114958487B (en) * | 2022-06-15 | 2024-03-22 | 银谷芳香科技有限公司 | Industrial extraction process method of Roman chamomile oil |
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2014
- 2014-06-05 CN CN201410246462.1A patent/CN104178346B/en active Active
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| Title |
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| 《天然产物有效成分超临界流体萃取过程的强化技术》;张炎强等;《广东化工》;20061231;第33卷(第5期);第22-25页 * |
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