CN101624557B - Method for extracting neroli absolute by supercritical carbon dioxide - Google Patents
Method for extracting neroli absolute by supercritical carbon dioxide Download PDFInfo
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- CN101624557B CN101624557B CN2009101045259A CN200910104525A CN101624557B CN 101624557 B CN101624557 B CN 101624557B CN 2009101045259 A CN2009101045259 A CN 2009101045259A CN 200910104525 A CN200910104525 A CN 200910104525A CN 101624557 B CN101624557 B CN 101624557B
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Abstract
The invention provides a method for extracting neroli absolute by supercritical carbon dioxide in combination with molecular distillation, and is characterized in that fresh orange blossoms are frozen and dried firstly, and then placed in an extraction kettle after being ground by a grinder; extraction are carried out twice under different temperatures and pressures, and extracts are merged, mixed and placed in a molecular still for separating and removing waxy component so as to obtain the neroli absolute. The invention has good extracting effect, high product yield, and low temperature in extraction separation process, thereby avoiding damages to aroma components due to high temperature without organic solvent residue, keeping pure natural performance of the neroli absolute, having convenient operation, and being applied to industrial production.
Description
Technical field
The present invention relates to the separation and purification of effective ingredients in plant, the method for contained orange flower absolute in particularly spending with the supercritical carbon dioxide extraction orange.
Background technology
Flores aurantii is a kind of famous and precious natural perfume, and its contained effective constituent orange flower absolute is applied among various daily chemical products and the food as high-grade perfume material.The existing method of extracting orange flower absolute is that the orange flower is processed flores aurantii medicinal extract with the sherwood oil lixiviate, adds 5～10 times of ethanol, and cold filtration is removed insoluble wax, and then be cooled to-18 ℃, refilters paraffin removal; Ethanolic soln is removed ethanol through underpressure distillation, promptly makes absolute oil.The shortcoming of this method is that fragrance is relatively poor, and color is darker, and yield is lower, residual human body is produced dysgenic organic solvent.
Summary of the invention
To the deficiency of prior art, it is good to the invention provides a kind of extracting effect, and yield is higher, and is pollution-free, and with the method for supercritical carbon dioxide extraction binding molecule distillation extraction orange flower absolute, the technical scheme of employing is following:
A kind of method with the supercritical carbon dioxide extraction orange flower absolute, its step is following: (1) is with the lyophilize of orange flower, with inserting extraction kettle after the kibbler pulverizing; (2) feeding carbonic acid gas with 15～30L/h flow velocity, is that 30～40 ℃, pressure are to carry out extraction first time under 10～20MPa condition in temperature, and extraction time 2～4h must the flores aurantii extract; (3) extraction kettle is boosted to 22～32MPa, temperature remains on 40～60 ℃, carries out the extraction second time, and extraction time 3～5h obtains extract for the second time;
(4) twice extract merged, mixing is put into the molecular still separation and is removed wax component, promptly obtains orange flower absolute.
Wherein the said orange of step (1) spends cryodesiccated temperature preferably-5～-35 ℃, and smashing fineness is 20～40 orders.
Wherein the said molecular still of step (4) vacuum tightness of removing wax component preferably is controlled at 50～90KPa, and temperature preferably is controlled at 30～60 ℃.
Supercritical carbon dioxide extraction is the chemical separation technology that develops rapidly both at home and abroad in recent years; Chemical reaction does not take place in used extraction agent carbon dioxide abstraction process; Have advantages such as flow process is simple, efficient, cold operation, and is pollution-free, be particularly suitable for the separation and purification of active ingredient of natural product.Distill the technology of producing the smart absolute oil of flores aurantii with the supercritical carbon dioxide extraction binding molecule at present and do not see that as yet report is arranged.In the operating process of supercritical carbon dioxide extraction method, should adjust with preferred relevant technical parameter, otherwise will have a strong impact on product yield and extraction effect according to the singularity of raw material.Particularly extraction for the first time is set in 30～40 ℃ with temperature in the present invention; Avoided that temperature is too high to be damaged some composition in the orange flower absolute; Extraction for the second time is controlled at 40～60 ℃ with temperature, and the composition that helps so further will not extracting for the first time extracts.The extract that obtains after twice extraction adopts the molecular still with protective value to remove wax component again, just reaches the object of the invention, obtains the smart absolute oil of colory flores aurantii.
The invention has the beneficial effects as follows and adopt supercritical carbon dioxide extraction binding molecule distillation extraction orange flower absolute, extracting effect is good, and product yield is high, quality better; Technical process is simple, and is easy to operate, and the extraction separation process temperature is low, avoided the destruction of high temperature to aroma component; Organic solvent-free is residual, keeps the pure natural property of orange flower absolute, but carbonic acid gas recycling is used; Nontoxic, non-environmental-pollution is applicable to suitability for industrialized production.
Specific embodiment (totally 5 examples)
Embodiment 1
Step is following: (1) is placed on temperature-5 ℃ lyophilize with 2000 gram orange flowers, is crushed to 40 order fineness with kibbler, inserts extraction kettle; (2) feeding carbonic acid gas with the 20L/h flow velocity, is that 30 ℃, pressure are to carry out extraction first time under the 12MPa condition in temperature, and extraction 2h must the flores aurantii extract; (3) extraction kettle is boosted to 25MPa, temperature remains on 50 ℃, carries out the extraction second time, and extraction 4.5h obtains extract for the second time; (4) twice extract merged, mixing is put into molecular still, under vacuum tightness 50KPa and 30 ℃ of conditions of temperature, separates and removes wax component, promptly obtains orange flower absolute 4.1 grams, absolute oil yield 0.205%.
Embodiment 2
Its step is following: (1) is placed on temperature-35 ℃ lyophilize with 2000 gram orange flowers, is crushed to 30 order fineness with kibbler, inserts extraction kettle; (2) feeding carbonic acid gas with the 25L/h flow velocity, is that 35 ℃, pressure are to carry out extraction first time under the 18MPa condition in temperature, and extraction 3h must the flores aurantii extract; (3) extraction kettle is boosted to 30MPa, temperature remains on 48 ℃, carries out the extraction second time, and extraction 5h obtains extract for the second time; (4) twice extract merged, mixing is put into molecular still, under vacuum tightness 70KPa and 60 ℃ of conditions of temperature, separates and removes wax component, promptly obtains orange flower absolute 4.35 grams, absolute oil yield 0.218%.
Embodiment 3
Step is with embodiment 1, and different is that the temperature that extracts the first time, the second time is respectively 33 ℃, 55 ℃, promptly obtains orange flower absolute 4.3 grams, absolute oil yield 0.215%.
Embodiment 4
Its step is following: (1) is placed on temperature-30 ℃ lyophilize with 5000 gram orange flowers, is crushed to 20 order fineness with kibbler, inserts extraction kettle; (2) feeding carbonic acid gas with the 30L/h flow velocity, is that 40 ℃, pressure are to carry out extraction first time under the 20MPa condition in temperature, and extraction 3.5h must the flores aurantii extract; (3) extraction kettle is boosted to 30MPa, temperature remains on 50 ℃, carries out the extraction second time, and extraction 5h obtains extract for the second time; (4) twice extract merged, mixing is put into molecular still, under vacuum tightness 90KPa and 60 ℃ of conditions of temperature, separates and removes wax component, promptly obtains orange flower absolute 10.5 grams, absolute oil yield 0.21%.
Embodiment 5
Step is with embodiment 4, and different is that the temperature that extracts the first time, the second time is respectively 38 ℃, 60 ℃, promptly obtains orange flower absolute 10.6 grams.Absolute oil yield 0.216%.
Claims (2)
1. method with the supercritical carbon dioxide extraction orange flower absolute, its step is following: (1) with the lyophilize of orange flower, inserts extraction kettle after pulverizing with kibbler; (2) feeding carbonic acid gas with 15～30L/h flow velocity, is that 30～40 ℃, pressure are to carry out extraction first time under 10～20MPa condition in temperature, and extraction time 2～4h must the flores aurantii extract; (3) extraction kettle is boosted to 22～32MPa, temperature remains on 40～60 ℃, carries out the extraction second time, and extraction time 3～5h obtains extract for the second time; (4) twice extract merged, mixing is put into the molecular still separation and is removed wax component, promptly obtains orange flower absolute; The vacuum degree control of said molecular still is at 50～90KPa, and temperature is controlled at 30～60 ℃.
2. the method with the supercritical carbon dioxide extraction orange flower absolute according to claim 1, wherein the said orange flower of step (1) lyophilize temperature is-5～-35 ℃, smashing fineness is 20～40 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009101045259A CN101624557B (en) | 2009-07-31 | 2009-07-31 | Method for extracting neroli absolute by supercritical carbon dioxide |
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| CN2009101045259A CN101624557B (en) | 2009-07-31 | 2009-07-31 | Method for extracting neroli absolute by supercritical carbon dioxide |
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| CN101624557A CN101624557A (en) | 2010-01-13 |
| CN101624557B true CN101624557B (en) | 2012-05-02 |
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| CN101928602B (en) * | 2010-08-30 | 2013-03-20 | 华南理工大学 | Method for separating paraffin from readymade oil |
| CN101993782A (en) * | 2010-12-01 | 2011-03-30 | 重庆市日用化学工业研究所 | Supercritical carbon dioxide extraction method of gardenia essential oil |
| CN102311880A (en) * | 2011-08-11 | 2012-01-11 | 魏立文 | Extraction method for extracting volatile oil from natural plant flowers |
| CN103007570B (en) * | 2012-12-10 | 2016-03-02 | 刘东波 | A kind of method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil |
| CN103305344B (en) * | 2013-06-18 | 2014-07-16 | 菏泽尧舜牡丹生物科技有限公司 | Method for extracting peony essence from fresh peony flowers |
| CN103627528A (en) * | 2013-06-30 | 2014-03-12 | 金玛瑙香水（明光）有限公司 | Method for extracting lavender essential oil |
| CN104982556B (en) * | 2015-06-30 | 2018-04-20 | 南阳汇萃植物制品有限公司 | A kind of cumin flavor oil and preparation method thereof |
| CN106318634A (en) * | 2016-08-28 | 2017-01-11 | 广西灏源盛世生物科技有限公司 | Method of extraction of orange blossom essential oil |
| CN109022121A (en) * | 2018-07-05 | 2018-12-18 | 紫云自治县紫香源农林科技有限责任公司 | A kind of extraction process of cinnamomum camphora oil |
| KR102645351B1 (en) * | 2021-08-02 | 2024-03-08 | 한국식품연구원 | Natural aroma composition using citrus flower and manufacturing method thereof |
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