CN100480364C - Technique for separating essential oil of spiceberry by method for breaking cell wall under normal temperature (or low temperature) and normal pressure - Google Patents
Technique for separating essential oil of spiceberry by method for breaking cell wall under normal temperature (or low temperature) and normal pressure Download PDFInfo
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- CN100480364C CN100480364C CNB2005100107279A CN200510010727A CN100480364C CN 100480364 C CN100480364 C CN 100480364C CN B2005100107279 A CNB2005100107279 A CN B2005100107279A CN 200510010727 A CN200510010727 A CN 200510010727A CN 100480364 C CN100480364 C CN 100480364C
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Abstract
The present invention relates to a technique for separating essential oil of perfume plant by adopting normal-temperature (or low-temperature) and normal-pressure cell wall-breaking method. Said invention is characterized by that it adopts a vibration type ultrafnie mechanical pulverizing equipment (below 200 meshes) with refrigeration function to break plant cell tissue and cell wall membrane of perfume plant whose perfume raw material content is above 80% in a fully-closed environment (using microscope to make detection) at normal temperature (or low temperature) and normal pressure, then utilizes the processes of water-washing, cold storage of freezing, standing still to make oil-water separation and high-speed centrifugal separation (3000 rpm) to obtain natural perfume plant essential oil.
Description
A kind of technology of extracting high-quality plant fragrance essential oil that is specifically designed to of technical field is the technology of using separating essential oil of spiceberry by method for breaking cell wall at normal temperatures and pressures.
This technology of background technology belongs to the utilisation technology category, comprises the application of biology, chemistry, physics, physical chemistry elementary principle and the application of novel mechanical equipment.Be the technology that is applicable to natural plant pefume processing.
Essential oil (Essential Oil) claims volatile oil, perfume oil again, is to adopt the general designation this plant characteristics fragrance, volatility oily material that has that various physical methods separate from the plant perfume material.Be the natural perfume goods the most traditional, the most large, that use is the most extensive, output is maximum.
Natural perfume plant generally all has uniqueness, nature, grace, comfortable fragrance and note, so the processing isolation technique of natural perfume always emphasizes to reduce sepn process to the destruction of its aroma component and losing of trace ingredients as far as possible, keep the distinctive natural note of various perfume materials, have the concentrated spice product of the complete odour characteristics of former natural perfume plant in the hope of preparation.Tradition natural perfume working method is because of himself inherent disadvantage, obviously do not reach this purpose, there are big gap (the citrous fruit peel essential oil of producing with cold grinding and cold-press, the spices essential oil of good heat resistance and itself need heat except the spices that could produce fragrance) in the natural essential oil product fragrance of extraction and perfume material itself.
The technology of a kind of normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall of summary of the invention is characterized in that said technology mainly comprises the steps:
(1) is chilled to-40 ℃～30 ℃ in advance with the ultra-fine mechanical crushing equipment start of the oscillatory type of band refrigerating function;
(2) spice berry that contains essential oil is carried out pre-treatment, the perfume material that particle diameter is bigger need be smashed particle diameter≤1 centimetre, adds the inhibitor mixed or the immersion of enzyme, and the contained enzyme of spice berry self damages essential oil when preventing cell wall breaking;
(3) the ultra-fine mechanical crushing equipment of the oscillatory type of utilizing precooling to finish is smashed the cell envelope more than 80% of the pretreated spice berry that contains essential oil in hermetic pulverizer;
(4) with the raw material after the water flushing processing that is added with 0.01mol/L alum, refrigeration is left standstill, and pectin, tannic acid, protein are fully precipitated, and oil reservoir is separated out on the surface, takes out the existing oil reservoir in surface, obtains slightly essential oil of part, and the elimination precipitation obtains oil-water mixture;
(5) utilize supercentrifuge separating oil water mixed liquid, the thick essential oil of the part of getting back;
(6) make with extra care after the thick essential oil merging with (4) and (5) gained, obtain the high-quality essential oil;
(7) filter residue in isolated water liquid and (4) in the distillation (5) obtains remaining essential oil.
Wherein the ultra-fine mechanical crushing equipment of oscillatory type of said band refrigerating function can be crushed to raw meal particle size and can pass through 200 mesh sieve holes under the condition of temperature≤48 ℃ in the step (1).The inhibitor of said enzyme comprises the class in reversible transglutaminase inhibitor, irreversible inhibitor and the disrupting agent in the step (2), comprises a kind of in sal epsom, yellow soda ash, calcium hydroxide, the proteolytic ferment.Said cell envelope more than 80% is smashed the result who is meant with after the microscopic examination plant cell tissue in the step (3) in hermetic pulverizer.Said refrigeration is left standstill and is meant and airtightly in 0-10 ℃ environment leaves standstill preservation in the step (4).Said supercentrifuge is meant the large vol whizzer of rotating speed 〉=3000 at full capacity rev/min in the step (5).Said making with extra care is meant that the thick essential oil to gained removes terpene, molecular distillation in the step (6).
This technology has solved the insurmountable key issue of traditional technology route, and following characteristic is arranged:
1. the processing technology routine of brand-new separating natural spice berry essential oil.
2. novel process is compared with traditional natural perfume complete processing, almost can overcome all disadvantages of traditional technology (particularly containing thermo-sensitivity composition or important trace ingredients in the natural perfume plant aroma component), isolated essential oil goods are evaluated through the perfumer, the complete characterization fragrance of the very approaching natural perfume material of being processed of fragrance.
3. new technology route is suitable for the high value natural plant pefume extracts essential oil separation of the bright leaf class of fresh flower, can remedy " supercritical CO preferably
2Fluid extraction natural perfume technology " the difficult deficiency that realizes the natural plant pefume of the bright leaf class of large-scale processing fresh flower.
4. the production process of new technology route does not relate to High Temperature High Pressure, does not use the inflammable and explosive solvent of volatility, has well solved the problem of traditional technology production safety.
5. energy-saving and environmental protection, scale production can have high input.
Description of drawings Fig. 1 is a normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall process route chart.
Embodiment: see following example:
1. the natural plant pefume extracts essential oil of fresh flower class is separated.
(1) the Flower of Bailan extracts essential oil is separated:
A. with the ultra-fine mechanical crushing equipment start of the oscillatory type of refrigerating function precooling, allow material tube temperature remain on 0 ℃～5 ℃;
B. take by weighing 1 kilogram of Flower of Bailan fresh flower, soak with the 5L saturated solution of magnesium sulfate of precooling at 0 ℃～5 ℃;
C. the ultra-fine mechanical crushing equipment of finishing with precooling immediately of oscillatory type is smashed the 95% above cell tissue and the cell envelope of pretreated Flower of Bailan fresh flower (sending into equipment together with soak solution) (handle getting final product in 15 minutes, available observation by light microscope detects) in hermetically sealed environment;
D. the raw material after handling with water (5L) flushing that is added with 0.01mol/L alum, to wash mixed solution fully stirs back refrigeration and leaves standstill (0～10 ℃, more than 1 hour, if the existing oil reservoir in surface this moment, can take out earlier, promptly get part Flower of Bailan essential oil), the elimination precipitation obtains oil-water mixture (the whole range request of crossing is finished) in closed environment;
E. use the rotating speed separating oil water mixed liquid of supercentrifuge, obtain the Flower of Bailan essential oil with 〉=3700r/min;
F. merge D, E gained Flower of Bailan essential oil, weighing can get about 1.5 grams of high quality white orchid essential oil;
G. distill the filter residue in the isolated water liquid and D among the E, obtain about 1 gram of remaining Flower of Bailan essential oil.
Gained high quality white orchid essential oil is light oily liquids, and perfumer's comment is: pure and fresh, the bright deep and remote fragrance of a flower, and head is fragrant perfect, the characteristic perfume of Flower of Bailan fresh flower, fragrance is sent out thoroughly, and lasting is general.
(2) extraction separation of Yilan Cananga odorata quintessence oil:
A. with the ultra-fine mechanical crushing equipment start of the oscillatory type of refrigerating function precooling, allow material tube temperature remain on 0 ℃～5 ℃;
B. take by weighing Yilan, 1 kilogram of Yilan fresh flower flower, soak with the aqueous solution that is added with the trace of albumin lytic enzyme (5L) of precooling at 0 ℃～5 ℃;
C. the ultra-fine mechanical crushing equipment of finishing with precooling immediately of oscillatory type is smashed the 95% above cell tissue and the cell envelope of pretreated Yilan, Yilan fresh flower (sending into equipment together with soak solution) (handle getting final product in 15 minutes, available observation by light microscope detects) in hermetically sealed environment;
D. the raw material after handling with water (5L) flushing that is added with 0.01mol/L alum, to wash mixed solution and fully stir the back quick freezing, freeze real after again room temperature thaw, leave standstill oily water separation (the existing oil reservoir in surface this moment, can take out earlier, promptly get part Yilan Cananga odorata quintessence oil), the elimination precipitation obtains oil-water mixture (the whole range request of crossing is finished) in closed environment;
E. use the rotating speed separating oil water mixed liquid of supercentrifuge, the part of getting back Yilan Cananga odorata quintessence oil with 〉=3700r/min;
F. merge D, E gained Yilan Cananga odorata quintessence oil, weighing can get the about 10-25 gram of high-quality Yilan Cananga odorata quintessence oil;
G. distill the filter residue in the isolated water liquid and D among the E, obtain the about 2-3 gram of remaining Yilan Cananga odorata quintessence oil.
Gained high-quality Yilan Cananga odorata quintessence oil is light oily liquids, and perfumer's comment is: the bright clear fragrance of a flower, and head is fragrant perfect, and the characteristic perfume of Yilan, Yilan fresh flower gives off a strong fragrance, and lasting still can.
2. the natural plant pefume extracts essential oil of bright leaf class is separated
The extraction separation of white orchid leaf essential oil:
A. with the ultra-fine mechanical crushing equipment start of the oscillatory type of refrigerating function precooling, allow material tube temperature remain on 0 ℃～5 ℃;
B. taking by weighing the bright leaf of 1 kilogram of white orchid leaf, shred particle diameter≤1 centimetre, is 10 sodium carbonate solution (5L) immersion at 0 ℃～5 ℃ pH value with precooling;
C. the ultra-fine mechanical crushing equipment of finishing with precooling immediately of oscillatory type is smashed the 95% above cell tissue and the cell envelope of the bright leaf of pretreated white orchid leaf (sending into equipment together with soak solution) (handle getting final product in 15 minutes, available observation by light microscope detects) in hermetically sealed environment;
D. the raw material after handling with water (5L) flushing that is added with 0.01mol/L alum, to wash mixed solution fully stirs back refrigeration and leaves standstill (0～10 ℃, more than 1 hour, if the existing oil reservoir in surface this moment, can take out earlier, promptly get part white orchid leaf essential oil), the elimination precipitation obtains oil-water mixture (the whole range request of crossing is finished) in closed environment;
E. use the rotating speed separating oil water mixed liquid of supercentrifuge, obtain the white orchid leaf essential oil with 〉=3700r/min;
F. merge D, E gained white orchid leaf essential oil, weighing can get about 1.2 grams of high-quality white orchid leaf essential oil;
G. distill the filter residue in the isolated water liquid and D among the E, obtain about 2 grams of remaining white orchid leaf essential oil.
Gained high-quality white orchid leaf essential oil is green oily liquids, and perfumer's comment is: delicate fragrance rhythm, with the sweet fragrance of a flower, and head is fragrant good, the characteristic perfume of the bright leaf of white orchid leaf, fragrance is sent out thoroughly, and lasting is general.
3. the natural plant pefume extracts essential oil of cauline leaf class is separated
The extraction separation of rosemary ethereal oil:
A. with the ultra-fine mechanical crushing equipment start of the oscillatory type of refrigerating function precooling, allow material tube temperature remain on 0 ℃～5 ℃;
B. taking by weighing the bright cauline leaf of 1 kilogram of Rosmarinus officinalis, shred particle diameter≤1 centimetre, is 10 aqua calcis (5L) immersion at 0 ℃～5 ℃ pH value with precooling;
C. the ultra-fine mechanical crushing equipment of finishing with precooling immediately of oscillatory type is smashed the 95% above cell tissue and the cell envelope of the bright cauline leaf of pretreated Rosmarinus officinalis (sending into equipment together with soak solution) (handle getting final product in 15 minutes, available observation by light microscope detects) in hermetically sealed environment;
D. the raw material after handling with water (5L) flushing that is added with 0.01mol/L alum, will wash mixed solution fully stir the back refrigerate and leave standstill (0～10 ℃, more than 1 hour, if the existing oil reservoir in surface this moment can take out earlier, promptly get the part rosemary ethereal oil), the elimination precipitation obtains oil-water mixture;
E. use the rotating speed separating oil water mixed liquid of supercentrifuge, obtain rosemary ethereal oil with 〉=3700r/min;
F. merge D, E gained rosemary ethereal oil, it is refining to remove terpene, and weighing can get the about 5-8 gram of rosemary ethereal oil;
G. distill the filter residue in the isolated water liquid and D among the E, obtain the about 2-3 gram of remaining rosemary ethereal oil.
The gained rosemary ethereal oil is green oily liquids, and perfumer's comment is: blue or green fragrant, refrigerant now herbal, and head is fragrant true to nature, the characteristic perfume of the bright leaf of Rosmarinus officinalis, fragrance is strong, saturating to be sent out, and lasting is general.
Branch, do, seed, bark, dry fruit, root class contain also available technology of essential oil fragrances plant and extract essential oil (the main note composition requires water insoluble).The essential oil fragrance that proposes is fine, complete characterization fragrance with perfume material, but these perfume materials or be worth cheap, main note composition good heat resistance, lasting lasting (as the banksia rose, the fragrant class perfume material of cream etc.), use the economic worth and the application value of this technology little, also just do not described in detail one by one here, it is as follows to take a single example: the extraction separation of sweet Fructus Foeniculi quintessence oil:
A. taking by weighing 1 kilogram of sweet sweet fennel seed of drying, is that 10 aqua calcis (10L) soaked 24 hours with precooling at 0 ℃～5 ℃ pH value;
B. with the ultra-fine mechanical crushing equipment start of the oscillatory type of refrigerating function precooling, allow material tube temperature remain on 0 ℃～5 ℃;
C. the ultra-fine mechanical crushing equipment of finishing with precooling of oscillatory type is smashed the 95% above cell tissue and the cell envelope of pretreated sweet sweet fennel seed (sending into equipment together with soak solution) (handle getting final product in 15 minutes, available observation by light microscope detects) in hermetically sealed environment;
D. the raw material after handling with water (10L) flushing that is added with 0.01mol/L alum, will wash mixed solution fully stir the back refrigerate and leave standstill (0～10 ℃, more than 1 hour, the existing oil reservoir in surface this moment can take out earlier, promptly gets the sweet Fructus Foeniculi quintessence oil of part), the elimination precipitation obtains oil-water mixture;
E. use the rotating speed separating oil water mixed liquid of supercentrifuge, obtain sweet Fructus Foeniculi quintessence oil with 〉=3700r/min;
F. merge D, the sweet Fructus Foeniculi quintessence oil of E gained, weighing can get about 20～35 grams of sweet Fructus Foeniculi quintessence oil;
G. distill the filter residue in the isolated water liquid and D among the E, obtain about 3～5 grams of remaining sweet Fructus Foeniculi quintessence oil.
The sweet Fructus Foeniculi quintessence oil of gained is the sap green oily liquids, and perfumer's comment is: hot note, with sweet herbal, the cured perfume (or spice) of fat and cream perfume (or spice), and head is fragrant good, and the characteristic perfume of sweet sweet fennel seed, fragrance are strong strongly, and lasting is lasting.
Claims (5)
1. the technology of a normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall is characterized in that said technology mainly comprises the steps:
(1) is chilled to-40 ℃～30 ℃ in advance with the ultra-fine mechanical crushing equipment start of the oscillatory type of band refrigerating function;
(2) spice berry that contains essential oil is carried out pre-treatment, the perfume material that particle diameter is bigger need be smashed particle diameter≤1 centimetre, adds a kind of in sal epsom, yellow soda ash, calcium hydroxide, the proteolytic ferment;
(3) the ultra-fine mechanical crushing equipment of the oscillatory type of utilizing precooling to finish is smashed the cell envelope more than 80% of the pretreated spice berry that contains essential oil to 200m in hermetic pulverizer;
(4) with the raw material after the water flushing processing that is added with 0.01mol/L alum, refrigeration is left standstill, and pectin, tannic acid, protein are fully precipitated, and oil reservoir is separated out on the surface, takes out the existing oil reservoir in surface, obtains slightly essential oil of part, and the elimination precipitation obtains oil-water mixture;
(5) utilize supercentrifuge separating oil water mixed liquid, the thick essential oil of the part of getting back;
(6) make with extra care after the thick essential oil merging with (4) and (5) gained, obtain the high-quality essential oil;
(7) filter residue in isolated water liquid and (4) in the distillation (5) obtains remaining essential oil.
2. the technology of normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall as claimed in claim 1 is characterized in that: wherein said cell envelope more than 80% is smashed the result who is meant with after the microscopic examination plant cell tissue in the step (3) in hermetic pulverizer.
3. the technology of normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall as claimed in claim 1 is characterized in that: wherein said refrigeration is left standstill and is meant and airtightly in 0-10 ℃ environment leaves standstill preservation in the step (4).
4. the technology of normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall as claimed in claim 1 is characterized in that: wherein said supercentrifuge is meant the large vol whizzer of rotating speed 〉=3000 at full capacity rev/min in the step (5).
5. the technology of normal temperature and pressure separating essential oil of spiceberry by method for breaking cell wall as claimed in claim 1 is characterized in that: wherein said making with extra care is meant that the thick essential oil to gained removes terpene, molecular distillation in the step (6).
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| CNB2005100107279A CN100480364C (en) | 2005-04-05 | 2005-04-05 | Technique for separating essential oil of spiceberry by method for breaking cell wall under normal temperature (or low temperature) and normal pressure |
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| CN102586023B (en) * | 2012-01-19 | 2013-07-03 | 仲恺农业工程学院 | Method for extracting citrus pericarp essential oil |
| CN102965190A (en) * | 2012-12-04 | 2013-03-13 | 师宗红盈食品有限公司 | Ginger essential oil extraction method |
| CN105232584A (en) * | 2015-09-30 | 2016-01-13 | 河南行知专利服务有限公司 | Decoction-free extraction process for precious Chinese herbal medicines |
| TWI584814B (en) * | 2016-03-23 | 2017-06-01 | Ren-Hao Liu | Extraction Methods and Extracts of Canna Plants and Their Uses |
| CN106947602A (en) * | 2017-05-03 | 2017-07-14 | 福建鑫绿林产品开发有限公司 | The high yield pulp1 production method and production line of a kind of fir essential oil |
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Non-Patent Citations (4)
| Title |
|---|
| 佛手油化学成分研究. 周露等.香料香精化妆品，第2卷. 2000 |
| 佛手油化学成分研究. 周露等.香料香精化妆品，第2卷. 2000 * |
| 玫瑰精油提取工艺研究. 马希汉等.林产化学与工业，第24卷. 2004 |
| 玫瑰精油提取工艺研究. 马希汉等.林产化学与工业，第24卷. 2004 * |
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