CN104004590B - DANGUIHUA method of extraction of essential oil - Google Patents
DANGUIHUA method of extraction of essential oil Download PDFInfo
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Abstract
The invention discloses a kind of DANGUIHUA method of extraction of essential oil, comprise the pre-treatment of DANGUIHUA raw material, extraction, essential oil collection step, the pre-treatment of described DANGUIHUA raw material is specially: pickle fresh flower with salt, sealing, be stored in freezer for subsequent use, while pickling, the consumption of salt is fresh flower weight 8%～12%, and in freezer, storage temperature is 15～20 DEG C. The present invention reaches by the pre-treatment to material, the technology such as suitable extracting parameter, introducing second distillation of setting the object of extracting DANGUIHUA volatile ingredient, do not introducing under the prerequisite of organic solvent, not only effectively ensure that in DANGUIHUA, most of volatile ingredient is suggested, avoid the introducing of non-DANGUIHUA derived essential oil, the recovery rate of DANGUIHUA essential oil is exceeded to 20% left and right compared with other distil process simultaneously, effectively improved DANGUIHUA essential oil yield in process of production.
Description
Technical field
The invention belongs to natural perfume material research and development field, be specifically related to a kind of DANGUIHUA extraction of essential oil technique.
Background technology
Orange osmanthus is the one of sweet osmanthus, belongs to the evergreen xylophyta of Oleaceae Osmanthus, opens Chinese red flower, and flowery odour is strong,In China, cultivation history is long, apart from the modern approximately history of existing 2500, originates in China Yangtze river basin to south China, southwestVarious places, generally cultivate with various places to the north of reaching southern ridge in the south in the Qinling Mountains. Be one of China's ten great tradition famous flowers, its flower is rare spice,Flower contains the multiple aromatic substances such as lactones in the last of the ten Heavenly stems, irisone, linalool oxide and nerol, can extract aromatic oil,Be used for allocating daily cosmetics, be also used as for a long time food flavor and be utilized.
At present, more than 30 of the built vertical orange osmanthus nursery stock bases of China's Fujian Province's Pucheng County, cultivate each age grade nursery stock more than 600Wan Zhu, aggregate resource cultivation scale exceedes 20,000 mu, produces more than 30 ten thousand kilograms of fresh sweet osmanthus per year, and flower production is fixed, butAt home to orange osmanthus fresh flower without add deep processing extraction process lack or more extensive, conventional medicinal extract extracts without advantage competitionPower, causes DANGUIHUA to be mainly used in eating raw in locality or makes osmanthus flower tea and be not used effectively, and its economic value added is notHeight, the chain of also failing to drive the industry further extends.
In order to utilize fresh flower, improve the economic benefit of orange osmanthus, the inventor carries sweet osmanthus active ingredient forefathersGet on the existing basis of research and carried out correlative study, propose a kind of DANGUIHUA volatile effective component extraction process, adoptThis technique can obtain volatile effective component in DANGUIHUA, and makes the more existing extracting method of the same race of its yield improve 20%Left and right under prerequisite with an organic solvent not, extracts to greatest extent volatile ingredient technology is provided from DANGUIHUAInstruct.
Summary of the invention
The object of the invention is, on the basis of existing extractive technique, to improve, provide a kind of DANGUIHUA essential oil to carryAccess method. The present invention reaches by the pre-treatment to material, the technology such as suitable extracting parameter, introducing second distillation of settingTo the object of extracting DANGUIHUA volatile ingredient, do not introducing under the prerequisite of organic solvent, improve carrying of existing extractive techniqueGet rate.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of DANGUIHUA method of extraction of essential oil, comprise the pre-treatment of DANGUIHUA raw material, extraction, essential oil collection stepSuddenly, the pre-treatment of described DANGUIHUA raw material is specially: pickle fresh flower with salt, sealing, be stored in freezer for subsequent use, salt while picklingConsumption be fresh flower weight 8%～12%, in freezer, storage temperature is 15～20 DEG C.
Preferably, described extraction is specially: adopt steam extraction device to carry out Steam Heating extraction, vapour pressure is controlled at0.4～0.7MPa, in the time that distillate starts to flow out, steam extraction device internal temperature is 95～105 DEG C. Control steam addsPressure, the temperature in when heat, make the outflow that distillate can be at the uniform velocity stable, and distillation duration is set rationally, can make raw material fillDivide and be extracted, do not waste again resource as far as possible.
Preferably, described extraction also comprises the step of distillation again, is specially: the distillate of described steam extraction deviceOutlet is connected with oil water separator, extracts after the distillate water-oil separating obtaining, and the efflux of oil water separator is carried out againInferior distillation, controlling vapo(u)rizing temperature is 90～100 DEG C, pressure is 1 atmospheric pressure.
Preferably, described oil water separator is bore 8～10cm, the oily light-water heavy duty oil separator of long 40～45cm.
Preferably, described essential oil is collected and is specially: after core intersection in oil water separator no longer increases, control distillateTemperature is 50～60 DEG C, after upper strata oil reservoir all melts, closes oil water separator lower layer of water flow export, and liquid level rises,When reaching after the height of oil-out, fluid oil flows out.
Preferably, the fluid oil of described outflow is collected in dark container, after static solidifying, and Physical withdrawing moisture, closeClose low temperature storage.
In DANGUIHUA method of extraction of essential oil of the present invention, described extraction procedure more specifically: check the sealing of extraction elementProperty, the DANGUIHUA of handling well is dropped in the material pot of extraction equipment, control according to the amount that drops into material and add the water yield,Amount of water is advisable for submergence raw material just, prevents that liquid level is too high, goes out along steam channel, pollutes essential oil; After being watered,Cover filler, check air-tightness, with anti-gas-leak; Open steam generator, open pipe valve, wait whole device logicalAfter gas is normal, shut gas valve, after vapour pressure rises to 0.4MPa, slowly open gas valve, make steam flatSteady supply; Open condensation cycle water, device, under normal operating conditions, regulates the flow velocity of condensed water, makes to steam gasOutflow is all in a liquid state; Distillate enters oil water separator, in separator, by after fluid cushion, presents water-oil separatingState, reaches after level altitude, and lower layer of water flows out from oil water separator, after collection, again separates, and controls and separatesThe vapo(u)rizing temperature of device is 90～100 DEG C of left and right, and pressure is 1 atmospheric pressure.
In DANGUIHUA method of extraction of essential oil of the present invention, described essential oil collection method is more specifically: treat in oil water separatorCore intersection, not after increase, regulates the flow velocity of condensed water, and efflux temperature is raise, be controlled within the scope of 50～60 DEG C,In oil water separator, solid-state orange osmanthus essential oil, along with after temperature raises, slowly presents liquid condition, after oil reservoir all melts,Close lower layer of water flow export, liquid level rises, and when reaching after the height of oil-out, fluid oil flows out, be collected in brown bottle,Labeling indicates essential oil title, the place of production, extraction time, removes moisture low temperature and preserves.
Compared with prior art, the beneficial effect that the present invention has is: the present invention can effectively extract in DANGUIHUA and containVolatile effective component, and ensure not introduce composition in other non-DANGUIHUA, extend the man-hour that adds of DANGUIHUA extraction of essential oilBetween, more traditional extracting mode is compared, and improves the yield of DANGUIHUA volatile effective component in 20% left and right, has improved orange osmanthusEconomic value added, for effective extraction of DANGUIHUA essential oil provides technological guidance, extended the industrial chain of orange osmanthus exploitation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail. Following examples will contribute to the technology people of this areaMember further understands the present invention, but does not limit in any form the present invention. It should be pointed out that the common skill to this areaArt personnel, without departing from the inventive concept of the premise, can also make some distortion and improvement. These all belong toProtection scope of the present invention.
Embodiment 1
The present embodiment relates to a kind of DANGUIHUA method of extraction of essential oil, carries out according to the following steps:
1, charging: the DANGUIHUA refrigerating after pickled is packed into the material pot of distilling apparatus in the freezer of 15～20 DEG C, chargingIn time, should ensure moisture and admittedly expect whole input in material pots.
2, unit state: except steam inlet links with steam generator, outside distillate outlet links with oil water separator, wholeIndividual device is in air-tight state, and air-tightness is better, prevents gas leak phenomenon.
3, extracting method:
(1) mode of heating: Steam Heating.
(2) extracting parameter: vapour pressure is controlled at 0.4MPa, internal temperature is at 95 DEG C.
(3) setting of oil water separator: it is suitable to choose according to capacity, the distillate rate of outflow and the essential oil character of deviceOil water separator, in this extraction process, the bore of oil water separator is 8～10cm, and length is that 40～45cm is advisable, and oil is lightWater heavy type, adopts glass tempering material, transparent visual.
(4) distillation again: again distill mode of heating to cushion the liquid reserving after static in oil water separatorFor direct electrical heating, heating and temperature control is at 90 DEG C, and pressure is 1 atmospheric pressure.
5, collect and store:
(1) collect: under orange osmanthus essential oil normal temperature, be solid-state, be reduce essential oil wall built-up lose, before collection by water-oil separatingOil reservoir in device dissolves, and solution temperature is unsuitable too high, prevents that essential oil is oxidized, is controlled at 50～60 DEG C, is collected in brownIn bottle.
(2), except moisture: essential oil must be taken portion of water out of after taking out, after essential oil is collected in container, leave standstill one sectionTime, natural coagulation, takes moisture wherein away with physical method.
(3) store: the essential oil after dewatering is contained in airtight brown container, carries out low-temperature storage.
Embodiment 2
The present embodiment relates to a kind of DANGUIHUA method of extraction of essential oil, carries out according to the following steps:
1, charging: the DANGUIHUA refrigerating after pickled is packed into the material pot of distilling apparatus in the freezer of 15～20 DEG C, dressWhen material, should ensure that moisture and solid material all drop in material pot.
2, unit state: except steam inlet links with steam generator, outside distillate outlet links with oil water separator, wholeIndividual device is in air-tight state, and air-tightness is better, prevents gas leak phenomenon.
3, extracting method:
(1) mode of heating: Steam Heating.
(2) extracting parameter: vapour pressure is controlled at 0.5MPa, internal temperature is at 100 DEG C.
(5) setting of oil water separator: it is suitable to choose according to capacity, the distillate rate of outflow and the essential oil character of deviceOil water separator, in this extraction process, the bore of oil water separator is 8～10cm, and length is that 40～45cm is advisable, and oil is lightWater heavy type, adopts glass tempering material, transparent visual.
(6) distillation again: again distill mode of heating to cushion the liquid reserving after static in oil water separatorFor direct electrical heating, heating and temperature control is at 95 DEG C, and pressure is 1 atmospheric pressure.
6, collect and store:
(1) collect: under orange osmanthus essential oil normal temperature, be solid-state, be reduce essential oil wall built-up lose, before collection by water-oil separatingOil reservoir in device dissolves, and solution temperature is unsuitable too high, prevents that essential oil is oxidized, is controlled at 50～60 DEG C, is collected in brownIn bottle.
(2), except moisture: essential oil must be taken portion of water out of after taking out, after essential oil is collected in container, leave standstill one sectionTime, natural coagulation, takes moisture wherein away with physical method.
(3) store: the essential oil after dewatering is contained in airtight brown container, carries out low-temperature storage.
Embodiment 3
The present embodiment relates to a kind of DANGUIHUA method of extraction of essential oil, carries out according to the following steps:
1, charging: the DANGUIHUA refrigerating after pickled is packed into the material pot of distilling apparatus in the freezer of 15～20 DEG C, chargingIn time, should ensure moisture and admittedly expect whole input in material pots.
2, unit state: except steam inlet links with steam generator, outside distillate outlet links with oil water separator, wholeIndividual device is in air-tight state, and air-tightness is better, prevents gas leak phenomenon.
3, extracting method:
(1) mode of heating: Steam Heating.
(2) extracting parameter: vapour pressure is controlled at 0.7MPa, internal temperature is at 105 DEG C.
(7) setting of oil water separator: it is suitable to choose according to capacity, the distillate rate of outflow and the essential oil character of deviceOil water separator, in this extraction process, the bore of oil water separator is 8～10cm, and length is that 40～45cm is advisable, and oil is lightWater heavy type, adopts glass tempering material, transparent visual.
(8) distillation again: again distill mode of heating to cushion the liquid reserving after static in oil water separatorFor direct electrical heating, heating and temperature control is at 100 DEG C, and pressure is 1 atmospheric pressure.
7, collect and store:
(1) collect: under orange osmanthus essential oil normal temperature, be solid-state, be reduce essential oil wall built-up lose, before collection by oil water separatorIn oil reservoir dissolve, solution temperature is unsuitable too high, prevents that essential oil is oxidized, is controlled at 50～60 DEG C, is collected in brown bottleIn.
(2), except moisture: essential oil must be taken portion of water out of after taking out, after essential oil is collected in container, leave standstill one sectionTime, natural coagulation, takes moisture wherein away with physical method.
(3) store: the essential oil after dewatering is contained in airtight brown container, carries out low-temperature storage.
By implementation and operation, result is as shown in table 1 below:
Table 1
Result from table 1 can find out, by this technique, in DANGUIHUA the extraction yield of volatile ingredient more existing with(petal under adopting is distilled on the spot, directly put in distillation equipment, its mode of heating is coal fire to plant extracting methodHeating, distillation parameter pressure values is about an atmospheric pressure, does not carry out second distillation) improve closely 20%, this increase rate isDo not introducing under the prerequisite of organic solvent, by improving, existing extraction process obtains.
Above specific embodiments of the invention are described. It will be appreciated that, the present invention is not limited toState specific implementations, those skilled in the art can make various distortion or amendment within the scope of the claims,This does not affect flesh and blood of the present invention.
Claims (3)
1. a DANGUIHUA method of extraction of essential oil, comprises the pre-treatment of DANGUIHUA raw material, extraction, essential oil collection step, itsBe characterised in that, the pre-treatment of described DANGUIHUA raw material is specially: pickle fresh flower with salt, sealing, is stored in freezer for subsequent usely, salts downTime processed, the consumption of salt is fresh flower weight 8%～12%, and in freezer, storage temperature is 15～20 DEG C;
Described extraction is specially: adopt steam extraction device to carry out Steam Heating extraction, and vapour pressure is controlled at 0.4～0.7MPa, in the time that distillate starts to flow out, steam extraction device internal temperature is 95～105 DEG C;
Described extraction also comprises the step of distillation again, is specially: distillate outlet and the oil of described steam extraction deviceSeparator connects, and extracts after the distillate water-oil separating obtaining, the efflux of oil water separator is distilled again,Controlling vapo(u)rizing temperature is 90～100 DEG C, and pressure is 1 atmospheric pressure;
Described oil water separator is bore 8～10 ㎝, the oily light-water heavy duty oil separator of long 40～45 ㎝.
2. DANGUIHUA method of extraction of essential oil according to claim 1, is characterized in that, described essential oil is collected concreteFor: after core intersection in oil water separator no longer increases, controlling distillate temperature is 50～60 DEG C, treats that upper strata oil reservoir is completePortion closes oil water separator lower layer of water flow export after melting, and liquid level rises, when reaching after the height of oil-out, and fluid oilFlow out.
3. DANGUIHUA method of extraction of essential oil according to claim 2, is characterized in that, the fluid oil of described outflowBe collected in dark container, after static solidifying, Physical withdrawing moisture, airtight low temperature storage.
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| CN105112164A (en) * | 2015-09-15 | 2015-12-02 | 福建玫瑰谷生态农业发展有限公司 | Method for extracting rose essential oil |
| CN107699345A (en) * | 2016-08-08 | 2018-02-16 | 庞锦霞 | A kind of method of osmanthus essential oil extraction |
| CN106367204A (en) * | 2016-08-31 | 2017-02-01 | 恒枫食品科技有限公司 | Osmanthus flower essence containing natural osmanthus flower fragrance and preparation method thereof |
| CN109576062A (en) * | 2019-02-12 | 2019-04-05 | 无锡薇泰药物技术有限公司 | A kind of Chinese yew hydrosol extraction process |
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