CN105969526A - Extraction method of dalbergia odorifera volatile oil - Google Patents
Extraction method of dalbergia odorifera volatile oil Download PDFInfo
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- CN105969526A CN105969526A CN201610339574.0A CN201610339574A CN105969526A CN 105969526 A CN105969526 A CN 105969526A CN 201610339574 A CN201610339574 A CN 201610339574A CN 105969526 A CN105969526 A CN 105969526A
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the field of pharmaceutical production, and in particular relates to an extraction method of dalbergia odorifera volatile oil. Aiming at the problems that the extraction method of the volatile oil in the prior art is high in energy consumption, long in time consumption, low in efficiency and oil yield, less in charging amount, not enough in purity after purification, and the like, the invention provides a new extraction method of the dalbergia odorifera volatile oil. The method comprises the three steps of medicine pretreatment, distilling extraction and oil-water separation. Furthermore, the method adopts the operation such as filling pure steam at uniform velocity for distilling and condensing by using a two-stage condenser pipe, thus improving the extraction efficiency; the extraction method is free from environmental pollution, safe and reliable, low in energy consumption, high in oil yield, simple in operation and low in cost, thus very easily realizing industrial production.
Description
Technical field
The invention belongs to pharmaceutical manufacturing field, be specifically related to the extracting method of a kind of volatile oil of Lignum Dalbergiae Odoriferae.
Background technology
Lignum Dalbergiae Odoriferae is leguminous plant Lignum Dalbergiae Odoriferae wingceltis Dalbergia odorifera T.Chen trunk and the dry duramen of root, main product in
The ground such as Hainan, Guangdong, Guangxi, Yunnan, have effect of removing stasis to stop bleeding, regulating QI to relieve pain, for epigastric pain, the stagnation of liver-QI side of body
Bitterly, thoracic obstruction twinge etc., its principle active component is volatile oil and flavone compound, and wherein Lignum Dalbergiae Odoriferae main body of oil is anti-
Formula nerolidol.Lignum Dalbergiae Odoriferae oil often is used for preparing " GUANXIN DANSHEN DIWAN ", " GUANXIN DANSHEN PIAN ", " double perfume (or spice) as raw material
Fat capsule ", it is widely used in the treatment of coronary heart disease clinically.
The conventional method extracting volatile oil of Lignum Dalbergiae Odoriferae has steam distillation and supercritical CO2Extraction etc..General pharmacy corporation
Extraction Lignum Dalbergiae Odoriferae oil uses conventional multi-function extractor to coordinate oil water separator employing to boil distillation and extraction method altogether with water and extracts.
This extracting method has some weak point following:
1) power consumption is relatively big, and during extraction, the solution in extraction pot must keep violent fluidized state, so the steam used
Measuring more, require that cooling system must be sufficiently large simultaneously, the cooling water inflow of consumption is bigger.
2) inefficient, general extraction time was at 22-26 hour.
3) volatile oil yield is relatively low, as a example by the medical material of oil content 2%, makes the most typically to extract about 24 hours,
The yield of volatile oil is at 1.0%-1.3%.
4) inventory is less, with 3m3As a example by extraction pot, single inventory is about 300 kilograms.
5) the volatile oil purity after extracting is inadequate, containing partial impurities and moisture, need to carry out refiltering and settlement treatment.
Supercritical CO2Extraction, though biological activity is difficult to be destroyed and simple to operate, energy consumption is low, yield is high, but its
Apparatus expensive, maintenance difficult, industrialized production should not be realized.
Summary of the invention
For prior art is boiled altogether distillation and extraction method and supercritical CO with water2The deficiency that extraction exists, the invention of the present invention
Purpose is to provide the extracting method of a kind of new volatile oil of Lignum Dalbergiae Odoriferae, it can overcome boil altogether with water distillation and extraction method power consumption big,
Efficiency is low, yield is low, inventory is few, purify after the purity problem such as not, and this method is simple to operate, and inventory is big, energy
Consuming low, yield is high, and with low cost, easily realizes industrialized production.
The technical problem to be solved in the present invention is to provide the extracting method of a kind of volatile oil of Lignum Dalbergiae Odoriferae, including three below step:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, the mix homogeneously that adds water after pulverizing carries out water profit,
Place, standby；Or immerse the container equipped with dehydrated alcohol or petroleum ether after choosing the dry duramen pulverizing of Lignum Dalbergiae Odoriferae wingceltis trunk and root
In, the volume of described dehydrated alcohol or petroleum ether is 5-8 times of medical material dry weight, supersound process 45-60min；Supersound process
After medical material put into Soxhlet reflux, the temperature in regulation reflux is 60-90 DEG C, and reflux, extract, 4-8h obtains backflow
Liquid, under 0.04-0.05Mpa pressure, 60-70 DEG C of temperature conditions, concentrates backflow, obtains crude extract；
B, distillation extraction: bottom the medical material after the water obtained in step a profit or crude extract being loaded, carrying of pure steam can be led directly to
Taking in tank, medical material is certain altitude to be accumulated in extraction pot, and medical material surface ensures smooth, has just started during logical steam slow in tank
Slowly opening steam valve, Steam pressure control is at 0.01-0.07MPa, and controlling the steam flow from extraction pot flows out is
80-100kg/h, distillation certain time, (depending on medical material inventory, learning through experimental example, evaporation capacity was the 3-of inventory
5 times can be extracted completely), obtain oil-containing mixed vapour；
C, oil-water separation: the oil-containing mixed vapour obtained in step b is existed by two-stage condensation device, control condensation temperature
85-95 DEG C, entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 65-75 DEG C, prepares fall
Fragrant volatile oil.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, grinding particle size described in step a is 2-10mm, preferably 2-4mm.
Take the Lignum Dalbergiae Odoriferae medical material of same batch, be ground into different grain size, take the medical material after same amount of pulverizing, by the inventive method
Straight-through vaporization method is extracted, result such as table 1, from result in table: be not the thinnest volatile oil of Lignum Dalbergiae Odoriferae of pulverizing medicinal materials
Yield is the highest, and medical material is during being ground into fine powder, and when destroying medical material internal organizational structure or pulverize, temperature raises, and makes
Become the loss of volatile oil；Additionally the inventive method is straight-through steam distillation, and pulverizing medicinal materials is meticulous causes the steam cannot be preferably
Penetrate medical material layer, it is impossible to taken out of well by the volatile oil in medical material and cause volatile oil yield to decline.
Table 1 pulverizing medicinal materials granularity is investigated
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the profit of water described in step a refers to add medical material weight 40%-60%
Water, after mixing place 10-15h.
Preferably, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the profit of water described in step a refers to add medical material weight 45%
Water, places 12h after mixing.
For improving the extraction yield of volatile oil of Lignum Dalbergiae Odoriferae, the medical material after pulverizing adds a small amount of water and carries out moistening, so can make
The medical material deliquescing being dried, histiocyte recovers native state, when beneficially steam penetrates medical material layer when distillation extraction after expanding
Cytoclasis and volatile oil is carried over.Still prevent medical material dust taken out of by steam and to improve volatile oil pure it addition, add water-wet
Degree.
Weighing and be crushed to the Lignum Dalbergiae Odoriferae medical material of 2-4mm in right amount, add different amounts of water and carry out water profit, the water profit time is 12h, point
Do not extract by the inventive method, obtain Lignum Dalbergiae Odoriferae oil, calculate Lignum Dalbergiae Odoriferae oil yield.
Table 2 water profit amount of water is investigated
| Amount of water | 20% | 30% | 40% | 45% | 50% | 60% | 70% | 80% |
| Oil yield | 1.15 | 1.37 | 1.76 | 1.84 | 1.78 | 1.70 | 1.44 | 1.21 |
As can be known from Table 2: amount of water 40%-60% volatile oil yield is more than 1.7%, and amount of water 40%-60% is excellent
Radix Ginseng selection number, and amount of water 45% is optimal.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, described in step b, ensure that the method that steam uniformly rises is:
Steam uniform device is installed bottom extraction pot, and has just started in tank slowly to open steam valve during logical steam.
In the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the steam flow flowed out in step b is investigated: weigh same batch Lignum Dalbergiae Odoriferae medicine
The each 600kg of material, carries out distillation extraction by the inventive method, controls extraction pot and flows out the different flow of steam, carries to volatile oil
Taking complete, record extracts duration and volatile oil yield, and the data obtained is shown in Table 3.
The investigation of the steam flow that table 3 extraction pot flows out
From table 3 it can be seen that steam flow is when 80-100kg/h, volatile oil yield is the highest, is more than 1.7%,
And extraction time is shorter, therefore preferably 80-100kg/h.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, described in step b, the medical material piling height in extraction pot is 1-3m,
And medical material surface to ensure smooth.
Medical material is piled up the highest more uniform in extraction pot, and extraction effect is more preferable.If medical material is not paved whole in tank, medical material
It is low that surface has height to have, and owing to steam would generally flow to the less direction of medical material, causes medical material to be heated inequality, and steam can not be equal
Even contact medical material layer, volatile oil is drawn not exclusively and the some vapor that is lost, finally affects volatile oil yield and has energy loss.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, distillation extraction time described in step b depending on medical material inventory,
Evaporation capacity is 3-5 times of inventory and can extract completely.If inventory is 600kg, the distillation extraction time is that 18-22h can
Extract completely.
Extract criterion the most completely: observe the glass visor of first-stage condenser lower end, see the most whether there is new oil droplet
Occur accumulation, as the most then illustrate the most extracted completely.
Inventory 600kg, carries out distillation extraction three batches by the inventive method, and related data record is shown in Table 3.
4 three batches, table extracts tables of data
| Batch | Extraction time (h) | Evaporation capacity (kg) | Volatile oil yield (%) |
| 1 | 19h | 2712kg | 1.81% |
| 2 | 20h | 2850kg | 1.87% |
| 3 | 18h | 2620kg | 1.77% |
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, condenser described in step c is two-stage condensation device, is divided into one-level
Condenser and secondary condenser.
Using two condensers, it is ensured that condensation effect, the tail vapour that first-stage condenser condensation is not fallen can pass through B-grade condensation
Device condenses.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the steam of band volatile oil described in step c flows before entering condenser
Amount is 80-100kg/h.
The invention have the benefit that the inventive method improves the oil yield of volatile oil of Lignum Dalbergiae Odoriferae, use straight-through pure steam extraction,
Steam can pass more medical material, and to reach volatile oil steam saturated vapor pressure at this temperature, steam takes away more waving
Hair oil.Another one reason, and compared with boiling distillation extraction altogether with water, water of the present invention is considerably less, only the 50% of inventory
Left and right, greatly reduces volatile oil meltage in water, thus improves volatile oil yield.With the medical material of oil content 2% it is
Example, uses the inventive method to extract, and the yield of volatile oil reaches about 1.8%, and traditional method is only about 1.2%.This
Inventive method less energy consumption, traditional distillation extraction that boils altogether with water needs to heat the water of the inventory 4-5 times amount of addition
To boiling and remaining fluidized state, the quantity of steam of needs is relatively big, and the inventive method is to be passed directly into pure steam, and steam is used
Measure and reduce about about 1/2 than traditional extraction process, enter the oil-containing quantity of steam in condenser and boil way of distillation minimizing altogether than with water about
About 1/2, therefore during condensation, the amount of cooling water used also greatly reduces, and reduces energy consumption.The inventive method extraction efficiency is high,
The extraction pot of same volume, the inventory using the inventive method is traditional boil the way of distillation altogether with water 2-2.5 times, because
Need not add substantial amounts of water, and medical material piling height can reach as high as 3 meters in extraction pot, and extraction time can shorten
15-30%, extraction efficiency significantly improves.Volatile oil purity obtained by the inventive method is higher, due to traditional extraction side
Method, when medical material seethes with excitement with water, is often brought part medical material impurity such as unqualified grade into, is needed filtration treatment, side of the present invention after extraction
The medical material that method is extracted be penetrate medical material by steam during the volatile oil of medical material is taken out of, the volatile oil of extraction is clean, it is not necessary to
Carry out filtering or settlement treatment i.e. can get the volatile oil that purity is higher.The inventive method does not uses any organic solvent, nothing
Environmental pollution, safe and reliable.The present invention is the new method that the extraction of volatile oil of Lignum Dalbergiae Odoriferae provides a kind of production suitable for industrialized,
The method equipment is simple, and easy to operate, small investment, operation expense are low, effectively reduce cost, improves economic effect
Benefit.
Detailed description of the invention
The invention provides the extracting method of a kind of volatile oil of Lignum Dalbergiae Odoriferae, comprise the following steps:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, the mix homogeneously that adds water after pulverizing carries out water profit,
Place, standby；Or immerse the container equipped with dehydrated alcohol or petroleum ether after choosing the dry duramen pulverizing of Lignum Dalbergiae Odoriferae wingceltis trunk and root
In, the volume of described dehydrated alcohol or petroleum ether is 5-8 times of medical material dry weight, supersound process 45-60min；Supersound process
After medical material put into Soxhlet reflux, the temperature in regulation reflux is 60-90 DEG C, and reflux, extract, 4-8h obtains backflow
Liquid, under 0.04-0.05Mpa pressure, 60-70 DEG C of temperature conditions, concentrates backflow, obtains crude extract；
B, distillation extraction: bottom the medical material after the water obtained in step a profit or crude extract being loaded, carrying of pure steam can be led directly to
Taking in tank, medical material is certain altitude to be accumulated in extraction pot, and medical material surface ensures smooth, has just started during logical steam slow in tank
Slowly opening steam valve, Steam pressure control at 0.01-0.07MPa, the steam flow controlling extraction pot outflow is
80-100kg/h, distillation certain time, (depending on medical material inventory, learning through experimental example, evaporation capacity was the 3-of inventory
5 times can be extracted completely), obtain oil-containing mixed vapour；
C, oil-water separation: the oil-containing mixed vapour obtained in step b is existed by two-stage condensation device, control condensation temperature
85-95 DEG C, entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 65-75 DEG C, prepares fall
Fragrant volatile oil.
Wherein, in order to accelerate extraction efficiency, improve volatile oil yield, save extraction time, the extraction of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae
In method, grinding particle size described in step a is 2-10mm, preferably 2-4mm.
Wherein, in order to during distillation extraction, volatile oil is drawn faster yield is higher, the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae is carried out
Water profit processes, and described water profit refers to add the water of medical material weight 40%-60%, places 10-15h after mixing.
Preferably, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the profit of water described in step a refers to add medical material weight 45%
Water, places 12h after mixing.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, described in step b, ensure that the method that steam uniformly rises is:
Steam uniform device is installed bottom extraction pot, and has just started in tank slowly to open steam valve during logical steam.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, described in step b, the medical material piling height in extraction pot is 1-3m,
And medical material surface to ensure smooth.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, distillation extraction time described in step b depending on medical material inventory,
Evaporation capacity is 3-5 times of inventory and can extract completely.Extract criterion the most completely: observe first-stage condenser lower end
Glass visor, see and the most whether have new oil droplet that accumulation occurs, as the most then illustrate the most extracted completely.
Wherein, run off to reduce the steam containing volatile oil, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, institute in step c
State condenser and use two-stage condensation device.Steam is after by one-level condensing tube, and the profit steam entrance two grades that failed to condensation is cold
Solidifying pipe, condenses further at B-grade condensation pipe.
Wherein, in the extracting method of above-mentioned volatile oil of Lignum Dalbergiae Odoriferae, the steam of band volatile oil described in step c flows before entering condenser
Amount is 80-100kg/h.
Below by embodiment, the detailed description of the invention of the present invention is described further, but the most therefore by the guarantor of the present invention
Scope of protecting limits in one embodiment.
Each embodiment and comparative example are all as a example by the Lignum Dalbergiae Odoriferae containing volatile oil about 2%.
Embodiment 1
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment: choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 2mm,
Medical material after pulverizing immerses equipped with in the container of petroleum ether, and the volume of described petroleum ether is 5 times of medical material dry weight, supersound process
45min；Soxhlet reflux put into by medical material after supersound process, and the temperature in regulation reflux is 60 DEG C, reflux, extract,
4h, obtains backflow, under 0.04Mpa pressure, 60 DEG C of temperature conditionss, concentrates backflow, obtains crude extract；
B, distillation extraction: can lead directly to bottom being loaded by the crude extract obtained in step a in the extraction pot of pure steam, medical material exists
Certain altitude to be accumulated in extraction pot, medical material surface ensures smooth, has just started slowly to open steam valve during logical steam in tank,
Steam pressure 0.01Mpa, the steam flow controlling to flow out from extraction pot is 80kg/h, the volatile oil when steam penetrates medical material layer
Being carried over therewith, condenser front end is installed steam-flow meter and is monitored the profit steam flow entering condenser at any time, and distillation is certain
Time, obtain oil-containing mixed vapour；
C, oil-water separation: the oil-containing mixed vapour obtained in step b is existed by two-stage condensation device, control condensation temperature
85 DEG C, entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 65 DEG C, prepares Lignum Dalbergiae Odoriferae volatilization
Oil.
Embodiment 2
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment: choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 4mm,
Medical material after pulverizing immerses equipped with in the container of petroleum ether, and the volume of described petroleum ether is 8 times of medical material dry weight, supersound process
60min；Soxhlet reflux put into by medical material after supersound process, and the temperature in regulation reflux is 90 DEG C, reflux, extract,
8h, obtains backflow, under 0.05Mpa pressure, 70 DEG C of temperature conditionss, concentrates backflow, obtains crude extract；
B, distillation extraction: can lead directly to bottom being loaded by the crude extract obtained in step a in the extraction pot of pure steam, medical material exists
Certain altitude to be accumulated in extraction pot, medical material surface ensures smooth, has just started slowly to open steam valve during logical steam in tank,
Steam pressure 0.07MPa, the steam flow controlling to flow out from extraction pot is 100kg/h, volatilizees when steam penetrates medical material layer
Oil is carried over therewith, and condenser front end is installed steam-flow meter and monitored the profit steam flow entering condenser at any time, distills one
Fix time, obtain oil-containing mixed vapour；
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 95 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 75 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 3
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment: choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 10mm,
Medical material after pulverizing immerses equipped with in dehydrated alcohol, and the volume of described dehydrated alcohol is 6 times of medical material dry weight, supersound process
50min；Soxhlet reflux put into by medical material after supersound process, and the temperature in regulation reflux is 70 DEG C, reflux, extract,
6h, obtains backflow, under 0.04Mpa pressure, 65 DEG C of temperature conditionss, concentrates backflow, obtains crude extract；
B, distillation extraction: can lead directly to bottom being loaded by the crude extract obtained in step a in the extraction pot of pure steam, medical material exists
Certain altitude to be accumulated in extraction pot, medical material surface ensures smooth, has just started slowly to open steam valve during logical steam in tank,
Steam pressure 0.07Mpa, the steam flow controlling to flow out from extraction pot is 100kg/h, volatilizees when steam penetrates medical material layer
Oil is carried over therewith, and condenser front end is installed steam-flow meter and monitored the profit steam flow entering condenser at any time, distills one
Fix time, obtain oil-containing mixed vapour；
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 90 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 70 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 4
Extract by the method outside technical solution of the present invention:
A, medical material pre-treatment: choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 6mm,
Medical material after pulverizing immerses equipped with in the container of dehydrated alcohol, and described dehydrated alcohol volume is 8 times of medical material dry weight, ultrasonic place
Reason 60min；Soxhlet reflux put into by medical material after supersound process, and the temperature in regulation reflux is 100 DEG C, backflow
Extract 8h, obtain backflow, under 0.03Mpa pressure, 50 DEG C of temperature conditionss, backflow is concentrated, is slightly carried
Thing；
B, distillation extraction: can lead directly to bottom being loaded by the crude extract obtained in step a in the extraction pot of pure steam, medical material exists
Certain altitude to be accumulated in extraction pot, medical material surface ensures smooth, has just started slowly to open steam valve during logical steam in tank,
Steam pressure 0.01Mpa, the steam flow controlling to flow out from extraction pot is 100kg/h, volatilize when steam penetrates medical material layer
Oil is carried over therewith, and condenser front end is installed steam-flow meter and monitored the profit steam flow entering condenser at any time, distills one
Fix time, obtain oil-containing mixed vapour；
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 80 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 70 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 5
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 2-4mm,
Medical material after pulverizing first carries out water profit, adds and drinks the water yield 40%, places 10 hours after mixing；
B, distillation extraction: can lead directly in the extraction pot of pure steam bottom the medical material loading after the water obtained in step a is moistened,
Piling height certain altitude wanted in extraction pot by medical material, and medical material surface ensures smooth, has just started slowly to open during logical steam in tank
Steam valve, steam pressure 0.01Mpa, the steam flow controlling extraction pot outflow is 80kg/h, distills certain time,
To oil-containing mixed vapour.
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 85 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 65 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 6
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 8-10mm,
Medical material after pulverizing first carries out water profit, adds and drinks the water yield 60%, places 15 hours after mixing；
B, distillation extraction: can lead directly in the extraction pot of pure steam bottom the medical material loading after the water obtained in step a is moistened,
Medical material wants piling height to be 1-3m in extraction pot, and medical material surface ensures smooth, has just started slowly to open during logical steam in tank
Steam valve, steam pressure 0.07Mpa, the steam flow controlling extraction pot outflow is 100kg/h, distills certain time,
Obtain oil-containing mixed vapour.
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 95 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 75 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 7
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 4-6mm,
Medical material after pulverizing first carries out water profit, adds and drinks the water yield 60%, places 15 hours after mixing；
B, distillation extraction: can lead directly in the extraction pot of pure steam bottom the medical material loading after the water obtained in step a is moistened,
Medical material wants piling height to be 1-3m in extraction pot, and medical material surface ensures smooth, has just started slowly to open during logical steam in tank
Steam valve, steam pressure 0.05Mpa, the steam flow controlling extraction pot outflow is 90kg/h, distills certain time,
To oil-containing mixed vapour.
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 80 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 70 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Embodiment 8
Volatile oil of Lignum Dalbergiae Odoriferae is extracted by technical solution of the present invention:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, pulverize, grinding particle size is about 2-4mm,
Medical material after pulverizing first carries out water profit, adds and drinks the water yield 45%, places 12 hours after mixing；
B, distillation extraction: can lead directly in the extraction pot of pure steam bottom the medical material loading after the water obtained in step a is moistened,
Medical material wants piling height to be 1-3m in extraction pot, and medical material surface ensures smooth, has just started slowly to open during logical steam in tank
Steam valve, steam pressure 0.03Mpa, the steam flow controlling extraction pot outflow is 90kg/h, distills certain time,
To oil-containing mixed vapour.
C, oil-water separation: the oil-containing mixed vapour obtained in step b passes through condenser, and control condensation temperature is at 90 DEG C, afterwards
Entering oil water separator, oil-water separation temperature controls to separate under the conditions of 70 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
Comparative example 9
Carry out extracting volatile oil of Lignum Dalbergiae Odoriferae with boiling distillation and extraction method altogether with water.
Adding the water accounting for container 3/4 in water vapour generating bottle, after whole distilling apparatus to be checked is air tight, outward winding T
Type pipe, is heated to boiling, when there being a large amount of water vapour produce and go out from the arm of T-shaped pipe, closes T-shaped pipe, water vapour
Enter in alembic, alembic loads the Lignum Dalbergiae Odoriferae wingceltis trunk after pulverizing and the dry duramen of root, starts distillation, work as effluent
During without obvious oil droplet, clear, stop distillation.
The result of each embodiment and comparative example is as shown in the table:
The extraction effect table of table 5 Different Extraction Method
Note: extraction time is the time extracted completely.
From table 5 result of the test, using technical solution of the present invention to carry out volatile oil of Lignum Dalbergiae Odoriferae extraction, purification efficiency is high, purifies the time
18-20h can extract completely, and purifies time 22-26h, side of the present invention with traditional distillation and extraction method that boils altogether with water
Method has effectively been saved the time, improves efficiency, and cooling water amount when decreasing steam consumption and condense, saves
Cost；On the other hand, the extraction yield of volatile oil of Lignum Dalbergiae Odoriferae is high, and its volatile oil yield of the Lignum Dalbergiae Odoriferae medical material of oil content 2% reaches
More than 1.7%, compare traditional method and improve 30%-40%, and volatile oil purity is high, is not required to through separating-purifying step,
Simplify operation, save cost.
Claims (10)
1. the extracting method of a volatile oil of Lignum Dalbergiae Odoriferae, it is characterised in that comprise the following steps:
A, medical material pre-treatment；Choosing Lignum Dalbergiae Odoriferae wingceltis trunk and the dry duramen of root, the mix homogeneously that adds water after pulverizing carries out water profit, puts
Put, standby；Or immerse in the container equipped with dehydrated alcohol or petroleum ether after choosing the dry duramen pulverizing of Lignum Dalbergiae Odoriferae wingceltis trunk and root,
The volume of described dehydrated alcohol or petroleum ether is 5-8 times of medical material dry weight, supersound process 45-60min；Medicine after supersound process
Soxhlet reflux put into by material, and the temperature in regulation reflux is 60-90 DEG C, and reflux, extract, 4-8h obtains backflow,
Under 0.04-0.05Mpa pressure, 60-70 DEG C of temperature conditions, backflow is concentrated, obtains crude extract；
B, distillation extraction: the extraction of pure steam bottom the medical material after the water obtained in step a profit or crude extract being loaded, can be led directly to
In tank, medical material is certain altitude to be accumulated in extraction pot, and medical material surface ensures smooth, has just started during logical steam slow in tank
Opening steam valve, Steam pressure control is at 0.01-0.07MPa, and the steam flow that extraction pot flows out controls at 80-100kg/h,
Distillation certain time, obtain oil-containing mixed vapour；
C, oil-water separation: by the oil-containing mixed vapour that obtains in step b by condenser, control condensation temperature at 85-95 DEG C,
Entering oil water separator afterwards, oil-water separation temperature controls to separate under the conditions of 65-75 DEG C, prepares volatile oil of Lignum Dalbergiae Odoriferae.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: pulverize grain described in step a
Degree is 2-10mm.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 2, it is characterised in that: pulverize grain described in step a
Degree is 2-4mm.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: the profit of water described in step a is
Refer to add the water of medical material weight 40%-60%, after mixing, place 10-15h.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 4, it is characterised in that: the profit of water described in step a is
Refer to add the water of medical material weight 45%, after mixing, place 12h.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: ensure described in step b to steam
The method that vapour uniformly rises is: installs steam uniform device bottom extraction pot, and has just started in tank slowly to open steaming during logical steam
Steam valve door.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: extraction pot described in step b
In medical material piling height be 1-3m, and medical material surfacing.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: distillation described in step b carries
Evaporation capacity was 3-5 times of inventory and can extract completely depending on medical material inventory the time that takes.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: condenser described in step c
For two-stage condensation device, it is divided into first-stage condenser and secondary condenser.
The extracting method of volatile oil of Lignum Dalbergiae Odoriferae the most according to claim 1, it is characterised in that: described in step c, band is waved
Before the steam entrance condenser of hair oil, flow is 80-100kg/h.
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| CN114507569A (en) * | 2022-02-28 | 2022-05-17 | 德格宗萨藏医药有限公司 | Extraction process of essential oil of Tibetan cedar at high altitude |
| CN114989894A (en) * | 2022-06-10 | 2022-09-02 | 吉水县金海天然香料油科技有限公司 | Method for extracting dalbergia wood volatile oil |
| CN114989894B (en) * | 2022-06-10 | 2023-12-22 | 吉水县金海天然香料油科技有限公司 | Extraction method of dalbergia wood volatile oil |
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