CN110437929A - A kind of camphor tree seed oil supercritical CO of response phase method optimization2Extraction process - Google Patents
A kind of camphor tree seed oil supercritical CO of response phase method optimization2Extraction process Download PDFInfo
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- CN110437929A CN110437929A CN201910856147.3A CN201910856147A CN110437929A CN 110437929 A CN110437929 A CN 110437929A CN 201910856147 A CN201910856147 A CN 201910856147A CN 110437929 A CN110437929 A CN 110437929A
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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Abstract
The invention discloses a kind of camphor tree seed oil supercritical COs of response phase method optimization2Extraction process includes the following steps: to pulverize and sieve Camphor Tree Seeds freeze-day with constant temperature；Camphor Tree Seeds after pulverizing and sieving are fitted into extraction kettle, extraction temperature, extracting pressure, extraction time and CO are adjusted2Flow is extracted to setting value, oil yield is calculated after extraction；On the basis of experiment of single factor, it is investigation factor that selecting, which influences three more significant factors to Camphor Tree Seeds oil yield, carries out response surface experiments design and is tested；Experimental data is analyzed and processed by software, establishes mathematical model with the process conditions of Optimized Extraction camphor tree seed oil；Influence of the experimental variable to the response of oil yield is analyzed according to the 3D figure of corresponding response surface, determines final optimum process condition.The oil yield of camphor tree seed oil is up to 38.89% under the process conditions, and mild condition, easy to operate, and the production suitable for camphor tree seed oil is extracted.
Description
Technical field
The invention belongs to field of chemical engineering, and in particular to a kind of camphor tree seed oil supercritical CO of response phase method optimization2It mentions
Taking technique.
Background technique
Camphor Tree Seeds, alias camphor tree pears, big Litsea pungens, camphor tree, camphorwood etc. are the seeds of aiphyllium camphor tree.Camphor tree conduct
One of maximum tree species of economic value in Lauraceae Cinnamomum, have splendid ecological and medicinal benefit, and stock number is huge.But at present
Camphor Tree Seeds are mostly handled with form of waste, and utilization rate is very small, cause the great wasting of resources.
The oil content of Camphor Tree Seeds is up to 40% or more, contains abundant fatty acid in seed oil, such as capric acid, lauric acid, flax
Acid, stearic acid, palmitinic acid etc., wherein two kinds of medium-chain fatty acids of capric acid C10 and lauric acid C12 account for 59.07% He respectively
37.22%, account for 95% of camphor tree seed oil or more.The disease resistance etc. of tomato plant can be enhanced in lauric acid C12；Capric acid C10 can be with
The anti-inflammatory drugs such as sodium houttuyfonate can also be reduced for treating the bacterium infection of the initiations such as pneumococcus, staphylococcus aureus
The content of cholesterol in serum, the illnesss such as treatment hyperlipidemia, thrombus.But it is less to the research of camphor tree seed oil at present, therefore camphor tree
Seed oil has wide development prospect.
Supercritical CO2Fluid extraction technology is the CO low with pressure, cheap and easy to get, environmentally protective using critical-temperature2As
The technology that solvent extracts.Compared with traditional extraction technology, it has, and high income, impurity content is low, oil quality is high,
The features such as process is succinct, low energy consumption.Response surface design method is to integrate the method for experimental design and modeling, in recent years
It is widely used in biotechnology.
Currently, camphor tree seed oil extraction process disclosed in the prior art haves the defects that oil yield is low.
Summary of the invention
The present invention is directed to overcome the deficiencies of the prior art and provide a kind of camphor tree seed oil supercritical CO of response phase method optimization2
Extraction process.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of camphor tree seed oil supercritical CO of response phase method optimization2Extraction process includes the following steps:
Step 1, it by Camphor Tree Seeds freeze-day with constant temperature, and pulverizes and sieves to the Camphor Tree Seeds after drying；
Step 2, the Camphor Tree Seeds after pulverizing and sieving are fitted into extraction kettle, adjust extraction temperature, extracting pressure, extraction time
And CO2Flow connects a receiving bottle in outlet valve and collects camphor tree seed oil, extracted, weighed after extraction to setting value
The weight of gained camphor tree seed oil simultaneously calculates oil yield；
Step 3, on the basis of experiment of single factor, selection on Camphor Tree Seeds oil yield Y influence more significant extraction temperature A,
Tri- factors of extracting pressure B and extraction time C are investigation factor, carry out response surface experiments design by Box-Behnken design method
And it is tested；
Step 4, experimental data is analyzed and processed by software, founding mathematical models are with Optimized Extraction camphor tree seed oil
Process conditions, prediction model are as follows:
Y=38.75+0.35*A+0.22*B+0.62*C+1.44*AB+0.19*AC+1.05*BC-2.2 1*A2-1.56*B2-
1.60*C2
A described in above formula is 45~65 DEG C, and B is 20~30MPa, and C is 30~90min；
Step 5, influence of three investigation factors to the response of oil yield is analyzed according to the 3D figure of corresponding response surface,
And the intuitively reciprocation between assay variable, determine final optimum process condition.
Further, the condition of dry Camphor Tree Seeds is 8 hours dry at 60 DEG C of constant temperature blast drying oven, screening in step 1
Condition was 60~80 meshes.
Further, it is 35~75 DEG C that extraction temperature is adjusted in step 2, and extracting pressure is 15~35MPa, and extraction time is
30~120min, and adjust CO2Flow is fixed as 2.0~2.5L/min.
Further, the oil yield calculation formula in step 2 is as follows:
A kind of camphor tree seed oil supercritical CO2Extraction process will be fitted into extraction kettle after Camphor Tree Seeds drying and crushing, adjust extraction
Temperature, extracting pressure, extraction time are respectively 57 DEG C, 27MPa, 69min, CO2Rate of discharge is 2.0~2.5L/min, in out
Mouth valve connects a receiving bottle and collects camphor tree seed oil, is extracted, is collected.
The utility model has the advantages that
(1) compared with traditional extraction technology, the present invention is by using supercritical CO2Technology is extracted, obtained camphor tree
Seed oil is faint yellow clear oily matter, has the fragrance that camphor tree seed oil is special, and with easy to operate, low energy consumption, without organic molten
The significant advantages such as agent residual, no pollution to the environment.Xu Liyong (development and utilization [J] Wanli College, Zhejiang of Xu Liyong Camphor Tree Seeds
Journal, 2000 (04): 21-22.) pass through solvent extraction camphor tree seed oil and other traditional technologies extractions camphor tree seed oil (Li Zhen
China, Wen Qiang wear the Camphor resources such as little Ying using the Jiangxi status and prospects [J] forestry science and technology, 2007 (06): 30-33+36.)
Oil yield is 3% or so, and best oil yield of the invention is 38.90%, in contrast oil yield is higher by nearly ten times.
(2) present invention is designed the extraction experiments of camphor tree seed oil using response phase method, by extraction temperature, extraction
Pressure, extraction time are investigated, and mathematical regression model is established, and analyze influence of each variable to Camphor Tree Seeds oil yield, and optimize
The process conditions of supercritical technology extraction camphor tree seed oil.By experimental verification, the reality of Camphor Tree Seeds oil yield under Optimal technique process
Testing value and match value has good degree of fitting, and the condition of optimization is suitable for the extraction of camphor tree seed oil.
(3) process conditions of extraction camphor tree seed oil provided by the invention are as follows: 57 DEG C of extraction temperature, extracting pressure 27MPa, extraction
Taking the time is respectively 69min, and mild condition, experimental cost is low, and extraction time is short.It can be the deep development and work of Camphor Tree Seeds product
Industry production provides support and thinking, with certain Technical Reference value and application and popularization value.
Detailed description of the invention
Fig. 1 is the influence of extracting pressure, extraction temperature, extraction time to Camphor Tree Seeds oil yield；
Fig. 2 is the 3D response surface figure that temperature and pressure, temperature and time, time and pressure influence Camphor Tree Seeds oil yield.
Specific embodiment
It is specific with reference to the accompanying drawings and examples to introduce essentiality content of the present invention, but guarantor of the invention is not limited with this
Protect range.
One, experimental material and instrument
1, experimental raw and reagent
Camphor Tree Seeds are purchased from Anhui Province Bozhou medicinal material market.
CO2(volume fraction > 99%) is purchased from Nanjing Shang Yuan industrial gasses factory.
2, instrument and equipment
BJ-300A multifunctional crusher (Deqing Bai Jie Electrical Appliances Co., Ltd)；BS124S assay balance (Beijing Sai Duolisi
Instrument Ltd.)；GZX-9070MBE electric heating constant-temperature blowing drying box (Shanghai Bo Xun Industrial Co., Ltd.)；60~80 meshes
(China Medicine University's storehouse)；TYW-2 air pressure pump (same electromechanical Co., Ltd, Suzhou City)；7071 supercritical CO 2 of model
Extraction equipment (Applied Separations company, the U.S.).
Two, experimental implementation process
A. low-temperature circulating cooler is opened, and temperature is set and is cooled down for 3.5 DEG C；
B. Camphor Tree Seeds are crushed, 60 DEG C are crossed 60~80 meshes after freeze-day with constant temperature 8 hours；
C. it weighs appropriate camphor tree powder of seeds to be placed in extraction kettle, extraction kettle both ends are sealed with absorbent cotton, are encrypted simultaneously
Seal is sealed against powder blocking pipeline；
D. extraction kettle is installed into pipeline according to the principle of " getting on, get off, big after first small "；
E., experimental temperature is set, is begun to warm up, and the temperature at reset valve is set and is heated for 100 DEG C；
F. after temperature reaches preset value, air pressure pump is opened, gas cylinder is opened and valve starts air inlet；
G. after air inlet for a period of time, gas cylinder and valve are closed, whether observation pressure declines, and checks the airtightness of extraction kettle；
It builds device again if not closed, places absorbent cotton and sealing ring；
H. confirm it is closed after, adjusting high-pressure pump knob, be forced into experiment needed for pressure；
I. after pressure stabilisation, receiving flask is connected at the corresponding outlet valve of extraction kettle；Outlet valve is opened, CO is adjusted2
Rate of discharge, start to extract；
J. timing when extraction starts, terminates after reaching the extraction time of setting；The weight of gained camphor tree seed oil is weighed, is calculated
Oil yield；
K. the level that response surface experiment is determined according to single factor test result carries out experiment using Box-Behnken design method and sets
Meter carries out analysis of experimental data using Design-Expert 8.0.6 software, determines the best of supercritical methanol technology extraction camphor tree seed oil
Process conditions.
Three, experiment of single factor
1, influence of the extracting pressure to Camphor Tree Seeds oil yield
Camphor tree powder of seeds after weighing 5.0g drying and sieving, is placed in extraction kettle.Extraction kettle both ends are sealed with absorbent cotton,
Blend rubber sealing ring is sealed.Extraction kettle after charging is installed to supercritical extraction unit, fixed constant temperature circulator
Temperature is 3.5 DEG C, CO2Outlet valve temperature is 100 DEG C, while fixed extractor kettle temperature degree is 45 DEG C.After set temperature to be achieved,
It opens high-pressure pump to pressurize, extracting pressure is respectively 15MPa, 20MPa, 25MPa, 30MPa, 35MPa.Adjust CO2Outlet valve,
Make CO2Rate of discharge is to terminate after extracting 60min within the scope of 2.0~2.5L/min.It is to investigate to refer to the oil yield of Camphor Tree Seeds
Mark, extracting pressure is to supercritical CO2Fig. 1 (a) is shown in the influence of technology extraction camphor tree seed oil.
2, influence of the extraction temperature to Camphor Tree Seeds oil yield
Camphor tree powder of seeds after weighing 5.0g drying and sieving, is placed in extraction kettle.Extraction kettle both ends are sealed with absorbent cotton,
Blend rubber sealing ring is sealed.Extraction kettle after charging is installed to supercritical extraction unit, fixed constant temperature circulator
Temperature is 3.5 DEG C, CO2Outlet valve temperature is 100 DEG C, at the same be arranged extraction kettle temperature be respectively 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C,
75℃.It after reaching this setting value to temperature, opens high-pressure pump and pressurizes, until extracting pressure is fixed as 25MPa.It adjusts
CO2Outlet valve makes CO2Rate of discharge is to terminate after extracting 60min within the scope of 2.0~2.5L/min.With the oil yield of Camphor Tree Seeds
For inspection target, extraction temperature is to supercritical CO2Fig. 1 (b) is shown in the influence of technology extraction camphor tree seed oil.
3, influence of the extraction time to Camphor Tree Seeds oil yield
Camphor tree powder of seeds after weighing 5.0g drying and sieving, is placed in extraction kettle.Extraction kettle both ends are sealed with absorbent cotton,
Blend rubber sealing ring is sealed.Extraction kettle after charging is installed to supercritical extraction unit, fixed constant temperature circulator
Temperature is 3.5 DEG C, CO2Outlet valve temperature is 100 DEG C, while it is 55 DEG C that extraction kettle temperature, which is fixedly installed,.Reach setting to temperature
After value, opens high-pressure pump and pressurize, extracting pressure is fixed as 25MPa.Adjust CO2Outlet valve makes CO2Rate of discharge is 2.0
Within the scope of~2.5L/min, setting extraction time is respectively 30min, 60min, 90min, 120min.With the oil yield of Camphor Tree Seeds
For inspection target, extraction time is to supercritical CO2Fig. 1 (c) is shown in the influence of technology extraction camphor tree seed oil.
Four, the extraction of response phase method optimization camphor tree seed oil
According to above-mentioned experiment of single factor as a result, experimental design is carried out using Box-Behnken design method, with Camphor Tree Seeds
Oil yield is response Y, extraction temperature A, extracting pressure B, and extraction time C is independent variable, carries out the response of Three factors-levels
Face experiment.Response surface experimental design is shown in Table 1.
1 response surface experimental level table of table
It is carried out according to above-mentioned table 1, multiple regression fitting has been carried out to data, has obtained camphor tree seed oil recovery rate Y (i.e. Camphor Tree Seeds
Oil yield) with extraction temperature A, the secondary multinomial regression model equation of extracting pressure B, extraction time C are as follows:
Y=38.75+0.35*A+0.22*B+0.62*C+1.44*AB+0.19*AC+1.05*BC-2.2 1*A2-1.56*B2-
1.60*C2
It is analyzed by software Design-Expert 8.0.6, obtains the results of analysis of variance of the regression model of table 2, and
Can intuitively interactive 3D response surface curve graph between situational variables, see Fig. 2.
2 regression model of table and variance analysis
Note: R2=0.9297；Adj R-Squared=0.8394；Adeq Precision=8.402
As can be seen from Table 2, the P value of the regression model is 0.0028 (< 0.05), and model has conspicuousness；And it loses quasi-
It is that 0.8895 (> 0.05) does not significantly illustrate there is good degree of fitting between the model and true value that item, which examines P value,.Model
Signal-to-noise ratio (Adeq Precision) value is 8.402 (> 4), also illustrates that the model has sufficiently strong signal strength, model has
Effect.
According to camphor tree seed oil recovery rate maximization principle, is solved using regression equation, obtain supercritical CO2Technology extracts camphor tree
The optimum process condition of seeds of trees oil are as follows: 56.73 DEG C of extraction temperature, extracting pressure 26.24MPa, extraction time 68.61min.It examines
Process conditions are modified to 57 DEG C of extraction temperature, extracting pressure 27MPa by the convenience for considering practical operation, and extraction time is
69min.Verification test is carried out, the recovery rate of obtained camphor tree seed oil is 38.13%, is differed with theoretical value (38.89%)
1.95%, within the scope of allowable error, illustrate through the regression equation to supercritical CO2Technology extraction camphor tree seed oil is analyzed
It is that reliably, can use the extraction that the process conditions carry out camphor tree seed oil with prediction.
The oil yield of camphor tree seed oil is up to 38.89% under the process conditions, and mild condition, easy to operate, is suitable for
The production of camphor tree seed oil is extracted.Support and thinking can be provided for the deep development and industrial production of Camphor Tree Seeds product, had certain
Technical Reference value and application and popularization value.
The effect of above-described embodiment is specifically to introduce essentiality content of the invention, but those skilled in the art should know
Protection scope of the present invention should not be confined to the specific embodiment by road.
Claims (5)
1. a kind of camphor tree seed oil supercritical CO of response phase method optimization2Extraction process, which comprises the steps of:
Step 1, it by Camphor Tree Seeds freeze-day with constant temperature, and pulverizes and sieves to the Camphor Tree Seeds after drying；
Step 2, the Camphor Tree Seeds after pulverizing and sieving are fitted into extraction kettle, adjust extraction temperature, extracting pressure, extraction time and CO2
Flow connects a receiving bottle in outlet valve and collects camphor tree seed oil, extracted, gained camphor tree is weighed after extraction to setting value
The weight of seeds of trees oil simultaneously calculates oil yield；
Step 3, on the basis of experiment of single factor, selection influences more significant extraction temperature A, extraction to Camphor Tree Seeds oil yield Y
Tri- factors of pressure B and extraction time C are investigation factor, carry out response surface experiments design by Box-Behnken design method and go forward side by side
Row experiment；
Step 4, experimental data is analyzed and processed by software, founding mathematical models are with the technique of Optimized Extraction camphor tree seed oil
Condition, prediction model are as follows:
Y=38.75+0.35*A+0.22*B+0.62*C+1.44*AB+0.19*AC+1.05*BC-2.2 1*A2-1.56*B2-
1.60*C2
A described in above formula is 45~65 DEG C, and B is 20~30MPa, and C is 30~90min；
Step 5, influence of three investigation factors to the response of oil yield is analyzed according to the 3D figure of corresponding response surface, and straight
The reciprocation between ground assay variable is seen, determines final optimum process condition.
2. extraction process according to claim 1, it is characterised in that: the condition of dry Camphor Tree Seeds is constant temperature drum in step 1
8 hours dry at 60 DEG C of wind drying box, screening condition was 60~80 meshes.
3. extraction process according to claim 1, it is characterised in that: adjusting extraction temperature in step 2 is 35~75 DEG C, extraction
Pressure power is 15~35MPa, and extraction time is 30~120min, and adjusts CO2Flow is fixed as 2.0~2.5L/min.
4. extraction process according to claim 1, it is characterised in that: the oil yield calculation formula in step 2 is as follows:
5. a kind of camphor tree seed oil supercritical CO2Extraction process, it is characterised in that: it will be fitted into extraction kettle after Camphor Tree Seeds drying and crushing,
Adjusting extraction temperature, extracting pressure, extraction time is respectively 57 DEG C, 27MPa, 69min, CO2Rate of discharge is 2.0~2.5L/
Min connects a receiving bottle in outlet valve and collects camphor tree seed oil, extracted, collected.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112940864A (en) * | 2021-02-02 | 2021-06-11 | 云南省农业科学院农产品加工研究所 | Microcapsule slow-release litsea essential oil applicable to meat product preservation |
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Application publication date: 20191112 |