CN109321360A - A kind of depickling refining methd of peony seed oil - Google Patents
A kind of depickling refining methd of peony seed oil Download PDFInfo
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- CN109321360A CN109321360A CN201811354399.8A CN201811354399A CN109321360A CN 109321360 A CN109321360 A CN 109321360A CN 201811354399 A CN201811354399 A CN 201811354399A CN 109321360 A CN109321360 A CN 109321360A
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- extraction
- carbon dioxide
- depickling
- peony
- seed oil
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
Abstract
The present invention provides a kind of depickling refining methds of peony seed oil, comprising: is extracted using supercritical carbon dioxide to the peony seeds crude oil, obtains purification peony seed oil；The pressure of the extraction is 15Mpa~25Mpa, and the temperature of extraction is 60 DEG C~80 DEG C.The present invention controls extracting pressure and extraction temperature, so that supercritical carbon dioxide has good solvability to the free fatty acid in peony seeds crude oil, and then free fatty acid is extracted from peony seeds crude oil, obtains purification peony seed oil.The purification peony seed oil that depickling refining methd provided by the invention obtains have the intrinsic smell of peony seed oil, free from extraneous odour, oil body clarification, in faint yellow, oil quality is good；And no solvent residue；Acid value is 0.83KOH mg/g, and acid value is low；Peroxide value is 0.23mmol/kg, illustrates that stability is good.
Description
Technical field
The present invention relates to edible oil extractive technique field more particularly to a kind of depickling refining methds of peony seed oil.
Background technique
Currently, the extracting mode of peony seed oil mainly have squeezing method, extraction method, prepressing extraction method, subcritical method and
Supercritical carbon dioxide extraction method etc..
Squeezing method is that raw material is first passed through to the technique for frying and being squeezed by physics mode, but a disadvantage is that seedcake Residual oil
Rate is high, and causes acid value and peroxide value to increase because heat treatment time is too long.
Extraction method is that oil plant is passed through high temperature using No. six solvent naphthas or the n-hexane principle that mixes similar to grease
Dissolution edible oil and fat are impregnated, are eaten using traditional " five is de- " (as depickling, decoloration, degumming, dehydration, deodorization) technique
The method of oil.The method biggest advantage is that oil yield is high (> 96%), but the disadvantage is that quality of crude oil is poor, subsequent technique is cumbersome,
And dissolvent residual is had, it causes damages to human health and environment.
Prepressing extraction method is to first pass through physics mode to squeeze out a part of grease, and remaining seedcake recycles extraction method
Remaining grease is extracted, the disadvantages of the method still has excessively high acid value, peroxide value and dissolvent residual.
Subcritical method is using butane to oil extraction, and the method is the disadvantage is that butane residual is serious.
Supercritical carbon dioxide extraction method is to certain special natural products using supercritical carbon dioxide with special molten
Solution effect carrys out the method for abstracting tree peony seed oil using the solvability of supercritical carbon dioxide and the relationship of its density.With it is above-mentioned
Unlike four kinds of extracting methods, due to CO2It is the nontoxic gas of colorless and odorless under fluid normality, after being separated with extraction component,
The absolutely not residual of solvent, extraction temperature is low, can be effectively prevented the oxidation of heat-sensitive ingredients, complete reservation biomass
Bioactivity is not necessarily to solvent recovery, and therefore, supercritical carbon dioxide extraction method is used widely.But faced at present using super
The problem of carbon dioxide extraction method still generally existing acid value of lipids extracted in boundary's is excessively high, does not meet national standard.
Summary of the invention
The purpose of the present invention is to provide a kind of depickling refining methds of peony seed oil；Using depickling purification side of the invention
The peony seed oil oil quality that method obtains is good, no solvent residue and acid value are low.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of depickling refining methds of peony seed oil, comprising the following steps: uses overcritical titanium dioxide
Carbon extracts peony seeds crude oil, obtains purification peony seed oil；The pressure of the extraction is 15Mpa~25Mpa, the temperature of extraction
Degree is 60 DEG C~80 DEG C.
Preferably, the time of the extraction is 30~120min.
Preferably, the extraction also obtains carrying the supercritical carbon dioxide of free fatty acid；It is also wrapped after the extraction
The separation to the supercritical carbon dioxide for carrying free fatty acid is included, the isolated temperature is 30 DEG C~60 DEG C, point
From pressure be 5Mpa~20Mpa.
Preferably, the depickling purification carries out in supercritical carbon dioxide extraction apparatus, to the overcritical titanium dioxide
Carbon extraction equipment be passed through carbon dioxide gas generate supercritical carbon dioxide, the carbon dioxide gas be passed through speed be 2~
20L/h。
Preferably, purity >=99.99% of the carbon dioxide gas.
Preferably, it after generating supercritical carbon dioxide, is continually fed into the supercritical carbon dioxide extraction apparatus male
Red seed crude oil is extracted, and the speed that is passed through of the peony seeds crude oil is 2~15mL/min.
Preferably, the peony seeds crude oil is obtained by peony seeds by cold pressing.
It preferably, further include being de-gassed to the peony seed oil being obtained by extraction after the extraction.
The present invention provides a kind of depickling refining methds of peony seed oil, comprising the following steps: uses overcritical titanium dioxide
Carbon extracts peony seeds crude oil, obtains purification peony seed oil；The pressure of the extraction is 15Mpa~25Mpa, the temperature of extraction
Degree is 60 DEG C~80 DEG C.It is 15Mpa~25Mpa that the present invention, which controls extracting pressure, and extraction temperature is 60 DEG C~80 DEG C, so that super face
Boundary's carbon dioxide has good solvability to the free fatty acid in peony seeds crude oil, and then insoluble to fatty glyceride
Solution, and then free fatty acid is extracted from peony seeds crude oil, obtain purification peony seed oil.Embodiment the result shows that, this
Smell, free from extraneous odour, the oil body that the purification peony seed oil that the depickling refining methd that invention provides obtains has peony seed oil intrinsic are clear
Clearly, in faint yellow, oil quality is good；And no solvent residue；Acid value is 0.83KOH mg/g, and acid value is low；Peroxide value is
0.23mmol/kg illustrates that stability is good.
In addition, the present invention also have instrumentation it is easy, can continuous production, be not required to recycling design, extraction efficiency it is high and
Energy consumption is less, save the cost, is easily enlarged the advantages that production.
Specific embodiment
The present invention provides a kind of depickling refining methds of peony seed oil, comprising the following steps: uses overcritical titanium dioxide
Carbon extracts peony seeds crude oil, obtains purification peony seed oil；The pressure of the extraction is 15Mpa~25Mpa, the temperature of extraction
Degree is 60 DEG C~80 DEG C.
In the present invention, the depickling purification carries out preferably in supercritical carbon dioxide extraction apparatus.The present invention is to institute
The structure for stating supercritical carbon dioxide extraction apparatus does not have particular/special requirement, the arbitrarily overcritical dioxy containing extraction kettle and separating still
Change carbon extraction equipment, present invention preferably employs continuous supercritical carbon dioxide extraction devices；It is overcritical using continous way
Carbon dioxide extraction apparatus has the advantages that instrumentation is simple, can be continuously produced.
The present invention is preferably passed through carbon dioxide gas to the supercritical carbon dioxide extraction apparatus, generates overcritical dioxy
Change carbon.In the present invention, the speed that is passed through of the carbon dioxide gas is preferably 2~20L/h, further preferably 5~15L/
H, more preferably 8~12L/h；The purity of the carbon dioxide gas is preferably >=99.99%.The present invention is by overcritical dioxy
Change in carbon extraction equipment and be passed through carbon dioxide gas, which can be changed into the supercritical carbon dioxide device
Supercritical carbon dioxide；After the present invention reaches the super critical condition (i.e. extraction temperature and extracting pressure) of setting, preferably continue to
Supercritical carbon dioxide extraction apparatus is continually fed into carbon dioxide gas, to guarantee continuously to generate overcritical titanium dioxide
Carbon, and then lasting extraction occurs.When the flow velocity of carbon dioxide gas of the present invention is excessive, supercritical carbon dioxide is in extraction kettle
During middle extraction free fatty acid, while triglycerides can be also extracted into separating still, recovery rate is caused to reduce；When described
When the flow velocity of carbon dioxide gas is too small, supercritical carbon dioxide cannot extract free fatty acid in extraction kettle completely, can shadow
Ring extraction efficiency and quality.
After the super critical condition (i.e. extraction temperature and extracting pressure) for reaching setting, the present invention is preferably to described overcritical two
Peony seeds crude oil is continually fed into carbonoxide extraction equipment to be extracted.In the present invention, the peony seeds crude oil is passed through speed
Degree is preferably 2~15mL/min, further preferably 4~10mL/min, most preferably 5~8mL/min.The present invention is to described male
The source of red seed crude oil does not have particular/special requirement, arbitrarily needs to carry out the peony seeds crude oil of depickling purification, of the present invention male
Red seed crude oil is preferably obtained by peony seeds through cold pressing.
It is passed through during peony seeds crude oil, the present invention extracts the peony seeds crude oil using supercritical carbon dioxide
It takes, obtains purification peony seed oil.In the present invention, the pressure of the extraction is 15Mpa~25Mpa, preferably 20~25Mpa；
The temperature of extraction is 60 DEG C~80 DEG C, preferably 65~75 DEG C.The present invention is by control extracting pressure and extraction temperature in the model
In enclosing, so that supercritical carbon dioxide has good solvability to the free fatty acid in peony seeds crude oil, and to fat
Acid glyceride does not dissolve then, and then free fatty acid is extracted from peony seeds crude oil, obtains the same of purification peony seed oil
When obtain carrying the supercritical carbon dioxide of free fatty acid.In the present invention, the time of the extraction be preferably 30~
120min, further preferably 60~120min.The present invention just isolates one preferably every extraction a period of time from separating still
Divide free fatty acid, preferably 20~40min of every extraction separates a free fatty acid.In the present invention, when extraction time is too long
When, after the completion of free-fat acid extraction, while triglycerides can be also extracted, influence recovery rate；When extraction time is too short, trip
It cannot be extracted completely from fatty acid.It is of the present invention extraction preferably in the extraction kettle of supercritical carbon dioxide extraction apparatus into
Row.
After extraction, the separation for the supercritical carbon dioxide that the present invention carries free fatty acid it is also preferable to include described pair.
In the present invention, the isolated temperature is preferably 30 DEG C~60 DEG C, further preferably 40~60 DEG C；The isolated pressure
Preferably 5Mpa~20Mpa, further preferably 5~15Mpa.Separation of the present invention is preferably in supercritical carbon dioxide extracting
Carried out in the separating still of device, supercritical carbon dioxide in extraction kettle by after the free-fat acid extraction in peony seeds crude oil,
It carries free fatty acid and enters the separating still of supercritical carbon dioxide device, when separation, supercritical carbon dioxide restores gas shape
State, the free fatty acid through supercritical carbon dioxide extracting are precipitated, and free fatty acid are obtained in separating still, in overcritical dioxy
The extraction kettle for changing carbon extraction equipment obtains purification peony seed oil.
After the extraction, the present invention is refined it is also preferable to include being de-gassed to the peony seed oil being obtained by extraction
Peony seed oil.Degassing process of the present invention preferably carries out under vacuum conditions, and the time of the degassing process is preferably 0.5
~2 hours, further preferably 1 hour.The present invention does not have particular/special requirement to the embodiment of the degassing process, using ability
Embodiment known to field technique personnel.
It is described in detail below with reference to depickling refining methd of the embodiment to peony seed oil provided by the invention, still
They cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
According to the parameter of table 1, set supercritical carbon dioxide device extraction kettle temperature as 72 DEG C, separating still temperature be 45
℃；Start to be passed through carbon dioxide gas (CO after reaching set temperature2Flow velocity is 10L/h), make its extraction kettle pressure 21Mpa,
Separating still pressure is 5Mpa, reaches 200mL peony seeds crude oil after pressure and to run to that continous way is super to face with flow velocity 6mL/min speed
In boundary's carbon dioxide extraction apparatus.It is all squeezed into peony seed oil, at this moment opens the free fatty acid that separating still picks out to be precipitated,
It then proceedes to run, picks out from separating still the free fatty acid to be precipitated every 30min, so repeatedly 3 times.
8mL free fatty acid and colloid finally are obtained from separating still altogether, extraction kettle picks out the purification peony seed oil of 190mL,
It puts it under vacuum (vacuum degree is -0.06MPa) and is de-gassed 1h.
Embodiment 2~4
Peony seeds crude oil is extracted and separated in the way of embodiment 1, conditional parameter is as shown in table 1.
Comparative example 1~3
Peony seeds crude oil is extracted and separated in the way of embodiment 1, conditional parameter is as shown in table 1.
The technological parameter of 1 Examples 1 to 4 of table and comparative example 1~3
The purification peony seed oil of Examples 1 to 4 and comparative example 1~3 is tested for the property, test result is shown in Table 2.Its
In, the peony seeds crude oil of Examples 1 to 4 and comparative example 1~3 is with a collection of peony seeds crude oil, and acid value is 8.6KOH after tested
mg/g。
2 Examples 1 to 4 of table and comparative example 1~3 refine the performance of peony seed oil
By the test result of table 2 it is found that peony seed oil depickling refining methd provided by the invention is obtained by controlling each parameter
The peony seed oil arrived have the intrinsic smell of peony seed oil, free from extraneous odour, oil body clarification, in faint yellow, oil quality is good；And without molten
Agent residual；Acid value is 0.83KOH mg/g, and acid value is low；Peroxide value is 0.23mmol/kg, illustrates that stability is good.And comparative example 1
~3 change the purification peony seed oil that extraction temperature, extracting pressure and carbon dioxide flow rate obtain on the basis of embodiment 1 respectively
Though color, smell and peroxide value, without significant change, acid value is higher.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of depickling refining methd of peony seed oil, comprising the following steps: using supercritical carbon dioxide to peony seeds crude oil
It is extracted, obtains purification peony seed oil；The pressure of the extraction is 15Mpa~25Mpa, and the temperature of extraction is 60 DEG C~80
℃。
2. depickling refining methd according to claim 1, which is characterized in that the time of the extraction is 30~120min.
3. depickling refining methd according to claim 1, which is characterized in that the extraction also obtains carrying free-fat
The supercritical carbon dioxide of acid；It further include point to the supercritical carbon dioxide for carrying free fatty acid after the extraction
From the isolated temperature is 30 DEG C~60 DEG C, and isolated pressure is 5Mpa~20Mpa.
4. depickling refining methd according to claim 1, which is characterized in that the depickling purification is in supercritical carbon dioxide
It is carried out in extraction equipment, is passed through carbon dioxide gas to the supercritical carbon dioxide extraction apparatus and generates overcritical titanium dioxide
The speed that is passed through of carbon, the carbon dioxide gas is 2~20L/h.
5. depickling refining methd according to claim 4, which is characterized in that the purity of the carbon dioxide gas >=
99.99%.
6. depickling refining methd according to claim 4, which is characterized in that after generating supercritical carbon dioxide, to described
It is continually fed into peony seeds crude oil in supercritical carbon dioxide extraction apparatus to be extracted, the speed that is passed through of the peony seeds crude oil is
2~15mL/min.
7. depickling refining methd according to claim 1, which is characterized in that the peony seeds crude oil is by peony seeds through too low
Temperature and pressure squeeze to obtain.
8. depickling refining methd according to claim 1, which is characterized in that further include to being obtained by extraction after the extraction
Peony seed oil be de-gassed.
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| CN201811354399.8A CN109321360A (en) | 2018-11-14 | 2018-11-14 | A kind of depickling refining methd of peony seed oil |
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| CN201811354399.8A CN109321360A (en) | 2018-11-14 | 2018-11-14 | A kind of depickling refining methd of peony seed oil |
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| CN101444239A (en) * | 2008-12-26 | 2009-06-03 | 北京工商大学 | Method for extracting peony seed oil |
| CN106967495A (en) * | 2017-02-13 | 2017-07-21 | 北京丹泽生态科技有限公司 | A kind of preparation method of peony seed oil |
| CN107057858A (en) * | 2017-04-27 | 2017-08-18 | 青岛利和萃取股份有限公司 | Reduce the supercritical carbon dioxide method for extracting and device of extract acid value |
| CN107287026A (en) * | 2017-08-11 | 2017-10-24 | 洛阳泽达慧康医药科技有限公司 | A kind of peony seed oil depickling extracting method |
| CN108060012A (en) * | 2017-12-19 | 2018-05-22 | 贵州航天乌江机电设备有限责任公司 | A kind of extracting method of peony seed oil |
-
2018
- 2018-11-14 CN CN201811354399.8A patent/CN109321360A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444239A (en) * | 2008-12-26 | 2009-06-03 | 北京工商大学 | Method for extracting peony seed oil |
| CN106967495A (en) * | 2017-02-13 | 2017-07-21 | 北京丹泽生态科技有限公司 | A kind of preparation method of peony seed oil |
| CN107057858A (en) * | 2017-04-27 | 2017-08-18 | 青岛利和萃取股份有限公司 | Reduce the supercritical carbon dioxide method for extracting and device of extract acid value |
| CN107287026A (en) * | 2017-08-11 | 2017-10-24 | 洛阳泽达慧康医药科技有限公司 | A kind of peony seed oil depickling extracting method |
| CN108060012A (en) * | 2017-12-19 | 2018-05-22 | 贵州航天乌江机电设备有限责任公司 | A kind of extracting method of peony seed oil |
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| 史小锋等: "超临界CO_2萃取牡丹籽油的研究进展 ", 《粮食加工》 * |
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