CN101649246B - Method for extracting and refining paeonia rockii seed oil - Google Patents
Method for extracting and refining paeonia rockii seed oil Download PDFInfo
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- CN101649246B CN101649246B CN 200910117449 CN200910117449A CN101649246B CN 101649246 B CN101649246 B CN 101649246B CN 200910117449 CN200910117449 CN 200910117449 CN 200910117449 A CN200910117449 A CN 200910117449A CN 101649246 B CN101649246 B CN 101649246B
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Abstract
The invention relates to a method for extracting and refining paeonia rockii seed oil. The method comprises the following steps: collecting seeds, unshelling, baking and frying, carrying out screw press, filtering, deacidifying, degumming, drying, decoloring, deodorizing in vacuum, adding an antioxidant and filling. After solid impurities and residues obtained by the screw press are broken up, ethylacetate is added, then refluxing extraction is carried out, and a solvent is recovered so as to obtain the paeonia rockii seed oil for cosmetics. A two-step method is used for extracting the paeonia rockii seed oil, wherein in the first step: primary pressed oil used for eating is obtained by physical pressing, and the produced paeonia rockii seed oil has higher oil recovery rate and no residual solvents and can be securely eaten; in the second step, the ethyl acetate is adopted for extraction, and ingredients for antioxidation, inflammation resistance, sun block, and the like in the paeonia rockii seed oil can be extracted and used for producing the cosmetics. The invention not only improves the oil recovery rate of paeonia rockii seeds, but also ensures that the effective ingredients in the paeonia rockii seeds are sufficiently utilized.
Description
Technical field
The high efficiency extraction that the present invention relates to tree peony deep process technology field, especially paeonia rockii seed oil is utilized technology, is the method for a kind of extraction and refining paeonia rockii seed oil specifically.
Background technology
Gansu is the important place of origin of Chinese tree peony, and the Gansu Paeonia papaveracea is as the second largest article population of Chinese tree peony, with its cold-resistant drought-enduring, plant is tall and big, solid power is strong etc., and characteristics are extensively cultivated in the various places, Gansu.For a long time; Mainly to sell with nursery stock be main to the tree peony of various places cultivations to view and admire, and the development and use of tree peony deep processed product but seem serious and lag behind that the production added value is very low; Do not form industrial chain; Particularly paeonia rockii seed has only and is used for breeding on a small quantity, and annual a large amount of seed falls in the ground in vain, the wasting of resources and serious.The Paeonia suffruticosa seed oleaginousness is nearly 30%, contains multiple unsaturated fatty acidss such as oleic acid, linolic acid, linolenic acid in the peony seed oil, and especially linolenic acid content reaches more than 40%.Linolenic acid is to increasing intelligence strengthening immunity, vision protection; Reduce fat brings high blood pressure down, lowering blood glucose; Suppress hemorrhagic disease of brain and thrombotic diseases, suppress the generation and the transfer of cancer, prevention myocardial infarction and cerebral infarction; Ammonium Glycyrrhizate property disease, preventing inflammation and reducing human aging etc. has obvious effect.Generally lack alpha-linolenic acid in the population of China meals at present, half of the not enough world health organisation recommendations amount of daily intaking amount, this also is to cause one of China's cardiovascular disorder, mellitus, near-sighted reason occurred frequently.China's medical circle and the expert of nutrition educational circles appeal the special alpha-linolenic acid that replenishes of national legislation one after another.Linolenic acid content is all very low in our the daily food, and it is linseed oil or perilla seed that the product that linolenic acid content in the market is high is mainly produced material, but since these two kinds crop yield is low, distribution range is narrow; Turnout is little; Cost is high, and fetch long price is difficult to satisfy great demand.Traditional oil expression technology oil yield is not high, can only obtain the fatty acid glycerine ester moiety in the tree peony seed.As a kind of oil plant of preciousness, the tree peony seed adopts tradition oil expression technology certainly will cause the waste of resource.If adopt modern solvent-extraction process, have certain dissolvent residual again, not only bad for eater's health, also can cause certain trouble to refining.
Summary of the invention
The present invention will solve the not high problem of traditional tree peony seed employing tradition technological oil yield of oil expression, and the process method of a kind of extraction and refining paeonia rockii seed oil is provided, and the head oil expression employing physical squeezing that is used to eat, and no solvent residue can relievedly eat; The seed oil that two procedures extract can fully leach the effective constituent in the tree peony seed again, can be used for the processing of other peony seed oil products, has improved the utilization ratio of peony seed oil greatly.
The present invention solves its technical problem through following technical proposals:
The method of a kind of extraction and refining paeonia rockii seed oil may further comprise the steps:
A. seed collection:
Pluck full ripe Paeonia papaveracea fruit, dry in the air 6-8 in dry ventilation and after Follicle radish fruit is all ftractureed, beat fruit, the tree peony seed is come off naturally;
B. shell, bake stir-fry:
Collect the tree peony seed that nature comes off, the roasting frying pan is sent in mechanical dejacketing, be warming up to gradually 120 ℃ evenly roasting fry, constantly stir-frying to 80% tree peony seed benevolence fries;
C. screw press and filtration:
The tree peony seed benevolence that roasting is fried is evenly sent into expeller continuously, and peony seed oil is extruded out under pressure, and the rotating speed of screw shaft is at 8-10r/min, and the crude oil that squeezes out is for use with oil filter solids filtered impurity residue, gets tree peony seed crude oil;
D. depickling:
Use 11% NaOH solution alkali-refining deacidification, adding alkali number is theoretical alkali charge and excess alkali quantity sum, and alkali lye divides three addings; The alkali refining initial temperature is 40 ℃; Stirring velocity is 60r/min when adding alkali, treat to reduce stirring velocity when oily soap separates, and the oil temperature that raises is to 60 ℃; Centrifugal treating under 5000r/min gets depickling oil then;
E. come unstuck:
Depickling oil is preheated to 60 ℃; Add the phosphoric acid of depickling oil mass 85%, the oil of phosphoric acid is 0.2% heavily, adds 60 ℃ of hot water of 3% behind the thorough mixing; Begin to stir with the 55r/min rotating speed; When the big phosphatide particle of sesame appears in oil surface, slow down stirring velocity, when the cohesion of phosphatide particle is obvious separate stage, stop to stir, utilize whizzer to remove phosphatide and get degummed oil to 15r/min;
F. dry, decolouring:
Control vacuum tightness is more than 93.3kPa, and oily temperature is heated to 90 ℃, and extremely white fog disappears in the pot, progressively in oil, puts into oil in the time of stirring and weighs 3% carclazyte, decolours 30 minutes, after the decolouring completion oily temperature is cooled to below 50 ℃, crosses and filters bleached oil;
G. vacuum deodorization:
Vacuum tightness is heated to 170-180 ℃ with bleached oil more than 101.2kPa, kept 3 hours, stops heating, treats that oily temperature is cooled to that vacuum breaker gets deodorised oil below 50 ℃.
H. add inhibitor:
Get the Tert. Butyl Hydroquinone of deodorization oil mass 0.01%, be made into 5～10% solution, add in the g step gained deodorization peony seed oil, continue to stir can 30 minutes with deodorization peony seed oil dissolving;
After the said c step, solid impurities and residues for use was broken up, adds 4 times and measure ETHYLE ACETATE, 75 ℃ of refluxed lixiviates 3 hours; Decompression and solvent recovery gets the used for cosmetic peony seed oil.
The present invention adopts two-step approach to extract peony seed oil, and the first step adopts physical squeezing, and the peony seed oil oil yield of production is higher, no solvent residue, edibility; Second step was adopted the ETHYLE ACETATE lixiviate, can anti-oxidant, the anti-inflammatory in the peony seed oil, the abundant lixiviate of composition such as sun-proof be come out, and was used for cosmetics production.Not only improved the oil yield of tree peony seed, and the effective constituent in the tree peony seed is fully used.
Embodiment
Below in conjunction with embodiment the present invention is further elaborated.
Embodiment 1
(1) seed collection: the mid or late August harvesting of paeonia szechuanica Fang garden is just ftractureed in Gansu; The purple plague purpura Mu Dan Follicle radish fruit of pericarp flavescence; Be placed on the place's seasoning of indoor shady and cool ventilation, stirred once, place and treated that its fruit all ftractureed in 6 days at a distance from two days; Beat to seed with wooden stick and all to come off, Paeonia suffruticosa seed 113kg.
(2) shelling, roasting are fried: get the tree peony seed, machine barking, removal of impurities.Tree peony seed after the decortication is put into pan, and little fire is fried slowly, and duty is stirred, and control tree peony seed temperature is at 120 ℃, fries to grind to open to the tree peony seed to be yellow.
(3) screw press and filtration: the tree peony seed benevolence that roasting is fried is cooled to 60 ℃ and evenly sends into the expeller squeezing continuously; Peony seed oil is extruded out under pressure; The rotating speed of screw shaft is at 8r/min; The crude oil that squeezes out filters with oil filter, and wherein residue is for use, gets head and presses tree peony seed crude oil 25kg.
(4) depickling: take by weighing 155g NaOH, being mixed with concentration is 11% alkali lye, divides to add for three times in the tree peony seed crude oil.The alkali refining initial temperature is at 40 ℃, and stirring velocity is 60r/min when adding alkali, treat to reduce stirring velocity when oily soap separates, and the oil temperature that raises is to 60 ℃, centrifugal treating under 5000r/min then, depickling oil.
(5) come unstuck: peony seed oil is preheated to about 60 ℃; The phosphoric acid that adds 50ml85%; The hot water that adds 60 ℃ of 750ml behind the thorough mixing begins to stir with the 55r/min rotating speed, when the big phosphatide particle of most sesames appears in oil surface, slows down stirring velocity gradually to 15r/min; When the cohesion of phosphatide particle is obvious separate stage, stop to stir, utilize whizzer to remove phosphatide and get degummed oil.
(6) dry, decolouring: control vacuum tightness is more than 93.3kPa, and oily temperature is heated to 90 ℃, and extremely white fog disappears in the pot; Progressively in oil, put into the 0.75kg carclazyte when stirring; Decoloured 30 minutes, decolouring is cooled to oily temperature below 50 ℃ rapidly after accomplishing, and filters as early as possible.
(7) vacuum deodorization: vacuum tightness remains on more than the 101.2kPa, and bleached oil is heated to 170 ℃, keeps 3 hours, stops heating, treats that oily temperature is cooled to vacuum breaker below 50 ℃.
(8) add inhibitor: take by weighing the 2.5g Tert. Butyl Hydroquinone,, stir, add then in the deodorised oil, continue to stir can about 30 minutes with the dissolving of 50ml peony seed oil.
Embodiment 2
(1) seed collection: the mid or late August harvesting of paeonia szechuanica Fang garden is just ftractureed in Gansu; The purple plague purpura Mu Dan Follicle radish fruit of pericarp flavescence; Be placed on the place's seasoning of indoor shady and cool ventilation, stirred once, place and treated that its fruit all ftractureed in 6 days at a distance from three days; Beat to seed with wooden stick and all to come off, Paeonia suffruticosa seed 113kg.
(2) shelling, roasting are fried: get the tree peony seed, machine barking, removal of impurities.Tree peony seed after the decortication is put into pan, and little fire is fried slowly, and duty is stirred, and control tree peony seed temperature is at 120 ℃, fries to grind to open to the tree peony seed to be yellow.
(3) screw press and filtration: the tree peony seed benevolence that roasting is fried is cooled to 60 ℃ and evenly sends into the expeller squeezing continuously; Peony seed oil is extruded out under pressure; The rotating speed of screw shaft is at 10r/min; The crude oil that squeezes out filters with oil filter, gets head and presses tree peony seed crude oil 25kg, and wherein residue is for use.
(4) the residue obtained 50kg of getting in the expressing process is broken up, add 200L ETHYLE ACETATE, 75 ℃ of refluxed lixiviate 3h.
(5) reclaim solvent, get the used for cosmetic peony seed oil.
Embodiment 3
(1) seed collection: the late August harvesting of paeonia szechuanica Fang garden is just ftractureed in Gansu; The purple plague purpura Mu Dan Follicle radish fruit of pericarp flavescence; Be placed on the place's seasoning of indoor shady and cool ventilation, stir once, place and treated that its fruit all ftractureed in 8 days at a distance from couple of days; Beat to seed with wooden stick and all to come off, Paeonia suffruticosa seed 55kg.
(2) shelling, roasting are fried: get the tree peony seed, machine barking, removal of impurities.Tree peony seed after the decortication is put into pan, and little fire is fried slowly, and duty is stirred, and control tree peony seed temperature is at 120 ℃, fries to grind to open to the tree peony seed to be yellow.
(3) screw press and filtration: the tree peony seed benevolence that roasting is fried is cooled to 60 ℃ and evenly sends into the expeller squeezing continuously; Peony seed oil is extruded out under pressure; The rotating speed of screw shaft is at 8-10r/min; The crude oil that squeezes out removes by filter wherein solid impurity with oil filter, gets head and presses tree peony seed crude oil 14kg.
(4) depickling: take by weighing 87g NaOH, being mixed with concentration is 11% left and right sides alkali lye, divides to add for three times in the tree peony seed crude oil.The alkali refining initial temperature is at 40 ℃, and stirring velocity is 60r/min when adding alkali, treat to reduce stirring velocity when oily soap separates, and the oil temperature that raises is to 60 ℃, centrifugal treating under 5000r/min then, depickling oil.
(5) come unstuck: peony seed oil is preheated to 60 ℃; The phosphoric acid that adds 28ml85%; The hot water that adds 60 ℃ of 420ml behind the thorough mixing begins to stir with the 55r/min rotating speed, when the big phosphatide particle of most sesames appears in oil surface, slows down stirring velocity gradually to 15r/min; When the cohesion of phosphatide particle is obvious separate stage, stop to stir, utilize whizzer to remove phosphatide and get degummed oil.
(6) dry, decolouring: control vacuum tightness is more than 93.3kPa, and oily temperature is heated to 90 ℃, and extremely white fog disappears in the pot; Progressively in oil, put into the 0.42kg carclazyte when stirring; Decoloured 30 minutes, decolouring is cooled to oily temperature below 50 ℃ rapidly after accomplishing, and filters as early as possible.
(7) vacuum deodorization: vacuum tightness remains on more than the 101.2kPa, and bleached oil is heated to 180 ℃, keeps 3 hours, stops heating, treats that oily temperature is cooled to vacuum breaker below 50 ℃.
(8) add inhibitor: take by weighing the 1.4g Tert. Butyl Hydroquinone,, stir, add then in the deodorised oil, continue to stir can 30 minutes with the dissolving of 14ml peony seed oil.
Claims (2)
1. one kind is extracted and the method for refining paeonia rockii seed oil, it is characterized in that may further comprise the steps:
A. seed collection: pluck full ripe Paeonia papaveracea fruit, dried in the air 6～8 days, beat fruit, the tree peony seed is come off naturally in dry ventilation;
B. shell, bake stir-fry:
Collect the tree peony seed that nature comes off, the roasting frying pan is sent in mechanical dejacketing, and temperature rises to 120 ℃ gradually, and evenly roasting is fried, and constantly stir-fries to 80% tree peony seed benevolence to fry;
C. screw press and filtration:
The tree peony seed benevolence that roasting is fried is evenly sent into expeller continuously, and peony seed oil is extruded out under pressure, and the rotating speed of screw shaft is at 8～10r/min, and the crude oil that squeezes out is for use with oil filter solids filtered impurity residue, gets tree peony seed crude oil;
D. depickling:
Use 11% NaOH solution alkali-refining deacidification, adding alkali number is theoretical alkali charge and excess alkali quantity sum, and alkali lye divides three addings; The alkali refining initial temperature is 40 ℃; Stirring velocity is 60r/min when adding alkali, treat to reduce stirring velocity when oily soap separates, and the oil temperature that raises is to 60 ℃; Centrifugal treating under 5000r/min gets depickling oil then;
E. come unstuck:
Depickling oil is preheated to 60 ℃; Adding concentration is 85% phosphoric acid, and the add-on of phosphoric acid accounts for 0.2% of depickling oil mass, adds 60 ℃ of hot water of depickling oil mass 3% behind the thorough mixing; Begin to stir with the 55r/min rotating speed; When the big phosphatide particle of sesame appears in oil surface, slow down stirring velocity, when the cohesion of phosphatide particle is obvious separate stage, stop to stir, utilize whizzer to remove phosphatide and get degummed oil to 15r/min;
F. dry, decolouring:
Control vacuum tightness is at 93.3kPa, and the degummed oil temperature is heated to 90 ℃, and white fog disappears to the pot, progressively in oil, puts into the carclazyte of degummed oil weight 3% in the time of stirring, decolour 30 minutes, and decolouring is cooled to oily temperature below 50 ℃ after accomplishing, filter bleached oil;
G. vacuum deodorization:
Vacuum tightness is heated to 170～180 ℃ at 101.2kPa with bleached oil, keeps 3 hours, stops heating, treats that oily temperature is cooled to vacuum breaker below 50 ℃, gets deodorised oil;
H. add inhibitor
Get the Tert. Butyl Hydroquinone of deodorization oil mass 0.01%, be made into 5～10% solution, add again in the g step gained deodorised oil, continue to stir can 30 minutes with deodorised oil.
2. a kind of the extraction and the method for refining paeonia rockii seed oil according to claim 1 after it is characterized in that c gone on foot said solid impurities and residues for use and break up, adds 4 times and measures ETHYLE ACETATE, 75 ℃ of refluxed lixiviates 3 hours; Decompression and solvent recovery gets the used for cosmetic peony seed oil.
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