CN106172884B - A kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae and preparation method thereof - Google Patents
A kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae and preparation method thereof Download PDFInfo
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- CN106172884B CN106172884B CN201610519776.3A CN201610519776A CN106172884B CN 106172884 B CN106172884 B CN 106172884B CN 201610519776 A CN201610519776 A CN 201610519776A CN 106172884 B CN106172884 B CN 106172884B
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- 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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
-
- 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
- C11B1/10—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
Abstract
The present invention discloses a kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae and preparation method thereof, the advanced formula oil of vitamin A strengthening wild almond Cortex Eucommiae, including eucommia ulmoides seed oil, mountain almond oil and vitamin A.The preparation method of eucommia ulmoides seed oil includes the following steps: supercritical extract (2) the seed of bark of eucommia crude oil refining of (1) seed of bark of eucommia crude oil；The preparation method of mountain almond oil includes the following steps: the de- bitter pre-treatment of (1) wild almond；(2) refining of wild almond crude oil.The eucommia ulmoides seed oil of preparation and mountain almond oil are mixed and added into vitamin A i.e. to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.The present invention can greatly improve people in daily life to the intake of vitamin A by the way that vitamin A is added in edible oil, and children is avoided to be deficient in vitamin A and depauperation.
Description
Technical field
The present invention relates to edible oils to develop and use field, and in particular to a kind of vitamin A strengthening wild almond Cortex Eucommiae is advanced to match
Square oil and preparation method thereof.
Background technique
China is that moderate vitamin A in children lacks country, and wherein city is slightly to lack, and rural area is Moderate deficiency, western
Area countryside is severe shortage.The reinforcing of vitamin A is the most effective approach for reducing vitamin A deficiency.The reinforcing of vitamin
Most importantly select suitable carrier.Energy is many as the carrier food of enhanced vitamin A, such as condiment, staple food, milk powder milk
Product, margarine etc..Optimal carrier or edible oil, first vitamin A are liposoluble vitamins, are soluble in edible oil,
It can be uniformly dispersed in edible oil；Vitamin A in conjunction with fatty acid formed ester than more stable, edible oil in other foods
It can make vitamin A and oxygen-barrier, be not easy to be oxidized decomposition, extend storage time；Fatty acid can promote the absorption of vitamin A
It utilizes；Vitamin A, which is added in edible oil, will not change original local flavor；No matter area, age, gender, can all take in daily certain
The edible oil of amount, and there is no the differences on the taste of region；The greasy and defecating feces excretion of edible oil ensure that amount has certainly
It is sex-limited, while also ensuring that edible vitamin A excessive will not be excessive；The simple process of vitamin A, cost are added in edible oil
Lower than other food, therefore, edible oil is the optimum carrier of enhanced vitamin A.
The nutritive value of edible oil depends primarily on monounsaturated fatty acids (oleic acid) content, the high nutriture value of oleic acid content
Value is just high.The alpha-linolenic acid (18:3) of 3 series of linoleic acid (18:2) and n-of 6 series of n-in polyunsaturated fatty acid is equal
Belong to essential fatty acid, i.e. body vital movement is essential, but body itself cannot synthesize, it is necessary to by food supply
Polyunsaturated fatty acid.Shortage can cause growth retardation, dysgenesia, skin injury and liver, kidney, nerve and vision etc.
Many-sided disease.If alpha-linolenic acid and linoleic ratio can be highly beneficial to human body close to the desirable level of 1:4.
The content of alpha-linolenic acid should be 2.5% or more, and it is just very useful to health that human body can take in 1g daily.
Eucommia ulmoides seed oil is rich in polyunsaturated fatty acid, and Linoleic acid accounts for 12% or so, and alpha-linolenic acid accounts for 60% or more,
Linolenic and linoleic is essential fatty acid, in addition it also contain a small amount of aucubin with tonifying liver effect at
Point, these all other greases cannot compare.Eucommia Oil is mainly by alpha-linolenic acid, oleic acid, linoleic acid, palmitinic acid, tristearin
The fatty acid such as acid, myristic acid composition, wherein unsaturated fatty acid is up to 90% or more, and essential fatty acid linoleic acid and
The content of alpha-linolenic acid is up to 70% or more, and especially alpha-linolenic acid content is up to 60% or so, protects with high nutrition
Strong value.
The oil content of wild almond is about 45% -60%, mainly by oleic acid, linoleic acid, palmitic acid, palmitoleic acid, Asia
The higher fatty acids composition of numb acid, saturated fatty acid content is seldom, and unsaturated fatty acid content is up to 95% or more, mountain almond oil
In in the unsaturated fatty acid that contains, oleic acid, linoleic acid and linolenic acid account for the 96.64% of fatty acid total amount.Contain in mountain almond oil
There is VE、VD3、VPEqual multivitamins, especially VD3Content be up to 5.01mg/100g, it is more rare in vegetable oil.VD3Shadow
The absorption and storage for ringing calcium, phosphorus in human body, play an important role in the mineralization of human body bone.
Summary of the invention
It is an object of the present invention to provide a kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae and its preparation sides
Method.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
A kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae, is made of eucommia ulmoides seed oil, mountain almond oil and vitamin A.
The mass ratio of the said vitamin A reinforcing advanced formula oil of ansu apricot Cortex Eucommiae, the eucommia ulmoides seed oil and mountain almond oil is 1:2
~1:5.
The mass ratio of the said vitamin A reinforcing advanced formula oil of ansu apricot Cortex Eucommiae, the eucommia ulmoides seed oil and mountain almond oil is 1:3
~1:4.
Said vitamin A strengthens the advanced formula oil of ansu apricot Cortex Eucommiae, and the content of the vitamin A is that every kilogram of vitamin A is strong
Changing vitamin A content in the advanced formula oil of ansu apricot Cortex Eucommiae is 5~20mg.
Said vitamin A strengthens the advanced formula oil of ansu apricot Cortex Eucommiae, and the content of the vitamin A is that every kilogram of vitamin A is strong
Changing vitamin A content in the advanced formula oil of ansu apricot Cortex Eucommiae is 10~15mg.
The mass ratio of the said vitamin A reinforcing advanced formula oil of ansu apricot Cortex Eucommiae, the eucommia ulmoides seed oil and mountain almond oil is 1:2
~1:5, the content of the vitamin A are that vitamin A content is 5 in every kilogram of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae
~20mg.
The mass ratio of the said vitamin A reinforcing advanced formula oil of ansu apricot Cortex Eucommiae, the eucommia ulmoides seed oil and mountain almond oil is 1:3
~1:4, the content of the vitamin A are that vitamin A content is 10 in every kilogram of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae
~15mg.
The preparation method that said vitamin A strengthens eucommia ulmoides seed oil in the advanced formula oil of ansu apricot Cortex Eucommiae includes the following steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil:
(1-1) seed of bark of eucommia supercritical CO2The pre-treatment of extraction: seed of bark of eucommia, which is dried, and is crushed to 40 mesh obtains seed of bark of eucommia powder,
Seed of bark of eucommia powder is first immersed in temperature is 50-60 DEG C, polyvinyl alcohol mass fraction is 0.5- in the poly-vinyl alcohol solution of 2-4wt%
1 hour, seed of bark of eucommia powder was ultrasonically treated while immersion, and ultrasonic frequency is 35KMz, and ultrasonic power is 260~400W, mistake
It filters and dry that seed of bark of eucommia powder, polyvinyl alcohol are polyvinyl alcohol 1788 or polyvinyl alcohol 1799；The preparation side of poly-vinyl alcohol solution
Method is as follows: polyvinyl alcohol is soaked in the ethanol solution that ethyl alcohol mass fraction is 70-85wt% 12-24 hours, filtering drying,
Then obtained polyvinyl alcohol is added in 50-60 DEG C of water, heating stirring 1 hour up to poly-vinyl alcohol solution
(1-2) seed of bark of eucommia powder supercritical CO2Extraction: seed of bark of eucommia powder obtained in step (1-1) is put into extraction kettle,
It for 30~80% aqueous solution is entrainer that ethyl alcohol or ethyl alcohol volumetric concentration are used in extraction process, and entrainer flow velocity is 1-3mL/
min；When using ethanol water for entrainer, the aqueous solution that ethyl alcohol volumetric concentration is 30% is passed through in extraction kettle first,
Then successively the aqueous solution that ethyl alcohol volumetric concentration is 40%, 50%, 60%, 70% and 80% is added in extraction kettle, ethyl alcohol
Aqueous solution that aqueous solution that aqueous solution that volumetric concentration is 30%, ethyl alcohol volumetric concentration are 40%, ethyl alcohol volumetric concentration are 50%,
The water that the aqueous solution and ethyl alcohol volumetric concentration that aqueous solution that ethyl alcohol volumetric concentration is 60%, ethyl alcohol volumetric concentration are 70% are 80%
Six kinds of ethanol waters of solution are passed through the ratio between time of extraction kettle are as follows: 2:3:1:1:1:2；Extracting pressure is 25~35MPa, extraction
Temperature is 45~50 DEG C, and extraction time is 1.5~2.5h, and separating pressure is 6~7MPa, and separation temperature is 45~50 DEG C, is obtained
Seed of bark of eucommia crude oil；
(2) seed of bark of eucommia crude oil refines, the specific steps are as follows:
Seed of bark of eucommia crude oil is placed in heating tank by (2-1), is warming up to 60~70 DEG C, and it is seed of bark of eucommia crude oil weight that weight, which is added,
0.05-0.25wt ‰, the phosphoric acid that concentration is 80-90wt%, react 45~55min；
Seed of bark of eucommia crude oil in heating tank is transferred in outer tank by (2-2), and the lye prepared in advance is added immediately, pours on one side
Lye at the uniform velocity stirs on one side, and mixing speed is 40~50 turns/min, reacts 10~15min, settles 4~6h；
In this step: lye is NaOH solution, and the ratio of NaOH solution and seed of bark of eucommia crude oil is 3:1~5:1/mL:g；Alkali
Changing temperature is 70~80 DEG C；
In this step: total alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are oil stream amount, unit Kg/h, AV are seed of bark of eucommia crude oil
Acid value, unit mgNaOH/g；
B. phosphoric acid alkali consumption NP: due to being added to phosphoric acid in the degumming of this technique, therefore lye addition is considered as neutralising phosphoric acid consumption
Alkali number；NP=1.22 × W, W H3PO4Additive amount, unit Kg/h, the amount of phosphoric acid is pure phosphoric acid amount here；
C. excess alkali quantity NC: excess alkali is 0.25~0.5wt% of oil mass, and NC=Q × 25%, Q are oil stream amount, unit is
Kg/h；
D. practical caustic soda amount NS: since caustic soda purity in the market differs, therefore while calculating, should be according to its NaOH actual content
It is converted: the NaOH percentage composition of practical caustic soda amount NS=(N+NP+NC)/commercially available alkali；
(2-3) takes supernatant, and the NaCl solution that NaCl mass fraction is 0.5-1.5wt%, NaCl solution additional amount is added
For seed of bark of eucommia crude oil weight 5-15wt%, at the uniform velocity stirs, 40~50 turns/min of revolving speed, settle 2h；
(2-4) takes supernatant, is 0.06~0.095Mpa in vacuum degree, temperature is dry under conditions of being 90~110 DEG C；
(2-5) enters bleacher, and vacuum degree is 0.06~0.095Mpa in bleacher, and temperature is 90~110 DEG C, toward decoloration
The food grade atlapulgite that seed of bark of eucommia crude oil weighs 2~4wt% is added in tank, reacts 45~55min；
(2-6) opens circulated filter system, carries out circulating filtration, until the clarification of seed of bark of eucommia crude oil；
(2-7) enter deodorizing tower in, in deodorizing tower vacuum degree be 0.0002MPa, temperature be 100~240 DEG C reaction 3~
5h；
In this step: deodorizing tower is to be applied in combination to carry out physical deacidification deodorization using physical refining tower, fatty acid supplementary set device；
(2-8) is naturally cooling to 100~170 DEG C, and water flowing acceleration is cooled to room temperature；
(2-9) carries out polishing filtering by bag filter, bestows the pressure of 4kg, and filtering obtains seed of bark of eucommia refined oil；
In this step: in bag filter the material of filter bag film be polyphenylene sulfide fibre, polyimides, aramid fiber or
One of polytetrafluoroethylene fibre；
In this step: the aperture size of filter bag film is 0.2~0.9nm in bag filter.
The preparation method that said vitamin A strengthens mountain almond oil in the advanced formula oil of ansu apricot Cortex Eucommiae includes the following steps:
(1) the de- bitter pre-treatment of wild almond:
The shelling of (1-1) wild almond hulling machine, first machine are screened, and then artificial screening obtains shelling wild almond；
Wild almond is poured into 60~120s in 90~100 DEG C of hot water by (1-2), be transferred to 4~10 DEG C of cold water impinging coolings 2~
5min；
(1-3), which pours into wild almond in peeling machine, to peel, and machine screens first, and then artificial screening obtains decortication ansu apricot
Benevolence；
Decortication wild almond is poured into 90~100 DEG C of hot water and carries out four immersions by (1-4), and water temperature is naturally cold in soaking process
But；2~4h is impregnated for the first time, is rinsed after pulling out with tap water；Second of 10~12h of immersion, is rinsed after pulling out with tap water；The
2~4h is impregnated three times, is rinsed after pulling out with tap water；4th 2~4h of immersion, is rinsed after pulling out with tap water；
(1-5) pours into the wild almond of de- hardship in drying pool, at 60~70 DEG C, air blast or microwave drying；When microwave drying,
Frequency using microwave drying is 2000~2400MHz, 1500~2800W of power, the bed of material with a thickness of 6~7cm；
(2) mountain almond oil extracts refining:
Pretreatment after the de- hardship of (2-1) wild almond: wild almond be crushed into 50 meshes and obtain wild almond powder, wild almond powder is soaked
Bubble is in the poly- second that temperature is 50-60 DEG C, polyvinyl alcohol mass fraction is 2-4wt%, polyethylene glycol mass fraction is 5-10wt%
0.5-1 hours in enol-polyglycol solution, wild almond powder is ultrasonically treated while immersion, and ultrasonic frequency is
35KHz, ultrasonic power are 260~400W, are filtered and dry that wild almond powder, polyvinyl alcohol are polyvinyl alcohol 1788 or poly- second
Enol 1799, polyethylene glycol are polyethylene glycol 200, polyethylene glycol 400 or Macrogol 600；
Polyvinyl alcohol-polyethylene glycol solution the preparation method is as follows: by polyvinyl alcohol be soaked in ethyl alcohol mass fraction be 70-
12-24 hours in the ethanol solution of 85wt%, then obtained polyvinyl alcohol is added in 50-60 DEG C of water by filtering drying,
Heating stirring 1 hour poly-vinyl alcohol solution, then add after polyethylene glycol stirring and dissolving polyvinyl alcohol-polyethylene glycol is molten
Liquid；
(2-2) low temperature squeezes mountain almond oil: expressing process uses purely physical pressing, and temperature controls between 35~55 DEG C,
Solid-liquid is subjected to the isolated wild almond dregs of rice and supernatant；The wild almond dregs of rice are added in the water of 3-6 times of its quality, utilize microwave
Reactor controls 55~60 DEG C of temperature of material, and being added account for wild almond dregs of rice mass fraction thereto is 0.055~0.065wt%'s
Compound enzyme digests 60~80min, is centrifuged to obtain thick wild almond crude oil, and the frequency of microwave reactor is 2500~3000MHz, power
1600~2500W；Compound enzyme includes protease and cellulase, and the mass ratio of protease and cellulase is 1:3~2:5；Egg
White enzyme includes neutral proteinase and alkali protease, and the mass ratio of neutral proteinase and alkali protease is 1:1~2:3；
The refining of (2-3) mountain almond oil:
(2-3-1) mixes supernatant and thick wild almond crude oil, obtains wild almond crude oil；
Wild almond crude oil is warming up to 60~70 DEG C by (2-3-2), and wild almond crude oil weight 0.05-0.15wt%, concentration is added
For the phosphoric acid of 75-95wt%, 25~35min is reacted；
(2-3-3) takes supernatant obtained in step (2-3-2), the water of wild almond crude oil weight 5-15wt% is added, at the uniform velocity
Stirring, revolving speed are 40~50 turns/min, settle 2h；
(2-3-4) takes supernatant obtained in step (2-3-3), vacuum degree be 0.06~0.095Mpa, temperature 90
It is dry under conditions of~110 DEG C；
(2-3-5) enters bleacher, and vacuum degree is 0.06~0.095Mpa in bleacher, temperature is 90~110 DEG C, is added
The food grade atlapulgite of wild almond crude oil weight 2wt%~4wt%, reacts 25~35min；
(2-3-6) opens circulated filter system, carries out circulating filtration, until filter liquor clarification；
(2-3-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 100~240 DEG C, reaction 2
~4h；
(2-3-8) is naturally cooling to 100~170 DEG C, and water flowing acceleration is cooled to room temperature；
(2-3-9) carries out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, obtains wild almond
Refined oil.
Beneficial effects of the present invention are as follows:
(1) Cortex Eucommiae crude oil is extracted using CO 2 supercritical, by the entrainer ethanol water for introducing various concentration
Greatly improve the recovery rate of aucubin in seed of bark of eucommia.Refining process is simple to operation, and deacid-deodoring process utilizes physics essence
Refining tower prevents the loss of effective component aucubin in eucommia ulmoides seed oil, and purifies seed of bark of eucommia by using nanoscale filter bag film
Oil, linolenic acid content is up to 61.71% in finally obtained seed of bark of eucommia refined oil, and rich in the peach leaf with liver-protecting function
Coral glycosides；
(2) mountain almond oil is squeezed using low-temperature physics, does not use organic solvent, without chemical contamination, refining process is simple
It is easy to operate, it all carries out under vacuum conditions, meets first-grade edible oil standard.The present invention is squeezed using low-temperature physics, is effectively kept away
The bioactivity for having exempted to damage protein, vitamin and unsaturated fatty acid in wild almond, in wild almond refined oil obtained
Saturated fatty acid content is low, and unsaturated fatty acid content is up to 95.34%, mid-oleic highest.The present invention also pass through by
Low-temperature physics squeezing is combined with microwave assisted aqueous extraction enzymatic isolation method, substantially increases the extraction efficiency of apricot kernel oil, and by ansu apricot
Benevolence carries out pre-treating technology, so that V in extraction processE、VD3Loss substantially reduce, improve V in wild almond refined oilE、VD3
Content；
(3) by adjusting the ratio of mountain almond oil and eucommia ulmoides seed oil, the ratio of saturated fatty acid in formula oil is greatly improved,
The especially content of alpha-linolenic acid.
(4) by the way that vitamin A is added in edible oil, people can be greatly improved in daily life to vitamin A
Intake avoids children from being deficient in vitamin A and depauperation；After storing the long period, the content of vitamin A is still very
Height can be used as the edible oil of supplement body vitamin A.
Detailed description of the invention
Fig. 1 is that eucommia ulmoides seed oil extracts refinery practice flow chart；
Fig. 2 is that mountain almond oil extracts refinery practice flow chart.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
First part: the preparation of eucommia ulmoides seed oil
Embodiment 1-1
A kind of eucommia ulmoides seed oil extraction refinery practice, includes the following steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil.
Seed of bark of eucommia is dried and crushed 40 meshes and obtains seed of bark of eucommia powder, seed of bark of eucommia powder is put into extraction kettle, extracting pressure
For 25MPa, extraction temperature is 45 DEG C, extraction time 1.5h, separating pressure 6MPa, and separation temperature is 45 DEG C, obtains Cortex Eucommiae
Seed crude oil.
(2) seed of bark of eucommia crude oil refines.
Seed of bark of eucommia crude oil is placed in heating tank by (2-1), is warming up to 60 DEG C, and it is seed of bark of eucommia crude oil weight that weight, which is added,
0.05wt ‰, the phosphoric acid that concentration is 80wt%, react 45min.
Seed of bark of eucommia crude oil in heating tank is transferred in outer tank by (2-2), and the aqueous slkali prepared in advance is added immediately, is leaned to one side
Enter lye at the uniform velocity to stir on one side, mixing speed is 40 turns/min, reacts 10min, settles 4h.
Lye is NaOH solution, and the ratio of NaOH solution and seed of bark of eucommia crude oil is 3:1mL/g；Alkalization temperature is 70 DEG C.Always
Alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are oil stream amount, unit Kg/h, AV are seed of bark of eucommia crude oil
Acid value, unit mgNaOH/g.
B. phosphoric acid alkali consumption NP: due to being added to phosphoric acid in the degumming of this technique, therefore lye addition is considered as neutralising phosphoric acid consumption
Alkali number；NP=1.22 × W, W H3PO4Additive amount, unit Kg/h, the amount of phosphoric acid is pure phosphoric acid amount here.
C. excess alkali quantity NC: excess alkali is the 0.5wt% of oil mass, and NC=Q × 50%, Q are oil stream amount, unit Kg/h.
D. practical caustic soda amount NS: since caustic soda purity in the market differs, therefore while calculating, should be according to its NaOH actual content
It is converted: the NaOH percentage composition of practical caustic soda amount NS=(N+NP+NC)/commercially available alkali.
(2-3) takes supernatant, and the NaCl solution that NaCl mass fraction is 0.5wt% is added, and NaCl solution additional amount is Du
Secondary seed crude oil weight 5wt%, at the uniform velocity stirs, 40 turns/min of revolving speed, settles 2h.
(2-4) takes supernatant, dry under the conditions of vacuum degree is 0.06Mpa, is at a temperature of 90 °C.
(2-5) enters bleacher, and vacuum degree is 0.06Mpa in bleacher, temperature is 90 DEG C, and Cortex Eucommiae is added into bleacher
The food grade atlapulgite of seed crude oil weight 2wt%, reacts 45min.
(2-6) opens circulated filter system, carries out circulating filtration, until the clarification of seed of bark of eucommia crude oil.
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 110 DEG C, reacts 3h；Deodorizing tower
It is to be applied in combination to carry out physical deacidification deodorization using physical refining tower and fatty acid supplementary set device.
(2-8) is naturally cooling to 100 DEG C, and water flowing acceleration is cooled to room temperature.
(2-9) carried out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtained seed of bark of eucommia essence
Oil refining；The material of filter bag film is polyphenylene sulfide fibre in bag filter；The aperture size of filter bag film in bag filter
For 0.2nm.
Embodiment 1-2
A kind of eucommia ulmoides seed oil extraction refinery practice, includes the following steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil.
Seed of bark of eucommia is dried and crushed 40 meshes and obtains seed of bark of eucommia powder, seed of bark of eucommia powder is put into extraction kettle, extracting pressure
For 35MPa, extraction temperature is 50 DEG C, extraction time 2.5h, separating pressure 7MPa, and separation temperature is 50 DEG C, obtains Cortex Eucommiae
Seed crude oil.
Use ethyl alcohol for entrainer in extraction process, entrainer flow velocity is 3mL/min.
(2) seed of bark of eucommia crude oil refines.
Seed of bark of eucommia crude oil is placed in heating tank by (2-1), is warming up to 70 DEG C, and it is seed of bark of eucommia crude oil weight that weight, which is added,
0.25wt ‰, the phosphoric acid that concentration is 90wt%, react 55min.
Seed of bark of eucommia crude oil in heating tank is transferred in outer tank by (2-2), and the aqueous slkali prepared in advance is added immediately, is leaned to one side
Enter lye at the uniform velocity to stir on one side, mixing speed is 50 turns/min, reacts 15min, settles 6h.
Lye is NaOH solution, and the ratio of NaOH solution and seed of bark of eucommia crude oil is 5:1mL/g；Alkalization temperature is 80 DEG C.Always
Alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are oil stream amount, unit Kg/h, AV are seed of bark of eucommia crude oil
Acid value, unit mgNaOH/g；
B. phosphoric acid alkali consumption NP: due to being added to phosphoric acid in the degumming of this technique, therefore lye addition is considered as neutralising phosphoric acid consumption
Alkali number；NP=1.22 × W, W H3PO4Additive amount, unit Kg/h, the amount of phosphoric acid is pure phosphoric acid amount here；
C. excess alkali quantity NC: excess alkali is the 0.25wt% of oil mass, and NC=Q × 25%, Q are oil stream amount, unit Kg/h；
D. practical caustic soda amount NS: since caustic soda purity in the market differs, therefore while calculating, should be according to its NaOH actual content
It is converted: the NaOH percentage composition of practical caustic soda amount NS=(N+NP+NC)/commercially available alkali.
(2-3) takes supernatant, and the NaCl solution that NaCl mass fraction is 1.5wt% is added, and NaCl solution additional amount is Du
Secondary seed crude oil weight 15wt%, at the uniform velocity stirs, 50 turns/min of revolving speed, settles 2h.
(2-4) takes supernatant, dry under conditions of vacuum degree is 0.095Mpa, temperature is 110 DEG C.
(2-5) enters bleacher, and vacuum degree is 0.095Mpa in bleacher, temperature is 110 DEG C, and Du is added into bleacher
The food grade atlapulgite of secondary seed crude oil weight 4wt%, reacts 55min.
(2-6) opens circulated filter system, carries out circulating filtration, until the clarification of seed of bark of eucommia crude oil.
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 120 DEG C, reacts 5h；Deodorizing tower
It is to be applied in combination to carry out physical deacidification deodorization using physical refining tower and fatty acid supplementary set device.
(2-8) is naturally cooling to 100 DEG C, and water flowing acceleration is cooled to room temperature.
(2-9) carried out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtained seed of bark of eucommia essence
Oil refining；The material of filter bag film is polytetrafluoroethylene fibre in bag filter；The aperture ruler of filter bag film in bag filter
Very little is 0.9nm.
Embodiment 1-3
A kind of eucommia ulmoides seed oil extraction refinery practice, includes the following steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil.
Seed of bark of eucommia is dried and crushed 40 meshes and obtains seed of bark of eucommia powder, seed of bark of eucommia powder is put into extraction kettle, extracting pressure
For 30MPa, extraction temperature is 48 DEG C, extraction time 2h, separating pressure 6.5MPa, and separation temperature is 50 DEG C, obtains Cortex Eucommiae
Seed crude oil.
It for 30~80% aqueous solution is entrainer that ethyl alcohol volumetric concentration is used in extraction process, and entrainer flow velocity is
2mL/min；The aqueous solution that ethyl alcohol volumetric concentration is 30% is passed through in extraction kettle first, then successively gradually respectively by ethyl alcohol body
The ethanol water that product concentration is 40%, 50%, 60%, 70% and 80% is added in extraction kettle, and ethyl alcohol volumetric concentration is
Aqueous solution that aqueous solution that 30% aqueous solution, ethyl alcohol volumetric concentration are 40%, ethyl alcohol volumetric concentration are 50%, ethyl alcohol volume are dense
Spend the aqueous solution for 60%, the aqueous solution that ethyl alcohol volumetric concentration is 70% and six kinds of second of aqueous solution that ethyl alcohol volumetric concentration is 80%
Alcohol solution is passed through kingfisher and takes the ratio between time of kettle are as follows: 2:3:1:1:1:2；That is: in the case that total extraction time is 2h, ethyl alcohol volume
Aqueous solution that aqueous solution that aqueous solution that concentration is 30%, ethyl alcohol volumetric concentration are 40%, ethyl alcohol volumetric concentration are 50%, ethyl alcohol
The aqueous solution that the aqueous solution and ethyl alcohol volumetric concentration that aqueous solution that volumetric concentration is 60%, ethyl alcohol volumetric concentration are 70% are 80%
Six kinds of ethanol waters successively each lead into the time span in extraction kettle are as follows: 24min, 36min, 12min, 12min, 12min,
24min。
(2) seed of bark of eucommia crude oil refines.
Seed of bark of eucommia crude oil is placed in heating tank by (2-1), is warming up to 65 DEG C, and it is seed of bark of eucommia crude oil weight that weight, which is added,
0.2wt ‰, the phosphoric acid that concentration is 85wt%, react 50min.
Seed of bark of eucommia crude oil in heating tank is transferred in outer tank by (2-2), and the aqueous slkali prepared in advance is added immediately, is leaned to one side
Enter lye at the uniform velocity to stir on one side, mixing speed is 50 turns/min, reacts 15min, settles 5h.
Lye is NaOH solution, and the ratio of NaOH solution and seed of bark of eucommia crude oil is 4:1mL/g；Alkalization temperature is 75 DEG C.Always
Alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are oil stream amount, unit Kg/h, AV are seed of bark of eucommia crude oil
Acid value, unit mgNaOH/g；
B. phosphoric acid alkali consumption NP: due to being added to phosphoric acid in the degumming of this technique, therefore lye addition is considered as neutralising phosphoric acid consumption
Alkali number；NP=1.22 × W, W H3PO4Additive amount, unit Kg/h, the amount of phosphoric acid is pure phosphoric acid amount here；
C. excess alkali quantity NC: excess alkali is the 0.4wt% of oil mass, and NC=Q × 40%, Q are oil stream amount, unit Kg/h；
D. practical caustic soda amount NS: since caustic soda purity in the market differs, therefore while calculating, should be according to its NaOH actual content
It is converted: the NaOH percentage composition of practical caustic soda amount NS=(N+NP+NC)/commercially available alkali.
(2-3) takes supernatant, and the NaCl solution that NaCl mass fraction is 1wt% is added, and NaCl solution additional amount is Cortex Eucommiae
Seed crude oil weight 10wt%, at the uniform velocity stirs, 50 turns/min of revolving speed, settles 2h.
(2-4) takes supernatant, dry under the conditions of vacuum degree is 0.08Mpa, is at a temperature of 90 °C.
(2-5) enters bleacher, and vacuum degree is 0.07Mpa in bleacher, temperature is 90 DEG C, and Cortex Eucommiae is added into bleacher
The food grade atlapulgite of seed crude oil weight 3wt%, reacts 50min.
(2-6) opens circulated filter system, carries out circulating filtration, until the clarification of seed of bark of eucommia crude oil.
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 120 DEG C, reacts 3~5h；It is de-
Smelly tower is to be applied in combination to carry out physical deacidification deodorization using physical refining tower and fatty acid supplementary set device.
(2-8) is naturally cooling to 100 DEG C, and water flowing acceleration is cooled to room temperature.
(2-9) carried out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtained seed of bark of eucommia essence
Oil refining；The material of filter bag film is polytetrafluoroethylene fibre in bag filter；The aperture ruler of filter bag film in bag filter
Very little is 0.2nm.
Embodiment 1-4
The difference of the present embodiment and embodiment 1-1 is: " seed of bark of eucommia powder being put into extraction kettle " it in step (1)
Before, first by seed of bark of eucommia powder be immersed in temperature be 60 DEG C, polyvinyl alcohol mass fraction be in the poly-vinyl alcohol solution of 4wt% it is 0.5 small
When, seed of bark of eucommia powder is ultrasonically treated while immersion, and ultrasonic frequency is 35KHz, ultrasonic power 350W, is filtered and dry
Seed of bark of eucommia powder is obtained, the polyvinyl alcohol of the present embodiment is polyvinyl alcohol 1788；Poly-vinyl alcohol solution the preparation method is as follows: by poly- second
Enol is soaked in the ethanol solution that ethyl alcohol mass fraction is 70wt% 24 hours, filtering drying, the polyethylene that then will be obtained
Alcohol is added in 60 DEG C of water, and heating stirring 1 hour up to poly-vinyl alcohol solution.
Embodiment 1-5
The difference of the present embodiment and embodiment 1-2 is: " seed of bark of eucommia powder being put into extraction kettle " it in step (1)
Before, seed of bark of eucommia powder is first immersed in temperature is 50 DEG C, polyvinyl alcohol mass fraction is 1 hour in the poly-vinyl alcohol solution of 2wt%,
Seed of bark of eucommia powder is ultrasonically treated while immersion, and ultrasonic frequency is 35KHz, ultrasonic power 350W, is filtered and dry
Seed of bark of eucommia powder, polyvinyl alcohol are polyvinyl alcohol 1799；Poly-vinyl alcohol solution the preparation method is as follows: polyvinyl alcohol is soaked in second
Alcohol mass fraction is 16 hours in the ethanol solution of 85wt%, then obtained polyvinyl alcohol is added to 60 DEG C by filtering drying
Water in, heating stirring 1 hour is up to poly-vinyl alcohol solution.
Embodiment 1-6
The difference of the present embodiment and embodiment 1-3 is: " seed of bark of eucommia powder being put into extraction kettle " it in step (1)
Before, seed of bark of eucommia powder is first immersed in temperature is 55 DEG C, polyvinyl alcohol mass fraction is 1 hour in the poly-vinyl alcohol solution of 3wt%,
Seed of bark of eucommia powder is ultrasonically treated while immersion, and ultrasonic frequency is 35KHz, ultrasonic power 350W, is filtered and dry
Seed of bark of eucommia powder, polyvinyl alcohol are polyvinyl alcohol 1788；Poly-vinyl alcohol solution the preparation method is as follows: polyvinyl alcohol is soaked in second
Alcohol mass fraction is 12 hours in the ethanol solution of 80wt%, then obtained polyvinyl alcohol is added to 55 DEG C by filtering drying
Water in, heating stirring 1 hour is up to poly-vinyl alcohol solution.
Palmitinic acid in the seed of bark of eucommia refined oil that embodiment 1-1~1-6 is obtained, stearic acid, oleic acid, linoleic acid plus linolenic acid
Content and the aucubin proportion of goods damageds are as shown in table 1；The seed of bark of eucommia refined oil physicochemical property that embodiment 1-1~1-6 is obtained is such as
Shown in table 1-2.
The aucubin proportion of goods damageds=(aucubin in the quality of aucubin-seed of bark of eucommia refined oil in seed of bark of eucommia
Quality) the quality * 100% of aucubin in/seed of bark of eucommia, aucubin content (mg/100g) and Du in seed of bark of eucommia
Aucubin content (mg/100g) is all made of detection method well known in the prior art in secondary seed refined oil.
The seed of bark of eucommia refined oil fatty acid composition and content that table 1-1 embodiment 1-1~1-6 is obtained
Note: the seed of bark of eucommia crude oil aerial shelf-life is no more than three months.
The seed of bark of eucommia refined oil physicochemical property that table 1-2 embodiment 1-1~1-6 is obtained
* the crude oil and refined oil extracted for corresponding embodiment
Second part: the preparation of mountain almond oil
Embodiment 2-1
A kind of mountain almond oil extraction refinery practice, includes the following steps:
(1) the de- bitter pre-treatment of wild almond.
The shelling of (1-1) wild almond hulling machine, first machine are screened, and then artificial screening obtains shelling wild almond；
Wild almond is poured into 60s in 90 DEG C of hot water by (1-2), is transferred to 4 DEG C of cold water impinging cooling 2min；
(1-3), which pours into wild almond in peeling machine, to peel, and machine screens first, and then artificial screening obtains decortication ansu apricot
Benevolence；
(1-4), which pours into decortication wild almond in 90 DEG C of hot water, carries out four immersions, water temperature natural cooling in soaking process；The
It is primary to impregnate 2h, it is rinsed after pulling out with tap water；Second of immersion 10h, is rinsed after pulling out with tap water；Third time impregnates 2h,
It is rinsed after pulling out with tap water；4th immersion 2h, is rinsed after pulling out with tap water；
(1-5) pours into the wild almond of de- hardship in drying pool, at 60 DEG C, forced air drying.
(2) mountain almond oil extracts refining.
It includes that cold pressing extracts mountain almond oil and mountain almond oil refining that mountain almond oil, which extracts refining,；
(2-0) cold pressing extracts in mountain almond oil step: expressing process uses purely physical pressing, and temperature is controlled 35
DEG C, solid-liquid is subjected to the isolated wild almond dregs of rice and supernatant.
Supernatant obtained in (2-1) collection step (2-0) is to get wild almond crude oil；
Wild almond crude oil is warming up to 60 DEG C by (2-2), and wild almond crude oil weight 0.05wt%, the phosphorus that concentration is 75wt% is added
Acid reacts 25min；
(2-3) takes supernatant obtained in step (2-2), and the water of wild almond crude oil weight 5wt% is added, at the uniform velocity stirs, turns
Speed is 40 turns/min, settles 2h；
(2-4) takes supernatant obtained in step (2-3), dry under the conditions of vacuum degree is 0.06Mpa, is at a temperature of 90 °C
It is dry；
(2-5) enters bleacher, and vacuum degree is 0.06Mpa in bleacher, temperature is 90 DEG C, and wild almond crude oil weight is added
The food grade atlapulgite of 2wt% reacts 25min；
(2-6) opens circulated filter system, carries out circulating filtration, until filter liquor clarification；
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 120 DEG C, reacts 2~4h；
(2-8) is naturally cooling to 100 DEG C, and water flowing acceleration is cooled to room temperature；
(2-9) carries out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtains wild almond essence
Oil refining.
Embodiment 2-2
A kind of mountain almond oil extraction refinery practice, includes the following steps:
(1) the de- bitter pre-treatment of wild almond.
The shelling of (1-1) wild almond hulling machine, first machine are screened, and then artificial screening obtains shelling wild almond；
Wild almond is poured into 120s in 100 DEG C of hot water by (1-2), is transferred to 10 DEG C of cold water impinging cooling 5min；
(1-3), which pours into wild almond in peeling machine, to peel, and machine screens first, and then artificial screening obtains decortication ansu apricot
Benevolence；
(1-4), which pours into decortication wild almond in 100 DEG C of hot water, carries out four immersions, water temperature natural cooling in soaking process；
4h is impregnated for the first time, is rinsed after pulling out with tap water；Second of immersion 12h, is rinsed after pulling out with tap water；Third time is impregnated
4h is rinsed after pulling out with tap water；4th immersion 4h, is rinsed after pulling out with tap water；
(1-5) pours into the wild almond of de- hardship in drying pool, and at 70 DEG C, the frequency of microwave drying, microwave drying is
2400MHz, power 2500W, the bed of material with a thickness of 6cm.
(2) mountain almond oil extracts refining.
It includes that cold pressing extracts mountain almond oil and mountain almond oil refining that mountain almond oil, which extracts refining,；
(2-0) cold pressing extracts in mountain almond oil step: expressing process uses purely physical pressing, and temperature is controlled 55
DEG C, solid-liquid is subjected to the isolated wild almond dregs of rice and supernatant.Then it carries out the post-processing of the wild almond dregs of rice: the wild almond dregs of rice is added to
In the water of 4 times of its quality, using the temperature 60 C of microwave reactor control material, the frequency of microwave reactor is 3000MHz, function
Rate 2500W, then the compound enzyme for accounting for that wild almond dregs of rice mass fraction is 0.065wt% is added thereto, 80min is digested, is centrifuged slightly
Wild almond crude oil；Compound enzyme includes protease and cellulase, and the mass ratio of protease and cellulase is 1:3；Protease packet
Include neutral proteinase and alkali protease, the mass ratio of neutral proteinase and alkali protease is 2:3.
(2-1) mixes supernatant obtained in step (2-0) and thick wild almond crude oil, obtains wild almond crude oil；
Wild almond crude oil is warming up to 70 DEG C by (2-2), and wild almond crude oil weight 0.15wt%, the phosphorus that concentration is 80wt% is added
Acid reacts 35min；
(2-3) takes supernatant obtained in step (2-2), and the water of wild almond crude oil weight 15wt% is added, at the uniform velocity stirs, turns
Speed is 50 turns/min, settles 2h；
(2-4) takes supernatant obtained in step (2-3), under the conditions of vacuum degree is 0.095Mpa, is at a temperature of 90 °C
It is dry；
(2-5) enters bleacher, and vacuum degree is 0.095Mpa in bleacher, temperature is 90 DEG C, and wild almond crude oil weight is added
The food grade atlapulgite of 4wt% reacts 35min；
(2-6) opens circulated filter system, carries out circulating filtration, until filter liquor clarification；
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 110 DEG C, reacts 2h；
(2-8) is naturally cooling to 100 DEG C, and water flowing acceleration is cooled to room temperature；
(2-9) carries out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtains wild almond essence
Oil refining.
Embodiment 2-3
The difference of the present embodiment and embodiment 2-1 is: before cold pressing extracts mountain almond oil in step (2-0),
Wild almond first be crushed into 50 meshes and obtain wild almond powder, it is 50 DEG C, polyvinyl alcohol quality that wild almond powder, which is then immersed in temperature,
0.5 hour in the polyvinyl alcohol-polyethylene glycol solution that score is 2wt%, polyethylene glycol mass fraction is 5wt%, wild almond powder
It being ultrasonically treated while immersion, ultrasonic power is 300W, supersonic frequency 30KHz, it filters and dry wild almond powder, then
Cold pressing is carried out to obtained wild almond powder and extracts mountain almond oil.
Polyvinyl alcohol is polyvinyl alcohol 1788, and polyethylene glycol is polyethylene glycol 200；Polyvinyl alcohol-polyethylene glycol solution
The preparation method is as follows: polyvinyl alcohol 1788 is soaked in the ethanol solution that ethyl alcohol mass fraction is 70wt% 12 hours, filtering
Obtained polyvinyl alcohol, is then added in 50 DEG C of water by drying, obtains poly-vinyl alcohol solution within heating stirring 1 hour, then again
Polyvinyl alcohol-polyethylene glycol solution is obtained after polyethylene glycol 200 stirring and dissolving is added.
Embodiment 2-4
The difference of the present embodiment and embodiment 2-2 is: before cold pressing extracts mountain almond oil, first by wild almond powder
Broken 50 mesh of mistake obtains wild almond powder, and wild almond powder is immersed in temperature is 60 DEG C, polyvinyl alcohol mass fraction is 3wt%, poly- second
Glycol mass fraction is that ultrasound is carried out while wild almond powder impregnates 1 hour in the polyvinyl alcohol-polyethylene glycol solution of 10wt%
Processing, ultrasonic power are 350W, supersonic frequency 40KHz, are filtered and dry that wild almond powder, polyvinyl alcohol are polyvinyl alcohol
1799, polyethylene glycol is polyethylene glycol 400；
Polyvinyl alcohol-polyethylene glycol solution the preparation method is as follows: polyvinyl alcohol 1799 is soaked in ethyl alcohol mass fraction
It is 12 hours in the ethanol solution of 85wt%, then obtained polyvinyl alcohol is added in 60 DEG C of water by filtering drying, heating
Stirring 1 hour poly-vinyl alcohol solution, then add after polyethylene glycol 400 stirring and dissolving polyvinyl alcohol-polyethylene glycol is molten
Liquid.
Palmitinic acid, palmitoleic acid, stearic acid, oleic acid, Asia in the wild almond refined oil that above-described embodiment 2-1~2-4 is obtained
Oleic acid and linolenic content are as shown in table 1；Grease in mountain almond oil recovery rate=wild almond refined oil quality/wild almond
Quality * 100%, VD3The proportion of goods damageds=(V in wild almondD3Quality-wild almond refined oil in VD3Quality) V in/wild almondD3's
Quality * 100%, VEThe proportion of goods damageds=(V in wild almondEQuality-wild almond refined oil in VEQuality) V in/wild almondEMatter
* 100% is measured, V in wild almondD3Content (mg/100g), V in wild almond refined oilD3Content (mg/100g), V in wild almondE
Content (mg/100g), V in wild almond refined oilEContent (mg/100g) be all made of detection side well known in the prior art
Method.
Gained wild almond refined oil fatty acid composition, content analysis and physicochemical property be such as into embodiment 2-4 by embodiment 2-1
Shown in table 2-1 and table 2-2.
Table 2-1 wild almond refined oil fatty acid composition and content analysis
| Embodiment 2-1 | Embodiment 2-2 | Embodiment 2-3 | Embodiment 2-4 | |
| Palmitinic acid | 3.05wt% | 3.50wt% | 3.48wt% | 3.55wt% |
| Palmitoleic acid | 0.49wt% | 0.60wt% | 0.58wt% | 0.61wt% |
| Stearic acid | 0.70wt% | 0.81wt% | 0.76wt% | 0.87wt% |
| Oleic acid | 58.19wt% | 62.42wt% | 64.52wt% | 66.91wt% |
| Linoleic acid | 23.54wt% | 27.21wt% | 26.65wt% | 27.71wt% |
| Alpha-linolenic acid | 0.08wt% | 0.11wt% | 0.10wt% | 0.11wt% |
| Mountain almond oil recovery rate | 62.21wt% | 79.36wt% | 62.87wt% | 79.76wt% |
| The vitamin E proportion of goods damageds | 19.68wt% | 13.74wt% | 5.12wt% | 1.83wt% |
| VD3The proportion of goods damageds | 20.26wt% | 15.19wt% | 6.34wt% | 2.10wt% |
Table 2-2 wild almond refined oil physicochemical property
Part III: the preparation of the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae:
Embodiment 3-1
The preparation method of the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae: the embodiment 1-1 eucommia ulmoides seed oil prepared is placed in
In mixer, be heated to 45 DEG C, stirring, mixing speed 45r/min, be then added embodiment 2-1 preparation mountain almond oil and
The mass ratio of vitamin A, eucommia ulmoides seed oil and mountain almond oil is 1:2.6, and the additional amount of vitamin A is to tie up in every kilogram of edible oil
Raw element A content is 15mg, continues to stir 2h, room temperature stands up to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.
Embodiment 3-2
The preparation method of the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae: the embodiment 1-2 eucommia ulmoides seed oil prepared is placed in
In mixer, be heated to 45 DEG C, stirring, mixing speed 45r/min, be then added embodiment 2-2 preparation mountain almond oil and
The mass ratio of vitamin A, eucommia ulmoides seed oil and mountain almond oil is 1:2.6, and the additional amount of vitamin A is to tie up in every kilogram of edible oil
Raw element A content is 15mg, continues to stir 2h, room temperature stands up to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.
Embodiment 3-3
The preparation method of the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae: the embodiment 1-5 eucommia ulmoides seed oil prepared is placed in
In mixer, be heated to 45 DEG C, stirring, mixing speed 45r/min, be then added embodiment 2-3 preparation mountain almond oil and
The mass ratio of vitamin A, eucommia ulmoides seed oil and mountain almond oil is 1:2.6, and the additional amount of vitamin A is to tie up in every kilogram of edible oil
Raw element A content is 15mg, continues to stir 2h, room temperature stands up to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.
Embodiment 3-4
The preparation method of the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae: the embodiment 1-6 eucommia ulmoides seed oil prepared is placed in
In mixer, be heated to 45 DEG C, stirring, mixing speed 45r/min, be then added embodiment 2-4 preparation mountain almond oil and
The mass ratio of vitamin A, eucommia ulmoides seed oil and mountain almond oil is 1:2.6, and the additional amount of vitamin A is to tie up in every kilogram of edible oil
Raw element A content is 15mg, continues to stir 2h, room temperature stands up to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.
After seeking vitamin A strengthening ansu apricot Cortex Eucommiae of the present invention advanced formula oil storage a period of time, vitamin A
Remaining content, carries out the following studies, by the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae prepared by embodiment 3-1 to 3-4
It is stored in the plastic bottle of transparent sealing, is placed at room temperature for, detect the remaining residue of vitamin A in formula oil in different time sections
Rate, as shown in table 3-1:
Note: the remaining percentage composition (wt%) of the vitamin A=advanced formula of correspondence time point vitamin A strengthening ansu apricot Cortex Eucommiae
When the quality of vitamin A in oil/initial in the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae vitamin A quality.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (3)
1. a kind of advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae, which is characterized in that by eucommia ulmoides seed oil, mountain almond oil and Wei Sheng
Plain A composition；
The mass ratio of the eucommia ulmoides seed oil and mountain almond oil is 1:3~1:4, and the content of the vitamin A is every kilogram of vitamin A
Strengthening vitamin A content in the advanced formula oil of ansu apricot Cortex Eucommiae is 10~15mg；
The preparation method of eucommia ulmoides seed oil includes the following steps:
(1) supercritical CO is used2Extraction process obtains seed of bark of eucommia crude oil:
(1-1) seed of bark of eucommia supercritical CO2The pre-treatment of extraction: seed of bark of eucommia, which is dried, and crushed 40 meshes obtains seed of bark of eucommia powder, first will
Seed of bark of eucommia powder is immersed in that temperature is 50-60 DEG C, polyvinyl alcohol mass fraction is that 0.5-1 is small in the poly-vinyl alcohol solution of 2-4wt%
When, seed of bark of eucommia powder is ultrasonically treated while immersion, and ultrasonic frequency is 35KMz, and ultrasonic power is 260~400W, filtering
And it is dry that seed of bark of eucommia powder, polyvinyl alcohol are polyvinyl alcohol 1788 or polyvinyl alcohol 1799；The preparation method of poly-vinyl alcohol solution
It is as follows: polyvinyl alcohol to be soaked in the ethanol solution that ethyl alcohol mass fraction is 70-85wt% 12-24 hours, filtering drying, so
Obtained polyvinyl alcohol is added in 50-60 DEG C of water afterwards, heating stirring 1 hour up to poly-vinyl alcohol solution
(1-2) seed of bark of eucommia powder supercritical CO2Extraction: seed of bark of eucommia powder obtained in step (1-1) is put into extraction kettle, is being extracted
Using ethyl alcohol volumetric concentration in the process for 30~80% aqueous solution is entrainer, and entrainer flow velocity is 1-3mL/min；Work as use
When ethanol water is entrainer, the aqueous solution that ethyl alcohol volumetric concentration is 30% is passed through in extraction kettle first, then successively will
The aqueous solution that ethyl alcohol volumetric concentration is 40%, 50%, 60%, 70% and 80% is added in extraction kettle, and ethyl alcohol volumetric concentration is
Aqueous solution that aqueous solution that 30% aqueous solution, ethyl alcohol volumetric concentration are 40%, ethyl alcohol volumetric concentration are 50%, ethyl alcohol volume are dense
Spend the aqueous solution for 60%, the aqueous solution that ethyl alcohol volumetric concentration is 70% and six kinds of second of aqueous solution that ethyl alcohol volumetric concentration is 80%
Alcohol solution is passed through the ratio between time of extraction kettle are as follows: 2:3:1:1:1:2；Extracting pressure be 25~35MPa, extraction temperature be 45~
50 DEG C, extraction time is 1.5~2.5h, and separating pressure is 6~7MPa, and separation temperature is 45~50 DEG C, obtains seed of bark of eucommia crude oil；
(2) seed of bark of eucommia crude oil refines, the specific steps are as follows:
Seed of bark of eucommia crude oil is placed in heating tank by (2-1), is warming up to 60~70 DEG C, and it is seed of bark of eucommia crude oil weight that weight, which is added,
0.05-0.25wt ‰, the phosphoric acid that concentration is 80-90wt%, react 45~55min；
Seed of bark of eucommia crude oil in heating tank is transferred in outer tank by (2-2), and the lye prepared in advance is added immediately, pours into lye on one side
It at the uniform velocity stirs on one side, mixing speed is 40~50 turns/min, reacts 10~15min, settles 4~6h；
In this step: lye is NaOH solution, and the ratio of NaOH solution and seed of bark of eucommia crude oil is 3:1~5:1/mL:g；Alkalization temperature
Degree is 70~80 DEG C；
In this step: total alkali consumption calculates according to the following steps:
A. theoretical caustic dosage N:N=7.13 × 10-4× AV × Q, Q are oil stream amount, unit Kg/h, AV are the acid of seed of bark of eucommia crude oil
Value, unit mgNaOH/g；
B. phosphoric acid alkali consumption NP: due to being added to phosphoric acid in the degumming of this technique, therefore lye addition is considered as neutralising phosphoric acid alkali consumption；
NP=1.22 × W, W H3PO4Additive amount, unit Kg/h, the amount of phosphoric acid is pure phosphoric acid amount here；
C. excess alkali quantity NC: excess alkali is 0.25~0.5wt% of oil mass, and NC=Q × 25%, Q are oil stream amount, unit Kg/h；
D. practical caustic soda amount NS: since caustic soda purity in the market differs, therefore while calculating, should carry out according to its NaOH actual content
Conversion: the NaOH percentage composition of practical caustic soda amount NS=(N+NP+NC)/commercially available alkali；
(2-3) takes supernatant, and the NaCl solution that NaCl mass fraction is 0.5-1.5wt% is added, and NaCl solution additional amount is Du
Secondary seed crude oil weight 5-15wt%, at the uniform velocity stirs, 40~50 turns/min of revolving speed, settles 2h；
(2-4) takes supernatant, is 0.06~0.095MPa in vacuum degree, temperature is dry under conditions of being 90~110 DEG C；
(2-5) enters bleacher, and vacuum degree is 0.06~0.095MPa in bleacher, and temperature is 90~110 DEG C, into bleacher
The food grade atlapulgite that seed of bark of eucommia crude oil weighs 2~4wt% is added, reacts 45~55min；
(2-6) opens circulated filter system, carries out circulating filtration, until the clarification of seed of bark of eucommia crude oil；
(2-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, and temperature is 100~240 DEG C of 3~5h of reaction；
In this step: deodorizing tower is to be applied in combination to carry out physical deacidification deodorization using physical refining tower, fatty acid trap；
(2-8) is naturally cooling to 100~170 DEG C, and water flowing acceleration is cooled to room temperature；
(2-9) carries out polishing filtering by bag filter, bestows the pressure of 4kg, and filtering obtains seed of bark of eucommia refined oil；
In this step: the material of filter bag film is polyphenylene sulfide fibre, polyimides, aramid fiber or poly- four in bag filter
One of vinyl fluoride fiber；
In this step: the aperture size of filter bag film is 0.2~0.9nm in bag filter.
2. the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae according to claim 1, which is characterized in that mountain almond oil
Preparation method includes the following steps:
(1) the de- bitter pre-treatment of wild almond:
The shelling of (1-1) wild almond hulling machine, first machine are screened, and then artificial screening obtains shelling wild almond；
Wild almond is poured into 60~120s in 90~100 DEG C of hot water by (1-2), is transferred to 4~10 DEG C of 2~5min of cold water impinging cooling；
(1-3), which pours into wild almond in peeling machine, to peel, and machine screens first, and then artificial screening obtains decortication wild almond；
(1-4), which pours into decortication wild almond in 90~100 DEG C of hot water, carries out four immersions, water temperature natural cooling in soaking process；
2~4h is impregnated for the first time, is rinsed after pulling out with tap water；Second of 10~12h of immersion, is rinsed after pulling out with tap water；Third
2~4h of secondary immersion, is rinsed after pulling out with tap water；4th 2~4h of immersion, is rinsed after pulling out with tap water；
(1-5) pours into the wild almond of de- hardship in drying pool, at 60~70 DEG C, air blast or microwave drying；When microwave drying, use
The frequency of microwave drying is 2000~2400MHz, 1500~2800W of power, the bed of material with a thickness of 6~7cm；
(2) mountain almond oil extracts refining:
Pretreatment after the de- hardship of (2-1) wild almond: wild almond be crushed into 50 meshes and obtain wild almond powder, wild almond powder is immersed in
The polyvinyl alcohol-that temperature is 50-60 DEG C, polyvinyl alcohol mass fraction is 2-4wt%, polyethylene glycol mass fraction is 5-10wt%
0.5-1 hours in polyglycol solution, wild almond powder is ultrasonically treated while immersion, and ultrasonic frequency is 35KHz, ultrasound
Power be 260~400W, filter and dry wild almond powder, polyvinyl alcohol is polyvinyl alcohol 1788 or polyvinyl alcohol 1799,
Polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400 or Macrogol 600；
Polyvinyl alcohol-polyethylene glycol solution the preparation method is as follows: by polyvinyl alcohol be soaked in ethyl alcohol mass fraction be 70-
12-24 hours in the ethanol solution of 85wt%, then obtained polyvinyl alcohol is added in 50-60 DEG C of water by filtering drying,
Heating stirring 1 hour poly-vinyl alcohol solution, then add after polyethylene glycol stirring and dissolving polyvinyl alcohol-polyethylene glycol is molten
Liquid；
(2-2) low temperature squeezes mountain almond oil: expressing process uses purely physical pressing, and temperature controls between 35~55 DEG C, will consolidate
Liquid carries out the isolated wild almond dregs of rice and supernatant；The wild almond dregs of rice are added in the water of 3-6 times of its quality, utilize microwave reaction
Device controls 55~60 DEG C of temperature of material, and the compounding for accounting for that wild almond dregs of rice mass fraction is 0.055~0.065wt% is added thereto
Enzyme digests 60~80min, is centrifuged to obtain thick wild almond crude oil, and the frequency of microwave reactor is 2500~3000MHz, power 1600
~2500W；Compound enzyme includes protease and cellulase, and the mass ratio of protease and cellulase is 1:3~2:5；Protease
Including neutral proteinase and alkali protease, the mass ratio of neutral proteinase and alkali protease is 1:1~2:3；
The refining of (2-3) mountain almond oil:
(2-3-1) mixes supernatant and thick wild almond crude oil, obtains wild almond crude oil；
Wild almond crude oil is warming up to 60~70 DEG C by (2-3-2), and wild almond crude oil weight 0.05-0.15wt%, concentration 75- is added
The phosphoric acid of 95wt% reacts 25~35min；
(2-3-3) takes supernatant obtained in step (2-3-2), and the water of wild almond crude oil weight 5-15wt% is added, at the uniform velocity stirs,
Revolving speed is 40~50 turns/min, settles 2h；
(2-3-4) takes supernatant obtained in step (2-3-3), vacuum degree is 0.06~0.095MPa, temperature is 90~110
It is dry under conditions of DEG C；
(2-3-5) enters bleacher, and vacuum degree is 0.06~0.095MPa in bleacher, temperature is 90~110 DEG C, and ansu apricot is added
The food grade atlapulgite of benevolence crude oil weight 2wt%~4wt%, reacts 25~35min；
(2-3-6) opens circulated filter system, carries out circulating filtration, until filter liquor clarification；
(2-3-7) enters in deodorizing tower, and vacuum degree is 0.0002MPa in deodorizing tower, temperature is 100~240 DEG C, reacts 2~4h；
(2-3-8) is naturally cooling to 100~170 DEG C, and water flowing acceleration is cooled to room temperature；
(2-3-9) carries out polishing filtering by bag filter, gives the pressure of 4kg, is filtered, and obtains wild almond refining
Oil.
3. the preparation method of any advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae of claim 1-2, feature exist
In eucommia ulmoides seed oil is placed in mixer, is heated to 40-50 DEG C, then mountain is added in stirring, mixing speed 40-60r/min
Apricot kernel oil and vitamin A continue to stir 1.5-2.5h, and room temperature stands up to the advanced formula oil of vitamin A strengthening ansu apricot Cortex Eucommiae.
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| CN103444911A (en) * | 2012-06-05 | 2013-12-18 | 张伟伟 | Medicinal and edible health care blending oil |
| CN103651949A (en) * | 2012-09-17 | 2014-03-26 | 莱阳齐花油脂科技有限公司 | Health-maintaining and weight-losing type blending oil |
| CN104012679A (en) * | 2013-03-29 | 2014-09-03 | 洛阳春魁农业开发有限公司 | Peony seed blend oil containing eucommia seed oil and preparation method of peony seed blend oil |
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| CN103444911A (en) * | 2012-06-05 | 2013-12-18 | 张伟伟 | Medicinal and edible health care blending oil |
| CN103651949A (en) * | 2012-09-17 | 2014-03-26 | 莱阳齐花油脂科技有限公司 | Health-maintaining and weight-losing type blending oil |
| CN104012679A (en) * | 2013-03-29 | 2014-09-03 | 洛阳春魁农业开发有限公司 | Peony seed blend oil containing eucommia seed oil and preparation method of peony seed blend oil |
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