CN104194920B - A kind of preparation method of fructus cannabis oil - Google Patents
A kind of preparation method of fructus cannabis oil Download PDFInfo
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- CN104194920B CN104194920B CN201410370953.7A CN201410370953A CN104194920B CN 104194920 B CN104194920 B CN 104194920B CN 201410370953 A CN201410370953 A CN 201410370953A CN 104194920 B CN104194920 B CN 104194920B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention discloses the preparation method of a kind of fructus cannabis oil, the method include fire fiber crops seed cleaning removal of impurities, high frequency vacuum drying, laser shell in advance, extrude that shelling, malleation be quenched, cold pressing, high-voltage pulse subcritical abstraction fructus cannabis cake, the step such as low temperature crystallization degumming and dewaxing, moving-bed type adsorption deacidification and filtration, the method has produces that efficiency is high, refining energy consumption is low, refining low, the advantages of environment protection of consumption.
Description
Technical field
The invention belongs to grease processing technology field, be specifically related to the preparation method of a kind of fructus cannabis oil.
Technical background
Fire fiber crops are that a kind of sunshine is short, annual, leaf palmation and mostly be dioecious herbaceous plant, have impoverishment tolerant
Property, resistance feature.The most many countries plantation industry fire fiber crops, China's fire fiber crops yield accounts for the 1/3 of world's fire fiber crops yield
Left and right, ranks first in the world.Common fire fiber crops seed benevolence oil content is 30%～40%, linoleic acid and linolenic ratio close to 2.5,
This ratio is the optimal proportion of needed by human body aliphatic acid.Fructus cannabis oil contains abundant trace mineral element, as phosphorus, iron,
Potassium, magnesium, zinc etc..Fructus cannabis oil has been applied to various food, chocolate including fire fiber crops, fire fiber crops cake, fire sesame candy fruit, fire pitted skin
The health food series such as bag and tea beverage.Fructus cannabis oil is the high-quality material of a kind of integration of drinking and medicinal herbs simultaneously, containing the richest
Rich phytosterol, by dietary int ake, can significantly reduce serum cholesterol, and have good antimicrobial antiphlogistic effect
Really；What in fructus cannabis oil, content was the highest is Gamma-Tocopherol, has substantially at aspects such as coronary heart disease, treatment and prevention of tumour and reduction DNA damages
Effect；Also fire flaxseed oil is suitable for doing oxidation resistant dietary sources to have researcher to find, it is eliminating DPPH free radical ability side
Face exceedes olive oil；It addition, containing more than 60 kind of phenols chemical substance in fructus cannabis oil, there is good non-oxidizability, relatively low
Dosage conditions under have the strongest Scavenging ability etc..
Traditional edible oil technology of preparing mainly uses pre-squeezing and extraction, the most again by chemical Degumming, chemistry
Crude oil is refined by depickling, high temperature decolouring and the technique such as high temperature deodorization, product based on I and II oil, its main disadvantages table
Now for using chemical reagent, overrefinement causes the natural activities such as vitamin E adjoint in grease, phytosterol, carotenoid
Material damage and destruction are serious, on the other hand, are easily generated trans-fatty acid during high temperature refinery, and bringing polycyclic aromatic hydrocarbon etc. into has
Pest matter.At present, for the problems referred to above, fructus cannabis oil preparation technique is studied by some researchers.
CN 1563306A discloses preparation method and the application of a kind of fructus cannabis oil, uses shelling cold press, then through filtering and
Centrifugal treating obtains cold press fructus cannabis oil, extracts cold pressed cake with propane or butane simultaneously, is refined by the extraction oil of acquisition again
And anti-oxidant treatment, it is thus achieved that refined fructus cannabis oil, it is eventually fabricated soft capsule, this technology can produce most fructus cannabis oil,
But it is not directed to the low-temperature refining technology of fructus cannabis oil.
CN 101177647A discloses a kind of fire fiber crops grease processing technique, use pneumatic conveying drying, shell, dry, quenched,
After normal temperature squeezing, centrifugal, filtration etc. process, it is thus achieved that cold press refines grease of fructus cannabis, and this technical application is reliable, but is not directed to
The low-temperature refining technology of fructus cannabis oil.
CN 102585999A discloses a kind of method of squeezing hemp seed oil, uses washing, heating using microwave, squeezes, filters
Producing with disinfecting steps, this technology is not directed to exuviating technology and the low-temperature refining technology of fructus cannabis oil of fire fiber crops seed.
CN 102816631A discloses a kind of method of acid system extrusion aqueous enzymatic extraction fire flaxseed oil fat, uses sulphur
Acid carries out pre-processing fructus cannabis, then extrusion, then carries out aqueous enzymatic method liquefaction, and this technology can obtain quality preferably fire fiber crops
Benevolence oil and fire fiber crops albumen, but it is not directed to exuviating technology and the low-temperature refining technology of fructus cannabis oil of fire fiber crops seed.
CN 103289819A discloses the technique of a kind of supercritical carbon dioxide extracting grease of fructus cannabis, and this technology has
The advantage such as pollution-free, no solvent residue, extraction temperature are low, use is safe, but it is not directed to exuviating technology and the fire of fire fiber crops seed
The low-temperature refining technology of fiber crops benevolence oil.
From the point of view of above-mentioned fructus cannabis oil preparation method, in the main extracting method still paying close attention to fructus cannabis oil, to fire fiber crops seed
Pretreatment exuviating technology and the low-temperature refining technical research of fructus cannabis oil more lack.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of fructus cannabis oil, fire fiber crops seed has been carried out pre-de-by this preparation method
Shell processes and have employed low-temperature refining technology, has that drying efficiency is high, refining energy consumption is low, refining consumes low, advantages of environment protection.
The above-mentioned purpose of the present invention is achieved through the following technical solutions: the preparation method of a kind of fructus cannabis oil, should
Method comprises the following steps:
(1) clear up, be dried: choose fresh fire fiber crops seed, after cleaning, use high frequency vacuum drying；
(2) shelling in advance: use laser to cut the fire fiber crops seed after step (1) high frequency vacuum drying, it is thus achieved that to shell in advance
The fire fiber crops seed processed；
(3) shelling: carry out extruding heat treatment by the fire fiber crops seed of step (2) pre-heat treatment, it is thus achieved that fructus cannabis and housing；
(4) malleation is quenched: use the moisture of the fructus cannabis obtained in malleation quenched mode regulating step (3)；
(5) cold pressing: use mechanical expression equipment that the fructus cannabis obtained in step (4) is carried out cold pressing, it is thus achieved that
Fructus cannabis crude oil 1 and squeezing fructus cannabis cake；
(6) high-voltage pulse subcritical abstraction: use high-voltage pulse subcritical abstraction mode to process the fire obtained in step (5)
Fiber crops benevolence cake, it is thus achieved that fructus cannabis crude oil 2 and the fructus cannabis dregs of rice；
(7) low temperature crystallization degumming and dewaxing: the fructus cannabis that the fructus cannabis crude oil 1 obtained in step (5) and step (6) obtain
Crude oil 2 adds filter aid be stirred, then uniform decrease in temperature, then carry out cold analysis process, obtain degumming dewaxing fire fiber crops through filtering
Benevolence oil；
(8) moving-bed type adsorption deacidification, filtration: add deacidification adsorbent in moving-burden bed reactor and step (7) is obtained
Degumming dewaxing fructus cannabis oil carry out depickling process, it is thus achieved that depickling fructus cannabis oil, after filtration seal preserve, i.e. obtain fructus cannabis
Oil.
The preparation method of the fructus cannabis oil in the present invention, include high frequency vacuum drying, laser shells in advance, malleation is quenched,
Cold pressing, high-voltage pulse subcritical abstraction, low temperature crystallization degumming and the technological means such as dewaxing, moving-bed type adsorption deacidification.
In the preparation method of this fructus cannabis oil:
Cleaning in step (1), is primarily referred to as selecting fresh fire fiber crops seed, cleaning be separated off weeds, plaster, stone,
Metal impurities.
The vacuum drying parameters of step (1) medium-high frequency is: frequency 6MHz～28MHz, voltage strength 1000V/cm～
3000V/cm, vacuum 300Pa～3000Pa, use high frequency vacuum drying to the weight/mass percentage composition of water in fire fiber crops seed be 7～
11%.
Parameters when using laser to cut in step (2) is: power 6W～50W, laser cutting speed 5mm/s
～35mm/s, use laser to cut, the width of the joint-cutting being cut to fire fiber crops seed is 0.5mm～3.5mm.
When the fire fiber crops seed of step (2) pre-heat treatment is carried out extruding heat treatment by step (3), the extrusion equipment of employing
Extruding hulling machine for toothed roller type, the husking yield of described fire fiber crops seed is 85%～98%.
The quenched mode of malleation described in step (4) is: fructus cannabis is inputted mixing plant, is uniformly passed through water, persistently stirs
Mixing 10min～30min, stir speed (S.S.) is 60 turns/min～180 turns/min；Proceeding in pressure vessel, arranging pressure is the most again
0.2MPa～3MPa, processes 15min～60min；Fructus cannabis water content after quenched is 7%～13%.
When using mechanical expression equipment that the fructus cannabis obtained in step (4) is carried out cold pressing in step (5), temperature is
25 DEG C～70 DEG C.
When step (6) using high-voltage pulse subcritical abstraction mode process the fructus cannabis cake obtained in step (5), every
Parameter is: pulse voltage 5kv～35kv, burst length 10 μ s～100 μ s, and the solvent used during subcritical abstraction is butane, sub-
Critical extracting pressure is 0.3MPa～1.5MPa, extraction time 0.8h～4.0h, and extraction temperature is 8 DEG C～50 DEG C.
The detailed process carrying out low temperature crystallization degumming and dewaxing treatment in step (7) is: the fructus cannabis obtained in step (5)
Adding filter aid in the fructus cannabis crude oil 2 that crude oil 1 and step (6) obtain and be stirred 15min～30min, stir speed (S.S.) is 20
Turning/min～80 turns/min, then uniform decrease in temperature is to 0 DEG C～16 DEG C, during uniform decrease in temperature stir speed (S.S.) be 5 turns/min～35 turns/
Min, temperature fall time is 2h～6h, maintain 4h～12h to carry out cold analysis process after temperature stabilization again, be eventually adding diatomite and adopt
Carrying out filtering with pressure type leaf filter and i.e. obtain degumming dewaxing fructus cannabis oil, wherein filter aid is fructus cannabis cake powder, described fire
The consumption of fiber crops benevolence cake powder accounts for fructus cannabis crude oil 1 and the 0.05%～0.3% of fructus cannabis crude oil 2 gross mass.
The filter aid fructus cannabis cake powder used in step (7), can use the fire obtained in above-mentioned steps of the present invention (5)
The fructus cannabis dregs of rice obtained in fiber crops benevolence cake and step (6) obtain after pulverizing, the mesh number of the fructus cannabis cake powder obtained after pulverizing
It is 60 mesh～120 mesh, it is also possible to obtain using commercially available fructus cannabis cake or the fructus cannabis dregs of rice to pulverize, but filter aid in the present invention
Consumption is little, and the fructus cannabis cake of present invention acquisition during preparing fructus cannabis oil and the fructus cannabis dregs of rice can enough be answered
With.
Step (8) adds in moving-burden bed reactor the degumming dewaxing fructus cannabis that step (7) is obtained by deacidification adsorbent
Oil carry out depickling process time, degumming dewaxing fructus cannabis oil be cycling in and out from bottom to top, deacidification adsorbent from top to down, wherein depickling
Temperature is 20 DEG C～70 DEG C, and adsorption time is 0.5h～3.5h.
Deacidification adsorbent of the present invention is become by alkaline bentonites soil, three kinds of mixed raw materials of silica and diatomite,
The weight/mass percentage composition of each raw material is: alkaline bentonites soil 45%～85%, silica 1 0%～50% and diatomite 5%～
20%.
Wherein said alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, NaOH
Consumption accounts for the 15～25% of bentonite gross mass.
The preparation process of wherein said deacidification adsorbent is: by alkaline bentonites soil, silica and diatomite at normal temperature
Lower grinding is i.e. prepared as deacidification adsorbent.
Compared with prior art, present invention have the advantage that
(1) the inventive method uses high frequency vacuum drying device regulation fire fiber crops seed moisture quickly and not damaged, it is adaptable to work
Industry metaplasia is produced；
(2) the inventive method employing pre-exuviating technology of laser matches with toothed roller type extruding hulling machine and beneficially improves fire fiber crops
The husking yield of seed；
(3) the inventive method uses the quenched fructus cannabis of malleation, has the advantages such as simple, low, efficiency Gao Yong of energy consumption of operation；
(4) the inventive method uses high-voltage pulse subcritical abstraction fructus cannabis cake, have that operation is simple, extraction efficiency high,
Advantages of environment protection；
(5) the inventive method uses low temperature crystallization degumming and dewaxing, simultaneously removing colloid and wax, operates simple and energy consumption
Low advantage；
(6) the inventive method uses moving-bed type adsorption deacidification, has deacidification efficiency high feature；
(7) in the inventive method integrated artistic combine that high frequency vacuum drying device is dried, laser shells in advance, toothed roller type extruding
Shelling, malleation is quenched, cold pressing, high-voltage pulse subcritical abstraction, low temperature crystallization degumming and dewaxing, moving-bed type adsorption deacidification
Etc. technology, having that energy consumption is low, refining consumption is low, product quality is high, advantages of environment protection.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that in embodiment of the present invention 1-6 prepared by fructus cannabis oil；
Fig. 2 is the oxidation induction period curve of fructus cannabis oil in the embodiment of the present invention 6.
Detailed description of the invention
Embodiment 1
As it is shown in figure 1, select fresh fire fiber crops seed, cleaning is separated off impurity, then fire fiber crops seed is delivered to high frequency true
Empty drying equipment is dried, its medium frequency be 27.12MHz voltage strength be 1500V/cm, vacuum 1000Pa, vacuum drying
To by the weight/mass percentage composition 8.5% of water in fire fiber crops seed, dried fire fiber crops seed is carried out pre-heat treatment, laser power 10W,
Laser cutting speed 10mm/s；The laser lancing width being cut to fire fiber crops seed is 1.5mm, is then sent to toothed roller type extruding shelling
Machine, the husking yield of its moderate heat fiber crops seed is 91.5%；Then, fructus cannabis input mixing plant, it is passed through water, continuously stirred 15min, stirs
Mixing speed is 90 turns/min；Proceeding in pressure vessel, arranging pressure is 0.6MPa the most again, process 30min, quenched after fire fiber crops
Benevolence water content is 9%；Then, fructus cannabis being conveyed into single screw press and squeezes, wherein fructus cannabis temperature is 50 DEG C, pressure
Squeeze and obtain fructus cannabis squeezing crude oil 1 and fructus cannabis cake；Fructus cannabis cake is put in the subcritical equipment of high-voltage pulse, in the present embodiment
The precritical detailed process of high-voltage pulse be referred to the postcritical operating process of high-voltage pulse, only pressure regulation and extract molten
Agent is different, and lower same, wherein pulse voltage 15kv, burst length 55 μ s, subcritical butane extracting pressure is 0.5MPa, extraction time
2.6h, extraction temperature is 25 DEG C, and after having extracted, decompression obtains extraction fructus cannabis crude oil 2；Then, at fructus cannabis crude oil 1 and fire
Fiber crops benevolence crude oil 2 adds helping of 0.08% (consumption of fructus cannabis cake powder accounting for the 0.08% of fructus cannabis crude oil gross mass, lower same)
(fructus cannabis cake powder is by entering above-mentioned that prepare or commercially available fructus cannabis cake or the fructus cannabis dregs of rice for filtering agent fructus cannabis cake powder
Row obtains after pulverizing, and the mesh number of the fructus cannabis cake powder obtained after pulverizing is 60 mesh～120 mesh, lower same), continuously stirred 20min,
Stir speed (S.S.) is 30 turns/min, is then cooled to 5 DEG C, and stir speed (S.S.) is 15 turns/min, and temperature fall time is 4h, after temperature stabilization again
Maintain 6h carry out cold analysis process, be subsequently adding diatomite and use pressure type leaf filter (unit type NYB-15, only enumerates,
It is not construed as limiting) filter, it is thus achieved that degumming dewaxing fructus cannabis oil；The fructus cannabis oil that degumming dewaxed again is cycling in and out from bottom to top,
From top to down, wherein depickling temperature controls at 45 DEG C deacidification adsorbent, adsorption time 1.5h；Finally depickling fructus cannabis oil is carried out
Filter, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline bentonites soil, 2. silica, 3. three kinds of diatomite is former
Abrasive lapping is prepared from, and shared by the most each raw material, mass percent is: alkaline bentonites soil: 75%；Silica: 15%；Diatom
Native: 10%, alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, and the consumption of NaOH accounts for swelling
The 15% of soil gross mass.
Embodiment 2
As it is shown in figure 1, select fresh fire fiber crops seed, cleaning is separated off impurity, then fire fiber crops seed is delivered to high frequency true
Empty drying equipment is dried, and its medium frequency is 27.12MHz, and voltage strength is 1000V/cm, vacuum 500Pa, vacuum drying
To by the weight/mass percentage composition 9.0% of water in fire fiber crops seed, dried fire fiber crops seed is carried out pre-heat treatment, laser power 15W,
Laser cutting speed 15mm/s, the width of the laser lancing being cut to fire fiber crops seed is 1.8mm, is then sent to toothed roller type extruding de-
Shell machine, wherein peeling rate is 92%；Then, fructus cannabis input mixing plant, it is passed through water, continuously stirred 18min, stir speed (S.S.) is
70 turns/min；Proceeding in pressure vessel, arranging pressure is 0.9MPa the most again, process 25min, quenched after fructus cannabis water content
It is 8.5%；Then, fructus cannabis being conveyed into twin-screw squeezer and squeezes, wherein fructus cannabis temperature is 45 DEG C, and squeezing obtains
Fructus cannabis squeezing crude oil 1 and fructus cannabis cake；Fructus cannabis cake is put in the subcritical equipment of high-voltage pulse, wherein pulse voltage
20kv, burst length 35 μ s, subcritical butane extracting pressure is 0.6MPa, extraction time 3.0h, and extraction temperature is 20 DEG C, extraction
After completing, decompression obtains extraction fructus cannabis crude oil 2；Then, fructus cannabis crude oil 1 and fructus cannabis crude oil 2 add 0.1% help
Filtering agent fructus cannabis cake powder, continuously stirred 15min, stir speed (S.S.) is 40 turns/min, is then cooled to 6 DEG C, and stir speed (S.S.) is 18
Turning/min, temperature fall time is 3.5h, maintains 5.5h to carry out cold analysis process again, be subsequently adding diatomite and use pressure after temperature stabilization
Power formula leaf filter filters, it is thus achieved that degumming dewaxing fructus cannabis oil；The fructus cannabis oil that degumming dewaxed again is cycling in and out from bottom to top,
From top to down, wherein depickling temperature controls at 40 DEG C deacidification adsorbent, adsorption time 1.2h；Finally depickling fructus cannabis oil is carried out
Filter, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline bentonites soil, 2. silica, 3. three kinds of diatomite is former
Abrasive lapping is prepared from, and shared by each raw material, mass percent is: alkaline bentonites soil: 60%；Silica: 35%；Diatomite:
5%, alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, and it is total that the consumption of NaOH accounts for bentonite
The 20% of quality.
Embodiment 3
As it is shown in figure 1, select fresh fire fiber crops seed, cleaning is separated off impurity, then fire fiber crops seed is delivered to high frequency true
Empty drying equipment is dried, and its medium frequency is 27.12MHz, and voltage strength is 1600V/cm, vacuum 800Pa, vacuum drying
To by the weight/mass percentage composition 8.0% of water in fire fiber crops seed, dried fire fiber crops seed is carried out pre-heat treatment, laser power 25W,
Laser cutting speed 25mm/s, the width of the laser lancing being cut to fire fiber crops seed is 2.0mm, is then sent to toothed roller type extruding de-
Shell machine, wherein peeling rate is 95%；Then, fructus cannabis input mixing plant, it is passed through water, continuously stirred 20min, stir speed (S.S.) is
60 turns/min；Proceeding in pressure vessel, arranging pressure is 0.9MPa the most again, process 16min, quenched after fructus cannabis water content
It is 9.5%；Then, fructus cannabis being conveyed into hydraulic squeezing press and squeezes, wherein fructus cannabis temperature is 35 DEG C, and squeezing obtains fire
Fiber crops benevolence squeezing crude oil 1 and fructus cannabis cake；Fructus cannabis cake is put in the subcritical equipment of high-voltage pulse, wherein pulse voltage 30kv,
Burst length 30 μ s, subcritical butane extracting pressure is 0.4MPa, extraction time 3.3h, and extraction temperature is 20 DEG C, and extraction completes
After, decompression obtains extraction fructus cannabis crude oil 2；Then, in fructus cannabis crude oil 1 and fructus cannabis crude oil 2, add the drainage of 0.12%
Agent fructus cannabis cake powder, continuously stirred 20min, stir speed (S.S.) is 35 turns/min, is then cooled to 10 DEG C, and stir speed (S.S.) is 20
Turning/min, temperature fall time is 3h, maintains 7h to carry out cold analysis process again, be subsequently adding diatomite and use pressure type after temperature stabilization
Leaf filter filters, it is thus achieved that degumming dewaxing fructus cannabis oil；The fructus cannabis oil that degumming dewaxed again is cycling in and out from bottom to top, depickling
From top to down, wherein depickling temperature controls at 40 DEG C adsorbent, adsorption time 1.8h；Finally depickling fructus cannabis oil was carried out
Filter, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline bentonites soil, 2. silica, 3. three kinds of diatomite is former
Abrasive lapping is prepared from, and shared by each raw material, mass percent is: alkaline bentonites soil: 80%；Silica: 10%；Diatomite:
10%, alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, and the consumption of NaOH accounts for bentonite
The 20% of gross mass.
Embodiment 4
The preparation method producing fructus cannabis oil that the present embodiment provides, as it is shown in figure 1, the method includes:
(1) cleaning: selecting fresh fire fiber crops seed, cleaning is separated off weeds, plaster, stone, metal impurities；
(2) high frequency vacuum drying: use the fire fiber crops seed moisture after cleaning in high frequency vacuum drying equipment regulating step (1),
High frequency vacuum drying parameter is: frequency is 6.78MHz, and voltage strength is 3000V/cm, vacuum 300Pa, and drying time is
30min, in dried fire fiber crops seed, moisture is 10.5%；
(3) shelling in advance: using dried fire fiber crops seed in laser appropriateness cutting process step (2), laser processing parameter is:
Power 6W, laser cutting speed 35mm/s, the laser lancing width being cut to fire fiber crops seed is 0.6mm；
(4) shelling: carry out extruding heat treatment by the fire fiber crops seed after step (3) in advance shelling, it is thus achieved that fructus cannabis and shell, extruding
Equipment is that toothed roller type extrudes hulling machine, and fire fiber crops seed husking yield is 85%；
(5) malleation is quenched: the moisture of the fructus cannabis that regulating step (4) obtains under positive pressure, and the quenched process of malleation is: will
Fructus cannabis input mixing plant, is uniformly passed through water, continuously stirred 10min, and stir speed (S.S.) is 180 turns/min, proceeds to resistance to the most again
In pressure vessel, arranging pressure is 0.2MPa, process 60min, quenched after fructus cannabis water content be 7%；
(6) cold pressing: use mechanical press that the fructus cannabis in step (5) is carried out cold pressing, it is thus achieved that fructus cannabis
Crude oil 1 and squeezing fructus cannabis cake, temperature for 25 DEG C during cold pressing fructus cannabis；
(7) high-voltage pulse subcritical abstraction: use high-voltage pulse subcritical extraction method to process fructus cannabis in step (6)
Cake, it is thus achieved that fructus cannabis crude oil 2 and the fructus cannabis dregs of rice, the detailed process of high-voltage pulse subcritical abstraction is: pulse voltage 5kv, pulse
Time 100 μ s, extractant is butane, and subcritical butane extracting pressure is 0.3MPa, extraction time 4.0h, and extraction temperature is 8
℃；
(8) low temperature crystallization degumming and dewaxing: the fire that the fructus cannabis crude oil 1 obtained in step (6) and/or step (7) obtain
Fiber crops benevolence crude oil 2 adds the filter aid fructus cannabis cake powder of 0.05% and is stirred, continuously stirred 15min, and stir speed (S.S.) is 80 turns/
min；Then being cooled to 0 DEG C, stir speed (S.S.) is 35 turns/min, and temperature fall time is 2h, maintains 12h again, then add after temperature stabilization
Enter diatomite and use pressure type leaf filter to filter；
(9) moving-bed type adsorption deacidification: add the degumming that step (8) is obtained by deacidification adsorbent in moving-burden bed reactor
Dewaxing fructus cannabis oil carries out depickling process, it is thus achieved that depickling fructus cannabis oil, and wherein deacidification adsorbent is by alkaline bentonites soil, silica
With three kinds of mixed raw materials of diatomite for forming, shared by each raw material, mass percent is: alkaline bentonites soil 45%, silica
50% and diatomite 5%；Alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, the use of NaOH
Amount accounts for the 25% of bentonite gross mass.
(10) filter: the depickling fructus cannabis oil that step (9) obtains is filtered, and airtight preservation.
Embodiment 5
The preparation method producing fructus cannabis oil that the present embodiment provides, as it is shown in figure 1, the method includes:
(1) cleaning: selecting fresh fire fiber crops seed, cleaning is separated off weeds, plaster, stone, metal impurities；
(2) high frequency vacuum drying: use the fire fiber crops seed moisture after cleaning in high frequency vacuum drying equipment regulating step (1),
High frequency vacuum drying parameter is: frequency is 13.56MHz, and voltage strength is 1000V/cm, vacuum 3000Pa, and drying time is
55min, in dried fire fiber crops seed, moisture is 9.6%；
(3) shelling in advance: using dried fire fiber crops seed in laser appropriateness cutting process step (2), laser processing parameter is:
Power 50W, laser cutting speed 5mm/s, the laser lancing width being cut to fire fiber crops seed is 3.0mm；
(4) shelling: carry out extruding heat treatment by the fire fiber crops seed after step (3) in advance shelling, it is thus achieved that fructus cannabis and shell, extruding
Equipment is that toothed roller type extrudes hulling machine, and fire fiber crops seed husking yield is 98%；
(5) malleation is quenched: the moisture of the fructus cannabis that regulating step (4) obtains under positive pressure, and the quenched process of malleation is: will
Fructus cannabis input mixing plant, is uniformly passed through water, continuously stirred 30min, and stir speed (S.S.) is 60 turns/min, proceeds to pressure the most again
In container, arranging pressure is 3MPa, process 15min, quenched after fructus cannabis water content be 13%；
(6) cold pressing: use mechanical press that the fructus cannabis in step (5) is carried out cold pressing, it is thus achieved that fructus cannabis
Crude oil 1 and squeezing fructus cannabis cake, temperature for 70 DEG C during cold pressing fructus cannabis；
(7) high-voltage pulse subcritical abstraction: use high-voltage pulse subcritical extraction method to process fructus cannabis in step (6)
Cake, it is thus achieved that fructus cannabis crude oil 2 and the fructus cannabis dregs of rice, the detailed process of high-voltage pulse subcritical abstraction is: pulse voltage 35kv, pulse
Time 10 μ s, extractant is butane, and subcritical butane extracting pressure is 1.5MPa, extraction time 0.8h, and extraction temperature is 50
℃；
(8) low temperature crystallization degumming and dewaxing: the fire that the fructus cannabis crude oil 1 obtained in step (6) and/or step (7) obtain
Fiber crops benevolence crude oil 2 adds the filter aid fructus cannabis cake powder of 0.3% and is stirred, continuously stirred 30min, and stir speed (S.S.) is 20 turns/
min；Then being cooled to 16 DEG C, stir speed (S.S.) is 5 turns/min, and temperature fall time is 6h, maintains 4h again, be subsequently adding after temperature stabilization
Diatomite also uses pressure type leaf filter to filter；
(9) moving-bed type adsorption deacidification: add the degumming that step (8) is obtained by deacidification adsorbent in moving-burden bed reactor
Dewaxing fructus cannabis oil carries out depickling process, it is thus achieved that depickling fructus cannabis oil, and wherein deacidification adsorbent is by alkaline bentonites soil, silica
With three kinds of mixed raw materials of diatomite for forming, shared by each raw material, mass percent is: alkaline bentonites soil 55%, silica
25% and diatomite 20%；Alkaline bentonites soil is made by bentonite and NaOH being ground at normal temperatures, NaOH
Consumption accounts for the 18% of bentonite gross mass.
(10) filter: the depickling fructus cannabis oil that step (9) obtains is filtered, and airtight preservation.
Embodiment 6
(1) the depickling fructus cannabis oil prepared in the embodiment of the present invention 1 is detected, it is thus achieved that the master of fructus cannabis oil
Want physical and chemical index as shown in table 1.
The main physical and chemical index of table 1 fructus cannabis oil
(2) the depickling fructus cannabis oil prepared in the embodiment of the present invention 1 is detected, it is thus achieved that the fat of fructus cannabis oil
Fat acid composition is as shown in table 2.
The aliphatic acid composition of table 2 fructus cannabis oil
| Inspection project | Testing result (%) | Detection foundation |
| Myristic acid | Do not detect | GB/T 17377-2008 |
| Palmitic acid | 6.3 | GB/T 17377-2008 |
| Palm monoenoic acid | 0.1 | GB/T 17377-2008 |
| Heptadecane acid | 0.1 | GB/T 17377-2008 |
| 17 carbon monoenoic acids | Do not detect | GB/T 17377-2008 |
| Stearic acid | 2.9 | GB/T 17377-2008 |
| Oleic acid | 12.2 | GB/T 17377-2008 |
| Linoleic acid | 56.4 | GB/T 17377-2008 |
| Leukotrienes | 20.5 | GB/T 17377-2008 |
| Arachidic acid | 0.6 | GB/T 17377-2008 |
| Peanut monoenoic acid | 0.3 | GB/T 17377-2008 |
| Peanut dienoic acid | 0.1 | GB/T 17377-2008 |
| Behenic acid | 0.2 | GB/T 17377-2008 |
| Other | 0.3 | GB/T 17377-2008 |
(3) the depickling fructus cannabis oil prepared in the embodiment of the present invention 1 is carried out sanitary index test, it is thus achieved that fire fiber crops
The sanitary index of benevolence oil is as shown in Table 3 below.
The sanitary index of table 3 fructus cannabis oil
(4) the depickling fructus cannabis oil prepared in the embodiment of the present invention 1 is carried out micro-nutrient composition test, it is thus achieved that
The micro-nutrient composition of fructus cannabis oil is as shown in Table 4 below.
Table 4 fructus cannabis oil micro-nutrient composition
| Unsaponifiable matter (%) | 2.8 | GB/T 5535.1-2008 |
| Phytosterol (mg/100g) | 66.6 | GB/T 25223-2010 |
| Chlorophyll (mg/kg) | 16.71 | SN/T 0801.21-2001 |
| Total phenol (mgSA/100g)) | 2.16 | Ultraviolet spectrophotometry |
| Vitamin E (mg/kg) | 576.5 | NY/T 1598-2008 |
(5) the depickling fructus cannabis oil prepared in the embodiment of the present invention 1 is carried out fructus cannabis oil oxidation stability test,
Test condition measures with reference to EN14112:2003；Test condition: 110 DEG C；Air mass flow: 10L/h, institute in test result such as Fig. 1
Showing, the oxidation induction period of depickling fructus cannabis oil is 2.01h/110 DEG C.
It can be seen that use the fructus cannabis oil that the preparation method in the present invention prepares from table 1-4 and Fig. 1, its reason
Change index meet relevant national standard, sanitary index meets national standard, fructus cannabis oil mainly by palmitic acid, palm monoenoic acid,
The groups such as heptadecane acid, stearic acid, oleic acid, linoleic acid, leukotrienes, arachidic acid, peanut monoenoic acid, peanut dienoic acid, behenic acid
Becoming, rich in micro-nutrient compositions such as phytosterol, total phenol and vitamin Es, antioxygenic property is good, the depickling fructus cannabis in the present invention
The oxidation induction period of oil is 2.01h/110 DEG C.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any Spirit Essence without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, be included in protection scope of the present invention.
Claims (5)
1. a preparation method for fructus cannabis oil, is characterized in that comprising the following steps:
(1) clear up, be dried: choose fresh fire fiber crops seed, after cleaning, use high frequency vacuum drying；
(2) shelling in advance: use laser to cut the fire fiber crops seed after step (1) high frequency vacuum drying, it is thus achieved that pre-heat treatment
Fire fiber crops seed；
(3) shelling: carry out extruding heat treatment by the fire fiber crops seed of step (2) pre-heat treatment, it is thus achieved that fructus cannabis and housing；
(4) malleation is quenched: use the moisture of the fructus cannabis obtained in malleation quenched mode regulating step (3)；
(5) cold pressing: use mechanical expression equipment that the fructus cannabis obtained in step (4) is carried out cold pressing, it is thus achieved that fire fiber crops
Benevolence crude oil 1 and squeezing fructus cannabis cake；
(6) high-voltage pulse subcritical abstraction: use high-voltage pulse subcritical abstraction mode to process the fructus cannabis obtained in step (5)
Cake, it is thus achieved that fructus cannabis crude oil 2 and the fructus cannabis dregs of rice；
(7) low temperature crystallization degumming and dewaxing: the fructus cannabis crude oil 2 obtained in step (5) acquisition fructus cannabis crude oil 1 and step (6)
Middle addition filter aid is stirred, then uniform decrease in temperature, then carries out cold analysis process, obtains degumming dewaxing fructus cannabis oil through filtering；
(8) moving-bed type adsorption deacidification, filtration: what step (7) was obtained by addition deacidification adsorbent in moving-burden bed reactor takes off
Glue dewaxing fructus cannabis oil carries out depickling process, it is thus achieved that depickling fructus cannabis oil, seals and preserves, i.e. obtain fructus cannabis oil after filtration；
The vacuum drying parameters of step (1) medium-high frequency is: frequency 6 MHz～28MHz, voltage strength 1000 V/cm～
3000V/cm, vacuum 300 Pa～3000Pa, use high frequency vacuum drying to the weight/mass percentage composition of water in fire fiber crops seed be 7 ~
11%；
Parameters when using laser to cut in step (2) is: power 6 W～50 W, laser cutting speed 5 mm/s
～35mm/s, the width of slit being cut to fire fiber crops seed is 0.5mm ~ 3.5mm；
The quenched mode of malleation described in step (4) is: fructus cannabis is inputted mixing plant, is uniformly passed through water, continuously stirred
10min～30min, stir speed (S.S.) is 60 turns/min～180 turns/min；Proceeding in pressure vessel, arranging pressure is the most again
0.2MPa～3MPa, process 15min～60min, quenched after fructus cannabis water content be 7%～13%；
When step (6) using high-voltage pulse subcritical abstraction mode process the fructus cannabis cake obtained in step (5), parameters
For: pulse voltage 5kv～35kv, burst length 10 s～100 s, the solvent used during subcritical abstraction is butane, subcritical
Extracting pressure is 0.3MPa～1.5MPa, extraction time 0.8h～4.0h, and extraction temperature is 8 DEG C～50 DEG C；
The detailed process carrying out low temperature crystallization degumming and dewaxing treatment in step (7) is: the fructus cannabis crude oil obtained in step (5)
1 and the fructus cannabis crude oil 2 that obtains of step (6) in add filter aid and be stirred 15min～30min, stir speed (S.S.) is 20 turns/
Min～80 turns/min, then uniform decrease in temperature is to 0 DEG C～16 DEG C, and during uniform decrease in temperature, stir speed (S.S.) is 5 turns/min～35 turns/min,
Temperature fall time is 2h～6h, maintains 4h～12h to carry out cold analysis process again, be eventually adding diatomite and use pressure after temperature stabilization
Formula leaf filter carries out filtering i.e. acquisition degumming dewaxing fructus cannabis oil, and wherein filter aid is fructus cannabis cake powder, described fructus cannabis cake
The consumption of powder accounts for fructus cannabis crude oil 1 and the 0.05%～0.3% of fructus cannabis crude oil 2 gross mass.
The preparation method of fructus cannabis oil the most according to claim 1, is characterized in that: step (2) shelled in advance in step (3)
When the fire fiber crops seed processed carries out extruding heat treatment, the extrusion equipment of employing is that toothed roller type extrudes hulling machine, described fire fiber crops seed
Husking yield is 85%～98%.
The preparation method of fructus cannabis oil the most according to claim 1, is characterized in that: use mechanical expression to set in step (5)
When the standby fructus cannabis to obtaining in step (4) carries out cold pressing, temperature is 25 DEG C～70 DEG C.
The preparation method of fructus cannabis oil the most according to claim 1, is characterized in that: at moving-burden bed reactor in step (8)
When the degumming dewaxing fructus cannabis oil that step (7) is obtained by middle addition deacidification adsorbent carries out depickling process, degumming dewaxing fructus cannabis
Oil is cycling in and out from bottom to top, and from top to down, wherein depickling temperature is 20 DEG C～70 DEG C to deacidification adsorbent, and adsorption time is 0.5h
～3.5h.
The preparation method of fructus cannabis oil the most according to claim 1, is characterized in that: described deacidification adsorbent is swollen by alkalescence
Profit soil, silica and three kinds of raw materials of diatomite are made, and the weight/mass percentage composition of each raw material is: alkaline bentonites soil 45%～85%,
Silica 1 0%～50% and diatomite 5%～20%.
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| CN109135912A (en) * | 2018-09-03 | 2019-01-04 | 无限极（中国）有限公司 | A kind of fructus cannabis oil and preparation method thereof |
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| CN101177647B (en) * | 2007-04-18 | 2010-11-03 | 广西巴马常春藤生命科技发展有限公司 | Laportea urentissima grease processing technology |
| CN102676290B (en) * | 2012-04-27 | 2013-10-30 | 无限极（中国）有限公司 | Ultrasonic assisted supercritical CO2 hemp seed oil extraction method |
| CN102669796A (en) * | 2012-05-30 | 2012-09-19 | 中国农业大学 | Chinese chestnut or castanea henryi unshelling method |
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