CN104194920A - Method for preparing hemp seed oil - Google Patents
Method for preparing hemp seed oil Download PDFInfo
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- CN104194920A CN104194920A CN201410370953.7A CN201410370953A CN104194920A CN 104194920 A CN104194920 A CN 104194920A CN 201410370953 A CN201410370953 A CN 201410370953A CN 104194920 A CN104194920 A CN 104194920A
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- hemp seed
- hemp
- seed oil
- seed
- oil
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- 239000010460 hemp oil Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 28
- 238000001291 vacuum drying Methods 0.000 claims abstract description 24
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000001125 extrusion Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 39
- 239000010779 crude oil Substances 0.000 claims description 38
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 33
- 239000000835 fiber Substances 0.000 claims description 24
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- 229940116226 behenic acid Drugs 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 229960004488 linolenic acid Drugs 0.000 description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 2
- 239000000944 linseed oil Substances 0.000 description 2
- 235000021388 linseed oil Nutrition 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 229960002969 oleic acid Drugs 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 230000001007 puffing effect Effects 0.000 description 2
- 229960004274 stearic acid Drugs 0.000 description 2
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- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005778 DNA damage Effects 0.000 description 1
- 231100000277 DNA damage Toxicity 0.000 description 1
- -1 DPPH free radical Chemical class 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 101100449533 Mus musculus Cxcl1 gene Proteins 0.000 description 1
- 235000021360 Myristic acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
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- 230000001741 anti-phlogistic effect Effects 0.000 description 1
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- 238000013459 approach Methods 0.000 description 1
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- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
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- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 1
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- 239000008157 edible vegetable oil Substances 0.000 description 1
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- 150000002989 phenols Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
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Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for preparing hemp seed oil. The method comprises the following steps of cleaning hemp seeds to remove impurities, carrying out high-frequency vacuum drying, pre-deshelling by virtue of laser, deshelling by virtue of extrusion, carrying out positive-pressure conditioning, pressing at a low temperature, carrying out high-voltage pulse subcritical extraction on hemp seed cakes, crystallizing and degumming at a low temperature, dewaxing, adsorbing and deacidifying on a moving bed, filtering and the like. The method has the advantages of high preparation efficiency, low refining energy consumption, low refining loss, environmental friendliness and the like.
Description
Technical field
The invention belongs to grease processing technology field, be specifically related to a kind of preparation method of Hemp Seed oil.
Technical background
Fire fiber crops are short, annual, leaf palmation at a kind of sunshine and mostly are dioecious herbaceous plant, have impoverishment tolerant, resistance feature.Many countries plantation industry fire is numb in the world at present, and China's numb output of fire accounts for 1/3 left and right of the numb output of world's fire, ranks first in the world.The numb seed benevolence of common fire oleaginousness is 30%～40%, and linolic acid and linolenic ratio approach 2.5, and this ratio is the optimum proportion of needed by human body lipid acid.Hemp Seed oil contains abundant trace mineral element, as phosphorus, iron, potassium, magnesium, zinc etc.Hemp Seed oil has been applied to various food, comprises that fire fiber crops are chocolate, fiery numb cake, fiery sesame candy fruit, the health food series such as fiery pitted skin bag and tea drink.Hemp Seed oil is a kind of high-quality material of integration of drinking and medicinal herbs simultaneously, contains extremely abundant plant sterol, by meals, takes in, and can significantly reduce serum cholesterol, and have good antimicrobial antiphlogistic effect; What in Hemp Seed oil, content was the highest is Gamma-Tocopherol, at aspects such as coronary heart disease, treatment and prevention of tumour and reduction DNA damages, has obvious effect; Also have investigator to find that fiery flaxseed oil is applicable to doing oxidation resistant meals resource, it is surpassing sweet oil aspect elimination DPPH free radical ability; In addition, in Hemp Seed oil, contain more than 60 kind of phenols chemical substance, there is good oxidation-resistance, under lower dosage condition, have very strong removing free radical ability etc.
Traditional edible oil technology of preparing is mainly to adopt pre-squeezing and solvent extraction, and then by techniques such as chemical Degumming, chemical deacidification, high temperature decolouring and high temperature deodorizations, crude oil is carried out to refining, product be take I and II oil as main, its main disadvantages shows as use chemical reagent, natural active matter losses such as the vitamin-E that overrefinement causes following in grease, plant sterol, carotenoid and destroy serious, on the other hand, in high temperature refining process, easily produce trans fatty acid, bring the objectionable impuritiess such as polycyclic aromatic hydrocarbons into.At present, for the problems referred to above, some investigators are studied Hemp Seed oil preparation technique.
CN 1563306A discloses a kind of preparation method and application of Hemp Seed oil, adopt shelling cold press, obtain cold press Hemp Seed oil with centrifugal treating after filtration again, simultaneously with propane or butane extraction cold pressed cake, the extraction oil of acquisition is refined and antioxidation treatment again, obtained refining Hemp Seed oil, finally make soft capsule, this technology can be produced most Hemp Seed oil, but does not relate to the low-temperature refining technology of Hemp Seed oil.
CN 101177647A discloses the numb grease processing technique of a kind of fire, after adopting air stream drying, shelling, oven dry, modified, normal temperature squeezing, centrifugal, filtration etc. to process, obtain the refining grease of fructus cannabis of cold press, this technical application is reliable, but does not relate to the low-temperature refining technology of Hemp Seed oil.
CN 102585999A discloses a kind of method of squeezing hemp seed oil, adopts washing, microwave heating, squeezing, filtration and disinfecting steps to produce, and this technology does not relate to the low-temperature refining technology of exuviating technology and the Hemp Seed oil of fiery numb seed.
CN 102816631A discloses a kind of method of acid system extruding puffing aqueous enzymatic extraction fire flaxseed oil fat, adopt sulfuric acid to carry out pre-treatment Hemp Seed, then extruding puffing, carry out again aqueous enzymatic method liquefaction, this technology can obtain the good Hemp Seed oil of quality and fiery numb albumen, but does not relate to the low-temperature refining technology of exuviating technology and the Hemp Seed oil of fiery numb seed.
CN 103289819A discloses a kind of technique of supercritical carbon dioxide extraction grease of fructus cannabis, the advantages such as that this technology has is pollution-free, no solvent residue, extraction temperature is low, use is safe, but do not relate to the low-temperature refining technology of exuviating technology and the Hemp Seed oil of fiery numb seed.
From above-mentioned Hemp Seed oil preparation method, mainly still pay close attention on the extracting method of Hemp Seed oil, the low-temperature refining technical study of the pre-treatment exuviating technology of the numb seed of fire and Hemp Seed oil is comparatively lacked.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of Hemp Seed oil, this preparation method has carried out pre-heat treatment and has adopted low-temperature refining technology the numb seed of fire, has that drying efficiency is high, refining energy consumption is low, low a, advantages of environment protection of refining consumption.
Above-mentioned purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of Hemp Seed oil, and the method comprises the following steps:
(1) cleaning, dry: choose fresh fire fiber crops seed, adopt high frequency vacuum drying after cleaning;
(2) shelling in advance: adopt laser to cut the fire fiber crops seed after step (1) high frequency vacuum drying, obtain the fire fiber crops seed of pre-heat treatment;
(3) shelling: the fire fiber crops seed of the pre-heat treatment of step (2) is pushed to heat treatment, obtain Hemp Seed and housing;
(4) malleation is modified: the moisture that adopts the Hemp Seed obtaining in the modified mode regulating step of malleation (3);
(5) low temperature pressing: adopt mechanical expression equipment to carry out low temperature pressing to the Hemp Seed obtaining in step (4), obtain Hemp Seed crude oil 1 and squeezing Hemp Seed cake;
(6) high-voltage pulse subcritical abstraction: adopt the Hemp Seed cake obtaining in high-voltage pulse subcritical abstraction mode treatment step (5), obtain Hemp Seed crude oil 2 and the Hemp Seed dregs of rice;
(7) low temperature crystallization comes unstuck and dewaxes: in the Hemp Seed crude oil 2 that the Hemp Seed crude oil 1 obtaining in step (5) and step (6) obtain, add flocculating aids to stir, then uniform decrease in temperature, carry out again cold analysis processing, obtain after filtration the dewaxing Hemp Seed oil that comes unstuck;
(8) moving-bed type adsorption deacidification, filtration: in moving-burden bed reactor, add the dewaxing Hemp Seed oil that comes unstuck that deacidification adsorbent obtains step (7) to carry out depickling processing, obtain depickling Hemp Seed oil, after filtering, sealing is preserved, and obtains Hemp Seed oil.
The preparation method of the Hemp Seed oil in the present invention, has comprised that high frequency vacuum drying, laser shell in advance, malleation is modified, low temperature pressing, high-voltage pulse subcritical abstraction, low temperature crystallization comes unstuck and the technique means such as dewaxing, moving-bed type adsorption deacidification.
In the preparation method of this Hemp Seed oil:
Cleaning in step (1), mainly refers to and selects fresh fire fiber crops seed, weeds, plaster, stone, metal impurities are removed in cleaning separation.
The vacuum drying parameters of step (1) medium-high frequency is: frequency 6MHz～28MHz, and voltage strength 1000V/cm～3000V/cm, vacuum tightness 300Pa～3000Pa, adopting high frequency vacuum drying to the quality percentage composition of water in fiery numb seed is 7～11%.
Parameters while adopting laser to cut in step (2) is: power 6W～50W, and laser cutting speed 5mm/s～35mm/s, adopts laser to cut, and the width that is cut to the joint-cutting of fiery numb seed is 0.5mm～3.5mm.
While the fire fiber crops seed of the pre-heat treatment of step (2) being pushed to heat treatment in step (3), the extrusion equipment of employing is toothed roller type extruding peeler, and the husking yield of described fire fiber crops seed is 85%～98%.
The modified mode of malleation described in step (4) is: Hemp Seed is inputted to whipping device, evenly pass into water, continue to stir 10min～30min, stir speed (S.S.) is 60 turn/min of turn/min～180; And then proceed in pressure vessel, it is 0.2MPa～3MPa that pressure is set, and processes 15min～60min; Hemp Seed water content after modified is 7%～13%.
While adopting mechanical expression equipment to carry out low temperature pressing to the Hemp Seed obtaining in step (4) in step (5), temperature is 25 ℃～70 ℃.
While adopting the Hemp Seed cake obtaining in high-voltage pulse subcritical abstraction mode treatment step (5) in step (6), parameters is: pulsed voltage 5kv～35kv, burst lengths 10 μ s～100 μ s, the solvent adopting during subcritical abstraction is butane, subcritical abstraction pressure is 0.3MPa～1.5MPa, extraction time 0.8h～4.0h, extraction temperature is 8 ℃～50 ℃.
In step (7), carry out that low temperature crystallization comes unstuck and the detailed process of dewaxing treatment is: in the Hemp Seed crude oil 2 that the Hemp Seed crude oil 1 obtaining in step (5) and step (6) obtain, add flocculating aids to stir 15min～30min, stir speed (S.S.) is 20 turn/min of turn/min～80, then uniform decrease in temperature to 0 ℃～16 ℃, during uniform decrease in temperature, stir speed (S.S.) is 5 turn/min of turn/min～35, temperature fall time is 2h～6h, , after temperature-stable, maintain again 4h～12h and carry out cold analysis processing, finally add diatomite and adopt pressure type leaf filter to filter and obtain the dewaxing Hemp Seed oil that comes unstuck, wherein flocculating aids is Hemp Seed cake powder, the consumption of described Hemp Seed cake powder accounts for 0.05%～0.3% of Hemp Seed crude oil 1 and Hemp Seed crude oil 2 total masses.
The flocculating aids Hemp Seed cake powder adopting in step (7), can adopt the Hemp Seed cake and the middle Hemp Seed dregs of rice that obtain of step (6) that in above-mentioned steps of the present invention (5), obtain to pulverize rear acquisition, the order number of the Hemp Seed cake powder obtaining after pulverizing is 60 order～120 orders, also can obtain adopting commercially available Hemp Seed cake or the Hemp Seed dregs of rice to pulverize, but the consumption of flocculating aids is little in the present invention, Hemp Seed cake and the Hemp Seed dregs of rice of the acquisition of the present invention in the process of preparing Hemp Seed oil can enough be applied.
While adding deacidification adsorbent to carry out depickling processing to the dewaxing Hemp Seed oil that comes unstuck of step (7) acquisition in step (8) in moving-burden bed reactor, the dewaxing Hemp Seed oil that the comes unstuck turnover that circulates from bottom to top, deacidification adsorbent from top to down, wherein depickling temperature is 20 ℃～70 ℃, and adsorption time is 0.5h～3.5h.
Deacidification adsorbent of the present invention is become by alkaline wilkinite, three kinds of mixed raw materials of silicon-dioxide and diatomite, and the quality percentage composition of each raw material is: alkaline wilkinite 45%～85%, silica 1 0%～50% and diatomite 5%～20%.
Wherein said alkaline wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 15～25% of wilkinite total mass.
The preparation process of wherein said deacidification adsorbent is: alkaline wilkinite, silicon-dioxide and diatomite are ground at normal temperatures and is prepared into deacidification adsorbent.
Compared with prior art, tool of the present invention has the following advantages:
(1) the inventive method adopts high frequency vacuum drying device to regulate fiery numb seed moisture fast and not damaged, is applicable to suitability for industrialized production;
(2) the inventive method adopts the pre-exuviating technology of laser to match and be conducive to improve the husking yield of fiery numb seed with toothed roller type extruding peeler;
(3) the inventive method adopts the modified Hemp Seed of malleation, has the advantages such as operation is simple and easy, energy consumption is low, efficiency Gao Yong;
(4) the inventive method adopts high-voltage pulse subcritical abstraction Hemp Seed cake, has that operation is simple and easy, extraction efficiency is high, advantages of environment protection;
(5) the inventive method adopts low temperature crystallization come unstuck and dewax, and removes colloid and wax simultaneously, operates the simple and easy and low advantage of energy consumption;
(6) the inventive method adopts moving-bed type adsorption deacidification, has the high feature of deacidification efficiency;
(7) in the inventive method, integrated artistic combines that high frequency vacuum drying device is dry, laser shells in advance, toothed roller type extruding shelling, malleation are modified, low temperature pressing, high-voltage pulse subcritical abstraction, low temperature crystallization comes unstuck and the technology such as dewaxing, moving-bed type adsorption deacidification, have 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 of Hemp Seed oil preparation in embodiment of the present invention 1-6;
Fig. 2 is the oxidation induction period curve of Hemp Seed oil in the embodiment of the present invention 6.
Embodiment
Embodiment 1
As shown in Figure 1, select fresh fire fiber crops seed, impurity is removed in cleaning separation, then the numb seed of fire is delivered to high frequency vacuum drying equipment and is dried, its medium frequency is that 27.12MHz voltage strength is 1500V/cm, vacuum tightness 1000Pa, vacuum-drying is extremely by the quality percentage composition 8.5% of water in the numb seed of fire, the numb seed of dried fire is carried out to pre-heat treatment, laser power 10W, laser cutting speed 10mm/s, the laser lancing width that is cut to fiery numb seed is 1.5mm, is then delivered to toothed roller type extruding peeler, and the husking yield of its moderate heat fiber crops seed is 91.5%, then, Hemp Seed input whipping device, passes into water, continues to stir 15min, and stir speed (S.S.) is 90 turn/min, and then proceed in pressure vessel, it is 0.6MPa that pressure is set, and processes 30min, the Hemp Seed water content after modified is 9%, then, Hemp Seed is conveyed into single screw press and squeezes, wherein Hemp Seed temperature is 50 ℃, and squeezing obtains Hemp Seed squeezing crude oil 1 and Hemp Seed cake, Hemp Seed cake is put into the subcritical equipment of high-voltage pulse, the precritical detailed process of high-voltage pulse in the present embodiment can be with reference to the postcritical operating process of high-voltage pulse, only pressure adjusting is different with extraction solvent, lower same, wherein pulsed voltage 15kv, burst lengths 55 μ s, subcritical butane extracting pressure is 0.5MPa, extraction time 2.6h, and extraction temperature is 25 ℃, after having extracted, decompression obtains extraction Hemp Seed crude oil 2, then, (consumption of Hemp Seed cake powder accounts for 0.08% of Hemp Seed crude oil total mass in Hemp Seed crude oil 1 and Hemp Seed crude oil 2, to add 0.08%, (Hemp Seed cake powder is by pulverizing rear acquisition by above-mentioned that prepare or commercially available Hemp Seed cake or the Hemp Seed dregs of rice for flocculating aids Hemp Seed cake powder down together), the order number of the Hemp Seed cake powder obtaining after pulverizing is 60 order～120 orders, lower same), continue to stir 20min, stir speed (S.S.) is 30 turn/min, then be cooled to 5 ℃, stir speed (S.S.) is 15 turn/min, temperature fall time is 4h, after temperature-stable, maintain again 6h and carry out cold analysis processing, then add diatomite and adopt pressure type leaf filter (unit type NYB-15, only for enumerating, be not construed as limiting) filter, the acquisition dewaxing Hemp Seed oil that comes unstuck, the dewaxing Hemp Seed oil that will come unstuck the again turnover that circulates from bottom to top, from top to down, wherein depickling temperature is controlled at 45 ℃ to deacidification adsorbent, adsorption time 1.5h, finally depickling Hemp Seed oil is filtered, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline wilkinite, and 2. silicon-dioxide, 3. three kinds of former abrasive lappings of diatomite are prepared from, and wherein the shared mass percent of each raw material is: alkaline wilkinite: 75%; Silicon-dioxide: 15%; Diatomite: 10%, alkaline wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 15% of wilkinite total mass.
Embodiment 2
As shown in Figure 1, select fresh fire fiber crops seed, impurity is removed in cleaning separation, then the numb seed of fire being delivered to high frequency vacuum drying equipment is dried, its medium frequency is 27.12MHz, voltage strength is 1000V/cm, vacuum tightness 500Pa, vacuum-drying, to by the quality percentage composition 9.0% of water in the numb seed of fire, is carried out pre-heat treatment, laser power 15W by the numb seed of dried fire, laser cutting speed 15mm/s, the width that is cut to the laser lancing of fiery numb seed is 1.8mm, is then delivered to toothed roller type extruding peeler, and wherein peeling rate is 92%; Then, Hemp Seed input whipping device, passes into water, continues to stir 18min, and stir speed (S.S.) is 70 turn/min; And then proceed in pressure vessel, it is 0.9MPa that pressure is set, and processes 25min, the Hemp Seed water content after modified is 8.5%; Then, Hemp Seed is conveyed into twin screw squeezing machine and squeezes, wherein Hemp Seed temperature is 45 ℃, and squeezing obtains Hemp Seed squeezing crude oil 1 and Hemp Seed cake; Hemp Seed cake is put into the subcritical equipment of high-voltage pulse, pulsed voltage 20kv wherein, burst lengths 35 μ s, subcritical butane extracting pressure is 0.6MPa, extraction time 3.0h, extraction temperature is 20 ℃, after having extracted, decompression obtains extraction Hemp Seed crude oil 2; Then, in Hemp Seed crude oil 1 and Hemp Seed crude oil 2, add 0.1% flocculating aids Hemp Seed cake powder, continue to stir 15min, stir speed (S.S.) is 40 turn/min, is then cooled to 6 ℃, and stir speed (S.S.) is 18 turn/min, temperature fall time is 3.5h, after temperature-stable, maintain again 5.5h and carry out cold analysis processing, then add diatomite and adopt pressure type leaf filter to filter, obtain the dewaxing Hemp Seed oil that comes unstuck; The dewaxing Hemp Seed oil that will come unstuck the again turnover that circulates from bottom to top, from top to down, wherein depickling temperature is controlled at 40 ℃ to deacidification adsorbent, adsorption time 1.2h; Finally depickling Hemp Seed oil is filtered, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline wilkinite, and 2. silicon-dioxide, 3. three kinds of former abrasive lappings of diatomite are prepared from, and the shared mass percent of each raw material is: alkaline wilkinite: 60%; Silicon-dioxide: 35%; Diatomite: 5%, alkaline wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 20% of wilkinite total mass.
Embodiment 3
As shown in Figure 1, select fresh fire fiber crops seed, impurity is removed in cleaning separation, then the numb seed of fire being delivered to high frequency vacuum drying equipment is dried, its medium frequency is 27.12MHz, voltage strength is 1600V/cm, vacuum tightness 800Pa, vacuum-drying, to by the quality percentage composition 8.0% of water in the numb seed of fire, is carried out pre-heat treatment, laser power 25W by the numb seed of dried fire, laser cutting speed 25mm/s, the width that is cut to the laser lancing of fiery numb seed is 2.0mm, is then delivered to toothed roller type extruding peeler, and wherein peeling rate is 95%; Then, Hemp Seed input whipping device, passes into water, continues to stir 20min, and stir speed (S.S.) is 60 turn/min; And then proceed in pressure vessel, it is 0.9MPa that pressure is set, and processes 16min, the Hemp Seed water content after modified is 9.5%; Then, Hemp Seed is conveyed into hydraulic squeezing press and squeezes, wherein Hemp Seed temperature is 35 ℃, and squeezing obtains Hemp Seed squeezing crude oil 1 and Hemp Seed cake; Hemp Seed cake is put into the subcritical equipment of high-voltage pulse, pulsed voltage 30kv wherein, burst lengths 30 μ s, subcritical butane extracting pressure is 0.4MPa, extraction time 3.3h, extraction temperature is 20 ℃, after having extracted, decompression obtains extraction Hemp Seed crude oil 2; Then, in Hemp Seed crude oil 1 and Hemp Seed crude oil 2, add 0.12% flocculating aids Hemp Seed cake powder, continue to stir 20min, stir speed (S.S.) is 35 turn/min, is then cooled to 10 ℃, and stir speed (S.S.) is 20 turn/min, temperature fall time is 3h, after temperature-stable, maintain again 7h and carry out cold analysis processing, then add diatomite and adopt pressure type leaf filter to filter, obtain the dewaxing Hemp Seed oil that comes unstuck; The dewaxing Hemp Seed oil that will come unstuck the again turnover that circulates from bottom to top, from top to down, wherein depickling temperature is controlled at 40 ℃ to deacidification adsorbent, adsorption time 1.8h; Finally depickling Hemp Seed oil is filtered, and airtight preservation.
In this example, the preparation method of deacidification adsorbent is: 1. alkaline wilkinite, and 2. silicon-dioxide, 3. three kinds of former abrasive lappings of diatomite are prepared from, and the shared mass percent of each raw material is: alkaline wilkinite: 80%; Silicon-dioxide: 10%; Diatomite: 10%, alkaline wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 20% of wilkinite total mass.
Embodiment 4
The preparation method who produces Hemp Seed oil that the present embodiment provides, as shown in Figure 1, the method comprises:
(1) cleaning: select fresh fire fiber crops seed, weeds, plaster, stone, metal impurities are removed in cleaning separation;
(2) high frequency vacuum drying: adopt the fiber crops of the fire after cleaning seed moisture in high frequency vacuum drying equipment regulating step (1), high frequency vacuum drying parameter is: frequency is 6.78MHz, voltage strength is 3000V/cm, vacuum tightness 300Pa, be 30min time of drying, and in dry rear fiery numb seed, moisture content is 10.5%;
(3) shelling in advance: adopt the numb seed of dried fire in laser appropriateness cutting process step (2), laser processing parameter is: power 6W, laser cutting speed 35mm/s, the laser lancing width that is cut to fiery numb seed is 0.6mm;
(4) shelling: the fire fiber crops seed after the pre-shelling of step (3) is pushed to heat treatment, obtain Hemp Seed and shell, extrusion equipment is toothed roller type extruding peeler, and fiery numb seed husking yield is 85%;
(5) malleation is modified: the moisture of the Hemp Seed that regulating step under positive pressure (4) obtains, the modified process of malleation is: Hemp Seed is inputted to whipping device, evenly pass into water, continue to stir 10min, stir speed (S.S.) is 180 turn/min, and then proceeds in pressure vessel, and it is 0.2MPa that pressure is set, process 60min, the Hemp Seed water content after modified is 7%;
(6) low temperature pressing: adopt mechanical expression machine to carry out low temperature pressing to the Hemp Seed in step (5), obtain Hemp Seed crude oil 1 and squeezing Hemp Seed cake, during low temperature pressing Hemp Seed, temperature is 25 ℃;
(7) high-voltage pulse subcritical abstraction: adopt Hemp Seed cake in high-voltage pulse subcritical extraction method treatment step (6), obtain Hemp Seed crude oil 2 and the Hemp Seed dregs of rice, the detailed process of high-voltage pulse subcritical abstraction is: pulsed voltage 5kv, burst lengths 100 μ s, extraction solvent is butane, subcritical butane extracting pressure is 0.3MPa, extraction time 4.0h, and extraction temperature is 8 ℃;
(8) low temperature crystallization comes unstuck and dewaxes: the Hemp Seed crude oil 2 that the Hemp Seed crude oil 1 obtaining in step (6) and/or step (7) obtain adds 0.05% flocculating aids Hemp Seed cake powder to stir, continue to stir 15min, stir speed (S.S.) is 80 turn/min; Then be cooled to 0 ℃, stir speed (S.S.) is 35 turn/min, and temperature fall time is 2h, maintains 12h after temperature-stable again, then adds diatomite and adopts pressure type leaf filter to filter;
(9) moving-bed type adsorption deacidification: add the dewaxing Hemp Seed oil that comes unstuck that deacidification adsorbent obtains step (8) to carry out depickling processing in moving-burden bed reactor, obtain depickling Hemp Seed oil, wherein deacidification adsorbent forms by alkaline wilkinite, silicon-dioxide and three kinds of mixed raw materials of diatomite are standby, and the shared mass percent of each raw material is: alkaline wilkinite 45%, silicon-dioxide 50% and diatomite 5%; Alkalescence wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 25% of wilkinite total mass.
(10) filter: the depickling Hemp Seed oil that step (9) is obtained filters, and airtight preservation.
Embodiment 5
The preparation method who produces Hemp Seed oil that the present embodiment provides, as shown in Figure 1, the method comprises:
(1) cleaning: select fresh fire fiber crops seed, weeds, plaster, stone, metal impurities are removed in cleaning separation;
(2) high frequency vacuum drying: adopt the fiber crops of the fire after cleaning seed moisture in high frequency vacuum drying equipment regulating step (1), high frequency vacuum drying parameter is: frequency is 13.56MHz, voltage strength is 1000V/cm, vacuum tightness 3000Pa, be 55min time of drying, and in dry rear fiery numb seed, moisture content is 9.6%;
(3) shelling in advance: adopt the numb seed of dried fire in laser appropriateness cutting process step (2), laser processing parameter is: power 50W, laser cutting speed 5mm/s, the laser lancing width that is cut to fiery numb seed is 3.0mm;
(4) shelling: the fire fiber crops seed after the pre-shelling of step (3) is pushed to heat treatment, obtain Hemp Seed and shell, extrusion equipment is toothed roller type extruding peeler, and fiery numb seed husking yield is 98%;
(5) malleation is modified: the moisture of the Hemp Seed that regulating step under positive pressure (4) obtains, the modified process of malleation is: Hemp Seed is inputted to whipping device, evenly pass into water, continue to stir 30min, stir speed (S.S.) is 60 turn/min, and then proceeds in pressure vessel, and it is 3MPa that pressure is set, process 15min, the Hemp Seed water content after modified is 13%;
(6) low temperature pressing: adopt mechanical expression machine to carry out low temperature pressing to the Hemp Seed in step (5), obtain Hemp Seed crude oil 1 and squeezing Hemp Seed cake, during low temperature pressing Hemp Seed, temperature is 70 ℃;
(7) high-voltage pulse subcritical abstraction: adopt Hemp Seed cake in high-voltage pulse subcritical extraction method treatment step (6), obtain Hemp Seed crude oil 2 and the Hemp Seed dregs of rice, the detailed process of high-voltage pulse subcritical abstraction is: pulsed voltage 35kv, burst lengths 10 μ s, extraction solvent is butane, subcritical butane extracting pressure is 1.5MPa, extraction time 0.8h, and extraction temperature is 50 ℃;
(8) low temperature crystallization comes unstuck and dewaxes: the Hemp Seed crude oil 2 that the Hemp Seed crude oil 1 obtaining in step (6) and/or step (7) obtain adds 0.3% flocculating aids Hemp Seed cake powder to stir, continue to stir 30min, stir speed (S.S.) is 20 turn/min; Then be cooled to 16 ℃, stir speed (S.S.) is 5 turn/min, and temperature fall time is 6h, maintains 4h after temperature-stable again, then adds diatomite and adopts pressure type leaf filter to filter;
(9) moving-bed type adsorption deacidification: add the dewaxing Hemp Seed oil that comes unstuck that deacidification adsorbent obtains step (8) to carry out depickling processing in moving-burden bed reactor, obtain depickling Hemp Seed oil, wherein deacidification adsorbent forms by alkaline wilkinite, silicon-dioxide and three kinds of mixed raw materials of diatomite are standby, and the shared mass percent of each raw material is: alkaline wilkinite 55%, silicon-dioxide 25% and diatomite 20%; Alkalescence wilkinite is by grinding wilkinite and sodium hydroxide to make at normal temperatures, and the consumption of sodium hydroxide accounts for 18% of wilkinite total mass.
(10) filter: the depickling Hemp Seed oil that step (9) is obtained filters, and airtight preservation.
Embodiment 6
(1) the depickling Hemp Seed oil preparing in the embodiment of the present invention 1 is detected, the main physical and chemical index of the Hemp Seed oil of acquisition is as shown in table 1.
The main physical and chemical index of table 1 Hemp Seed oil
(2) the depickling Hemp Seed oil preparing in the embodiment of the present invention 1 is detected, the lipid acid of the Hemp Seed oil of acquisition forms as shown in table 2.
The lipid acid of table 2 Hemp Seed oil forms
| Interventions Requested | Detected result (%) | Detect foundation |
| Myristic acid | Do not detect | GB/T?17377-2008 |
| Palmitinic 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 |
| Linolic acid | 56.4 | GB/T?17377-2008 |
| Linolenic acid | 20.5 | GB/T?17377-2008 |
| Eicosanoic acid | 0.6 | GB/T?17377-2008 |
| Peanut monoenoic acid | 0.3 | GB/T?17377-2008 |
| Peanut diolefinic 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 Hemp Seed oil preparing in the embodiment of the present invention 1 is carried out to sanitary index test, the sanitary index of the Hemp Seed oil of acquisition as shown in Table 3 below.
The sanitary index of table 3 Hemp Seed oil
(4) the depickling Hemp Seed oil preparing in the embodiment of the present invention 1 is carried out to micro-nutrient composition test, the micro-nutrient composition of the Hemp Seed oil of acquisition as shown in Table 4 below.
Table 4 Hemp Seed oil micro-nutrient composition
| Unsaponifiables (%) | 2.8 | GB/T?5535.1-2008 |
| Plant sterol (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 Hemp Seed oil preparing in the embodiment of the present invention 1 is carried out to the test of Hemp Seed oil oxidative stability, test condition is measured with reference to EN14112:2003; Test condition: 110 ℃; Air flow quantity: 10L/h, as shown in fig. 1, the oxidation induction period of depickling Hemp Seed oil is 2.01h/110 ℃ to test result.
From table 1-4 and Fig. 1, can find out, the Hemp Seed oil that adopts the preparation method in the present invention to prepare, its physical and chemical index meets relevant national standard, sanitary index meets national standard, Hemp Seed oil is mainly comprised of palmitinic acid, palm monoenoic acid, heptadecane acid, stearic acid, oleic acid, linolic acid, linolenic acid, eicosanoic acid, peanut monoenoic acid, peanut diolefinic acid, behenic acid etc., be rich in the micro-nutrient compositions such as plant sterol, total phenol and vitamin-E, antioxidant property is good, and the oxidation induction period of the depickling Hemp Seed oil in the present invention is 2.01h/110 ℃.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, be included in protection scope of the present invention.
Claims (10)
1. a preparation method for Hemp Seed oil, is characterized in that comprising the following steps:
(1) cleaning, dry: choose fresh fire fiber crops seed, adopt high frequency vacuum drying after cleaning;
(2) shelling in advance: adopt laser to cut the fire fiber crops seed after step (1) high frequency vacuum drying, obtain the fire fiber crops seed of pre-heat treatment;
(3) shelling: the fire fiber crops seed of the pre-heat treatment of step (2) is pushed to heat treatment, obtain Hemp Seed and housing;
(4) malleation is modified: the moisture that adopts the Hemp Seed obtaining in the modified mode regulating step of malleation (3);
(5) low temperature pressing: adopt mechanical expression equipment to carry out low temperature pressing to the Hemp Seed obtaining in step (4), obtain Hemp Seed crude oil 1 and squeezing Hemp Seed cake;
(6) high-voltage pulse subcritical abstraction: adopt the Hemp Seed cake obtaining in high-voltage pulse subcritical abstraction mode treatment step (5), obtain Hemp Seed crude oil 2 and the Hemp Seed dregs of rice;
(7) low temperature crystallization comes unstuck and dewaxes: in the Hemp Seed crude oil 2 of step (5) acquisition Hemp Seed crude oil 1 and step (6) acquisition, add flocculating aids to stir, then uniform decrease in temperature, carry out again cold analysis processing, obtain after filtration the dewaxing Hemp Seed oil that comes unstuck;
(8) moving-bed type adsorption deacidification, filtration: in moving-burden bed reactor, add the dewaxing Hemp Seed oil that comes unstuck that deacidification adsorbent obtains step (7) to carry out depickling processing, obtain depickling Hemp Seed oil, after filtering, sealing is preserved, and obtains Hemp Seed oil.
2. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: the vacuum drying parameters of step (1) medium-high frequency is: frequency 6MHz～28MHz, voltage strength 1000V/cm～3000V/cm, vacuum tightness 300Pa～3000Pa, adopting high frequency vacuum drying to the quality percentage composition of water in fiery numb seed is 7～11%.
3. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: the parameters while adopting laser to cut in step (2) is: power 6W～50W, laser cutting speed 5mm/s～35mm/s, the width of slit that is cut to fiery numb seed is 0.5mm～3.5mm.
4. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: while the fire fiber crops seed of the pre-heat treatment of step (2) being pushed to heat treatment in step (3), the extrusion equipment adopting is toothed roller type extruding peeler, and the husking yield of the numb seed of described fire is 85%～98%.
5. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: the modified mode of malleation described in step (4) is: Hemp Seed is inputted to whipping device, evenly pass into water, continue to stir 10min～30min, stir speed (S.S.) is 60 turn/min of turn/min～180; And then proceed in pressure vessel, it is 0.2MPa～3MPa that pressure is set, and processes 15min～60min, the Hemp Seed water content after modified is 7%～13%.
6. the preparation method of Hemp Seed oil according to claim 1, is characterized in that: while adopting mechanical expression equipment to carry out low temperature pressing to the Hemp Seed obtaining in step (4) in step (5), temperature is 25 ℃～70 ℃.
7. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: while adopting the Hemp Seed cake obtaining in high-voltage pulse subcritical abstraction mode treatment step (5) in step (6), parameters is: pulsed voltage 5kv～35kv, burst lengths 10 μ s～100 μ s, the solvent adopting during subcritical abstraction is butane, subcritical abstraction pressure is 0.3MPa～1.5MPa, extraction time 0.8h～4.0h, and extraction temperature is 8 ℃～50 ℃.
8. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: in step (7), carry out that low temperature crystallization comes unstuck and the detailed process of dewaxing treatment is: in the Hemp Seed crude oil 2 that the Hemp Seed crude oil 1 obtaining in step (5) and step (6) obtain, add flocculating aids to stir 15min～30min, stir speed (S.S.) is 20 turn/min of turn/min～80, then uniform decrease in temperature to 0 ℃～16 ℃, during uniform decrease in temperature, stir speed (S.S.) is 5 turn/min of turn/min～35, temperature fall time is 2h～6h, after temperature-stable, maintain again 4h～12h and carry out cold analysis processing, finally add diatomite and adopt pressure type leaf filter to filter and obtain the dewaxing Hemp Seed oil that comes unstuck, wherein flocculating aids is Hemp Seed cake powder, the consumption of described Hemp Seed powder accounts for 0.05%～0.3% of Hemp Seed crude oil 1 and Hemp Seed crude oil 2 total masses.
9. the preparation method of Hemp Seed oil according to claim 1, it is characterized in that: while adding deacidification adsorbent to carry out depickling processing to the dewaxing Hemp Seed oil that comes unstuck of step (7) acquisition in step (8) in moving-burden bed reactor, the dewaxing Hemp Seed oil that the comes unstuck turnover that circulates from bottom to top, deacidification adsorbent from top to down, wherein depickling temperature is 20 ℃～70 ℃, and adsorption time is 0.5h～3.5h.
10. the preparation method of Hemp Seed oil according to claim 9, it is characterized in that: described deacidification adsorbent is made by alkaline wilkinite, silicon-dioxide and three kinds of raw materials of diatomite, and the quality percentage composition of each raw material is: alkaline wilkinite 45%～85%, silica 1 0%～50% and diatomite 5%～20%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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