CN102120946B - Method for producing germ oil, oligosaccharides and protein concentrate by using soybean germs - Google Patents
Method for producing germ oil, oligosaccharides and protein concentrate by using soybean germs Download PDFInfo
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Abstract
The invention discloses a method for producing products such as soybean germ oil, soybean germ protein concentrate, soybean oligosaccharides, soybean saponins and soybean isoflavones by using soybean germs, and relates to the field of deep grain processing. The method comprises the following steps of: performing online stabilization treatment on the soybean germs; performing normal temperature extraction and low temperature desolventizing by taking subcritical fluid as a lytic enzyme to produce the soybean germ oil; extracting polar ingredients such as the soybean oligosaccharides and the like from the defatted soybean germs by taking subcritical liquid ammonia and the like as lytic enzymes, and separating the oligosaccharides, the isoflavones and the saponins from the extract and purifying; and separating the soybean germ protein concentrate from the liquid ammonia extract, namely a low temperature soybean gear meal. When the method is used, five products such as the germ oil, the oligosaccharides, the soybean protein concentrate and the like can be obtained simultaneously, so that the full utilization of the soybean germs is realized, and production cost is low; reextraction can be completed in different extraction stages of the same leaching equipment, so that investment is saved; and zero emission is realized, so that the method is environmentally-friendly.
Description
Technical field
The present invention relates to grain intensive processing field, refer in particular to a kind of take soybean germ as raw material, adopt the method for subcritical fluids stepwise solvent extraction, coproduction soybean embryo fat/oil, soybean oligosaccharide, soybean germ protein concentrate, Soyasaponin and soybean isoflavones.
Background technology
Soybean germ is the basis that the soybean seed grows, and has special composition and nutritive value, though its quality only accounts for 2.0 ~ 2.5% of soybean gross weight, contains abundant isoflavones, saponin, oligose, V
EWith several physiological active substances such as plant sterols.According to document, the content of various nutritive ingredients sees Table 1 in the soybean germ.
The trophic component of table 1 soybean germ
| Composition | Moisture | Crude fat | Crude protein | Robust fibre | Ash content | Oligose | General glycoside | Isoflavones |
| Content (%) | 9.3 | 10.2 | 38.6 | 7.7 | 4.6 | 14.3 | 4.25 | 3.2 |
Soybean germ contains seven large characteristic chemical constituents:
(1) oil composition of plant sterol soybean germ sees Table 2, and wherein unsaponifiable matter content 11.5%, take β-sitosterol as main, is up to 7.25%.β-sitosterol is the widest a kind of sterol that distributes in the Vegetable oil lipoprotein, generally accounts for more than 60% of total sterol, and other is Stigmasterol, campesterol, ergosterol etc.β-sitosterol content is nearly 20 times of sterol content in the cotyledon in the soybean germ, and is suitable with the deodorization distillate of soybean.
Soybean embryo fat/oil contains abundant natural phytosterin, can suppress the absorption of cholesterol in human body, thereby has the absorption that reduces total cholesterol level and LDL-C in the blood.
The oil composition of table 2 soybean germ
| Composition | C16:0 | C18:0 | C18:1 | C18:2 | C18:3 | β-sitosterol | V E | Phosphatide |
| Content (%) | 13.2 | 3.0 | 6.7 | 52.7 | 23.7 | 7.25 | 0.46 | 4.35 |
(2) the linolenic acid soybean embryo fat/oil contains abundant unsaturated fatty acids, wherein contains the linolenic acid more than 25%, and shelter has first of the germ oil.Linolenic acid is a kind of indispensable fatty acid, also is a kind of lipid acid of very easily oxidation, and it coexists as in the soybean germ with the isoflavones and the saponin that have than the strong anti-oxidation effect.
(3) the vitamin-E soybean embryo fat/oil contains the tocopherol about 0.5%, can match in excellence or beauty with wheatgerm oil (0.2～0.55%), apparently higher than cotyledon oil; But in soybean germ and the cotyledon oil all take Gamma-Tocopherol as main, account for respectively 76.1% and 65.3%, and in the wheatgerm oil take alpha-tocopherol as main component (more than 60%), although the physiological action of Gamma-Tocopherol than alpha-tocopherol a little less than, its oxidation-resistance is the strongest.
(4) containing isoflavones about 3% in the isoflavones soybean germ, is 30～60 times of cotyledon, accounts for 30～50% of soybean total isoflavone.
(5) containing saponin about 6% in the saponin soybean germ, is to extract the good raw material of Soyasaponin.Isoflavones and saponin all are a kind of protective substance, and the protection soybean germ is not encroached on by insect and harmful microbe in the rudiment process, equally protects the lipoid composition in the plumule not oxidized yet.
(6) contain oligose about 15% in the oligose soybean germ, its main component is stachyose, raffinose and sucrose.Soybean oligosaccharide can activate the interior bifidus bacillus of enteron aisle and promote its growth and breeding, and prevention, treatment constipation and diarrhoea can not cause that the tooth dental caries become, and also can be used as diabetics, adiposis patient and hypoglycemia patient's protective foods simultaneously.
(7) the soybean protein soybean germ contains the albumen more than 38%, and its amino acid forms similar to amino acid composition in the soybean cotyledon.Soybean germ albumen is as the integral part of soybean protein, and the same with soybean protein have very high nutritive value and a physiological function, such as the strengthen muscle effect, strengthens the effects such as immunologic function.
Because soybean germ is rich in β-sitosterol, isoflavones, saponin and V
EEtc. the various active composition, become in recent years research and development focus both domestic and external.
Chinese patent 00804213.6 discloses the method that the soybean germ raw material is rich in a kind of soybean embryo fat/oil and production, and the technique of producing the soybean germ raw material comprises kibbles mill, screening, pneumatic separation etc.Then adopt organic solvent (such as normal hexane) to leach soybean embryo fat/oil.The employing organic solvent leaches, because solvent boiling point is generally greater than 60 ℃, the solvent that removes in mixing oil and the wet dregs of rice must make its temperature rise to more than 100 ℃, can cause in the oil protein denaturation in thermo-sensitivity composition deterioration by oxidation, the dregs of rice.Even adopt low temperature desolventizing equipment, but complicated operation, consume highly, cause low temperature desolventizing dregs of beans production cost too high, greatly affect economic benefit.In addition, this patent has only been utilized the lipid in the soybean germ, does not relate to the problem of complex utilization of the compositions such as albumen in the dregs of rice, isoflavones and saponin.
Chinese patent 200810137429 discloses a kind of supercritical CO
2The production technique of extracting soybean germ oil adopts this method gained soybean germ oil quality high, and extraction time is short, energy consumption is low.But because its treatment capacity is little, equipment investment is large, so that the soybean embryo fat/oil product cost is higher, thereby this technology commercialization application is restricted.Simultaneously, this patent also is only to have utilized the lipid in the soybean germ, does not relate to equally the comprehensive utilization technique of the compositions such as albumen in the dregs of rice, isoflavones and saponin.
Chinese patent 200510011328 discloses by the method for extracting soybean isoflavones, soybean saponin, soybean oligosaccharide and soybean protein concentrate in skimmed soy beans such as soybean defatted soybean meal or the embryo.The quality condition of the undeclared skimmed soy beans plumule of the inventor dregs of rice, if the dregs of rice that high temperature drying obtains will cause its finished product--poor quality and the yield of soybean protein concentrate are low, and the method does not relate to the problem of utilizing of soybean embryo fat/oil yet.In addition, the method during alcohol solvent, needs the pyroprocessing more than 100 ℃ in removing the dregs of rice, cause protein denaturation.Though this patent relies on the technique means such as enzymolysis and spraying drying, make the NSI of product 〉=80%, the production cost of soybean germ albumen can be very high.
In addition, fat hydrolase in the soybean germ and fats oxidn enzyme activity are very high, after soybean germ separates from soybean, above-mentioned enzyme activity will further be strengthened, oxidation products of fatty acids is especially one of main source of strong beany flavor in the plumule of soybean, and how the passivation enzyme activity is the key of producing high-quality soybean embryo fat/oil.
In order to overcome the only unilateral part component (such as grease, soybean oligosaccharide, soybean isoflavones, Soyasaponin) of utilizing in the soybean germ of existing method; Supercritical CO
2Extraction equipment has high input, yields poorly, production cost is high; No. six solvent extractions (normal hexane is main) are the deficiency such as deterioration in quality in desolvation process, the present invention is take subcritical fluids as lyase, substep extracts germ oil, oligose, isoflavones, saponin and the five kinds of products of functional germ protein powder in the soybean germ successively, realized the complete utilization of soybean germ, significantly reduced production cost, and Effective Raise quality product, increased economic benefit.
Summary of the invention
The invention provides a kind of take soybean germ as raw material, the method for coproduction soybean embryo fat/oil, soybean oligosaccharide, soybean isoflavones, Soyasaponin and five kinds of products of soybean germ protein concentrate.
The technical solution adopted for the present invention to solve the technical problems is: at first soybean germ is carried out stabilization treatment, passivation fat hydrolase and lipoxidase wherein; Then adopt the extraction of subcritical fluids normal temperature, low temperature desolventizing, produce soybean embryo fat/oil, and prepare pure soybean embryo fat/oil; Extract remainder is take subcritical liquefied ammonia etc. as lyase, low-temperature extraction soybean oligosaccharide isopolarity composition wherein, and separation and purification soybean oligosaccharide, soybean isoflavones and Soyasaponin; At last, from the extract remainder (the low temperature soybean germ dregs of rice) of liquefied ammonia, separate the soybean germ protein concentrate.
Method of the present invention is specifically carried out according to following step:
(1) stabilization of soybean germ:The fresh soyabean plumule enters stabilizing device, carries out blunt enzyme and processes;
(2) soybean germ roll embryo:To through the soybean germ of step (1) stabilization treatment, roll into the following thin slice of 0.5mm, preferred 0.3～0.4mm;
(3) subcritical fluid extraction of soybean embryo fat/oil:Take subcritical fluids as lyase, the soybean germ of processing roll embryo through step (2) carries out countercurrent leaching 1～5 time, extraction time 30～180 minutes, solid-liquid ratio 1:1～6,10～40 ℃ of extraction temperature, extracting pressure 0.2～0.8MPa.Mixing oil and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state.The solvent gas that evaporates from mixing oil and the wet dregs of rice recycles behind compressed machine compression, the condensation liquefaction again.Gained extract soybean germ crude oil adopts conventional winterization, alkali refining and decoloration process, obtains refining soybean germ oil production.
(4) extraction of soybean oligosaccharide, isoflavones and saponin:The extract remainder skimmed soy beans plumule that step (3) is obtained, cross 30～60 mesh sieves after pulverizing, adopt subcritical fluids (such as liquefied ammonia) for lyase or in subcritical fluids, add entrainment agent, carry out countercurrent leaching 1～5 time, solid-liquid ratio 1:1 ~ 6,30～180 minutes time, 10～40 ℃ of temperature, extracting pressure 0.2～1.6MPa.Extraction liquid and the wet dregs of rice that extraction obtains enter vapo(u)rization system, and precipitation under decompression state is extracted thing soybean oligosaccharide mixture and the extract remainder low temperature soybean germ dregs of rice.The solvent gas that reduction vaporization goes out recycles behind compressed machine compression, the condensation liquefaction again.
(5) soybean oligosaccharide is refining.To the extract that step (4) obtains, with 80～100% ethanol (v/v) extraction, preferred 95% medical alcohol (v/v), extraction is extracted thing and extract remainder.Wherein extract remainder is soybean germ oligose crude product.This crude product can be further with the water dissolution of 2～8 times of quality, and centrifugal, supernatant liquor adopts massfraction 0.1～5.0% activated carbon decolorizing, filters, and filtrate decompression is concentrated, obtains the soybean oligosaccharide slurry, and the oligomeric Icing Sugar of the soybean germ that obtains making with extra care is pulverized in vacuum-drying.
(6) preparation of soybean isoflavones.To the extract that step (5) obtains, after reduction vaporization is removed ethanol below 50 ℃, then add the water dissolution of 1～10 times of quality in the residue, centrifugal, obtain supernatant liquor and throw out, 50 ℃ of lower vacuum-dryings of described throw out 1～4 hour obtain highly purified soybean isoflavones.
(7) preparation of Soyasaponin.The supernatant liquor that step (6) is obtained, after adopting macroporous resin adsorption 0.5～2h, then use 50～90% ethanol (v/v) to carry out wash-out, 50 ℃ of lower reduction vaporizations of elutriant are removed ethanol, and be concentrated into 1/5～1/10 of original volume, 50 ℃ of lower vacuum-drying 1～4h of concentrated solution obtain highly purified Soyasaponin.
(8) preparation of low temperature soybean germ protein concentrate.To the extract remainder low temperature soybean germ dregs of rice that step (4) obtains, behind micronizing or Ordinary pulverization, cross 30～120 mesh sieves, obtain soybean germ albumen crude product; Add 2～6 times of quality, 60～100% ethanol (v/v) in the soybean germ albumen crude product, washing is filtered, the 50 ℃ of lower reduction vaporizations of the wet dregs of rice after the washing are removed ethanol after, vacuum-drying 1～4h obtains refining soybean germ protein concentrate.
Wherein said step (3)
The extraction of soybean oligosaccharide, isoflavones and saponin, can also ethanol be solvent, carry out countercurrent leaching 1～5 time, alcohol concn is 60～80%(v/v), solid-liquid ratio 1:1～5, extraction time 30～180 minutes, 35～60 ℃ of extraction temperature; Then solid-liquid separation, extraction liquid and the wet dregs of rice enter respectively vapo(u)rization system, precipitation under decompression state; Extract remainder skimmed soy beans plumule obtains pulverous soybean germ protein concentrate crude product through desolvation with after pulverizing, and behind the liquid phase Recycled ethanol solvent, is extracted the mixture that thing is soybean oligosaccharide, soybean isoflavones and Soyasaponin; The ethanol that evaporates in the solid-liquid two-phase can be recycled.
Wherein said soybean germ stabilization comprises online and processed offline dual mode, preferred online stabilization wherein, online treatment are namely carried out immediately stabilization treatment, processed offline to the soybean germ of just having separated and are about to soybean germ and collect to concentrate and carry out stabilization treatment; Described stabilization treatment method comprises the means such as microwave, steam treatment, hot blast or extruding puffing, wherein preferred microwave and steam treatment; When adopting microwave, microwave power 0.05～5.0kW/kg soybean germ, the microwave action time is 1～10min; When adopting the high pressure steam stabilization, vapor pressure 3～7kg, treatment time 5～30min.
Wherein said subcritical fluids is butane, propane, dme, liquefied petroleum gas (LPG) (LPG) or liquefied ammonia etc., wherein preferred butane, liquefied ammonia; Described entrainment agent comprises ethanol, methyl alcohol etc., preferred alcohol wherein, and the massfraction that adds entrainment agent is 0.1～5%.
Wherein the described operating process of step (3,4) all is to finish under the processing condition of complete closed, select butane etc. from soybean germ oil and grease extracting, select oligose in the extraction skimmed soy beans plumules such as ethanol or liquefied ammonia etc., twice extraction can be finished in the different extraction sections in same leaching plant, also can finish respectively in the leaching plant of two series connection.
Winterization, alkali refining and the decoloration process of routine in the wherein said step (3), the sodium hydroxide that at first adds massfraction 0.05～0.25% in the crude oil, stirring velocity is 40～70 to turn/min, after finishing neutralization reaction, speed drops to 10～30 and turns/min, continue to stir 10～30min, oil is warming up to 90～95 ℃, and adds strong mixing or use airflow stirring instead according to neat soap flocculation situation.When the obvious sedimentation of neat soap, stop to stir, 4～6h is left standstill in insulation, and with the soft water washing of oil mass 10～15%, temperature is not less than 85 ℃ subsequently, and stirring velocity should be moderate therebetween, makes oil mixing with water even, washs 2～4 times.Then carry out adsorption bleaching, sorbent material is take atlapulgite as main, and adds a small amount of gac (atlapulgite quality 5～10%), and the sorbent material consumption is 1～7% of quality of crude oil, 80～110 ℃ of adsorption temps, and stirring velocity≤80 turn/min, decolouring 15～30min.The last grease that slowly stirs is cooled to 4～6 ℃, and insulation 12～36h filters, and obtains the soybean germ refining oil.
Advantage of the present invention:
(1) the present invention adopts the subcritical fluid extraction technology, 5 products such as high-quality soybean embryo fat/oil, soybean oligosaccharide, soybean isoflavones, Soyasaponin and soybean germ protein concentrate have been obtained simultaneously, realize the complete utilization of soybean germ, and realized zero release;
(2) the present invention adopts subcritical fluid extraction soybean embryo fat/oil and soybean oligosaccharide, and normal temperature extraction, low temperature desolventizing belong to non-hot-work, and finish whole production process under the condition of starvation, thereby kept to greatest extent linolenic acid in the soybean embryo fat/oil, V
EWith the not oxidation of thermo-sensitivity composition, the soybean germ albumen unchangeability such as β-sitosterol, good product quality;
(3) method of the present invention is produced soybean embryo fat/oil, soybean germ protein concentrate, finishes continuously under the processing condition of complete closed, has simplified goods batch, and the products production cost is low;
(4) the present invention adopts lipase and the lipoxidase in the online stabilization technology passivation soybean germ, has effectively prevented becoming sour of soybean germ, and soybean germ crude oil acid value is low, has significantly improved the yield of soybean embryo fat/oil;
(5) reextraction of the present invention (step 3,4) can be finished in the different extraction sections in same set of leaching plant, has significantly saved facility investment;
(6) to adopt butane, liquefied ammonia and edible ethanol be spe medium in the present invention, avoided the pollution of organic solvent to product, and product meets food security standard;
(7) the extraction lyase that uses of each operation of the present invention is all recyclable and recycle, and has reduced on the one hand production cost, simultaneously also environmental protection.
Description of drawings
Fig. 1 is the method process flow diagram of soybean germ coproduction germ oil, oligose and protein concentrate.
Embodiment
Below in conjunction with embodiment the present invention is further elaborated.
Embodiment 1
The fresh soyabean plumule that oil pressing factory's production line has just been separated is carried by transfer roller, enters the microwave device, the enzyme that goes out, and processing condition are: microwave power 0.15kW/kg plumule, microwave action time 5min.The soybean germ that to process through microwave utilizes flaker to roll into the thin slice of 0.4mm.
Get above-mentioned soybean germ 1000kg, take liquefied butane as lyase, carry out countercurrent leaching 3 times, extraction time 45 minutes, feed liquid mass ratio 1:3,25 ℃ of extraction temperature.Mixing oil and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state.Obtain soybean germ crude oil 95kg, skimmed soy beans plumule 902kg.The butane gas that evaporates from mixing oil and the wet dregs of rice recycles behind compressed machine compression, the condensation liquefaction again.
Get soybean germ crude oil 50kg, at first toward the sodium hydroxide that wherein adds quality of crude oil mark 0.1%, stirring velocity is 60 to turn/min, after finishing neutralization reaction, speed drops to 10 and turns/min, continues to stir 20min and makes the neat soap flocculation, and oil is warming up to 90 ℃, when the obvious sedimentation of neat soap, stop to stir, 6h is left standstill in insulation, and the soft water with quality of crude oil 10% washs subsequently, 85 ℃ of profit temperature are washed 2 times.Then the sorbent material that adds quality of crude oil 2%, sorbent material be take atlapulgite as main (gac that wherein contains quality 5%), 90 ℃ of oil temperatures, and stirring velocity 50 turns/min, bleaching time 25min.The last grease that slowly stirs is cooled to 5 ℃, and insulation 24h filters, and obtains soybean germ refining oil 41kg.
Extracting degreasing soybean germ 100kg, pulverize, cross 30 sieves, adopt liquefied ammonia to carry out countercurrent leaching 3 times, feed liquid mass ratio 1:4, extraction time 45 minutes, 25 ℃ of extraction temperature, the extraction extraction liquid and the wet dregs of rice that obtain enter vapo(u)rization system, and precipitation under decompression state obtains mixture 8.9kg and the low temperature soybean germ dregs of rice 88kg of soybean oligosaccharide, soybean isoflavones, Soyasaponin.The solvent gas that reduction vaporization goes out recycles behind compressed machine compression, the condensation liquefaction again.
Get the mixture 1kg of soybean oligosaccharide, soybean isoflavones, Soyasaponin, with medical alcohol (V/V) extraction of concentration 95%.Extract remainder is soybean germ oligose crude product 512g, crude product is further after the water dissolution with 4 times of quality, centrifugal, supernatant liquor adds the gac of massfraction 0.2%, filter, filtrate decompression is concentrated, obtains the soybean oligosaccharide slurry, vacuum-drying obtains the oligomeric Icing Sugar 356g of soybean germ that makes with extra care after the pulverizing.After 50 ℃ of lower reduction vaporizations of its extract are removed ethanol, add the water dissolution of 5 times of quality, centrifugal being precipitated and supernatant liquor, 50 ℃ of lower vacuum-drying 2.5h of throw out obtain soybean isoflavones 155g.Supernatant liquor is through AB-8 macroporous resin adsorption 2h, and the ethanol elution with 75%, elutriant are evaporated to 1/10,55 ℃ of vacuum-drying 1.5h of original volume, obtain Soyasaponin 198g.
Get low temperature soybean germ dregs of rice 10kg, after the pulverizing, cross 80 mesh sieves, obtain soybean germ protein concentrate crude product 9.8kg, again with the washing of 90% ethanolic soln of 4 times of weight, after the filtration, the 50 ℃ of lower reduction vaporizations of the plumule dregs of rice after the washing are removed ethanol after, and vacuum-drying 1.5h, the soybean germ protein concentrate 8.2kg that obtains making with extra care.
Embodiment 2
The fresh soyabean plumule that low temperature soybean protein manufacturing enterprise has just separated is carried by transfer roller, enters the steam stable gasifying device, and enzyme goes out.Processing condition are: the plumule 500kg that once feeds intake, vapor pressure 5kg, treatment time 8min.Then, will through the soybean germ of steam stable processing, utilize flaker to roll into the thin slice of 0.5mm.
Get above-mentioned soybean germ 1000kg, take liquefied butane as lyase, carry out countercurrent leaching 2 times, extraction time 30 minutes, solid-liquid ratio 1:3,25 ℃ of extraction temperature.Mixing oil and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state.Obtain soybean germ crude oil 86kg, skimmed soy beans plumule 901kg.The solvent gas that evaporates from mixing oil and the wet dregs of rice recycles behind compressed machine compression, the condensation liquefaction again.
Get soybean germ crude oil 50kg, at first toward the sodium hydroxide that wherein adds quality of crude oil mark 0.1%, stirring velocity is 60 to turn/min, after finishing neutralization reaction, speed drops to 10 and turns/min, continues to stir 20min and makes the neat soap flocculation, and oil is warming up to 90 ℃, when the obvious sedimentation of neat soap, stop to stir, 6h is left standstill in insulation, and the soft water with quality of crude oil 10% washs subsequently, 85 ℃ of profit temperature are washed 2 times.Then the sorbent material that adds quality of crude oil 2%, sorbent material be take atlapulgite as main (wherein containing 5% gac), 90 ℃ of oil temperatures, and stirring velocity 50 turns/min, bleaching time 25min.The last grease that slowly stirs is cooled to 5 ℃, and insulation 24h filters, and obtains soybean germ refining oil 42kg.
Extracting degreasing soybean germ 100kg pulverizes, and crosses 60 mesh sieves, adopts 4 countercurrent leachings of ethanol, and alcohol concn is 80%(v/v), solid-liquid ratio 1:3, extraction time 120 minutes, 50 ℃ of extraction temperature; Then solid-liquid separation, extraction liquid and the wet dregs of rice enter respectively vapo(u)rization system, precipitation under decompression state; Extract remainder obtains pulverous soybean germ protein concentrate crude product 89kg through desolvation with after pulverizing.Behind the liquid phase Recycled ethanol solvent, obtain the mixture 9.5kg of soybean oligosaccharide, soybean isoflavones and Soyasaponin; The ethanol that evaporates in the solid-liquid two-phase can be recycled.
Get the mixture 1kg of soybean oligosaccharide, soybean isoflavones, Soyasaponin, with concentration 95% medical alcohol (v/v) extraction.Its extract remainder is soybean germ oligose crude product 535g, crude product is further after the water dissolution with 3 times of quality, centrifugal, supernatant liquor interpolation massfraction is 0.2% gac, filter, filtrate decompression is concentrated, obtains the soybean oligosaccharide slurry, vacuum-drying obtains the oligomeric Icing Sugar 386g of soybean germ that makes with extra care after the pulverizing.Its extract adds the water dissolution of 6 times of quality after ethanol is removed in evaporation, centrifugal being precipitated and supernatant liquor, and 50 ℃ of lower vacuum-drying 3h of throw out obtain soybean isoflavones 172g.Through AB-8 macroporous resin adsorption 1.5h, being washed till pol with distilled water is zero degree, uses 70% ethanol elution again with supernatant liquor, and elutriant is evaporated to 1/10,55 ℃ of vacuum-drying 3.5h of original volume, obtains Soyasaponin 226g.
Get soybean germ dregs of rice 10kg, after the pulverizing, cross 80 mesh sieves, obtain soybean germ protein concentrate crude product 9.8kg.
Embodiment 3
The fresh soyabean plumule that oil pressing factory's production line has just been separated is carried by transfer roller, enters the microwave device, the enzyme that goes out, and processing condition are: microwave power 0.15kW/kg plumule, microwave action time 5min.The soybean germ that to process through microwave utilizes flaker to roll into the thin slice of 0.4mm.
Get above-mentioned soybean germ 1000kg, take liquefaction LPG as lyase, carry out countercurrent leaching 2 times, extraction time 60 minutes, solid-liquid ratio 1:4,25 ℃ of extraction temperature.Mixing oil and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state.The solvent gas that evaporates from mixing oil and the wet dregs of rice recycles behind compressed machine compression, the condensation liquefaction again.Obtain soybean germ crude oil 89kg, skimmed soy beans plumule 900kg.Adopt conventional winterization, alkali refining and decoloration process, obtain refining soybean germ oil production 62kg.
Get soybean germ crude oil 50kg, at first toward the sodium hydroxide that wherein adds quality of crude oil mark 0.2%, stirring velocity is 50 to turn/min, after finishing neutralization reaction, speed drops to 15 and turns/min, continues to stir 20min and makes the neat soap flocculation, and oil is warming up to 95 ℃, when the obvious sedimentation of neat soap, stop to stir, 4h is left standstill in insulation, and the soft water with quality of crude oil 15% washs subsequently, 90 ℃ of profit temperature are washed 3 times.Then the sorbent material that adds quality of crude oil 3%, sorbent material be take atlapulgite as main (wherein containing 10% gac), 110 ℃ of oil temperatures, and stirring velocity 50 turns/min, bleaching time 20min.The last grease that slowly stirs is cooled to 5 ℃, and insulation 20h filters, and obtains soybean germ refining oil 40kg.
Extracting degreasing soybean germ 100kg, pulverize, cross 30 sieves, adopt subcritical butane (wherein add mass ratio be 1% ethanol), carry out countercurrent leaching 3 times, solid-liquid ratio 1:4, extraction time 45 minutes, 25 ℃ of extraction temperature, extraction liquid and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state obtains mixture 7.8kg and the low temperature soybean germ dregs of rice 92kg of soybean oligosaccharide, soybean isoflavones, Soyasaponin.The solvent gas that reduction vaporization goes out recycles behind compressed machine compression, the condensation liquefaction again.
Get the mixture 1kg of soybean oligosaccharide, soybean isoflavones, Soyasaponin, with medical alcohol (v/v) extraction of concentration 95%.Its extract remainder is soybean germ oligose crude product 505g, crude product is further after the water dissolution with 4 times of quality, centrifugal, supernatant liquor interpolation massfraction is 0.5% gac, filter, filtrate decompression is concentrated, obtains the soybean oligosaccharide slurry, vacuum-drying obtains the oligomeric Icing Sugar 348g of soybean germ that makes with extra care after the pulverizing.Its extract adds the water dissolution of 3 times of quality after ethanol is removed in evaporation, centrifugal being precipitated and supernatant liquor, and 50 ℃ of lower vacuum-drying 1.5h of throw out obtain soybean isoflavones 137g.Through AB-8 macroporous resin adsorption 2h, being washed till pol with distilled water is zero degree, uses 80% ethanol elution again with supernatant liquor, and elutriant is evaporated to 1/8,55 ℃ of vacuum-drying 1.5h of original volume, obtains Soyasaponin 175g.
Get low temperature soybean germ dregs of rice 10kg, after the micronizing, obtain soybean germ protein concentrate crude product 9.9kg; Again with the washing of 90% ethanolic soln of 4 times of weight, after the filtration, with the 50 ℃ of lower reduction vaporizations of the plumule dregs of rice after the washing, and the vacuum-drying 1.5h soybean germ protein concentrate 8.5kg that can obtain making with extra care.
Claims (5)
1. the method for soybean germ coproduction germ oil, oligose and protein concentrate is characterized in that carrying out according to following step:
(1) stabilization of soybean germ: the fresh soyabean plumule, enter stabilizing device, carry out blunt enzyme and process;
(2) soybean germ roll embryo: will through the soybean germ of step (1) stabilization treatment, roll into the following thin slice of 0.5mm;
(3) subcritical fluid extraction of soybean embryo fat/oil: the soybean germ of processing roll embryo through step (2) take subcritical fluids as solvent, carry out countercurrent leaching 1～5 time, extraction time 30～180 minutes, solid-liquid ratio 1:1～6,10～40 ℃ of extraction temperature, extracting pressure 0.2～0.8MPa; Mixing oil and the wet dregs of rice that extraction obtains enter vapo(u)rization system, precipitation under decompression state; The solvent gas that evaporates from mixing oil and the wet dregs of rice recycles behind compressed machine compression, the condensation liquefaction again; Get extract soybean germ crude oil, adopt conventional winterization, alkali refining and decoloration process, obtain refining soybean germ oil production;
(4) extraction of soybean oligosaccharide, isoflavones and saponin: the extract remainder skimmed soy beans plumule that step (3) is obtained, cross 30～60 mesh sieves after pulverizing, adopt subcritical fluids to be solvent or in subcritical fluids, to add entrainment agent, carry out countercurrent leaching 1～5 time, solid-liquid ratio 1:1 ~ 6,30～180 minutes time, 10～40 ℃ of temperature, extracting pressure 0.2～1.6MPa; Extraction liquid and the wet dregs of rice that extraction obtains enter vapo(u)rization system, and precipitation under decompression state is extracted thing soybean oligosaccharide mixture and the extract remainder low temperature soybean germ dregs of rice; The solvent gas that reduction vaporization goes out recycles behind compressed machine compression, the condensation liquefaction again;
(5) soybean oligosaccharide is refining: to the extract that step (4) obtains, be 80～100% alcohol extractions with volumetric concentration, extraction is extracted thing and extract remainder; Wherein extract remainder is soybean germ oligose crude product; This crude product is further used the water dissolution of 2～8 times of quality, and is centrifugal, and supernatant liquor adopts massfraction 0.1～5.0% activated carbon decolorizing, filters, and filtrate decompression is concentrated, obtains the soybean oligosaccharide slurry, and the oligomeric Icing Sugar of the soybean germ that obtains making with extra care is pulverized in vacuum-drying;
(6) preparation of soybean isoflavones: the extract that step (5) is obtained, after reduction vaporization is removed ethanol below 50 ℃, then the water dissolution that adds 1～10 times of quality in the residue, centrifugal, obtain supernatant liquor and throw out, 50 ℃ of lower vacuum-dryings of described throw out 1～4 hour obtain highly purified soybean isoflavones;
(7) preparation of Soyasaponin: the supernatant liquor that step (6) is obtained, after adopting macroporous resin adsorption 0.5～2h, then be that 50～90% ethanol carries out wash-out with volumetric concentration, 50 ℃ of lower reduction vaporizations of elutriant are removed ethanol, and be concentrated into 1/5～1/10 of original volume, 50 ℃ of lower vacuum-drying 1～4h of concentrated solution obtain highly purified Soyasaponin;
(8) preparation of low temperature soybean germ protein concentrate: to the extract remainder low temperature soybean germ dregs of rice that step (4) obtains, behind micronizing or Ordinary pulverization, cross 30～120 mesh sieves, obtain soybean germ albumen crude product; Add 2～6 times of quality in the soybean germ albumen crude product, volumetric concentration is 60～100% ethanol, washing is filtered, the 50 ℃ of lower reduction vaporizations of the wet dregs of rice after the washing are removed ethanol after, vacuum-drying 1～4h obtains refining soybean germ protein concentrate.
2. the method for soybean germ coproduction germ oil according to claim 1, oligose and protein concentrate, it is characterized in that wherein the described soybean germ stabilization treatment of step (1) is online or processed offline dual mode, wherein said online treatment is namely carried out immediately stabilization treatment, wherein said processed offline to the soybean germ of just having separated and is about to soybean germ and collects to concentrate and carry out stabilization treatment; Described stabilization treatment method comprises microwave, steam treatment, hot blast or extruding puffing means, when adopting microwave, and microwave power 0.05～5.0kW/kg soybean germ, the microwave action time is 1～10min; When adopting the high pressure steam stabilization, vapor pressure 3～7kg, treatment time 5～30min.
3. the method for soybean germ coproduction germ oil according to claim 1, oligose and protein concentrate, it is characterized in that wherein said subcritical fluids is butane, propane, dme, liquefied petroleum gas (LPG) or liquefied ammonia, described entrainment agent comprises ethanol or methyl alcohol, and the massfraction that adds entrainment agent is 0.1～5%.
4. the method for soybean germ coproduction germ oil according to claim 1, oligose and protein concentrate, it is characterized in that wherein step (3) and (4) described operating process all are to finish under the processing condition of complete closed, select butane from soybean germ oil and grease extracting, select the oligose in ethanol or the liquefied ammonia extraction skimmed soy beans plumule, finish in the different extraction sections of twice extraction in same leaching plant, perhaps in the leaching plant of two series connection, finish respectively.
5. the method for soybean germ coproduction germ oil according to claim 1, oligose and protein concentrate, it is characterized in that wherein winterization, alkali refining and the decoloration process of the described routine of step (3), carry out according to following step: at first in crude oil, add the sodium hydroxide that accounts for quality of crude oil mark 0.05～0.25%, stirring velocity is 40～70 to turn/min, after finishing neutralization reaction, speed drops to 10～30 and turns/min, continue to stir 10～30min, oil is warming up to 90～95 ℃, and adds strong mixing or use airflow stirring instead according to neat soap flocculation situation; When the obvious sedimentation of neat soap, stop to stir, 4～6h is left standstill in insulation, and with the soft water washing of oil mass 10～15%, temperature is not less than 85 ℃ subsequently, and stirring velocity should be moderate therebetween, makes oil mixing with water even, washs 2～4 times; Then carry out adsorption bleaching, sorbent material is take atlapulgite as main, and adds 5～10% the gac that accounts for the atlapulgite quality, and the sorbent material consumption is 1%～7% of quality of crude oil, 80～110 ℃ of adsorption temps, and stirring velocity≤80 turn/min, decolouring 15～30min; The last grease that slowly stirs is cooled to 4～6 ℃, and insulation 12～36h filters, and obtains the soybean germ refining oil.
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| CN103013652A (en) * | 2012-12-07 | 2013-04-03 | 江南大学 | Process for simultaneous extraction of lipid and oligosaccharide from soybean |
| CN103242951A (en) * | 2013-05-06 | 2013-08-14 | 广西工学院 | Method for improving oil extraction pre-treatment technology |
| CN103497830A (en) * | 2013-10-11 | 2014-01-08 | 江南大学 | High-quality wheat germ oil and subcritical preparation method thereof |
| HRP20221346T1 (en) * | 2015-09-07 | 2022-12-23 | George Stantchev | Extraction apparatus and method thereof |
| CN106236818B (en) * | 2016-08-02 | 2019-05-17 | 宝健（北京）生物技术有限公司 | A method of extracting phytosterol from soybean stem cell culture |
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