CN101283746B - Process for extracting the soyabean oligosaccharides by air-float purification and film integration - Google Patents
Process for extracting the soyabean oligosaccharides by air-float purification and film integration Download PDFInfo
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- CN101283746B CN101283746B CN2008100644893A CN200810064489A CN101283746B CN 101283746 B CN101283746 B CN 101283746B CN 2008100644893 A CN2008100644893 A CN 2008100644893A CN 200810064489 A CN200810064489 A CN 200810064489A CN 101283746 B CN101283746 B CN 101283746B
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Abstract
The invention relates to a method for extracting edible oligosaccharides, specifically a method for extracting soybean oligosaccharides from soybean whey liquid by flotation purification and membrane concentration. The method comprises the following steps: thermal coagulation, cooling, high-speed centrifugal separation, pH adjustment and flocculation, secondary high-speed centrifugal separation, flotation separation, first-stage ultrafiltration, decolorization with ion exchange resin, electrodialysis desalination, further desalination with ion exchange resin, second-stage ultrafiltration, reverse osmosis concentration, activated carbon decolorization, diatomite filtration, terminal ultrafiltration and negative-pressure evaporation concentration. The invention has the advantages that: 1. based on the reasonable combination of proper molecular weight cut-off of ultrafiltration membrane and membrane assembly, operation mode and efficient cleaning, the method works continuously and stablyfor long time; 2. the method realizes the pretreatment by using multi-stage high-efficiency centrifugal separation technique, without using filter aids and producing pollutants, and the separated protein residue can be recycled; and 3. the method has simple process and low equipment and operation costs.
Description
Technical field: the present invention relates to a kind of method of extracting edible oligose, be specially a kind of method, from soybean whey liquid, extract soybean oligosaccharide with air-float purification, the integrated extraction soybean oligosaccharide of film.
Background technology: soybean oligosaccharide through biological action, produces gases such as carbonic acid gas in intestines, make the uncomfortable flatulence phenomenon of people and cause, and can not be absorbed by human consumption, is considered to not be the nutrient substance of human body, thereby has negated the utility value of soybean oligosaccharide.But along with people are by discovering in recent years, soybean oligosaccharide is not to be the material of flatulence effect, the growth of what is more important and human body, body eubolism, prevents and treats the best breeding material of all closely bound up bifidus bacillus of eqpidemic disease.The peculiar a series of unique physiological functions of soybean oligosaccharide make people more and more pay attention to development and use to it.
Soybean whey water is to produce the high concentrated organic wastewater that produces in the food processes such as soybean protein isolate, protein concentrate (acid system) and bean curd, and its major ingredient is: protein, carbohydrate, salt.Traditional way is directly discharged it as the refuse that has no utility value, or through biochemical simple process discharging, has not only polluted environment, and wasted the material very useful to Human Physiology, i.e. soybean oligosaccharide and whey-protein etc.
Contain major ingredient such as whey-protein, carbohydrate, salt in the soybean whey liquid, wherein carbohydrate accounts for 0.5%-1.0%, the monose (glucose) that comprises disaccharide (sucrose), trisaccharide (Fructus Kaki glycoside) and tetrose (stachyose) and trace, whey-protein accounts for 0.1%-0.5%, salt accounts for 0.2%-1%, comprise organic salt and inorganic salt, total solidity thing accounts for 0.8%-2.5%.
Adopt membrane separation technique from soybean whey liquid, to extract soybean oligosaccharide.Soybean whey liquid purifying method commonly used: but remove in the soybean whey liquid heat-coagulation or add the protein that flocculation agent can flocculate with flame filter press, and then hold back remaining albumen with ultra-filtration membrane and purify soybean whey liquid, owing to contain the good small molecular protein of thermostability in the whey liquid, heating or adding under the condition of flocculation agent, still some small molecular protein is difficult to coagulative precipitation, therefore by filtering method, be difficult to protein contained in the soybean whey liquid is thoroughly separated.So also there are some technical difficult problems in actual applications in this method.Its main concrete difficult problem is as follows:
1, membrane pollution problem.It is membrane pollution problem that ultrafiltration is used for the maximum problem of the current existence of soybean whey liquid component separation.According to the difference of soybean whey protein and soybean oligosaccharide and salt molecular weight, with the ultra-filtration membrane of certain molecular weight cut-off, the whey-protein in the soybean whey liquid to be held back, soybean oligosaccharide and salt see through ultra-filtration membrane, make two components obtain separating.Because whey-protein has certain viscosity, easily be attached on the film, form gel, cause fenestra to stop up, thereby cause membrane flux to be decayed rapidly, ultrafiltration can not normally be carried out.
2, film cleans problem.Soybean whey liquid pre-treatment, method commonly used are heating and add flocculation agent, make the protein denaturation post precipitation, with flame filter press albumen sepn are removed again.Owing to contain all good small molecular protein of stability under some thermostability and the ionogen condition in the soybean whey liquid, therefore can not albumen sepn is complete with filtering method, or misoperation is run albumen, will cause serious membrane pollution problem, although take diversified purging method, also be difficult to return to original flux, even ultra-filtration membrane can't normally be moved.
3, environmental pollution problem.Owing to usually with the protein in the flame filter press separation soybean whey liquid, just must add a large amount of diatomite, therefore in operational process, will produce a large amount of diatomite and proteic mixed waste, and cause the pollution of environment as flocculating aids
Summary of the invention: the object of the present invention is to provide execute-in-place, simple in structure, with low cost, easy to operate, use a kind of flexibly pre-treatment complete, do not produce that pollutent, film contamination resistance are strong, film long service life, easy cleaning, flow are big, stable, improve the product yield, the method for the integrated extraction soybean oligosaccharide of air-float purification, film that quality is high.The object of the present invention is achieved like this: it comprises and adds that heat-coagulation, cooling, high speed centrifugation separate, pH value is regulated flocculation, the separation of secondary high speed centrifugation, dissolved air flotation, one-level ultrafiltration, ion-exchange resin decolorization, electrodialytic desalting, ion exchange resin advanced desalination, two-stage ultrafiltering, reverse osmosis concentration, activated carbon decolorizing, diatomite filtration, terminal ultrafiltration, negative pressure evaporation are concentrated.Concrete steps are as follows:
(1) add heat-coagulation, at first with soybean whey liquid under pH value=4.5--4.7 condition, be heated to 95 ℃--in the time of 100 ℃, kept 20--30 minute, make the whey-proteins denature in the whey liquid, coagulative precipitation;
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, its temperature be dropped to below 42 ℃;
(3) high speed centrifugation separates, and whey liquid after will cooling off is sent into high-speed centrifuge and carried out the solid, liquid separation, and solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar;
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the whey-protein flocculation sediment;
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus;
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 35 ℃ of 0.3Mpa-0.5Mpa PH=4.5-9 feeding liquid temperature--40 ℃ of liquid level 800-1200mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting;
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid, hollow-fibre membrane is molecular weight cut-off 10000-20000, PH=2-12, operating pressure are 0.1Mpa-0.5Mpa, 35 ℃ of feeding temperatures--40 ℃;
(8) ion-exchange resin decolorization is sent into the ion-exchange resin decolorization system with the one-level ultrafiltration through whey liquid and is decoloured, flow velocity 10-15 rice/hour, 30 ℃ of temperature--35 ℃;
(9) electrodialytic desalting through the whey liquid of ion-exchange resin decolorization, still contains certain salt, it is sent into electrodialysis carry out desalination, makes specific conductivity that whey sees through liquid less than below the 50 μ s/cm, and ratio of desalinization reaches more than 98%;
(10) ion exchange resin advanced desalination also has a spot of salt through the whey liquid behind the electrodialytic desalting, and it is sent into ion exchange resin column again, carries out further desalination and metal ion, and its specific conductivity is reached below the 10 μ s/cm;
(11) two-stage ultrafiltering is sent the whey liquid of previous step into the two-stage ultrafiltering system and is carried out removal of impurities, and hollow-fibre membrane is molecular weight cut-off 10000-20000, and PH=2-12, operating pressure are 0.1Mpa-0.5Mpa, 35 ℃ of feeding temperatures--and 40 ℃;
(12) reverse osmosis concentration makes concentration of oligosaccharide in the whey liquid solution by 1%-1.2%, is concentrated into 8%-10%.Water more than 90% sees through, and does not contain sugar, as the process water reuse;
(13) activated carbon decolorizing, with the reverse osmosis concentrated liquid glucose that is reduced to 8%-10%, be heated to 80 ℃-85 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac sent into filter, the filtering gac with pump;
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again;
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite, the oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear;
(16) negative pressure evaporation concentrates, through the pol after the reverse osmosis concentration is 8%-10%, will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system, under negative pressure, 80 ℃ of-85 ℃ of operational conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into water cooler, when temperature drops to below 25 ℃, pack to be pulpous state soybean oligosaccharide finished product.Advantage of the present invention is: 1, adopt the small molecular protein in the air-float purification removal whey liquid, create prerequisite for preventing that film from polluting.2, adopt the reasonable combination of suitable membrane molecular weight cut-off and membrane module, and the operational mode that adopts, effective purging methods etc. guarantee operation steady in a long-term.3, repeatedly efficient centrifugal isolation technique is adopted in pre-treatment, need not add any flocculating aids, does not produce any pollutent, and isolated albumen slag can be recycled.4, work simplification, facility investment and working cost are low.5, energy-conservation.The membrane sepn process does not undergo phase transition, and energy consumption is low, and adopts clear energy sources---electric power, so membrane separation technique claims power-saving technology again.Adopt reverse osmosis membrane that the soybean protein isolate whey water is concentrated, do not need steam, can save total energy consumption more than 70%.6, the true qualities, this flavor and the nutritive ingredient that keep soybean oligosaccharide.Membrane sepn is to carry out under normal temperature low pressure, and protein, electrodialytic desalting, reverse osmosis concentration etc. are held back in ultrafiltration, and membrane process does not need heating, no phase transformation.Avoid the generation of phenomenons such as sugared thermolysis and variable color, kept former coloured, the flavor and the nutritive ingredient of product.7, after soya whey wastewater is handled through membrane sepn, but the cleaning reuse.
Description of drawings: Fig. 1 is a structural principle block diagram of the present invention.
Embodiment:
(1) add heat-coagulation, at first with soybean whey liquid under pH value=4.5--4.7 condition, be heated to 95 ℃--in the time of 100 ℃, kept 20--30 minute, make the whey-proteins denature in the whey liquid, coagulative precipitation.
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, its temperature be dropped to below 42 ℃.
(3) high speed centrifugation separates, and will cool off the back whey liquid, sends into high-speed centrifuge and carries out the solid, liquid separation.Solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar.
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the whey-protein flocculation sediment.
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus.
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 35 ℃ of 0.3Mpa-0.5Mpa PH=4.5-9 feeding liquid temperature--40 ℃ of liquid level 800-1200mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting.
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular weight cut-off 10000-20000, its PH=2-12.Film toughness height, flux are big, antipollution, easy cleaning, and have backwashing function, operating pressure 0.1Mpa-0.5Mpa, and 35 ℃ of feeding temperatures--40 ℃.
(8) ion-exchange resin decolorization, the one-level ultrafiltration is sent into the ion-exchange resin decolorization system through whey liquid decolours, looking decolorizing effect regularly regenerates to ion exchange resin, flow velocity 10-15 rice/hour, 30 ℃ of temperature--35 ℃, the spent ion exchange resin decolouring is improved the quality of products, reduce gac and diatomaceous consumption, and the quantity discharged of waste material.
(9) electrodialytic desalting, the whey liquid through ion-exchange resin decolorization still contains certain salt, and it can influence the local flavor of product.It is sent into electrodialysis carry out desalination, make specific conductivity that whey sees through liquid less than below the 50 μ s/cm, ratio of desalinization reaches more than 98%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialytic desalting, it is sent into ion exchange resin column again, carry out further desalination and metal ion, its specific conductivity is reached below the 10 μ s/cm, thoroughly remove hardship, saline taste and heavy metal etc. in the whey liquid.
(11) two-stage ultrafiltering is for holding back the impurity that electrodialysis and ion exchange resin system bring into.It is sent into the two-stage ultrafiltering system, and to carry out removal of impurities supermembrane molecular weight cut-off be the hollow-fibre membrane of 10000--20000, PH=2-12, film toughness height, flux are big, antipollution, easy cleaning, and have backwashing function, operating pressure 0.1Mpa-0.5Mpa, 30 ℃-40 ℃ of feeding temperatures.
(12) reverse osmosis concentration is for improving the concentration of soybean oligosaccharide, save energy, soybean whey liquid after ultrafiltration purification, electrodialysis and ion exchange resin desalination, decolouring, carry out reverse osmosis concentration, make concentration of oligosaccharide in its solution, be concentrated into 8%-10% by 1%-1.2%.Water more than 90% sees through, and does not contain sugar, as the process water reuse.
(13) activated carbon decolorizing, with the reverse osmosis concentrated liquid glucose that is reduced to 8%-10%, be heated to 80 ℃-85 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac is sent into filter with pump, gac is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again.
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear.
(16) negative pressure evaporation concentrates, and through the pol 8%-10% after the reverse osmosis concentration, relative volume is big, easily becomes sour, and the shelf lives is short, and therefore bad transportation will further concentrate.Will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system.Under negative pressure, 80 ℃ of-85 ℃ of operational conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into water cooler, when temperature drops to below 25 ℃, pack to be soybean pulpous state oligose finished product.
Embodiment 1:(1) add heat-coagulation, at first with soybean whey liquid under pH value=4.5 conditions, be heated to 95 ℃, kept 20 minutes, make the whey-proteins denature in the whey liquid, coagulative precipitation.
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, make its temperature drop to 35 ℃.
(3) high speed centrifugation separates, and will cool off the back whey liquid, sends into high-speed centrifuge and carries out the solid, liquid separation.Solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar.
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 10% concentration, regulates PH=7 and makes the whey-protein flocculation sediment.
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus.
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 0.3Mpa, PH=4.5,35 ℃ of feeding liquid temperature, liquid level 800mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting.
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid.Adopt the hollow-fibre membrane of molecular weight cut-off 10000, its PH=2.Film toughness height, flux are big, antipollution, easy cleaning, and have backwashing function, operating pressure 0.1Mpa, 35 ℃ of feeding temperatures.
(8) ion-exchange resin decolorization, the one-level ultrafiltration is sent into the ion-exchange resin decolorization system through whey liquid decolours, looking decolorizing effect regularly regenerates to ion exchange resin, 10 meters/hour of flow velocitys, 30 ℃ of temperature, the spent ion exchange resin decolouring is improved the quality of products, reduce gac and diatomaceous consumption, and the quantity discharged of waste material.
(9) electrodialytic desalting, the whey liquid through ion-exchange resin decolorization still contains certain salt, and it can influence the local flavor of product.It is sent into electrodialysis carry out desalination, make specific conductivity that whey sees through liquid less than 35 μ s/cm, ratio of desalinization reaches 98%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialytic desalting, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its specific conductivity reach 8 μ s/cm, thoroughly remove hardship, saline taste and heavy metal etc. in the whey liquid.
(11) two-stage ultrafiltering is for holding back the impurity that electrodialysis and ion exchange resin system bring into.It is sent into the two-stage ultrafiltering system, and to carry out removal of impurities supermembrane molecular weight cut-off be 10000 hollow-fibre membrane, PH=2, operating pressure 0.1Mpa, 30 ℃ of feeding temperatures.
(12) reverse osmosis concentration is for improving the concentration of soybean oligosaccharide, save energy, soybean whey liquid after ultrafiltration purification, electrodialysis and ion exchange resin desalination, decolouring, carry out reverse osmosis concentration, make concentration of oligosaccharide in its solution, be concentrated into 8% by 1%.90% water sees through, and does not contain sugar, as the process water reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 8% the liquid glucose that is reduced to, be heated to 80 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac sent into filter with pump, gac is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again.
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear.
(16) negative pressure evaporation concentrates, and through the pol 8% after the reverse osmosis concentration, relative volume is big, easily becomes sour, and the shelf lives is short, and therefore bad transportation will further concentrate.Will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system.Under negative pressure, 80 ℃ of operational conditions of temperature, its pol is concentrated to 76% by 8%, and then cools off with being pumped into water cooler, when temperature drops to 24 ℃, pack to be soybean pulpous state oligose finished product.
Embodiment 2:(1) add heat-coagulation, at first with soybean whey liquid under pH value=4.7 conditions, when being heated to 100 ℃, kept 30 minutes, make the whey-proteins denature in the whey liquid, coagulative precipitation.
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, make its temperature drop to 42 ℃.
(3) high speed centrifugation separates, and will cool off the back whey liquid, sends into high-speed centrifuge and carries out the solid, liquid separation.Solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar.
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 30% concentration, regulates PH=9 and makes the whey-protein flocculation sediment.
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus.
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 0.5Mpa, PH=9, feeding liquid temperature, 40 ℃, liquid level 1200mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting.
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular weight cut-off 20000, its PH=12.Operating pressure 0.5Mpa, 40 ℃ of feeding temperatures.
(8) ion-exchange resin decolorization, the one-level ultrafiltration is sent into the ion-exchange resin decolorization system through whey liquid decolours, looking decolorizing effect regularly regenerates to ion exchange resin, flow velocity rice/hour, 35 ℃ of temperature, the spent ion exchange resin decolouring is improved the quality of products, reduce gac and diatomaceous consumption, and the quantity discharged of waste material.
(9) electrodialytic desalting, the whey liquid through ion-exchange resin decolorization still contains certain salt, and it can influence the local flavor of product.It is sent into electrodialysis carry out desalination, make specific conductivity that whey sees through liquid less than 40 μ s/cm, ratio of desalinization reaches 99%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialytic desalting, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its specific conductivity reach 10 μ s/cm, thoroughly remove hardship, saline taste and heavy metal etc. in the whey liquid.
(11) two-stage ultrafiltering is for holding back the impurity that electrodialysis and ion exchange resin system bring into.It is sent into the two-stage ultrafiltering system, and to carry out removal of impurities supermembrane molecular weight cut-off be 20000 hollow-fibre membrane, PH=12, and operating pressure 0.5Mpa,, 40 ℃ of feeding temperatures.
(12) reverse osmosis concentration is for improving the concentration of soybean oligosaccharide, save energy, soybean whey liquid after ultrafiltration purification, electrodialysis and ion exchange resin desalination, decolouring, carry out reverse osmosis concentration, make concentration of oligosaccharide in its solution, be concentrated into 10% by 1.2%.97 water sees through, and does not contain sugar, as the process water reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 10% the liquid glucose that is reduced to, be heated to 85 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac sent into filter with pump, gac is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again.
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear.
(16) negative pressure evaporation concentrates, and through the pol 10% after the reverse osmosis concentration, relative volume is big, easily becomes sour, and the shelf lives is short, and therefore bad transportation will further concentrate.Will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system.Under negative pressure, 85 ℃ of operational conditions of temperature, its pol is concentrated to 78% by 10%, and then cools off with being pumped into water cooler, when temperature drops to 25 ℃, pack to be soybean pulpous state oligose finished product.
Embodiment 3:(1) add heat-coagulation, at first with soybean whey liquid under the condition of pH value=4., when being heated to 98 ℃, kept 25 minutes, make the whey-proteins denature in the whey liquid, coagulative precipitation.
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, make its temperature drop to 40 ℃.
(3) high speed centrifugation separates, and will cool off the back whey liquid, sends into high-speed centrifuge and carries out the solid, liquid separation.Solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar.
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 25% concentration, regulates PH=8 and makes the whey-protein flocculation sediment.
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus.
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 35 ℃ of 0.4Mpa, PH=7, feeding liquid temperature--40 ℃, liquid level 1000mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting.
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular weight cut-off 15000, its PH=10.Operating pressure 0.4Mpa, 38 ℃ of feeding temperatures.
(8) ion-exchange resin decolorization, the one-level ultrafiltration is sent into the ion-exchange resin decolorization system through whey liquid decolours, looking decolorizing effect regularly regenerates to ion exchange resin, 13 meters/hour of flow velocitys, 33 ℃ of temperature, the spent ion exchange resin decolouring is improved the quality of products, reduce gac and diatomaceous consumption, and the quantity discharged of waste material.
(9) electrodialytic desalting, the whey liquid through ion-exchange resin decolorization still contains certain salt, and it can influence the local flavor of product.It is sent into electrodialysis carry out desalination, make specific conductivity that whey sees through liquid less than 48 μ s/cm, ratio of desalinization reaches 99%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialytic desalting, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its specific conductivity reach 9 μ s/cm, thoroughly remove hardship, saline taste and heavy metal etc. in the whey liquid.
(11) two-stage ultrafiltering is for holding back the impurity that electrodialysis and ion exchange resin system bring into.It is sent into the two-stage ultrafiltering system, and to carry out removal of impurities supermembrane molecular weight cut-off be 15000 hollow-fibre membrane, PH=11, and operating pressure 0.4Mpa,, 38 ℃ of feeding temperatures.
(12) reverse osmosis concentration is for improving the concentration of soybean oligosaccharide, save energy, soybean whey liquid after ultrafiltration purification, electrodialysis and ion exchange resin desalination, decolouring, carry out reverse osmosis concentration, make concentration of oligosaccharide in its solution, be concentrated into 9% by 1.1%.Water more than 99% sees through, and does not contain sugar, as the process water reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 9% the liquid glucose that is reduced to, be heated to 84 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac sent into filter with pump, gac is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again.
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear.
(16) negative pressure evaporation concentrates, and through the pol 9% after the reverse osmosis concentration, relative volume is big, easily becomes sour, and the shelf lives is short, and therefore bad transportation will further concentrate.Will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system.Under negative pressure, 84 ℃ of operational conditions of temperature, its pol is concentrated to 77% by 9%, and then cools off with being pumped into water cooler, when temperature drops to 23 ℃, pack to be soybean pulpous state oligose finished product.
Claims (1)
1. the method for an air-float purification, the integrated extraction soybean oligosaccharide of film, it comprises and adds that heat-coagulation, cooling, high speed centrifugation separate, pH value is regulated flocculation, the separation of secondary high speed centrifugation, dissolved air flotation, one-level ultrafiltration, ion-exchange resin decolorization, electrodialytic desalting, ion exchange resin advanced desalination, two-stage ultrafiltering, reverse osmosis concentration, activated carbon decolorizing, diatomite filtration, terminal ultrafiltration, negative pressure evaporation are concentrated, it is characterized in that:
(1) add heat-coagulation, at first with soybean whey liquid under pH value=4.5--4.7 condition, be heated to 95 ℃--in the time of 100 ℃, kept 20--30 minute, make the whey-proteins denature in the whey liquid, coagulative precipitation;
(2) cooling will add the heat-coagulation whey liquid and send into water cooler, with the water coolant indirect heat exchange, its temperature be dropped to below 42 ℃;
(3) high speed centrifugation separates, and whey liquid after will cooling off is sent into high-speed centrifuge and carried out the solid, liquid separation, and solid phase is discharged, and liquid phase is sent into pH value and regulated the flocculation jar;
(4) pH value is regulated flocculation, and supercentrifuge is told liquid phase, sends into pH value and regulates the flocculation jar, under 30 rev/mins of agitation conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the whey-protein flocculation sediment;
(5) the secondary high speed centrifugation separates, and will regulate pH value flocculation sediment whey liquid, sends into high-speed centrifuge, carries out the secondary solid, liquid and separates, and solid phase is discharged, and liquid phase is sent into air-floating apparatus;
(6) dissolved air flotation, to also contain solubility whey-protein and the proteic whey liquid of polypeptide small molecule, be input in the air-floating apparatus: the air pressure in the air-floating apparatus is 35 ℃ of 0.3Mpa-0.5Mpa PH=4.5-9 feeding liquid temperature--40 ℃ of liquid level 800-1200mm, surfactants such as the soluble protein in the clear liquid, polypeptide, accumulate in liquid-gas interface, and float, foam and whey liquid are separated to solution top formation foam layer, purifying whey liquid prevents that film from polluting;
(7) one-level ultrafiltration is sent the whey liquid behind the air-float purification into the one-level ultrafiltration, further holds back residual protein and colloidalmaterial in the whey liquid, hollow-fibre membrane is molecular weight cut-off 10000-20000, PH=2-12, operating pressure are 0.1Mpa-0.5Mpa, 35 ℃ of feeding temperatures--40 ℃;
(8) ion-exchange resin decolorization is sent into the ion-exchange resin decolorization system with the one-level ultrafiltration through whey liquid and is decoloured, flow velocity 10-15 rice/hour, 30 ℃ of temperature--35 ℃;
(9) electrodialytic desalting through the whey liquid of ion-exchange resin decolorization, still contains certain salt, it is sent into electrodialysis carry out desalination, makes specific conductivity that whey sees through liquid less than below the 50 μ s/cm, and ratio of desalinization reaches more than 98%;
(10) ion exchange resin advanced desalination also has a spot of salt through the whey liquid behind the electrodialytic desalting, and it is sent into ion exchange resin column again, carries out further desalination and metal ion, and its specific conductivity is reached below the 10 μ s/cm;
(11) two-stage ultrafiltering is sent the whey liquid of previous step into the two-stage ultrafiltering system and is carried out removal of impurities, and hollow-fibre membrane is molecular weight cut-off 10000-20000, and PH=2-12, operating pressure are 0.1Mpa-0.5Mpa, 35 ℃ of feeding temperatures--and 40 ℃;
(12) reverse osmosis concentration makes concentration of oligosaccharide in the whey liquid solution by 1%-1.2%, is concentrated into 8%-10%.Water more than 90% sees through, and does not contain sugar, as the process water reuse;
(13) activated carbon decolorizing, with the reverse osmosis concentrated liquid glucose that is reduced to 8%-10%, be heated to 80 ℃-85 ℃ after, add 3 ‰ gac again, under agitation condition, decoloured 30 minutes, and then the mixed solution of liquid glucose and gac sent into filter, the filtering gac with pump;
(14) diatomite filtration at first adds pre-removing in the liquid with 3% diatomite, sends into diatomite filter after mixing and removes in advance, after forming filtering layer, with the mixed solution of sugar with gac, sends into the diatom filter and carries out the filtering gac again;
(15) terminal ultrafiltration, in the soybean oligosaccharide liquid of filtering gac, residual a spot of gac and diatomite, the oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes gac and diatomite, makes its clear;
(16) negative pressure evaporation concentrates, through the pol after the reverse osmosis concentration is 8%-10%, will be by the liquid glucose of terminal ultrafiltration, again with being pumped into triple effect negative pressure evaporation system, under negative pressure, 80 ℃ of-85 ℃ of operational conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into water cooler, when temperature drops to below 25 ℃, pack to be pulpous state soybean oligosaccharide finished product.
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| CN102827687A (en) * | 2012-09-17 | 2012-12-19 | 东北农业大学 | Extraction method of soybean oligosaccharides |
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| CN104530143B (en) * | 2014-12-31 | 2017-01-11 | 东北农业大学 | Method for preparing soybean whey oligosaccharide through coupling of heating, flocculating, air floating and ultra-filtering |
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| CN114292966A (en) * | 2021-12-23 | 2022-04-08 | 巴彦淖尔华恒生物科技有限公司 | Separation method and application of flocculation protein in starch sugar solution |
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