CN101283746A - 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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- 240000007842 Glycine max Species 0.000 title claims abstract description 58
- 235000010469 Glycine max Nutrition 0.000 title claims abstract description 58
- 229920001542 oligosaccharide Polymers 0.000 title claims abstract description 35
- 150000002482 oligosaccharides Polymers 0.000 title claims abstract description 35
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 9
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- 238000005189 flocculation Methods 0.000 claims abstract description 33
- 230000016615 flocculation Effects 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 31
- 238000000909 electrodialysis Methods 0.000 claims abstract description 30
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 27
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 25
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 25
- 239000012528 membrane Substances 0.000 claims abstract description 24
- 238000004042 decolorization Methods 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000005345 coagulation Methods 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 52
- 239000011780 sodium chloride Substances 0.000 claims description 29
- WQZGKKKJIJFFOK-GASJEMHNSA-N D-Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 25
- 239000008103 glucose Substances 0.000 claims description 25
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- 238000007667 floating Methods 0.000 claims description 18
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000835 fiber Substances 0.000 claims description 12
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- 239000007787 solid Substances 0.000 claims description 12
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- 239000012141 concentrate Substances 0.000 claims description 11
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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 stably for 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 compound sugar, be specially a kind of method, from soybean whey liquid, extract soyabean oligosaccharides with air-float purification, the integrated extraction soyabean oligosaccharides of film.
Background technology:
Soyabean oligosaccharides through biological agent, produces gases such as carbon dioxide 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 of human body, thereby has negated the value of soyabean oligosaccharides.But along with people are by discovering in recent years, soyabean oligosaccharides 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 Bifidobacterium of eqpidemic disease.The peculiar a series of unique physiological functions of soyabean oligosaccharides make people more and more pay attention to development and use to it.
Soy-bean 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 Main Ingredients and Appearance is: protein, carbohydrate, salt.Traditional way is directly discharged it as the refuse that has no value, or through biochemical simple process discharging, has not only polluted environment, and wasted the material very useful to Human Physiology, i.e. soyabean oligosaccharides and lactalbumin etc.
Contain Main Ingredients and Appearances such as lactalbumin, 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, lactalbumin accounts for 0.1%-0.5%, salt accounts for 0.2%-1%, comprise organic salt and inorganic salts, total solidity thing accounts for 0.8%-2.5%.
Adopt membrane separation technique from soybean whey liquid, to extract soyabean oligosaccharides.Soybean whey liquid purification method commonly used: but remove in the soybean whey liquid heat-coagulation or add the protein that flocculant can flocculate with flame filter press, and then hold back remaining albumen with milipore filter and purify soybean whey liquid, owing to contain the good small molecular protein of heat endurance in the whey liquid, heating or adding under the condition of flocculant, still some small molecular protein is difficult to coagulative precipitation, therefore the method by filtering is 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 soyabean oligosaccharides and salt molecular weight, with the milipore filter of certain molecular cut off, the lactalbumin in the soybean whey liquid to be held back, soyabean oligosaccharides and salt see through milipore filter, make two components obtain separating.Because lactalbumin 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 preliminary treatment, method commonly used are heating and add flocculant, make the albuminous degeneration post precipitation, with flame filter press Protein Separation are removed again.Owing to contain all good small molecular protein of stability under some heat endurance and the electrolyte condition in the soybean whey liquid, therefore can not Protein Separation is complete with the method for filtering, or misoperation is run albumen, will cause serious membrane pollution problem, although take diversified cleaning method, also be difficult to return to original flux, even milipore filter 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 running, will produce a large amount of diatomite and the mixed waste of albumen, and cause the pollution of environment as filter aid
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 preliminary treatment complete, do not produce that pollutant, 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 soyabean oligosaccharides 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, electrodialysis desalination, 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid, hollow-fibre membrane is molecular 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) electrodialysis desalination through the whey liquid of ion-exchange resin decolorization, still contains certain salt, it is sent into electrodialysis carry out desalination, makes electrical conductivity that whey sees through liquid less than below the 50 μ s/cm, and salt rejection rate reaches more than 98%;
(10) ion exchange resin advanced desalination also has a spot of salt through the whey liquid behind the electrodialysis desalination, and it is sent into ion exchange resin column again, carries out further desalination and metal ion, and its electrical 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 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 fresh water (FW) 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 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon sent into filter, the filtering active carbon with pump;
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again;
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite, the oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 operating conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into cooler, when temperature drops to below 25 ℃, pack to be pulpous state soyabean oligosaccharides 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 suitable retaining molecular weight and the reasonable combination of membrane module, and the operational mode that adopts, effective cleaning methods etc. guarantee operation steady in a long-term.3, repeatedly efficient centrifugal isolation technics is adopted in preliminary treatment, need not add any filter aid, does not produce any pollutant, and isolated albumen slag can be recycled.4, work simplification, equipment investment and operating cost are low.5, energy-conservation.The film separation 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 nutritional labeling that keep soyabean oligosaccharides.It is to carry out under normal temperature low pressure that film separates, and protein, electrodialysis desalination, 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 thermal decomposition and variable color, kept former coloured, the flavor and the nutritional labeling of product.7, after the soya whey wastewater process film separating treatment, but the cleaning reuse.
Description of drawings:
Fig. 1 is a structural principle block diagram of the present invention.
The specific 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular cut off 10000-20000, its PH=2-12.Film-strength 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 active carbon and diatomaceous consumption, and the discharge capacity of waste material.
(9) electrodialysis desalination, 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 electrical conductivity that whey sees through liquid less than below the 50 μ s/cm, salt rejection rate reaches more than 98%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialysis desalination, it is sent into ion exchange resin column again, carry out further desalination and metal ion, its electrical 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 cut off be the hollow-fibre membrane of 10000--20000, PH=2-12, film-strength 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 soyabean oligosaccharides, energy savings, 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 fresh water (FW) 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 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon is sent into filter with pump, active carbon is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again.
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 storage life 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 operating conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into cooler, when temperature drops to below 25 ℃, pack to be soybean pulpous state compound sugar 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 10% concentration, regulates PH=7 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid.Adopt the hollow-fibre membrane of molecular cut off 10000, its PH=2.Film-strength 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 active carbon and diatomaceous consumption, and the discharge capacity of waste material.
(9) electrodialysis desalination, 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 electrical conductivity that whey sees through liquid less than 35 μ s/cm, salt rejection rate reaches 98%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialysis desalination, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its electrical 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 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 soyabean oligosaccharides, energy savings, 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 fresh water (FW) reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 8% the liquid glucose that is reduced to, be heated to 80% after, add 3 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon sent into filter with pump, active carbon is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again.
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 storage life 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 operating conditions of temperature, its pol is concentrated to 76% by 8%, and then cools off with being pumped into cooler, when temperature drops to 24 ℃, pack to be soybean pulpous state compound sugar 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 30% concentration, regulates PH=9 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular 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 active carbon and diatomaceous consumption, and the discharge capacity of waste material.
(9) electrodialysis desalination, 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 electrical conductivity that whey sees through liquid less than 40 μ s/cm, salt rejection rate reaches 99%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialysis desalination, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its electrical 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 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 soyabean oligosaccharides, energy savings, 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 fresh water (FW) reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 10% the liquid glucose that is reduced to, be heated to 85% after, add 3 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon sent into filter with pump, active carbon is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again.
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 storage life 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 operating conditions of temperature, its pol is concentrated to 78% by 10%, and then cools off with being pumped into cooler, when temperature drops to 25 ℃, pack to be soybean pulpous state compound sugar 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 25% concentration, regulates PH=8 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid.The present invention adopts the hollow-fibre membrane of molecular 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 active carbon and diatomaceous consumption, and the discharge capacity of waste material.
(9) electrodialysis desalination, 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 electrical conductivity that whey sees through liquid less than 48 μ s/cm, salt rejection rate reaches 99%.
(10) ion exchange resin advanced desalination, also have a spot of salt through the whey liquid behind the electrodialysis desalination, it is sent into ion exchange resin column again, carry out further desalination and metal ion, make its electrical 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 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 soyabean oligosaccharides, energy savings, 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 fresh water (FW) reuse.
(13) activated carbon decolorizing, with reverse osmosis concentrated 9% the liquid glucose that is reduced to, be heated to 84% after, add 3 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon sent into filter with pump, active carbon is filtered.
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again.
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite.The oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 storage life 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 operating conditions of temperature, its pol is concentrated to 77% by 9%, and then cools off with being pumped into cooler, when temperature drops to 23 ℃, pack to be soybean pulpous state compound sugar finished product.
Claims (1)
1, the method for a kind of air-float purification, the integrated extraction soyabean oligosaccharides 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, electrodialysis desalination, 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 cooler, with the cooling water 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 stirring conditions, adds the sodium hydroxide solution of 10%--30% concentration, regulates PH=7-9 and makes the lactalbumin 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, the whey liquid of solubility lactalbumin and polypeptide small molecule albumen will also be contained, 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, surface reactive materials such as the soluble protein in the clear liquid, polypeptide, accumulate in gas-liquid interface, and float, foam and whey liquid are separated to solution top formation froth bed, 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 colloidal substance in the whey liquid, hollow-fibre membrane is molecular 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) electrodialysis desalination through the whey liquid of ion-exchange resin decolorization, still contains certain salt, it is sent into electrodialysis carry out desalination, makes electrical conductivity that whey sees through liquid less than below the 50 μ s/cm, and salt rejection rate reaches more than 98%;
(10) ion exchange resin advanced desalination also has a spot of salt through the whey liquid behind the electrodialysis desalination, and it is sent into ion exchange resin column again, carries out further desalination and metal ion, and its electrical 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 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 fresh water (FW) 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 ‰ active carbon again, under stirring condition, decoloured 30 minutes, and then the mixed liquor of liquid glucose and active carbon sent into filter, the filtering active carbon with pump;
(14) diatomite filtration at first adds pre-removing in the liquid with 3 ‰ diatomite, sends into diatomite filter after mixing and carries out precoating, after forming filtering layer, with the mixed liquor of sugar with active carbon, sends into the diatom filter and carries out the filtering active carbon again;
(15) terminal ultrafiltration, in the soyabean oligosaccharides liquid of filtering active carbon, residual a spot of active carbon and diatomite, the oligomeric liquid glucose in back that will decolour is sent into the terminal ultrafiltration, removes active carbon 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 operating conditions of temperature, its pol is concentrated to 76%-78% by 8%-10%, and then cools off with being pumped into cooler, when temperature drops to below 25 ℃, pack to be pulpous state soyabean oligosaccharides finished product.
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