CN101503469A - Method for extracting soy protein, oligosaccharide and isoflavone from soybean whey by two-stage two-segment film - Google Patents

Method for extracting soy protein, oligosaccharide and isoflavone from soybean whey by two-stage two-segment film Download PDF

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CN101503469A
CN101503469A CNA2009101162924A CN200910116292A CN101503469A CN 101503469 A CN101503469 A CN 101503469A CN A2009101162924 A CNA2009101162924 A CN A2009101162924A CN 200910116292 A CN200910116292 A CN 200910116292A CN 101503469 A CN101503469 A CN 101503469A
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soybean
soybean protein
isoflavones
oligosaccharide
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CN101503469B (en
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洪光明
罗建平
潘利华
徐学玲
查学强
叶忠东
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Huangshan Jialong Green Food Co ltd
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Jialong Green Food Co Ltd Of Huangshan Tourism Group
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Abstract

The invention relates to a method for extracting soy protein, oligosaccharide and isoflavone by a two-stage two-section membrane, which solves the problem of comprehensive extraction and utilization of soybean protein, oligosaccharide and isoflavone in soybean yellow serofluid. The method comprises four operating steps of: preprocessing: centrifuging the soybean yellow serofluid so as to remove bean dregs, suspended matter and the like and obtain supernatant fluid A; hyperfiltration: processing the supernatant fluid A by a two-stage two-section membrane system, realizing separation of soy protein with soy isoflavones and soy oligosaccharide and obtaining soy protein finished product with the content of more than 90 percent; absorption and reverse osmosis: processing permeate liquid by a macroporous absorbent resin column and a reverse osmosis membrane system, then carrying out concentration and spray drying and obtaining the soy oligosaccharide finished product with the content of more than 80 percent; and elution: carrying out dissolution and elution to soy isoflavone absorbed by the macroporous absorbent resin with 80 percent of methanol or alcohol, then carrying out concentration and spray drying and obtaining the soy isoflavone finished product with the content of more than 50 percent. The method has simple technique and convenient operation.

Description

Two-stage two-segment film extracts the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean
Technical field
The present invention relates to utilize membrane separation technique from yellow plasm of soybean, to extract soybean protein, soybean oligosaccharide and soybean isoflavones functional factor product, belong to soybean deep processing and waste water reclaiming technical field.
Background technology
The a large amount of waste water that produce in the production process of bean product such as traditional bean curd, dried bean curd, the skin of soya-bean milk and soybean protein are called the bean curd whey wastewater, are commonly called as yellow seriflux.According to statistics, 1 ton of (t) soybean of every processing will be discharged 2-5 ton (t) yellow seriflux.Be rich in the functional factor extensively be familiar with such as soy-protein, soybean oligosaccharide, soybean isoflavones etc. in the yellow seriflux.Find after testing, the soybean isoflavones that contains in the yellow seriflux account for contained soybean isoflavones in the soy material 50%, stachyose 83%, raffinose 94%, proteinic 17%, have the selective separation recovery value.As far back as the seventies, Goldsmith has just carried out and utilizes membrane technique to reclaim the whey protein in the soya whey wastewater and the research of oligose, but disperse again because the scale of general Bean Products Factory is less, fund and technical force's deficiency, and recycling and problem of environmental pollution to functional factor are also paid little attention to, therefore, yellow plasm of soybean still is discharged as waste liquid so far, is not fully used.Therefore, seek the yellow seriflux treatment process of a kind of technical feasibility, industrial economy, environment protection standard, to promoting resource rational utilization, solving crisis of resource and environmental pollution has direct realistic meaning.
Treatment process to soybean processing waste water has anaerobic-aerobic biological treatment, evaporation concentration method, fermentation method and ultrafiltration-reverse osmosis-electroosmose process at present.Anaerobic-aerobic biological treatment treatment effect instability wherein; The evaporation concentration method energy consumption is big, and facility investment and working cost height were promoted in industrial being difficult to; The fermentation method products obtained therefrom is second-rate, mostly is small molecular protein sugar, and yields poorly; There is the shortcoming of operation of equipment complexity in ultrafiltration-reverse osmosis-electroosmose process.Membrane sepn be utilize a special manufacturing, have and select diactinic film, try hard to recommend outside moving down to the heterogeneity in liquid phase or the gas phase mixture separate, purification, spissated advanced machining technology.Membrane separation technique is easy and simple to handle with it, separation efficiency is high and the advantage such as low that consumes energy becomes the requisite technology of biologic separation and purification process.Adopt membrane separation technique to handle the Chinese patent that the existing publication number of soybean processing waste water is respectively CN4560047A and CN01336333A.Publication number provides a kind of method of utilizing Bean Products Factory's waste water to produce soybean isoflavones for the patent of invention of CN4560047A, but this technology does not relate to how extracting soybean protein and soybean oligosaccharide from yellow plasm of soybean.Publication number provides a kind of method of utilizing soybean processing waste water to produce soybean whey protein and soybean oligosaccharide for the patent of invention of CN01336333A, and how this patent of invention extracts isoflavones from yellow plasm of soybean if not relating to; And added in this extractive technique and contained Ca 2+Flocculation agent, concentration polarization and film very easily take place to be polluted, cause membrane flux to descend.
Summary of the invention
In order to solve the comprehensive extraction and application problem of soybean protein in the yellow plasm of soybean, oligose and isoflavones, the invention provides the method for soybean protein, oligose and isoflavones in the employing two-stage two-segment film extraction yellow plasm of soybean that a kind of technology is simple, easy to operate, added value is high.
The technical solution that realizes above-mentioned purpose is as follows:
The method that two-stage two-segment film extracts soybean protein, oligose and isoflavones in the yellow plasm of soybean comprises following operation steps:
(1), pre-treatment:
The yellow plasm of soybean that produces in the bean product production process directly through the centrifugal pre-treatment of whizzer, to remove bean dregs, suspended substance wherein, is obtained supernatant A;
(2), ultrafiltration:
Is 50000-100000 daltonian one-level one section ultra-filtration membrane ultrafiltration by molecular weight cut-off with supernatant A under temperature 20-50 ℃, pressure 0.5-1.5Mpa, obtains soybean protein concentrated solution P1A, and obtains ultrafiltration and see through liquid B 0Again ultrafiltration is seen through liquid B 0By molecular weight cut-off is two sections ultra-filtration membrane ultrafiltration of 3000 daltonian one-levels, obtains soybean protein concentrated solution P1 B, and obtain ultrafiltration through liquid B; Merge soybean protein concentrated solution P1 AWith soybean protein concentrated solution P1 BPromptly obtain soybean protein concentrated solution P1, soybean protein concentrated solution P1 is concentrated into solid content through thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean protein finished product of content more than 90%;
(3), absorption and reverse osmosis:
Ultrafiltration is seen through the adsorption column of liquid B through macroporous adsorbent resin; Soybean isoflavones is by the absorption of the adsorption column of macroporous adsorbent resin, and soybean oligosaccharide flows out from the adsorption column of macroporous adsorbent resin, collects effluent liquid C; Effluent liquid C by reverse osmosis membrane system, is obtained soybean oligosaccharide concentrated solution P2; Soybean oligosaccharide concentrated solution P2 is concentrated into solid content through thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean oligosaccharide finished product of content more than 80%;
(4), wash-out:
Earlier with the water elution liquid of deionized water wash-out adsorption column to the effluent liquid solid substance, the back with the methyl alcohol more than 80% or ethanol under the flow velocity of 1-3BV/h the wash-out adsorption column to the alcohol eluen that flows out isoflavone-containing; Alcohol eluen is concentrated into solid content with thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean isoflavones finished product of content more than 50%.
Whizzer in the step (1) is a disk centrifugal separator, and centrifuging temperature is 10-60 ℃, and working flow is 1-2L/min.
The processing condition of one section ultra-filtration membrane ultrafiltration of one-level or two sections ultra-filtration membrane ultrafiltration of one-level are in the step (2): temperature 20-50 ℃, pressure 0.5-1.5Mpa.
Reverse osmosis pressure described in the step (3) is 0.2-2.0Mpa.
The potting resin of adsorption column described in the step (3) is D101 or AB-8 nonpolar macroporous adsorption resin.
The inlet temperature 125-130 of described spray-drying tower ℃, air outlet temperature 80-85 ℃.
The working conditions of described thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃.Thin film evaporation reclaims the methyl alcohol or the ethanol that obtain and can be used as the eluent recycling in the described step (4).
Useful technique effect of the present invention is embodied in the following aspects:
1, this technology has overcome problems of the prior art and deficiency, has the advantages that technology is simple, flow process is short, cost is low, is fit to large, medium and small different scales bean product processing enterprise.
2, the present invention has realized the recycling of yellow plasm of soybean, has not only obtained the three kind biologically active substances useful to HUMAN HEALTH, and has reduced environmental pollution, has important economic benefit, social benefit and environmental benefit.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described by embodiment.
Embodiment 1:
Referring to Fig. 1, the method that two-stage two-segment film extracts soybean protein, oligose and isoflavones in the yellow plasm of soybean comprises following operation steps:
Step 1: pre-treatment
The yellow plasm of soybean that produces in the bean product production process is collected into wastewater trough, entering rotating speed through the waste water force (forcing) pump is that 10000r/min disk centrifugal separator above, that flow is 2L/min carries out centrifugal pre-treatment, centrifuging temperature is 10-60 ℃, to remove wherein bean dregs, particle, suspended substance etc., obtain supernatant A;
Step 2: ultrafiltration
Is 50000-100000 daltonian one-level one section ultrafiltration membrane system by molecular weight cut-off successively with the supernatant A that obtains after the pre-treatment under temperature 20-50 ℃, pressure 0.5-1.5Mpa condition, obtains soybean protein concentrated solution P1 A, and obtain ultrafiltration membrane permeate liquid B 0Again with ultrafiltration membrane permeate liquid B 0By molecular weight cut-off is two sections ultrafiltration membrane system of 3000 daltonian one-levels, and the realization soybean protein separates with soybean isoflavones, soybean oligosaccharide, obtains soybean protein concentrated solution P1 B, and obtain ultrafiltration through liquid B; Merge soybean protein concentrated solution P1 AWith soybean protein concentrated solution P1 BPromptly obtain soybean protein concentrated solution P1, soybean protein concentrated solution P1 is concentrated into solid content through falling-film evaporator reaches 25%-30%, the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃; Enter spray-drying tower again, inlet temperature 125-130 ℃, air outlet temperature 80-85 ℃, to obtain the soybean protein part finished product of content more than 90%.
Step 3: absorption and reverse osmosis
Resulting ultrafiltration in the step 2 is seen through liquid B from bottom to top through an adsorption column that is assembled with the AB-8 macroporous adsorbent resin; The adsorption column group is made up of three adsorption columns, and ultrafiltration sees through liquid B in succession continuously in an orderly manner by three adsorption columns; Be filled with according to the AB-8 macroporous adsorbent resin that sees through liquid weight 10% in every three adsorption columns; Soybean isoflavones is by resin absorption, and soybean oligosaccharide flows out from resin column, collects effluent liquid C; By reverse osmosis membrane system, reverse osmosis pressure is 0.2-2.0Mpa, obtains soybean oligosaccharide concentrated solution P2 with effluent liquid C; Soybean oligosaccharide concentrated solution P2 is concentrated into solid content through falling-film evaporator reaches 25%-30%, the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃; Enter spray-drying tower again, inlet temperature 125-130 ℃, air outlet temperature 80-85 ℃, to obtain the soybean oligosaccharide finished product of content more than 80%.
Adsorption column potting resin or employing D101 nonpolar macroporous adsorption resin.
Step 4: wash-out
After adsorption operations is finished, use deionized water wash-out adsorption column to effluent liquid solid content<0.5% (refractometer analysis) earlier, the back obtains water elution liquid and alcohol eluen with the wash-out adsorption column under the flow velocity of 1-3BV/h of the methyl alcohol more than 80% to effluent liquid isoflavone content<0.001% (spectrophotometric analysis); Alcohol eluen concentrates with thin-film evaporator, and the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09Mpa, temperature 50-60 ℃, and be concentrated into solid content and reach 25%-30%; Enter spray-drying tower again, inlet temperature 125-130 ℃, air outlet temperature 80-85 ℃, to obtain the soybean isoflavones finished product of content more than 50%.
Embodiment 2
Step 1: pre-treatment
Getting the 1000L yellow plasm of soybean, to add rotating speed be that 20000r/min disk centrifugal separator above, that flow is 2L/min carries out centrifugal pre-treatment, and centrifuging temperature is 10-60 ℃, to remove wherein bean dregs, particle, suspended substance etc., obtains the 974L supernatant A;
Step 2: ultrafiltration
Is 50000-100000 daltonian one-level one section ultrafiltration membrane system by molecular weight cut-off successively with the supernatant A that obtains after the pre-treatment under 20-50 ℃, 0.5-1.5Mpa working pressure, obtains soybean protein concentrated solution P1 A, and obtain ultrafiltration membrane permeate liquid B 0Again with ultrafiltration membrane permeate liquid B 0By molecular weight cut-off is two sections ultrafiltration membrane system of 3000 daltonian one-levels, and the realization soybean protein separates with soybean isoflavones, soybean oligosaccharide, obtains soybean protein concentrated solution P1 B, and obtain ultrafiltration through liquid B; Merge soybean protein concentrated solution P1 AWith soybean protein concentrated solution P1 BPromptly obtain soybean protein concentrated solution P1, soybean protein concentrated solution P1 is concentrated into solid content through falling-film evaporator reaches 25%-30%, the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃; Enter spray-drying tower again, inlet temperature 125-130 ℃, air outlet temperature 80-85 ℃, to obtain soybean protein part finished product 995g of content 91.2%.
Step 3: absorption and reverse osmosis
Resulting ultrafiltration in the step 2 is seen through liquid B from bottom to top through an adsorption column that is assembled with the AB-8 macroporous adsorbent resin; The adsorption column group is made up of three adsorption columns, and ultrafiltration sees through liquid B in succession continuously in an orderly manner by three adsorption columns; Be filled with according to the AB-8 macroporous adsorbent resin that sees through liquid weight 10% in every three adsorption columns; Soybean isoflavones is by resin absorption, and soybean oligosaccharide flows out from resin column, collects effluent liquid C; Effluent liquid C by reverse osmosis membrane system, is obtained soybean oligosaccharide concentrated solution P2; Soybean oligosaccharide concentrated solution P2 is concentrated into solid content through falling-film evaporator reaches 25%-30%, the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃; Enter spray-drying tower again, inlet temperature 125-130 ℃, air outlet temperature 80-85 ℃, to obtain the soybean oligosaccharide finished product 12450g of content 80.6%.
Step 4: wash-out
After adsorption operations is finished, use deionized water wash-out adsorption column to effluent liquid solid content<0.5% (refractometer analysis) earlier, the back obtains water elution liquid and alcohol eluen with the wash-out adsorption column under the flow velocity of 1-3BV/h of the ethanol more than 80% to effluent liquid isoflavone content<0.001% (spectrophotometric analysis); Alcohol eluen concentrates with thin-film evaporator, the working conditions of thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃; And be concentrated into solid content and reach 25%-30%, enter spray-drying tower again, 125 ℃ of inlet temperature, 80 ℃ of air outlet temperatures are to obtain the soybean isoflavones finished product 64g of content 52.1%.

Claims (7)

1, two-stage two-segment film extracts the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean, it is characterized in that comprising following operation steps:
(1), pre-treatment:
The yellow plasm of soybean that produces in the bean product production process directly through the centrifugal pre-treatment of whizzer, to remove bean dregs, suspended substance wherein, is obtained supernatant A;
(2), ultrafiltration:
Is 50000-100000 daltonian one-level one section ultra-filtration membrane ultrafiltration by molecular weight cut-off with supernatant A under temperature 20-50 ℃, pressure 0.5-1.5Mpa, obtains soybean protein concentrated solution P1 A, and obtain ultrafiltration through liquid B 0Again ultrafiltration is seen through liquid B 0By molecular weight cut-off is two sections ultra-filtration membrane ultrafiltration of 3000 daltonian one-levels, obtains soybean protein concentrated solution P1 B, and obtain ultrafiltration through liquid B; Merge soybean protein concentrated solution P1 AWith soybean protein concentrated solution P1 BPromptly obtain soybean protein concentrated solution P1, soybean protein concentrated solution P1 is concentrated into solid content through thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean protein finished product of content more than 90%;
(3), absorption and reverse osmosis:
Ultrafiltration is seen through the adsorption column of liquid B through macroporous adsorbent resin; Soybean isoflavones is by the absorption of the adsorption column of macroporous adsorbent resin, and soybean oligosaccharide flows out from the adsorption column of macroporous adsorbent resin, collects effluent liquid C; Effluent liquid C by reverse osmosis membrane system, is obtained soybean oligosaccharide concentrated solution P2; Soybean oligosaccharide concentrated solution P2 is concentrated into solid content through thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean oligosaccharide finished product of content more than 80%;
(4), wash-out:
Earlier with the water elution liquid of deionized water wash-out adsorption column to the effluent liquid solid substance, the back with the methyl alcohol more than 80% or ethanol under the flow velocity of 1-3BV/h the wash-out adsorption column to the alcohol eluen that flows out isoflavone-containing; Alcohol eluen is concentrated into solid content with thin-film evaporator reaches 25%-30%, enter spray-drying tower again and carry out spraying drying, obtain the soybean isoflavones finished product of content more than 50%.
2, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the whizzer in the step (1) is a disk centrifugal separator, and centrifuging temperature is 10-60 ℃, and working flow is 1-2L/min.
3, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the processing condition of one section ultra-filtration membrane ultrafiltration of one-level or two sections ultra-filtration membrane ultrafiltration of one-level are in the step (2): temperature 20-50 ℃, pressure 0.5-1.5Mpa.
4, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the reverse osmosis pressure described in the step (3) is 0.2-2.0Mpa.
5, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the potting resin of adsorption column described in the step (3) is D101 or AB-8 nonpolar macroporous adsorption resin.
6, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the inlet temperature 125-130 of described spray-drying tower ℃, air outlet temperature 80-85 ℃.
7, extract the method for soybean protein, oligose and isoflavones in the yellow plasm of soybean according to the described two-stage two-segment film of claim 1, it is characterized in that: the working conditions of described thin-film evaporator: vacuum tightness 0.08-0.09MPa, temperature 50-60 ℃.
CN2009101162924A 2009-03-06 2009-03-06 Method for extracting soy protein, oligosaccharide and isoflavone from soybean whey by two-stage two-segment film Active CN101503469B (en)

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EP2301367A1 (en) * 2009-09-28 2011-03-30 WhiteWave Services, Inc. Soy beverage substantially free of isoflavones and method of production
CN102827687A (en) * 2012-09-17 2012-12-19 东北农业大学 Extraction method of soybean oligosaccharides
CN103265614A (en) * 2013-05-28 2013-08-28 宜宾学院 Method for extracting soy protein, oligosaccharide and isoflavone from soybean wastewater by one-step process
CN106282258A (en) * 2016-09-24 2017-01-04 合肥信达膜科技有限公司 A kind of soybean isoflavone isolation technics
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US8597712B2 (en) 2009-09-28 2013-12-03 Whitewave Services, Inc. Soy beverage substantially free of isoflavones and method of production
CN102827687A (en) * 2012-09-17 2012-12-19 东北农业大学 Extraction method of soybean oligosaccharides
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CN106923197A (en) * 2015-12-30 2017-07-07 丰益(上海)生物技术研发中心有限公司 A kind of soybean water extract of low anti-nutrition component and preparation method thereof
CN106282258A (en) * 2016-09-24 2017-01-04 合肥信达膜科技有限公司 A kind of soybean isoflavone isolation technics
CN108308368A (en) * 2018-03-21 2018-07-24 山东禹王生态食业有限公司 A kind of soybean protein bean clear water processing system and processing method
CN108308368B (en) * 2018-03-21 2021-05-28 山东禹王生态食业有限公司 Soybean protein clear water treatment system and method
CN108587798A (en) * 2018-04-09 2018-09-28 吕慧琴 A kind of natural handguard dish washing detergent and preparation method thereof
CN110003289A (en) * 2019-05-08 2019-07-12 江苏博晟康生物科技有限公司 A method of the yellow serofluid improving biological transformation ratio prepares soyabean oligosaccharides
CN111944010A (en) * 2020-08-20 2020-11-17 运城学院 Equipment and method for extracting soybean protein, isoflavone and oligosaccharide from bean product wastewater
CN111944010B (en) * 2020-08-20 2023-05-09 运城学院 Extraction equipment and method for soybean protein, isoflavone and oligosaccharide in bean product wastewater
CN112456713A (en) * 2020-11-24 2021-03-09 广东闻扬环境科技有限公司 Process and equipment for recovering and treating protein in bean product wastewater
CN113355372A (en) * 2021-06-10 2021-09-07 苏州金记食品有限公司 Process for purifying soybean whey and extracting soybean isoflavone aglycone

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