CN104630316A - Integrated technology for extracting proteins and phytin from corn steep liquor - Google Patents
Integrated technology for extracting proteins and phytin from corn steep liquor Download PDFInfo
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- CN104630316A CN104630316A CN201310559888.8A CN201310559888A CN104630316A CN 104630316 A CN104630316 A CN 104630316A CN 201310559888 A CN201310559888 A CN 201310559888A CN 104630316 A CN104630316 A CN 104630316A
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Abstract
The invention discloses an integrated technology for extracting proteins and phytin from corn steep liquor. The technology comprises the following steps: adding protease to the corn steep liquor, carrying out an enzymatic hydrolysis reaction to obtain a corn steep liquor enzymatic hydrolysis liquid, removing impurities from the corn steep liquor enzymatic hydrolysis liquid, carrying out membrane filtration on the impurity removed corn steep liquor enzymatic hydrolysis liquid to obtain a trapped fluid and a permeate liquid; processing the permeate liquid to obtain a required finished phytin product; and processing the trapped fluid to prepare a required protein product. During the corn steep liquor enzymatic hydrolysis, the enzymatic hydrolysis reaction is terminated when the hydrolysis degree of macromolecular proteins in the corn steep liquor is 2-50%. The integrated technology for extracting proteins and phytin from corn steep liquor maximally extracts proteins in the corn steep liquor without influencing the membrane flux, and makes other macromolecular organic components furthest extracted and converted to form corresponding products without influencing the quality of the phytin product.
Description
Technical field
The present invention relates to and a kind ofly extract the composite technology of albumen and Phytin with corn slurries for raw material, belong to integral cereal and utilize field of deep.
Background technology
Corn is the traditional farm crop of China, accounts for 30% of total output of grain, in the development of national economy, has very important status.Corn more than 80% composition is starchy material, therefore a large amount of for the production of starch, but in starch production process, when can produce a large amount of by products as wet milling process production W-Gum, first corn grain to be placed in water and soak, and add certain pharmaceutical chemicals, as sulfurous acid, the waste water stayed after corn soaking is called soak water of maize or corn steeping water, and general one ton of corn can produce 0.8m
3immersion water.
Early stage soak water of maize or its concentrated product corn steep liquor are nearly all fallen by as discharge of wastewater thus bring serious environmental pollution, or adopt alkali (liming or the sodium hydroxide etc.) precipitator method to extract thick Phytin from soak water of maize or corn steep liquor, Phytin is the general term of phytin or phytic acid ca, be the main raw material preparing inositol, it extracts what in fact obtain is phytic acid in soak water of maize or corn steep liquor.But said extracted technique just extracts Phytin, also rationally effective exploitation is not all obtained containing organic compositions such as protein (amino acid), lactic acid, carbohydrates in its raffinate, bring serious environmental pollution on the contrary, thus make part Phytin manufacturing enterprise be closed by force or ban.
Disclosing a kind of in Chinese patent literature CN103214512A take defatted rice bran as the technique of prepared using membrane technique high-purity phytic acid, from angles of product, the object of this technique is to extract highly purified phytic acid, the macromolecular substance such as protein, polysaccharide that removing has an impact to its purity as far as possible, do not consider effective Utilizing question of these compositions, because in above-mentioned technique, the high precision of ultra-filtration membrane retains, make to retain in product and also contain other a large amount of macromolecular substance except containing except albumen, make protein content in trapped fluid extremely low; From technique be, the molecular weight that its ultra-filtration membrane used need retain is 3000 dalton, its membrane pore size is minimum, although this aperture can remove the materials such as the larger protein of molecular weight, but these albumen can bring fouling membrane to cause the decline of membrane flux, general at about 20LMH or below, separation efficiency is extremely low, its industrial application critical constraints.
Chinese patent literature CN102689947A discloses a kind of method adopting level Four membrane concentration soak water of maize, the method passes through backwash, by retain in film filter colloid, microorganism, protein, carbohydrate, molten phosphorus substance, amino acid and micro-wash-out, obtain the corn steep liquor concentrated, so that the processing and utilization that corn steep liquor is follow-up.Above-mentionedly prepare in the process of corn steep liquor, proteolytic enzyme is added in soak water of maize, protein molecule is cut into molecular weight about 30,000 protein, it is the blocking in order to reduce film in several leading level filtration procedure, but the part small molecular protein increased when degrading large molecular weight protein still can affect carrying out smoothly of fourth stage membrane filtration program, the raising of its overall flux is limited, and the corn slurries that aforesaid method obtains are not suitable for the use extracting Phytin, its major cause is, the major protein affecting Phytin purity in actually operating from corn steep liquor during alkali collection Phytin be molecular weight about 30,000 protein, and the protein of the corn steep liquor that aforesaid method obtains exactly containing about 30,000 molecular weight, therefore the corn steep liquor directly using this patented method to produce still does not obtain the higher Phytin product of purity by Silvola recovery.
In sum, if while extracting high purity Phytin, other macromole organic composition farthest can also be extracted and change into corresponding product, not only can realize the comprehensive utilization of resource, increase the new economic benefit of Phytin manufacturing enterprise, meanwhile, become simple terminal and administer as from watershed management, realize the reduction of discharging of pollutent, thus greatly alleviate load and the treatment cost of end contamination improvement.
Summary of the invention
For solving in prior art, due to the problem of the exhaust emission environment of other organic composition in the technique extracting Phytin from soak water of maize, and then a kind of composite technology extracting albumen and Phytin from corn slurries is provided, it, can also the various byproduct such as coproduction albumen and feed while extraction high purity Phytin.
For this reason, the technical scheme that the application takes is:
From corn slurries, extract a composite technology for albumen and Phytin, comprise the steps,
(1) in corn slurries, add proteolytic enzyme carry out enzyme digestion reaction and obtain corn steep liquor enzymolysis solution, wherein, described proteolytic enzyme is acidic incision proteolytic enzyme, the add-on of described proteolytic enzyme is that (u is enzyme activity unit to 5 ~ 500u/g dry, 5 ~ 500u/g represents that the amount adding proteolytic enzyme in every g dry is 5 ~ 500 enzyme activity unit u), temperature of reaction 35 DEG C ~ 55 DEG C, enzymolysis time is 1 ~ 24h;
(2) impurity in described corn steep liquor enzymolysis solution is removed;
(3) the corn steep liquor enzymolysis solution of removing impurity is carried out membrane filtration, obtain trapped fluid and permeate;
(4) in described permeate, calcium salt or calcium hydroxide aqueous solution is added, wherein, in calcium and permeate, the mass ratio of dry-matter is 1:10 ~ 1:40, after using sodium hydroxide solution regulator solution pH value to 6.7 ~ 7.5 again, the filter residue obtained by Plate Filtration is thick Phytin, described thick Phytin obtains required Phytin finished product through refining, oven dry, pulverizing, and sheet frame filtered solution passes through concentrated as feed or fermentation industry raw material;
(5) described trapped fluid is through diafiltration, dry obtained required protein product.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, the hydrolysis degree of high molecular weight protein in corn slurries described in described step (1), to account for the percent basis of protein ingredient total density value in non-enzymolysis stoste in the total density value difference of more than 2kDa protein ingredient before and after enzymolysis according to sodium dodecyl sulfate polyacrylamide gel electrophoresis of protein under reductive condition, when being 2% ~ 50%, stop described enzyme digestion reaction.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, in described step (1), also comprise the step regulating reacting liquid pH value to 3.5-5.0.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, in described step (1), the add-on of described proteolytic enzyme is 10 ~ 200u/g dry, temperature of reaction 45 DEG C ~ 55 DEG C, and enzymolysis time is 2 ~ 12h, and the pH value of reaction solution is 3.8-4.2.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, described step (1) also comprises the step that the enzyme that goes out is lived.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, described corn slurries are soak water of maize or soak water of maize thickened pulp.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, described in described step (3), corn steep liquor enzymolysis solution temperature is 25 ~ 65 DEG C, and pH value is 3.5 ~ 5.0, operating pressure 1 ~ 8Bar.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, the film that membrane filtration described in described step (3) uses for aperture in the ultra-filtration membrane of 20kDa-200kDa or aperture the microfiltration membrane at 20-100nm.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, the film that membrane filtration described in described step (3) uses be tubular membrane, rolled film or flat sheet membrane;
The film that membrane filtration described in described step (3) uses is hollow-fibre membrane, metallic membrane, ceramic membrane, organic membrane, mineral membrane or membrane bioreactor.
Above-mentionedly extract in the composite technology of albumen and Phytin from corn slurries, in described corn slurries, dry matter content is 5-30wt%, pH value 3.5-4.5.
Compared with prior art, the application's tool has the following advantages:
(1) composite technology extracting albumen and Phytin from corn slurries provided by the invention, add acid endo-protease and carry out enzyme digestion reaction under given conditions, thus the specific protein in corn slurries is degraded, when not affecting membrane flux, be extracted the albumen in corn slurries to greatest extent, under the condition not affecting Phytin quality product, other macromole organic composition farthest can also be extracted and change into corresponding product, solve in prior art the pollution reducing film when membrane pore size extracts merely Phytin, or in order to reduce fouling membrane, improve membrane pore size or the simple loss adding the protein ingredient that proteolytic enzyme causes, and the environmental pollution brought thus.
(2) composite technology extracting albumen and Phytin from corn slurries provided by the invention, the hydrolysis degree of high molecular weight protein in described corn slurries after enzymolysis in step (1), to account for the percent basis of protein ingredient total density value in non-enzymolysis stoste in the total density value difference of more than 2kDa protein ingredient before and after enzymolysis according to sodium dodecyl sulfate polyacrylamide gel electrophoresis of protein under reductive condition, described enzyme digestion reaction is stopped when being 2% ~ 50%, thus will the major protein molecular degradation of Phytin recovery purity be affected, not only change bulk of molecule, also can change the original space conformation of protein molecular simultaneously, the surface charge of the protein molecular in corn steep liquor enzymolysis solution and hydrophobic region are changed, thus and reactive force between existing membrane material reduce, and then decrease fouling membrane, improve membrane flux, the composite technology extracting albumen and Phytin from corn slurries provided by the invention, average flux more than 50LMH can be reached within the time that membrane sepn runs two hours or more continuously, substantially increase membrane sepn efficiency.
(3) composite technology extracting albumen and Phytin from corn slurries provided by the invention, the hydrolysis degree of high molecular weight protein in described corn slurries after enzymolysis in step (1), to account for the percent basis of protein ingredient total density value in non-enzymolysis stoste in the total density value difference of more than 2kDa protein ingredient before and after enzymolysis according to sodium dodecyl sulfate polyacrylamide gel electrophoresis of protein under reductive condition, when being 2% ~ 50%, stop described enzyme digestion reaction.Due to the protein in corn steep liquor, based on about 30kDa protein molecular, can precipitate when alkali collection Phytin product thereupon, affect Phytin purity, and this protein part can be degraded at the enzyme of the application, change its pH-solvability, both the blocking of film is avoided in the interaction having decreased itself and film, the molecule avoiding again a small amount of non-tunicle to retain is separated out when alkali collection Phytin, thus improve the purity of Phytin, and the amount that the protein molecular after enzymolysis in corn steep liquor enzymolysis solution carries phytic acid declines, be beneficial to being separated of phytic acid and albumen in subsequent technique, and then after decreasing separation, the phytic acid carried in protein molecular, be extracted the productive rate of Phytin to a certain extent, in the application, Phytin purity reaches more than 80%, yield can reach more than 90%, obviously be better than traditional Phytin extraction process, protein product is containing albumen more than 40%, and while being separated Phytin product, have also obtained the product containing albumen, the composition in this product all derives from corn steep liquor itself, introduces, can be used for animal-feed or other purposes without allogenic material.
(4) composite technology extracting albumen and Phytin from corn slurries provided by the invention, the corn steep liquor extracted after Phytin still can continue concentrated as feed or substratum, and due to the extraction of Phytin, decrease corn steep liquor as phytic acid during feed on zootrophic impact, and the Partial digestion of high molecular weight protein more has and utilizes digesting and assimilating of animal.
(5) composite technology extracting albumen and Phytin from corn slurries provided by the invention, this technique is separated in backward immersion water adds proteolytic enzyme with immersion water completing corn kernel, does not impact albumen in corn kernel.
(6) composite technology extracting albumen and Phytin from corn slurries provided by the invention, this technique does not produce new waste water except a small amount of water used of Membrane cleaning in production process.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the schematic diagram of present invention process flow process;
Fig. 2 is sds polyacrylamide gel electrophoresis of protein analysis chart under the reductive condition that uses the hydrolysis degree analysis of high molecular weight protein in corn steep liquor.
Embodiment
Technique provided by the invention is applicable to all corn steep liquors or soak water of maize, is preferably applicable to corn steep liquor that dry matter content is 5-30wt%, pH value 3.5-4.5 or soak water of maize.
In present invention process, measure product Phytin content assaying method and use " People's Republic of China's chemical industry standard HG2683-95 " to measure phytic acid content, then be scaled Phytin content according to following formula:
Phytin content=C1 × 1.39
In formula, phytic acid mass percentage concentration in C1-product, %;
The mass conversion coefficient of 1.39-Phytin and phytic acid.
In present invention process, the determining the protein quantity method in protein product that measures uses " mensuration of national food safety standard GB5009.5-2010-Protein in Food ", and protein conversion factor is 6.25.
In present invention process, the method for calculation of membrane sepn average flux (J) are as follows:
Wherein, t collects time (unit: second) of permeate, V be within t second, receive permeate rise number, S is the effective filtration area (m of film
2), the unit of J is LMH, namely per membrane area filtration permeate per hour rise number.
Embodiment 1
Getting dry matter content is 10wt%, measured value at pH3.9(23 DEG C ± 2 DEG C) corn steep liquor be raw material, aspartic protease (Sigma is added in the corn steep liquor squeezed in storage tank, aspartic protease P0107Sigma), and by following enzymatic hydrolysis condition enzymolysis: temperature 50 C, pH3.9, enzyme concentration is 200u/g dry, the enzymolysis reaction (now enzymolysis time is 8 hours) when the hydrolysis degree of high molecular weight protein in reaction solution is 20%, the corn steep liquor after enzymolysis is by after the larger solid particle polluter in strainer removing slurry; Re-using film pore footpath is that the ceramic membrane of 100nm filters corn steep liquor enzymolysis solution, wherein, this process feed temperature is 55 DEG C, measured value at pH3.9(23 DEG C ± 2 DEG C), operating pressure 5Bar, time 2h, membrane sepn average flux is 70LMH, and corn steep liquor enzymolysis solution is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%, wherein, the mass ratio of calcium and dry-matter is 1:30.Again by measured value at sodium hydroxide solution adjustment pH to 6.8(23 DEG C ± 2 DEG C of 10%) after, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 83%, yield is 91%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 41% through diafiltration, drying and other steps.
In the present embodiment, the mensuration of hydrolysis degree is realized (shown in Fig. 2) by following methods: left figure is the sds polyacrylamide gel electrophoresis figure of No. 1,2, sample (swimming lane 1,2), and swimming lane 3 is standard molecular weight albumen; Right figure is greater than density value analysis chart corresponding to 2kDa zone of protein in No. 1,2, sample.Interpolation 10%(v/v to preparing) beta-mercaptoethanol enzymolysis before No. 2, sample carries out resolving gel concentration after No. 1, sample and enzymolysis is 15%(w/v) polyacrylamide gel electrophoresis, and use coomassie brilliant blue staining (the left figure of Fig. 2).Use ImageJ software to carry out ribbon density analysis (the right figure of Fig. 2) to the band being greater than 2kDa in gel, the total density value that No. 1, sample is D
1, the total density value that No. 2, sample is D
2, then,
Hydrolysis degree=the 1-D of high molecular weight protein
2/ D
1=20%.
Embodiment 2
Getting dry matter content is 5%, the corn steep liquor of pH value 4.5 is raw material, acidic incision proteolytic enzyme (Wuxi biotechnology company limited of Jie Neng section is added in the corn steep liquor squeezed in storage tank, aspartic protease GC106), and by following enzymatic hydrolysis condition enzymolysis: temperature 35 DEG C, pH4.5, enzyme concentration is 5u/g dry, enzymolysis time is 18h, and now, the hydrolysis degree of high molecular weight protein is 5%.Corn steep liquor after enzymolysis is by after the larger solid particle polluter in strainer removing slurry; The polyvinylidene fluoride flat film re-using molecular weight cut-off 190kDa filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 25 DEG C, and pH is 4.5, operating pressure 2Bar, time 2.5h.Membrane sepn average flux is 55LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:40.Again by after the sodium hydroxide solution adjustment pH to 7.1 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 81%, yield is 92%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 45% through diafiltration, drying and other steps.
Embodiment 3
Getting dry matter content is 30%, the corn steep liquor of pH value 3.5 is raw material, aspartic protease (Su Kehan biotechnology company limited is added in the corn steep liquor squeezed in storage tank, aspartic protease SUKAPro AC), and by following enzymatic hydrolysis condition enzymolysis: temperature 45 C, pH3.5, enzyme concentration is 500u/g dry, enzymolysis time is 10h, and now, the hydrolysis degree of high molecular weight protein is 48%.Corn steep liquor after enzymolysis is by after the larger solid particle polluter in strainer removing slurry; Re-using film pore footpath is that the tube type metal film of 50nm filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 63 DEG C, and pH is 3.5, operating pressure 8Bar, time 2h.Membrane sepn average flux is 50LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:10.Again by after the sodium hydroxide solution adjustment pH to 7.5 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 86%, yield is 95%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 46% through diafiltration, drying and other steps.
Embodiment 4
Getting dry matter content is 12%, the corn steep liquor of pH value 4.0 is raw material, in the corn steep liquor squeezed in storage tank, add a kind of Validase TSP Concentrate II (derive from Validase TSP Concentrate II, Novi letter Neutrase), and by following enzymatic hydrolysis condition enzymolysis: temperature 55 DEG C, uses sodium hydroxide solution to regulate pH to 5.0, enzyme concentration is 50u/g dry, enzymolysis time is 24h, and now, the hydrolysis degree of high molecular weight protein is 3%.Corn steep liquor after enzymolysis is by after the larger solid particle polluter in strainer removing slurry; The polysulfones rolled film re-using molecular weight cut-off 100kDa filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 35 DEG C, and pH is 5.0, operating pressure 3.5Bar, time 2h.Membrane sepn average flux is 60LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:22.Again by after the sodium hydroxide solution adjustment pH to 6.9 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 85%, yield is 92%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 53% through diafiltration, drying and other steps.
Embodiment 5
Getting dry matter content is 12%, the corn steep liquor of pH value 4.0 is raw material, papoid (Jie Woli biological products company limited is added in the corn steep liquor squeezed in storage tank, papoid), and by following enzymatic hydrolysis condition enzymolysis: temperature 45 C, uses sodium hydroxide solution to regulate pH to 5.0, enzyme concentration is 100u/g dry, enzymolysis time is 4h, and now, the hydrolysis degree of high molecular weight protein is 25%.Corn steep liquor after enzymolysis is by after the larger solid mechanical granule foreign in strainer removing slurry; Re-using film pore footpath is that the tube type metal film of 20nm filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 50 DEG C, and pH is 4.0, operating pressure 4Bar, time 2.5h.Membrane sepn average flux is 53LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:20.Again by after the sodium hydroxide solution adjustment pH to 7.1 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 84%, yield is 92%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 48% through diafiltration, drying and other steps
Embodiment 6
Getting dry matter content is 17%, the corn steep liquor of pH value 4.0 is raw material, aspartic protease (Su Kehan biotechnology company limited is added in the corn steep liquor squeezed in storage tank, aspartic protease SUKAPro AC), and by following enzymatic hydrolysis condition enzymolysis: temperature 45 C, uses hydrochloric acid soln to regulate pH to 3.5, enzyme concentration is 100u/g dry, enzymolysis time is 2h, and now, the hydrolysis degree of high molecular weight protein is 10%.Corn steep liquor after enzymolysis by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; The polysulfones flat sheet membrane re-using molecular weight cut-off 20kDa is filtered corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 45 DEG C, and pH is 3.5, operating pressure 4.0Bar, time 3h.Membrane sepn average flux is 51LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:20.Again by after the sodium hydroxide solution adjustment pH to 7.1 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 86%, yield is 92%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 58% through diafiltration, drying and other steps.
Embodiment 7
Getting dry matter content is 10%, the corn steep liquor of pH value 3.8 is raw material, aspartic protease (the biochemical company limited in gold source, Zhengzhou City is added in the corn steep liquor squeezed in storage tank, aspartic protease 537), and by following enzymatic hydrolysis condition enzymolysis: temperature 35 DEG C, pH3.8, enzyme concentration is 10u/g dry, enzymolysis time is 1h, and now, the hydrolysis degree of high molecular weight protein is 2%.Corn steep liquor after enzymolysis by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; Re-using aperture is that the ceramic membrane of 70nm filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 65 DEG C, and pH is 3.8, operating pressure 3.5Bar, time 2h.Membrane sepn average flux is 58LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:30.Again by after the sodium hydroxide solution adjustment pH to 6.7 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 81%, yield is 90%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 44% through diafiltration, drying and other steps.
Embodiment 8
Getting dry matter content is 13%, the corn steep liquor of pH value 4.2 is raw material, aspartic protease (the biochemical company limited in gold source, Zhengzhou City is added in the corn steep liquor squeezed in storage tank, aspartic protease 537), and by following enzymatic hydrolysis condition enzymolysis: temperature 50 C, pH4.2, enzyme concentration is 500u/g dry, enzymolysis time is 12h, and now, the hydrolysis degree of high molecular weight protein is 50%.Corn steep liquor after enzymolysis by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; The polysulfones rolled film re-using molecular weight cut-off 100kDa filters corn steep liquor enzymolysis solution, and wherein, this process operation temperature is 55 DEG C, and pH is 4.2, operating pressure 1.0Bar, time 3h.Membrane sepn average flux is 52LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of the membrane filtration aqua calcis through first adding 10%.Wherein, the mass ratio of calcium and dry-matter is 1:20.Again by after the sodium hydroxide solution adjustment pH to 7.1 of 10%, obtain thick Phytin by Plate Filtration, obtaining through refining, oven dry, pulverising step the Phytin finished product that purity is 85%, yield is 92%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 50% through diafiltration, drying and other steps.
Comparative example 1
Getting dry matter content is 17%, and the corn steep liquor of pH value 4.0 is raw material, and corn steep liquor by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; The polysulfones rolled film re-using molecular weight cut-off 3kDa filters corn steep liquor, and wherein, this process operation temperature is 45 DEG C, and pH is 4.0, operating pressure 4.0Bar, time 0.45h.Membrane sepn average flux is 15LMH.Corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of membrane filtration, through the aqua calcis first adding 10%, after regulating pH to 6.0, obtains thick Phytin by Plate Filtration, through refining, dry, pulverising step obtaining the Phytin finished product that purity is 73%, yield is 80%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 25% through diafiltration, drying and other steps.
In this comparative example; the purity of Phytin product and yield are not high; and the operating time is 0.45h; because when proceeding to this time; the transitory flux of film have dropped the over half of initial flux, necessary stop cleaning, and average flux now only has 15LMH; the feed liquid that the very low very difficult process of flux is relatively large, this also have impact on the production efficiency of Phytin.In addition, the protein product purity obtained is not high yet.
Comparative example 2
Getting dry matter content is 17%, and the corn steep liquor of pH value 4.0 is raw material, adds Sumizyme MP (Novi letter alcalase2.4L) in corn steep liquor.And by following enzymatic hydrolysis condition enzymolysis: temperature 45 C, pH.35, enzyme concentration is 100u/g dry, and enzymolysis time is 2h, and now, the hydrolysis degree of high molecular weight protein is 1%.Corn steep liquor after enzymolysis by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; The polysulfones rolled film re-using molecular weight cut-off 3kDa filters corn steep liquor, and wherein, this process operation temperature is 45 DEG C; pH is 4.0; operating pressure 4.0Bar, time 20min, membrane sepn average flux is 12LMH; the transitory flux of 20min caudacoria drops to original half; need stop cleaning, again film was carried out, for obtaining the product of higher yields to residue feed liquid; need stop cleaning repeatedly to reach more than hundred times, final corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of membrane filtration, through the aqua calcis first adding 10%, after regulating pH to 6.0, obtains thick Phytin by Plate Filtration, through refining, dry, pulverising step obtaining the Phytin finished product that purity is 72%, yield is 81%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 50% through diafiltration, drying and other steps.
In addition; once run no cease turbine sweep clean; then under above-mentioned identical membrane filtration operation condition; after being filled into 1 hour, because the blocked filtration of film stops substantially, a large amount of corn slurries are stored in trapped fluid; the quantity of permeate is little; the purity of its Phytin finished product is 72%, but yield is less than 10%, obtains the butt protein content of protein product also below 10%.
Comparative example 3
Getting dry matter content is 17%, and the corn steep liquor of pH value 4.0 is raw material, adds Sumizyme MP (Novi letter alcalase2.4L) in corn steep liquor.And by following enzymatic hydrolysis condition enzymolysis: temperature 45 C, pH.35, enzyme concentration is 100u/g dry, and enzymolysis time is 2h, and now, the hydrolysis degree of high molecular weight protein is 1%.Corn steep liquor after enzymolysis by the larger solid mechanical granule foreign in strainer removing slurry, and uses aperture to be after the microfiltration membrane equipment of 5 μm removes little suspended particle; The polysulfones rolled film re-using molecular weight cut-off 20kDa filters corn steep liquor, and wherein, this process operation temperature is 45 DEG C; pH is 4.0; operating pressure 4.0Bar, time 30min, membrane sepn average flux is 18LMH; the transitory flux of 30min caudacoria drops to original half; need stop cleaning, again film was carried out, for obtaining the product of higher yields to residue feed liquid; need stop cleaning repeatedly to reach more than 40 times, final corn steep liquor is divided into trapped fluid and permeate two portions.The permeate of membrane filtration, through the aqua calcis first adding 10%, after regulating pH to 6.0, obtains thick Phytin by Plate Filtration, through refining, dry, pulverising step obtaining the Phytin finished product that purity is 71%, yield is 85%.Sheet frame filtered solution concentrates after acid adjustment whitewashes for fiber feedstuff.The trapped fluid of membrane sepn obtains the protein product of butt protein content 50% through diafiltration, drying and other steps.
In addition; once run no cease turbine sweep clean; then under above-mentioned identical membrane filtration operation condition; after being filled into 1 hour, because the blocked filtration of film stops substantially, a large amount of corn slurries are stored in trapped fluid; the quantity of permeate is little; the purity of its Phytin finished product is 72%, but yield is less than 10%, obtains the butt protein content of protein product also below 10%.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (10)
1. from corn slurries, extract a composite technology for albumen and Phytin, comprise the steps,
(1) in corn slurries, add proteolytic enzyme carry out enzyme digestion reaction and obtain corn steep liquor enzymolysis solution, wherein, described proteolytic enzyme is acidic incision proteolytic enzyme, and the add-on of described proteolytic enzyme is 5 ~ 500u/g dry, temperature of reaction 35 DEG C ~ 55 DEG C, and enzymolysis time is 1 ~ 24h;
(2) impurity in described corn steep liquor enzymolysis solution is removed;
(3) the corn steep liquor enzymolysis solution of removing impurity is carried out membrane filtration, obtain trapped fluid and permeate;
(4) in described permeate, calcium salt or calcium hydroxide aqueous solution is added, wherein, in calcium and permeate, the mass ratio of dry-matter is 1:10 ~ 1:40, after using sodium hydroxide solution regulator solution pH value to 6.7 ~ 7.5 again, the filter residue obtained by Plate Filtration is thick Phytin, described thick Phytin obtains required Phytin finished product through refining, oven dry, pulverizing, and sheet frame filtered solution passes through concentrated as feed or fermentation industry raw material;
(5) described trapped fluid is through diafiltration, dry obtained required protein product.
2. the composite technology extracting albumen and Phytin from corn slurries according to claim 1, is characterized in that,
The hydrolysis degree of high molecular weight protein in corn slurries described in described step (1), to account for the percent basis of protein ingredient total density value in non-enzymolysis stoste in the total density value difference of more than 2kDa protein ingredient before and after enzymolysis according to sodium dodecyl sulfate polyacrylamide gel electrophoresis of protein under reductive condition, when being 2% ~ 50%, stop described enzyme digestion reaction.
3. the composite technology extracting albumen and Phytin from corn steep liquor according to claim 1 and 2, is characterized in that,
The step regulating reacting liquid pH value to 3.5-5.0 is also comprised in described step (1).
4. the composite technology extracting albumen and Phytin from corn slurries according to claim 3, is characterized in that,
In described step (1), the add-on of described proteolytic enzyme is 10 ~ 200u/g dry, temperature of reaction 45 DEG C ~ 55 DEG C, and enzymolysis time is 2 ~ 12h, and the pH value of reaction solution is 3.8-4.2.
5. the composite technology extracting albumen and Phytin from corn steep liquor according to claim 4, is characterized in that,
Described step (1) also comprises the step that the enzyme that goes out is lived.
6., according to the arbitrary described composite technology extracting albumen and Phytin from corn steep liquor of claim 1-5, it is characterized in that,
Described corn slurries are soak water of maize or soak water of maize thickened pulp.
7. according to claim 6 is that prepared using membrane technique produces albumen and Phytin technique with corn steep liquor, it is characterized in that,
Described in described step (3), corn steep liquor enzymolysis solution temperature is 25 ~ 65 DEG C, and pH value is 3.5 ~ 5.0, operating pressure 1 ~ 8Bar.
8., according to the arbitrary described composite technology extracting albumen and Phytin from corn steep liquor of claim 1-7, it is characterized in that,
The film that membrane filtration described in described step (3) uses for aperture in the ultra-filtration membrane of 20kDa-200kDa or aperture the microfiltration membrane at 20-100nm.
9. the composite technology extracting albumen and Phytin from corn steep liquor according to claim 8, is characterized in that,
The film that membrane filtration described in described step (3) uses is tubular membrane, rolled film or flat sheet membrane;
The film that membrane filtration described in described step (3) uses is hollow-fibre membrane, metallic membrane, ceramic membrane, organic membrane, mineral membrane or membrane bioreactor.
10. the composite technology extracting albumen and Phytin from corn steep liquor according to claim 9, is characterized in that, in described corn slurries, dry matter content is 5-30wt%, pH value 3.5-4.5.
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