CN102010441B - Process of preparing phytic acid/sodium phytate and co-producing corn proteins by using corn as raw material - Google Patents
Process of preparing phytic acid/sodium phytate and co-producing corn proteins by using corn as raw material Download PDFInfo
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Abstract
The invention discloses a process of preparing phytic acid/sodium phytate and co-producing corn proteins by using corn as a raw material, comprising the following steps: directly extracting the phytic acid from a corn soak solution through an ion exchange resin adsorption method, and replacing the precipitating, the filtering and the washing of the calcium phytate with the adsorption and the desorption of the resin, thereby greatly shortening the process and improving the quality. The average yield of the phytic acid can be more than 96%, and the proteins in the extracting process can be precipitated to use as the feed. In addition, the solution after the extracting of the phytic acid is unpolluted and can be used to produce the corn steep liquor. The process provided by the invention has low energy consumption, no environmental pollution, simple process, good production quality and high yield.
Description
Technical field
The present invention relates to a kind of is the technology of feedstock production phytic acid/sodium phytate and coproduction zein with the soak water of maize.
Background technology
Phytic acid (phytic acid) is a kind of organo phosphorous compounds that extensively is present in the plant seed, and chemical name is hexalin six SULPHOSUCCINIC ACID ESTERs, has another name called myo-Inositol hexaphosphate; Chemical formula C6H18P6024, molecular weight 660.08, the faint yellow or tawny thick liquid of outward appearance; Be acid, soluble in water, be insoluble in organic solvents such as alcohol, benzene, chloroform; Exist with the free state form hardly, usually with calcium, magnesium, potassium double salt (Fei Ting, form phytic) is present in kind skin, the plumule place of cereal, oil crops; In rice bran, maize germ wheat bran, cottonseed, Semen Brassicae campestris, wherein phytic acid content is higher in rice bran, maize germ and the wheat bran.
Sodium phytate is the salt derivative of phytic acid; It is except the major applications characteristic with phytic acid; Also wider range of application is arranged than phytic acid; Like conduct: the additive of the special efficacy auxiliary agent of the standard reagent of the fermentation accelerant in the fermentation industry, Biochemical Research and analysis, scavenger specially and daily use chemicals industry (toothpaste, cosmetics) etc.And have transportation, storage, characteristics such as easy to use, therefore more and more receive people's attention.
Phytic acid, unique physiology, pharmacology merit property and the chemical property of sodium phytate make it obtain in fields such as medicine, chemical industry, daily-use chemical industry, light industry, food, health care, metallurgy, plastics, printing, metal finishing, high-grade fruit freshness preserving, lipid-antioxidant activities to use extremely widely.Phytic acid is looked for " natural article " by developed countries such as America and Europe, Japan, Israel at present, classifies the important material product as, and turnout and demand increase year by year.
China is the big country of maize planting, and W-Gum output is considerable.Present at home general wet processes corn, need adopting temperature in the course of processing is that 50 ℃, concentration are the immersion to the peace and quiet about 55h of corn of 0.25% sulfurous sour water.The volume of soaked in water is almost equal with the corn volume that is soaked, and discharges through the back that recycles of certain process.The simplest recoverying and utilizing method of soak water of maize is the raw material that its simmer down to steeping water is made for fermentation industries such as microbiotic and monosodium glutamate.But because W-Gum production increase in recent years is very fast, the outlet of steeping water has also become problem, and particularly the new way of handling soak water of maize must be sought in the relatively more concentrated producing region of W-Gum factory.
Discovering in recent years is that raw material can directly extract phytic acid and sodium phytate with the soak water of maize, and this research provides new method for corn deep processing, is again that the production of phytic acid and sodium phytate has improved new raw material approach simultaneously.Fei Tingfa is mainly adopted in the production of sodium phytate at present, and this method energy consumption is big, and environmental pollution is serious, complex process, and of poor quality, waste material can not fully utilize.
Summary of the invention
To above-mentioned prior art, the invention provides a kind of is the technology of feedstock production phytic acid/sodium phytate and coproduction zein with the soak water of maize, has both improved the purity of phytic acid, sodium phytate, has reclaimed the albumen sub product simultaneously again.
The present invention realizes through following technical scheme:
A kind of is the technology of feedstock production phytic acid/sodium phytate and coproduction zein with the corn, may further comprise the steps:
(1) corn steeping water pretreatment: in water, 0.2% the zeyssatite that adds corn weight is to remove soluble protein and starch with corn soaking; Boil 3～5min, make residual SO
2Be heated the volatilization and remove, materials such as protein are separated out by thermocoagulation, suction filtration, cleaner liquid; At this moment, the phytin double salt in the cleaner liquid is present in the cleaner liquid with the form of phytin hydrogen salt;
(2) decolouring: above-mentioned cleaner liquid, with gac decolouring 40min under 75～80 ℃ of 1% (M/V), suction filtration must be filtrated.To filtrate in 40～50 ℃, be evaporated to 20% of original volume under the condition of vacuum tightness 0.02～0.2MPa, get liquid concentrator;
(3) cross positive resin column (Z type): the liquid concentrator in the step (2), cross post with the speed of 2～4BV/h, purpose is that the cation replacements such as calcium magnesium in the solution are come out; Prevent when crossing negative resin, to generate calcium hydroxide; Depositions such as Marinco H are stopped up the resin space, and experiment can't be carried out; Make phytin hydrogen salt change into phytic acid simultaneously, prevent in the process of precipitating proteins, to cause the loss of phytic acid.In this process, need to remove more completely the positively charged ions such as calcium magnesium in the phytic acid acid salt solution, 2～3 the positive resin columns of generally will connecting; After crossing positive resin column, gained solution is carried out the mensuration of calcium ions and magnesium ions, calcium ions and magnesium ions carries out subsequent processing after reaching controlling index;
(4) secondary decolourization: behind the positive resin of above-mentioned mistake, add the gac of 1.0% (M/V) in the gained solution, suction filtration gets secondary decolourization filtrating;
(5) regulate pH: with the above-mentioned secondary decolourization filtrating that obtains, regulate pH value to 6～8, suction filtration, the gained filter residue is zein, and gained filtrating is the thick solution of sodium phytate;
(6) concentrate: gained in the step (5) is filtrated at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is 18～25mg/mL, gets concentrated filtrate;
(7) cross positive resin (Z type): purpose is to regulate pH value to 2～3 of above-mentioned concentrated filtrate, and phytic acid and phytate are adsorbed in following negative resin adsorption process fully;
(8) cross negative resin post (Z type): the concentrated filtrate after step (7) is handled is crossed post with the speed of 2～4BV/h, and in this process, phytic acid is attracted on the negative resin; After crossing post; Washing earlier to be to remove the impurity such as protein of resin surface, and using massfraction then is that 0.3% sodium hydroxide solution prewashing is removed pigment and is soluble in the impurity of diluted alkaline, and using massfraction again is 0.6% sodium hydroxide solution wash-out; Fraction collection; Get sodium phytate solution, concentrated, dry, promptly obtain the finished product sodium phytate.
Further comprising the steps of: cationic exchange coloum (Z type) is crossed with the gained sodium phytate solution in (9), promptly gets plant acid solution.
In the said step (3), confirm controlling index that calcium ions and magnesium ions will reach according to water hardness, for: less than 25 degree.
Regulating the used solution of pH in the said step (5) is sodium hydroxide solution.
In the above-mentioned technology, the method for the concentration of mensuration phytic acid or sodium phytate is following: adopt thorium nitrate 99.99004323A8urity titration measuring phytic acid content: get quantity of sample and add in the Erlenmeyer flask, inwardly add 30～50mL zero(ppm) water, use 0.3moL/L HNO again
3Regulate between pH value to 1.9～2.2, solution is heated to 60 ℃, add 1 0.5% xylenol orange indicator, use the thorium nitrate 99.99004323A8urity titration fast, become pink and 30s to solution by yellow and do not fade and be terminal point.The calculation formula of phytic acid content is:
Phytic acid content=0.33mV/w
In the formula, m-thorium nitrate 99.99004323A8urity solution quality concentration, mg/mL; The volume of V-thorium nitrate 99.99004323A8urity solution consumption, mL; The w-sample quality, g; 0.33-the mass conversion coefficient of phytic acid and thorium nitrate 99.99004323A8urity.
After utilizing prepared of the present invention to obtain plant acid solution, sodium phytate solution; Crystallization can be adopted following method: respectively with plant acid solution, sodium phytate solution at 40～60 ℃; Concentrating under reduced pressure under the condition of vacuum tightness 0.02～0.2MPa; Obtain certain density plant acid solution, simultaneously sodium phytate solution is continued to be concentrated into the adularescent deposition and occur, be transferred in the dry good small beaker in 0～4 ℃ of following low temperature crystallization.Centrifugal: use whizzer, spinning 5min under 5000rpm, drying obtains sodium phytate finished product purity 99.53%, and the phytic acid recovery reaches more than 85%.
Technology of the present invention transfers the pH to 7.23 of solution because after corn steeping water has been crossed once positive resin, when having reclaimed zein, improved the purity of phytic acid, sodium phytate greatly.The phytic acid of producing is an off-white powder for extremely flaxen phytic acid, sodium phytate.Improved the quality of phytic acid, sodium phytate greatly.
The present invention adopts the ion exchange resin absorption method directly from soak water of maize, to extract phytic acid; Removed the process of phytic acid ca deposition, filtration and washing; Become the absorption of resin and resolve additive process, flow process shortens greatly, and quality improves greatly; The average yield of phytic acid can reach more than 96%, and can precipitate protein in the leaching process as the usefulness of feed.In addition, the solution behind the extraction phytic acid is not contaminated, still can be used to produce steeping water.Technology energy consumption of the present invention is low, non-environmental-pollution, and technology is simple, and the products obtained therefrom quality is good, and productive rate is high.
The present invention is a raw material with corn steeping water; Preparation phytic acid, sodium phytate reclaimed zein simultaneously, improved the purity of phytic acid, sodium phytate; If will realize industrialized production; To be expected to enlarge our company's corn deep processing industrial chain, improve the added value that company's W-Gum is produced, bring bigger economic benefit and social benefit.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
Get 2000mL corn water, add 5% chitosan 100ml, in 50 ℃ of flocculation 30min.The gac of adding 1.5% is in 80 ℃ of 30min that decolour down, and suction filtration must be filtrated, and filtrating is concentrated into volume 560mL, solid substance 35.3%, phytic acid content 42.69mg/mL.Cross the D301 Zeo-karb, add 1.5% activated carbon decolorizing, be concentrated into 368mL; Solid content 20.8% is got this solution of 166mL, and the sodium hydroxide solution with 30% is transferred pH to 7.21; Stir 20min, suction filtration carries out solid-liquid separation, and phytic acid content is 19.50mL thorium nitrate 99.99004323A8urity/mL filtrating in the gained filtrating; Solid substance is 21.8%, and filtrating is at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is to cross Zeo-karb behind 18～25mg/mL.Filtrating is diluted to 500mL, crosses negative resin (negative resin 250mL humid volume decolours No. 2), washing is used 0.3% sodium hydroxide 500mL wash-out removal of impurities, 0.6% sodium hydroxide 1000mL wash-out again.Fraction collection, the purity that obtains sodium phytate are up to 99.53%, and the recovery of phytic acid reaches more than 85%, and protein recovery is up to 95%.
Embodiment 2:
Get 2000mL corn water, add 5% chitosan 100ml, in 50 ℃ of flocculation 30min.The gac of adding 1.5% is in 80 ℃ of 30min that decolour down, and suction filtration must be filtrated, and filtrating is concentrated into volume 560mL, solid substance 35.3%, phytic acid content 42.69mg/mL.Cross the D301 Zeo-karb, add 1.5% activated carbon decolorizing, be concentrated into 368mL; Solid content 20.8% is got this solution of 166mL, and the sodium hydroxide solution with 30% is transferred pH to 7.21; Stir 20min, suction filtration carries out solid-liquid separation, and phytic acid content is 19.50mL thorium nitrate 99.99004323A8urity/mL filtrating in the gained filtrating; Solid substance is 21.8%, and filtrating is at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is to cross Zeo-karb behind 18～25mg/mL.Filtrating is diluted to 500mL, crosses negative resin (Zhejiang win honour for D301 negative resin 250mL humid volume), washing is used 0.3% sodium hydroxide 500mL wash-out removal of impurities, 0.6% sodium hydroxide 1000mL wash-out again.Fraction collection, the purity that obtains sodium phytate are up to 93.65%, and the recovery of phytic acid reaches 73%, and protein recovery is up to 95%.
Embodiment 3:
Get 2000mL corn water, add 5% chitosan 100ml, in 50 ℃ of flocculation 30min.The gac of adding 1.5% is in 80 ℃ of 30min that decolour down, and suction filtration must be filtrated, and filtrating is concentrated into volume 560mL, solid substance 35.3%, phytic acid content 42.69mg/mL.Cross the D301 Zeo-karb, add 1.5% activated carbon decolorizing, be concentrated into 368mL; Solid content 20.8% is got this solution of 166mL, and the sodium hydroxide solution with 30% is transferred pH to 7.21; Stir 20min, suction filtration carries out solid-liquid separation, and phytic acid content is 19.50mL thorium nitrate 99.99004323A8urity/mL filtrating in the gained filtrating; Solid substance is 21.8%, and filtrating is at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is to cross Zeo-karb behind 18～25mg/mL.Filtrating is diluted to 500mL, crosses negative resin (negative resin 250mL humid volume decolours No. 1), washing is used 0.3% sodium hydroxide 500mL wash-out removal of impurities, 0.6% sodium hydroxide 1000mL wash-out again.Fraction collection, the purity that obtains sodium phytate are up to 87%, and the recovery of phytic acid reaches 69.7%, and protein recovery is up to 95%.
Claims (3)
1. one kind is the technology of feedstock production sodium phytate and coproduction zein with the corn, it is characterized in that, may further comprise the steps: (1) corn steeping water pretreatment: with corn soaking in water; 0.2% the zeyssatite that adds corn weight; Boil 3 ~ 5min, suction filtration gets cleaner liquid; At this moment, the phytin double salt in the cleaner liquid is present in the cleaner liquid with the form of phytin hydrogen salt;
(2) decolouring: above-mentioned cleaner liquid, the gac with 1% is in 75～80 ℃ of 40min that decolour down, and suction filtration must be filtrated, and will filtrate then in 40～50 ℃, is evaporated to 20% of original volume under the condition of vacuum tightness 0.02～0.2MPa, gets liquid concentrator;
(3) cross positive resin column: the above-mentioned liquid concentrator that obtains, cross post with the speed of 2～4BV/h, the cation replacement in the solution is come out; After crossing positive resin column, gained solution is carried out the mensuration of calcium ions and magnesium ions, calcium ions and magnesium ions carries out subsequent processing after reaching controlling index; Confirm controlling index that calcium ions and magnesium ions will reach according to water hardness, for: less than 25 degree;
(4) secondary decolourization: the gac of adding 1.0% in the gained solution behind the positive resin of above-mentioned mistake, suction filtration gets secondary decolourization filtrating;
(5) regulate pH: with the above-mentioned secondary decolourization filtrating that obtains, regulate pH value to 6～8, suction filtration, the gained filter residue is zein, and gained filtrating is the thick solution of sodium phytate;
(6) concentrate: gained in the step (5) is filtrated at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is 18～25mg/mL, gets concentrated filtrate;
(7) cross positive resin: purpose is to regulate pH value to 2 ~ 3 of above-mentioned concentrated filtrate;
(8) cross the negative resin post: the concentrated filtrate after step (7) is handled is crossed post with the speed of 2～4BV/h, and in this process, phytic acid is attracted on the negative resin; After crossing post, 0.3% sodium hydroxide solution prewashing is used in washing then earlier, uses 0.6% sodium hydroxide solution wash-out again, and fraction collection gets sodium phytate solution, and is concentrated, dry, promptly obtains the finished product sodium phytate.
2. one kind is the technology of feedstock production phytic acid/sodium phytate and coproduction zein with the corn, it is characterized in that: may further comprise the steps:
(1) corn steeping water pretreatment: corn soaking in water, is added 0.2% zeyssatite of corn weight, boils 3 ~ 5min, suction filtration, cleaner liquid; At this moment, the phytin double salt in the cleaner liquid is present in the cleaner liquid with the form of phytin hydrogen salt;
(2) decolouring: above-mentioned cleaner liquid, the gac with 1% is in 75～80 ℃ of 40min that decolour down, and suction filtration must be filtrated, and will filtrate then in 40～50 ℃, is evaporated to 20% of original volume under the condition of vacuum tightness 0.02～0.2MPa, gets liquid concentrator;
(3) cross positive resin column: the above-mentioned liquid concentrator that obtains, cross post with the speed of 2～4BV/h, the cation replacement in the solution is come out; After crossing positive resin column, gained solution is carried out the mensuration of calcium ions and magnesium ions, calcium ions and magnesium ions carries out subsequent processing after reaching controlling index; Confirm controlling index that calcium ions and magnesium ions will reach according to water hardness, for: less than 25 degree;
(4) secondary decolourization: the gac of adding 1.0% in the gained solution behind the positive resin of above-mentioned mistake, suction filtration gets secondary decolourization filtrating;
(5) regulate pH: with the above-mentioned secondary decolourization filtrating that obtains, regulate pH value to 6～8, suction filtration, the gained filter residue is zein, and gained filtrating is the thick solution of sodium phytate;
(6) concentrate: gained in the step (5) is filtrated at 40～60 ℃, and being evaporated to phytic acid concentration under the condition of vacuum tightness 0.02～0.2MPa is 18～25mg/mL, gets concentrated filtrate;
(7) cross positive resin: purpose is to regulate pH value to 2 ~ 3 of above-mentioned concentrated filtrate;
(8) cross the negative resin post: the concentrated filtrate after step (7) is handled is crossed post with the speed of 2～4BV/h, and in this process, phytic acid is attracted on the negative resin; After crossing post, 0.3% sodium hydroxide solution prewashing is used in washing then earlier, uses 0.6% sodium hydroxide solution wash-out again, and fraction collection gets sodium phytate solution, and is concentrated, dry, obtains the finished product sodium phytate;
(9) the gained sodium phytate solution is crossed cationic exchange coloum, promptly get plant acid solution.
3. according to claim 1 is the technology of feedstock production sodium phytate and coproduction zein with the corn, it is characterized in that: regulating the used solution of pH in the said step (5) is sodium hydroxide solution.
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| CN102746332B (en) * | 2012-07-19 | 2015-12-09 | 中粮生物化学（安徽）股份有限公司 | A kind of method of corn soaking water extraction Phytin |
| CN105001257A (en) * | 2015-06-03 | 2015-10-28 | 山东大宗生物开发股份有限公司 | Method for extracting calcium-magnesium phytate from corn soaked liquid |
| CN106616347A (en) * | 2016-11-19 | 2017-05-10 | 陈桂龙 | Comprehensive utilization method for corn germs |
| CN109170220A (en) * | 2018-11-06 | 2019-01-11 | 赵琪 | A kind of curing method of corn pulp |
| CN110483240A (en) * | 2019-08-02 | 2019-11-22 | 潍坊盛泰药业有限公司 | A kind of soak water of maize method of comprehensive utilization |
| CN113861236B (en) * | 2021-10-18 | 2023-09-05 | 山东寿光巨能金玉米开发有限公司 | Method for preparing calcium phytate by purifying phytic acid |
| CN114195292B (en) * | 2021-12-16 | 2023-08-25 | 山东省鲁洲食品集团有限公司 | Method for removing phosphorus from starch sugar rabbet sewage |
| CN114031058B (en) * | 2021-12-22 | 2023-09-12 | 诸城市浩天药业有限公司 | Method for producing inositol and potassium dihydrogen phosphate by adopting corn steep liquor and produced inositol and potassium dihydrogen phosphate |
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| CN101638436A (en) * | 2009-09-07 | 2010-02-03 | 山东龙力生物科技股份有限公司 | Extracted corn protein and production method thereof |
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| CN101638436A (en) * | 2009-09-07 | 2010-02-03 | 山东龙力生物科技股份有限公司 | Extracted corn protein and production method thereof |
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