CN116102589A - Method for extracting sodium phytate from corn steep liquor - Google Patents
Method for extracting sodium phytate from corn steep liquor Download PDFInfo
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- CN116102589A CN116102589A CN202211615869.8A CN202211615869A CN116102589A CN 116102589 A CN116102589 A CN 116102589A CN 202211615869 A CN202211615869 A CN 202211615869A CN 116102589 A CN116102589 A CN 116102589A
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- sodium phytate
- corn steep
- steep liquor
- resin column
- phytic acid
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- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 title claims abstract description 77
- 229940083982 sodium phytate Drugs 0.000 title claims abstract description 77
- 240000008042 Zea mays Species 0.000 title claims abstract description 42
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 42
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 42
- 235000005822 corn Nutrition 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 39
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 40
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 38
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 38
- 229940068041 phytic acid Drugs 0.000 claims abstract description 35
- 239000000467 phytic acid Substances 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 33
- 239000012528 membrane Substances 0.000 claims abstract description 30
- 238000002791 soaking Methods 0.000 claims abstract description 16
- 229920002472 Starch Polymers 0.000 claims abstract description 13
- 235000019698 starch Nutrition 0.000 claims abstract description 13
- 239000008107 starch Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 65
- 239000003513 alkali Substances 0.000 claims description 20
- 238000001728 nano-filtration Methods 0.000 claims description 18
- 150000001450 anions Chemical class 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 229920006395 saturated elastomer Polymers 0.000 claims description 13
- 239000003480 eluent Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical group [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000003957 anion exchange resin Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 16
- 238000000926 separation method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 241000196324 Embryophyta Species 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 238000011010 flushing procedure Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- -1 directly neutralize Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- RDOWQLZANAYVLL-UHFFFAOYSA-N phenanthridine Chemical compound C1=CC=C2C3=CC=CC=C3C=NC2=C1 RDOWQLZANAYVLL-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229940049805 hexasodium phytate Drugs 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 238000012696 Interfacial polycondensation Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KETSPIPODMGOEJ-UHFFFAOYSA-B dodecasodium;(2,3,4,5,6-pentaphosphonatooxycyclohexyl) phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OC1C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C1OP([O-])([O-])=O KETSPIPODMGOEJ-UHFFFAOYSA-B 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/117—Esters of phosphoric acids with cycloaliphatic alcohols
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting sodium phytate from corn steep liquor, and belongs to the technical field of sodium phytate extraction. The invention adsorbs corn soaking water phytic acid through one-step method resin, then adopts membrane separation to remove impurities and a chromatographic column to remove impurities, introduces inorganic matters and organic matters into raw corn steep liquor, and ensures that the removal rate of the inorganic matters and the organic matters is over 99 percent, thereby ensuring that the finished product of high-quality sodium phytate is produced in the subsequent process. The corn soaking water which is the production raw material of the invention is a byproduct of a starch plant, is cheap and easy to obtain, and changes waste into valuable. The membrane separation concentration and chromatographic column impurity removal are adopted, the salt and organic matters are thoroughly separated, the product purity is high, and the requirements of high-end clients can be met.
Description
Technical Field
The invention belongs to the technical field of sodium phytate extraction, and particularly relates to a method for extracting sodium phytate from corn steep liquor.
Background
At present, two main processes for producing phytic acid are available, one is to take phenanthridine as a raw material, add the phenanthridine into dilute hydrochloric acid, acid hydrolysis to obtain a mixed solution of phytic acid and calcium chloride, the mixed solution is subjected to cation exchange resin to remove calcium ions to obtain a mixed solution of phytic acid and hydrochloric acid, the mixed solution is subjected to acrylic acid anion resin saturated adsorption, then a large amount of water is used for washing off chloride ions, sodium hydroxide is used for resolving to obtain sodium phytate feed liquid, sodium hydroxide is added into the sodium phytate feed liquid to adjust the pH value, and the feed liquid is concentrated, crystallized and dried to obtain sodium phytate.
The other process is to use phytic acid and sodium hydroxide as raw materials, directly neutralize, concentrate, crystallize and dry to obtain the finished phytic acid.
Disclosure of Invention
The invention aims to provide a method for extracting sodium phytate from corn steep liquor, which is characterized in that corn steep water phytic acid is adsorbed by a one-step method resin, membrane separation and impurity removal and chromatographic column impurity removal are adopted in the follow-up process, and inorganic matters and organic matters are introduced into raw corn steep liquor, so that the removal rate of the inorganic matters and the organic matters is over 99%, and the guarantee is provided for the production of high-quality sodium phytate finished products in the subsequent process.
The invention is realized by the following technical scheme:
a method for extracting sodium phytate from corn steep liquor, the method comprising: adding liquid alkali into the sodium phytate feed liquid, regulating, vacuum concentrating, cooling, centrifuging to obtain crystals, and drying to obtain a sodium phytate finished product.
Preferably, the pH value of the sodium phytate feed liquid is 8-9.
Preferably, the pH value of the sodium phytate feed liquid after the liquid alkali adding adjustment is 12-12.5.
Preferably, after the vacuum concentration, the concentration specific gravity is 1.38 to 1.40.
Preferably, the temperature is not higher than 30-35 ℃ when the temperature is reduced.
Preferably, the drying temperature is 50-80 ℃.
The invention adsorbs corn soaking water phytic acid through one-step method resin, then adopts membrane separation to remove impurities and a chromatographic column to remove impurities, introduces inorganic matters and organic matters into raw corn steep liquor, and ensures that the removal rate of the inorganic matters and the organic matters is over 99 percent, thereby ensuring that the finished product of high-quality sodium phytate is produced in the subsequent process.
Preferably, the preparation method of the sodium phytate feed liquid comprises the following steps:
(1) After the corn soaking water in the starch factory is subjected to sedimentation and impurity removal treatment, the obtained corn soaking liquid primary pulp enters an anion resin column for saturated adsorption, and when the phytic acid content of effluent reaches 80% of the organic phosphorus content of the primary pulp, the adsorption is finished;
(2) Ejecting corn steep liquor primary pulp in the anion resin column of the step (1) by using water, washing the anion resin column by using clear water, and eluting by using alkali liquor to obtain crude sodium phytate feed liquid with pH value not higher than 10;
(3) Decoloring, filtering, concentrating and separating impurities by a chromatographic column, wherein the mass ratio of the crude sodium phytate feed liquid in the step (2) to the active carbon is 1:0.15-0.20 wt%.
Preferably, the anion resin column cyclic saturation adsorption treatment includes: after the anion resin column adsorbs the extracted primary pulp, when the phytic acid content in the effluent liquid is 10wt% of the phytic acid content in the extracted primary pulp, the effluent liquid circularly enters the extracted primary pulp, and the anion resin column circularly performs saturated adsorption until the phytic acid content in the effluent liquid is not less than 80wt% of the phytic acid content in the extracted primary pulp;
the anion resin column is a free amine type acrylic acid anion exchange resin column.
Preferably, in the step (2), the eluent mixture obtained after alkali liquor elution enters a decoloring tank, and activated carbon with the mass ratio of 1:0.15-0.20 wt% is added for decoloring.
Preferably, in the step (3), the filtering is performed by adopting a cloth bag filtering device with the aperture of 2 μm;
the concentration adopts nanofiltration membrane filtration concentration treatment, and the molecular weight cut-off of the membrane is 150-200D.
Nanofiltration membranes have pore diameters above 1nm, typically 1-2nm. Is a functional semipermeable membrane that allows the permeation of solvent molecules or certain low molecular weight solutes or low-valent ions. It is a special and very promising separation membrane variety, it is named because of the size of the trapped substance about nanometers, it traps the molecular weight of the organic matter about 150-500, the ability to trap soluble salt is between 2-98%, desalt the monovalent anion salt solution is lower than the high-valence anion salt solution. Is used for removing organic matters and chromaticity of surface water, removing hardness of groundwater, partially removing soluble salts, concentrating fruit juice, separating useful substances in medicines, and the like. Nanofiltration membranes are mostly composite membranes, and the surface separation layer is composed of polyelectrolyte, so that the nanofiltration membranes have a certain retention rate on inorganic salts. Nanofiltration membranes commercialized abroad mostly compound an ultrathin separation layer with nanoscale pore diameter on a microporous base membrane by an interfacial polycondensation and condensation method. Nanofiltration membranes are capable of trapping nanoscale (0.001 microns) materials. The operation interval of the nanofiltration membrane is between ultrafiltration and reverse osmosis, the molecular weight of the trapped organic matters is about 200-800MW, the capacity of trapping dissolved salts is 20% -98%, the removal rate of soluble monovalent ions is lower than that of high-valence ions, the nanofiltration is generally used for removing organic matters, pigments and hardness and radium in surface water and underground water, and the dissolved salts are partially removed, so that useful substances in food and medicine production are extracted and concentrated. The operating pressure of nanofiltration membranes is generally 3.5-30bar.
The cloth bag filter device is a novel filter system and has the advantages of high filter precision, large treatment capacity, low cost, convenience and rapidness in use and maintenance, complete specification, various materials, wide application range and the like. The method is mainly applied to: food, health, pharmaceutical, etc. The bag filters are divided into single bags and multiple bags according to the number of bags, and are divided into side-inlet type and top-inlet type according to the positions of the feed holes, and the side-inlet type is replaced by the top-inlet type. In addition, an interlayer filter which is generally of a double-layer structure can be provided according to the requirement of the filtering temperature of a user, and steam or heat conducting oil can be introduced into the interlayer to maintain or improve the temperature of fluid, prevent the fluid from solidifying, improve the filtering speed of viscous liquid or meet the requirement of the next working procedure on the temperature.
Compared with the prior art, the invention has at least the following technical effects:
the invention discloses a method for extracting sodium phytate from corn soaking liquid, which is a novel method for preparing sodium phytate by taking corn soaking water as a raw material through a novel method such as saturated adsorption elution, membrane separation concentration, chromatographic separation impurity removal and the like. The method adopts acrylic acid anion resin to adsorb phytic acid in corn soaking liquid in a saturated manner, a certain amount of water is used for washing residual corn soaking water after adsorption is finished, then 5-6% sodium hydroxide is used for desorption to obtain crude sodium phytate feed liquid containing chloride, 0.02% active carbon is added into the crude sodium phytate feed liquid for decoloration and filtration, nanofiltration membrane is used for filtration and concentration of filtrate to obtain feed liquid with the concentration of sodium phytate of more than 12%, chromatographic columns are used for separating the feed liquid, organic and inorganic impurities are removed, pure sodium phytate feed liquid is obtained, pH value of the sodium phytate feed liquid is adjusted to be 12-12.5 by adding liquid alkali, and the feed liquid is concentrated, cooled, crystallized and centrifugally separated to obtain a high-quality sodium phytate finished product.
And secondly, as the phytic acid sodium is produced by using the phytin as a raw material and adopting a multi-step ion exchange process for removing impurities, the acid-base consumption is high, and a large amount of sewage is discharged. The invention adsorbs corn soaking water phytic acid through one-step resin, then adopts membrane separation to remove impurities and a chromatographic column to remove impurities, the removal rate of inorganic matters and organic matters is introduced into raw material corn steep liquor to be over 99 percent, and the invention provides guarantee for the production of high-quality sodium phytate finished products in the subsequent working procedure.
Thirdly, the corn soaking water which is the production raw material of the invention is a byproduct of a starch plant, is cheap and easy to obtain, and changes waste into valuable.
And fourthly, membrane separation concentration and chromatographic column impurity removal are adopted, salt and organic matters are thoroughly separated, the product purity is high, and the requirements of high-end customers can be met.
Drawings
FIG. 1 is a schematic flow chart of a method for extracting sodium phytate in example 1;
fig. 2 is a schematic diagram of a sodium phytate product prepared by the method of example 1.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the following examples, which are to be construed as merely illustrative and not limitative of the scope of the invention, but are not intended to limit the scope of the invention to the specific conditions set forth in the examples, either as conventional or manufacturer-suggested, nor are reagents or apparatus employed to identify manufacturers as conventional products available for commercial purchase.
The technical scheme of a specific implementation mode of the invention is as follows:
a processing method for extracting phytic acid from corn soaking water is characterized by comprising the following steps:
(1) Delivering corn steep liquor discharged from starch production to a settling tank, standing for settling, separating solids such as starch and protein, filtering supernatant by using a bedroom spiral filter, further throttling suspended impurities, delivering filtrate to a polypropylene resin column for adsorbing phytic acid, delivering effluent to the primary pulp settling tank when the phytic acid content of the effluent reaches 10% of that of primary pulp, circularly saturated adsorbing, and delivering the effluent to the primary pulp 80% after saturated adsorbing, wherein the adsorbed corn steep liquor and the separated solids impurities are completely returned to a starch plant for concentrating and utilizing.
(2) And (3) ejecting the primary pulp in the resin column by using water, filtering liquid by using a nanofiltration membrane, and flushing impurities in the resin column by using a small amount of clear water until effluent liquid has no obvious suspended impurities.
(3) Preparing 5-6% diluted alkali liquor for eluting, collecting front-section and middle-section sodium phytate eluates to a decolorizing tank, stopping collecting when the pH value of the eluent mixture reaches 8-9, wherein the collecting liquid is hexasodium phytate or heptasodium phytate. And collecting the eluent at the later stage to an alkali distribution tank for applying the alkali distribution eluent.
(4) After the elution is finished, the resin column is washed by water and a small amount of water, and then a new round of adsorption is carried out.
(5) Adding 0.2% active carbon into the crude phytic acid feed liquid for decoloring, and obtaining clear and transparent crude phytic acid feed liquid through a plate frame.
(6) The plate and frame filtrate is finely filtered by a cloth bag filter.
(7) The crude sodium phytate is filtered and concentrated by using a nanofiltration membrane, the trapped fluid is sodium phytate feed liquid, the filtered fluid contains chloride and small molecular organic matters, and the filtered fluid is used for collecting temporary fluid for flushing the resin column in the step (2) and the step (4).
(8) And separating and removing impurities from the membrane concentrated and trapped about 15% sodium phytate feed liquid by using a chromatographic column to obtain pure sodium phytate feed liquid.
(9) The pH value of the sodium phytate liquid separated by the chromatographic column is 8-9, and the pH value is regulated to 12-12.5 by alkali liquor.
(10) Vacuum concentrating the sodium phytate feed liquid with pH value regulated, controlling concentration end specific gravity to 1.38-1.40, cooling and crystallizing the concentrated paste, discharging and centrifuging at temperature lower than 30-35 deg.C, drying, rinsing with purified water, drying again, and taking out sodium phytate wet crystal.
(11) Drying the wet crystallization at 50-80 ℃, and sieving the dried product to obtain a sodium phytate finished product.
Example 1: the specific flow is shown in figure 1:
a processing method for extracting phytic acid from corn soaking water is characterized by comprising the following steps:
(1) Delivering corn steep liquor discharged from starch production to a settling tank, standing for settling, separating solids such as starch and protein, filtering supernatant by using a bedroom spiral filter, further throttling suspended impurities, delivering filtrate to a polypropylene resin column for adsorbing phytic acid, delivering effluent to the primary pulp settling tank when the phytic acid content of the effluent reaches 10% of that of primary pulp, circularly saturated adsorbing, and delivering the effluent to the primary pulp 80% after saturated adsorbing, wherein the adsorbed corn steep liquor and the separated solids impurities are completely returned to a starch plant for concentrating and utilizing.
(2) And (3) ejecting the primary pulp in the resin column by using water, filtering liquid by using a nanofiltration membrane, and flushing impurities in the resin column by using a small amount of clear water until effluent liquid has no obvious suspended impurities.
(3) Preparing 5-6% diluted alkali liquor for eluting, collecting front-section and middle-section sodium phytate eluates to a decolorizing tank, stopping collecting when the pH value of the eluent mixture reaches 9, wherein the collecting liquid is hexasodium phytate or heptasodium phytate. And collecting the eluent at the later stage to an alkali distribution tank for applying the alkali distribution eluent.
(4) After the elution is finished, the resin column is washed by water and a small amount of water, and then a new round of adsorption is carried out.
(5) Adding 0.2% active carbon into the crude phytic acid feed liquid for decoloring, and obtaining clear and transparent crude phytic acid feed liquid through a plate frame.
(6) The plate and frame filtrate is finely filtered by a cloth bag filter.
(7) The crude sodium phytate is filtered and concentrated by using a nanofiltration membrane, the trapped fluid is sodium phytate feed liquid, the filtered fluid contains chloride and small molecular organic matters, and the filtered fluid is used for collecting temporary fluid for flushing the resin column in the step (2) and the step (4).
(8) And separating and removing impurities from the membrane concentrated and trapped about 15% sodium phytate feed liquid by using a chromatographic column to obtain pure sodium phytate feed liquid.
(9) The pH value of the sodium phytate liquid separated by the chromatographic column is 9, and the pH value is regulated to 12.5 by alkali liquor.
(10) Vacuum concentrating the sodium phytate feed liquid with pH value regulated, controlling concentration end specific gravity to 1.38-1.40, cooling and crystallizing the concentrated paste, discharging and centrifuging at temperature lower than 30 deg.c, spin-drying, eluting with purified water, spin-drying again, and taking out sodium phytate wet crystal.
(11) And drying the wet crystallization at 50 ℃, and sieving the dried product to obtain a sodium phytate finished product.
Example 2:
a processing method for extracting phytic acid from corn soaking water is characterized by comprising the following steps:
(1) Delivering corn steep liquor discharged from starch production to a settling tank, standing for settling, separating solids such as starch and protein, filtering supernatant by using a bedroom spiral filter, further throttling suspended impurities, delivering filtrate to a polypropylene resin column for adsorbing phytic acid, delivering effluent to the primary pulp settling tank when the phytic acid content of the effluent reaches 10% of that of primary pulp, circularly saturated adsorbing, and delivering the effluent to the primary pulp 80% after saturated adsorbing, wherein the adsorbed corn steep liquor and the separated solids impurities are completely returned to a starch plant for concentrating and utilizing.
(2) And (3) ejecting the primary pulp in the resin column by using water, filtering liquid by using a nanofiltration membrane, and flushing impurities in the resin column by using a small amount of clear water until effluent liquid has no obvious suspended impurities.
(3) Preparing 5-6% diluted alkali liquor for eluting, collecting front-section and middle-section sodium phytate eluates to a decolorizing tank, stopping collecting when the pH value of the eluent mixture reaches 8, wherein the collecting liquid is hexasodium phytate or heptasodium phytate. And collecting the eluent at the later stage to an alkali distribution tank for applying the alkali distribution eluent.
(4) After the elution is finished, the resin column is washed by water and a small amount of water, and then a new round of adsorption is carried out.
(5) Adding 0.2% active carbon into the crude phytic acid feed liquid for decoloring, and obtaining clear and transparent crude phytic acid feed liquid through a plate frame.
(6) The plate and frame filtrate is finely filtered by a cloth bag filter.
(7) The crude sodium phytate is filtered and concentrated by using a nanofiltration membrane, the trapped fluid is sodium phytate feed liquid, the filtered fluid contains chloride and small molecular organic matters, and the filtered fluid is used for collecting temporary fluid for flushing the resin column in the step (2) and the step (4).
(8) And separating and removing impurities from the membrane concentrated and trapped about 15% sodium phytate feed liquid by using a chromatographic column to obtain pure sodium phytate feed liquid.
(9) The pH value of the sodium phytate liquid separated by the chromatographic column is 8, and the pH value is regulated to 12 by alkali liquor.
(10) Vacuum concentrating the sodium phytate feed liquid with pH value regulated, controlling concentration end specific gravity to 1.38-1.40, cooling and crystallizing the concentrated paste, discharging and centrifuging at temperature lower than 35 deg.C, drying, rinsing with purified water, drying again, and taking out sodium phytate wet crystal.
(11) And drying the wet crystals at the temperature of 80 ℃, and sieving the dried product to obtain a sodium phytate finished product.
As shown in fig. 2, a sodium phytate sample picture was prepared by the extraction method of example 1.
Experimental example:
sodium phytate samples were prepared in 4 batches using the extraction method of example 1 above. Wherein the samples are respectively batch 1 sample, batch 2 sample, batch 3 sample, and batch 4 sample.
Conclusion: each of the above samples was sodium phytate obtained by the extraction method of example 1, and the samples obtained for different batches were tested, showing that the sodium phytate obtained by the extraction method of example 1 meets the national standard.
Comparative example 1: the nanofiltration membrane filtration concentration treatment in step (7) in the method of example 1 was removed, and the other steps were the same as in example 1.
Comparative example 1 and example 1 obtained sample results: comparative example 1 yielded a sample that was chloride-free.
Comparative example 2: the step (8) column separation and impurity removal treatment in the method of example 1 was omitted, and the other steps were the same as in example 1.
Comparative example 2 and example 1 obtained sample results: the inorganic phosphorus, chloride, sulfate and calcium salt indexes of the produced samples of comparative example 2 are unstable, and part of batches are unqualified.
Comparative example 3: step (7) and step (8) in the method of example 1 were deleted, and the other steps were the same as in example 1.
Comparative example 3 and example 1 obtained sample results: the indexes of inorganic phosphorus, chloride, sulfate and calcium salt of the samples produced in the comparative example 3 are unstable, part of batches are unqualified, organic matters in the feed liquid are separated and removed through the step (7) and the step (8), the crystallization paste obtained in the concentration step is sticky, and the crystallization yield is greatly reduced.
Finally, it should be noted that: the foregoing description is only of the preferred embodiments of the invention and is not intended to limit the scope of the invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for extracting sodium phytate from corn steep liquor, comprising: adding liquid alkali into the sodium phytate feed liquid to adjust the pH value, then carrying out vacuum concentration, cooling and centrifuging to obtain crystals, and drying to obtain a sodium phytate finished product.
2. The method for extracting sodium phytate from corn steep liquor according to claim 1, wherein the pH of the sodium phytate liquor is 8-9.
3. The method for extracting sodium phytate from corn steep liquor according to claim 1, wherein the pH of the sodium phytate liquor after alkali addition adjustment is 12-12.5.
4. The method of claim 1, wherein the concentration ratio is 1.38-1.40 after vacuum concentration.
5. The method of claim 1, wherein the temperature is no higher than 35 ℃.
6. The method of claim 1, wherein the drying temperature is 50-80 ℃.
7. The method for extracting sodium phytate from corn steep liquor according to claim 1, wherein the preparation method of the sodium phytate feed liquor is as follows:
(1) After the corn soaking water in the starch factory is subjected to sedimentation and impurity removal treatment, the obtained corn soaking liquid primary pulp enters an anion resin column for circulating saturated adsorption, and when the phytic acid content of effluent reaches 80% of the organic phosphorus content of the primary pulp, the adsorption is finished;
(2) Ejecting corn steep liquor primary pulp in the anion resin column of the step (1) by using water, washing the anion resin column by using clear water, and eluting by using alkali liquor to obtain crude sodium phytate feed liquid with pH value not higher than 10;
(3) Decoloring, filtering, concentrating and separating impurities by a chromatographic column according to the mass ratio of the crude sodium phytate feed liquid in the step (2) to the active carbon of 1:15wt% -20wt%.
8. The method for extracting sodium phytate from corn steep liquor as claimed in claim 7, wherein the anion resin column circulating saturation adsorption treatment comprises: after the anion resin column adsorbs the extracted primary pulp, when the phytic acid content in the effluent liquid is 10wt% of the phytic acid content in the extracted primary pulp, the effluent liquid circularly enters the extracted primary pulp, and the anion resin column circularly performs saturated adsorption until the phytic acid content in the effluent liquid is not less than 80wt% of the phytic acid content in the extracted primary pulp;
the anion resin column is a free amine type acrylic acid anion exchange resin column.
9. The method for extracting sodium phytate from corn steep liquor as claimed in claim 7, wherein in the step (2), the eluent mixture obtained after the alkaline solution elution is returned to the original eluent for recycling.
10. The method for extracting sodium phytate from corn steep liquor according to claim 7, wherein in the step (3), the fine filtration treatment is carried out by adopting a cloth bag filter with a pore diameter of 2 μm;
the concentration adopts nanofiltration membrane filtration concentration treatment, and the molecular weight cut-off of the membrane is 150-200D.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117448390A (en) * | 2023-12-25 | 2024-01-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117448390A (en) * | 2023-12-25 | 2024-01-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
| CN117448390B (en) * | 2023-12-25 | 2024-03-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
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