CN115160108B - Process for preparing inositol and phosphoric acid - Google Patents
Process for preparing inositol and phosphoric acid Download PDFInfo
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- CN115160108B CN115160108B CN202211081319.2A CN202211081319A CN115160108B CN 115160108 B CN115160108 B CN 115160108B CN 202211081319 A CN202211081319 A CN 202211081319A CN 115160108 B CN115160108 B CN 115160108B
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- inositol
- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 100
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 50
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 title claims abstract description 47
- 229960000367 inositol Drugs 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 75
- 229920005989 resin Polymers 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 50
- 238000001914 filtration Methods 0.000 claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 35
- 239000012528 membrane Substances 0.000 claims abstract description 30
- 238000001728 nano-filtration Methods 0.000 claims abstract description 30
- 239000000706 filtrate Substances 0.000 claims abstract description 27
- 239000000047 product Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000008213 purified water Substances 0.000 claims abstract description 21
- 150000001450 anions Chemical class 0.000 claims abstract description 19
- 239000012466 permeate Substances 0.000 claims abstract description 18
- 239000006228 supernatant Substances 0.000 claims abstract description 18
- 239000012530 fluid Substances 0.000 claims abstract description 16
- 240000008042 Zea mays Species 0.000 claims abstract description 11
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 11
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 11
- 150000001768 cations Chemical class 0.000 claims abstract description 11
- 235000005822 corn Nutrition 0.000 claims abstract description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 16
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000004925 Acrylic resin Substances 0.000 claims description 7
- 229920000178 Acrylic resin Polymers 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 7
- 229920001429 chelating resin Polymers 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000012465 retentate Substances 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- 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 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 239000007787 solid Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 11
- 239000012065 filter cake Substances 0.000 description 10
- 125000002091 cationic group Chemical group 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000002585 base Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000002386 leaching Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 4
- 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 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 235000002949 phytic acid Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 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 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000467 phytic acid Substances 0.000 description 2
- 229940068041 phytic acid Drugs 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/185—Preparation neither from elemental phosphorus or phosphoric anhydride nor by reacting phosphate-containing material with an acid, e.g. by reacting phosphate-containing material with an ion-exchange resin or an acid salt used alone
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of inositol and byproduct production, in particular to a process method for preparing inositol and phosphoric acid, which comprises the following steps: (1) Taking supernatant obtained after standing and settling corn soaking water, and passing through an anion resin column; (2) Washing the resin column with purified water in countercurrent, washing with hydrochloric acid solution, and collecting effluent liquid; (3) Concentrating the effluent by using a nanofiltration membrane, and respectively collecting the trapped fluid and the permeate; (4) Taking trapped fluid to enter a cation resin column, and collecting effluent for later use; (5) Taking effluent, hydrolyzing, filtering, and collecting filtrate for later use; (6) Filtering the filtrate with nanofiltration membrane, and separating the collected permeate with simulated moving bed system to obtain phosphoric acid phase and inositol phase; decolorizing, filtering and concentrating the phosphoric acid phase to obtain a phosphoric acid product; and (3) concentrating, crystallizing and recrystallizing the inositol phase to obtain an inositol finished product. The inositol product and the phosphoric acid product with high quality can be obtained by adopting the process method.
Description
Technical Field
The invention relates to the technical field of inositol and byproduct production, in particular to a process method for preparing inositol and phosphoric acid.
Background
The prior art is that corn steep water passes through a weak alkaline ion exchange resin column, phytic acid in the corn steep water is adsorbed and then desorbed by using hydrochloric acid or a chloride salt solution as a desorbent, collected desorption liquid is subjected to ultrafiltration membrane filtration and nanofiltration membrane concentration to obtain phytic acid (neutralized by alkali substances) or a phytate solution, and then hydrolysis is carried out to obtain a mixed solution of inositol and phosphate. Although phosphate as a byproduct brings economic benefits to enterprises, the economic value is not high, the process difference of different salts is large, a large amount of solid materials need to be treated in the preparation process, dust pollution and inositol loss are easily caused, and three wastes are generated. Therefore, in order to solve the above problems, a process for preparing inositol and phosphoric acid is researched and researched.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the process method for preparing the inositol and the phosphoric acid is provided, the inositol and the phosphoric acid by-products can be obtained simultaneously by utilizing the production process, the benefit is increased for enterprises, and the inositol phase and the phosphoric acid phase can be better separated by adopting the simulated moving bed separation.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a process for the preparation of inositol and phosphoric acid, said process comprising the steps of:
(1) Taking supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anion resin column in a countercurrent manner, and collecting effluent liquid and returning the effluent liquid to a starch factory;
(2) Counter-current washing the anion resin column in the step (1) by purified water until the protein content in effluent water is less than 0.05w/v%, then forward washing the anion resin column by 5wt% hydrochloric acid solution, and collecting effluent liquid for later use;
(3) Concentrating the effluent liquid collected in the step (2) by adopting a nanofiltration membrane, and respectively collecting trapped fluid and permeate liquid; then, thoroughly washing the collected trapped fluid by pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the trapped liquid for standby in the step (3), enabling the trapped liquid to flow into a cation resin column positively, and collecting effluent liquid for standby;
(5) Hydrolyzing the effluent liquid collected in the step (4) at 160-190 ℃ under 0.6-0.8Mpa for 9-11h, filtering, and collecting filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by adopting a nanofiltration membrane, washing the nanofiltration membrane by adopting purified water, returning the collected trapped fluid to the step (5) for continuous hydrolysis, and separating the collected permeate by adopting a simulated moving bed system to obtain a phosphoric acid phase and an inositol phase; decolorizing, filtering and concentrating the phosphoric acid phase to obtain a phosphoric acid product; and (3) concentrating, crystallizing and recrystallizing the inositol phase to obtain an inositol finished product.
As an improved technical scheme, the filler in the anion resin column in the step (1) is gel type weak base acrylic resin LKA98.
As an improved technical scheme, the supernatant in the step (1) enters a resin column according to the flow rate of 1.0-1.5 BV/h.
As an improved technical scheme, the purified water in the step (2) enters a resin column at the flow rate of 2-4 BV/h; the dosage of the hydrochloric acid is 1.4-1.6BV of resin volume, and the hydrochloric acid enters the resin column at the flow rate of 0.3-0.6 BV/h.
As an improved technical scheme, the trapped fluid collected in the step (4) flows into the resin column according to the inflow of 0.5-0.8BV/h.
As an improved technical proposal, the filler in the cation resin in the step (4) is strong acid cation chelating resin ZGD851.
As an improved technical scheme, the molecular weight cut-off of the nanofiltration membrane in the step (3) and the nanofiltration membrane in the step (6) is 500 daltons.
As an improved technical scheme, when the simulated moving bed system is adopted in the step (4) for separation, the filler in the chromatogram is ZGSPC106Ca resin, the mobile phase is deionized water, the pressure is 0-0.6Mpa, the separation temperature is 22-55 ℃, the feeding flow is 20-50L/h, the flow of the mobile phase is 100-160L/h, and the valve switching time is 4-8min.
After the technical scheme is adopted, the invention has the beneficial effects that:
the method comprises the steps of enabling supernatant after standing and settling corn soaking water to pass through an anion resin column, flushing the resin column with a purified aqueous solution, flushing the resin column with a hydrochloric acid solution, concentrating collected effluent liquid through a nanofiltration membrane, enabling trapped fluid collected after the purified water is thoroughly washed to enter a cation resin column, adsorbing calcium and magnesium ions through the cation resin column, hydrolyzing the effluent liquid collected after the column is passed, filtering the filtrate collected after the column is filtered, continuously filtering the filtrate through the nanofiltration membrane, thoroughly washing the purified water, returning the collected trapped fluid to hydrolysis, combining the collected permeate liquid and the thoroughly washed water, and separating through a simulated moving bed separation system (a filler in a chromatogram is gel-type strong-acid cation exchange resin, a mobile phase is purified water, the pressure is 0.1-0.35Mpa, the separation temperature is 22-55 ℃, the feeding flow is 20-50L/h, the flow rate of the entering the mobile phase is 100-160L/h, and the valve switching time is 4-8 min), obtaining a muscle alcohol phase and a phosphoric acid phase after separation, and decolorizing, filtering and concentrating the collected phosphoric acid phase to obtain a phosphoric acid product; concentrating, crystallizing and recrystallizing the collected inositol phase to obtain an inositol product; the method can obtain high-quality inositol products and phosphoric acid products, meet the requirements of customers on different products, increase the product types and benefits of enterprises, avoid resource waste and reduce environmental pollution; the whole process method does not generate three wastes, and increases economic benefits for enterprises.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The moving bed in the simulated moving bed separation system comprises 6 chromatographic columns which are sequentially connected in series end to end, the total area is divided into 4 areas, one column is arranged in a Z1 area, two columns are arranged in a Z2 area, two columns are arranged in a Z3 area, one column is arranged in a Z4 area, the packing in the chromatogram is ZGSPC106Ca resin, the mobile phase is purified water, the pressure is 0.1-0.35Mpa, the separation temperature is 22-55 ℃, the feeding flow is 20-50L/h, the inflow mobile phase flow is 100-160L/h, and the valve switching time is 4-8min.
Example 1
A process for the preparation of inositol and phosphoric acid comprising the steps of:
(1) Taking 46L of supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anion resin column of 4L of resin filler (gel type weak base acrylic resin LKA 98) in a countercurrent manner at the flow rate of 1.0BV/h, and returning effluent liquid to a starch factory after collecting the effluent liquid;
(2) Washing the anion resin column in the step (2) by purified water in a countercurrent way at the flow rate of 2BV/h until the protein content in effluent water is less than 0.05w/v%, washing the resin column by a resin volume of 1.4BV and a 5wt% hydrochloric acid solution in a positive flow way at 0.3BV/h, and collecting 6L effluent liquid for later use;
(3) Concentrating the effluent collected in the step (2) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), and respectively collecting 1.6L of cut-off liquid and 4.4L of permeate (hydrochloric acid solution for preparing the next batch of washing resin columns); then, thoroughly washing the collected trapped fluid by using pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the retentate reserved in the step (3), positively flowing into a cationic resin column (the filler is strongly acidic cationic chelating resin ZGD 851) at a flow rate of 0.5BV/h, and collecting the effluent for later use;
(5) Transferring the effluent liquid collected in the step (4) into an enamel pressure kettle, hydrolyzing for 9 hours at 160 ℃ and under 0.6Mpa, and filtering to collect filtrate for later use;
(6) Taking the filtrate obtained in the step (5), filtering by adopting a nanofiltration membrane (with the molecular weight cutoff being 500 daltons), then flushing the nanofiltration membrane by adopting purified water (until the solid content of the permeate is measured by a refractometer), returning 0.6L of the collected retentate to the step (5) for continuous hydrolysis, and separating 2.0L of the collected permeate by adopting a simulated moving bed system (the filler in the chromatogram is ZGSPC106Ca resin), wherein the mobile phase is deionized water, the pressure is 0.1MPa, the separation temperature is 22 ℃, the feed flow is 20L/h, the flow of the mobile phase is 100L/h, and the valve switching time is 4 min) to obtain a phosphoric acid phase and an inositol phase; decolorizing the phosphoric acid phase (adding 5 ‰ of active carbon), filtering, and concentrating to obtain phosphoric acid product; heating and concentrating inositol phase to solid content of 50 w/w, maintaining the temperature to 95-100 deg.C, adding medical active carbon with dry weight of 2% to the inositol phase (specifically, inositol phase is heated and concentrated to solid content of 50 w/w), maintaining the temperature, stirring, decolorizing for 0.5 hr, maintaining the temperature, filtering, and removing active carbon. And (3) raising the temperature of the filtrate to 100 ℃ for full dissolution, cooling to 28-32 ℃ for filtration, compacting the filter cake, filtering without water drops, leaching the filter cake with a small amount of normal temperature water, and drying to obtain the inositol finished product.
Example 2
A process for the preparation of inositol and phosphoric acid comprising the steps of:
(1) Taking 46L of supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anion resin column of 4L of resin filler (gel type weak base acrylic resin LKA 98) in a countercurrent manner at the flow rate of 1.2BV/h, and returning effluent liquid to a starch factory after collecting the effluent liquid;
(2) Counter-current washing the anion resin column in the step (2) by purified water according to the flow rate of 2-4BV/h until the protein content in effluent water is less than 0.05w/v%, then washing the resin column by resin volume of 1.45BV and 5wt% hydrochloric acid solution according to the positive current of 0.4BV/h, and collecting effluent liquid of 6L for later use;
(3) Concentrating the effluent collected in the step (2) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), and respectively collecting 1.6L of cut-off liquid and 4.4L of permeate (hydrochloric acid solution for preparing the next batch of washing resin columns); then, thoroughly washing the collected trapped fluid by pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the retentate reserved in the step (3), positively flowing into a cationic resin column (the filler is strongly acidic cationic chelating resin ZGD 851) at a flow rate of 0.6BV/h, and collecting the effluent for later use;
(5) Transferring the effluent liquid collected in the step (4) into an enamel pressure kettle, hydrolyzing for 9.5h at 170 ℃ and 0.65Mpa, and filtering to collect filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), washing the nanofiltration membrane by using purified water (the solid content of the filtrate is measured by a refractometer to be 0 percent), returning 0.6L of the collected cut-off to the step (5) for continuous hydrolysis, and separating 2.0L of the collected permeate by using a simulated moving bed system (the filler in the chromatogram is ZGSPC106Ca resin), wherein the mobile phase is deionized water, the pressure is 0.15MPa, the separation temperature is 30 ℃, the feed flow rate is 28L/h, the flow phase flow rate is 115L/h, and the valve switching time is 5 min) to obtain a phosphoric acid phase and an inositol phase; decolorizing the phosphoric acid phase (adding 5 ‰ of active carbon based on phosphoric acid phase weight), filtering, and concentrating to obtain phosphoric acid product; heating and concentrating inositol phase to solid content of 50 w/w, maintaining the temperature to 95-100 deg.C, adding medical active carbon with dry weight of 2% to the inositol phase (specifically, inositol phase is heated and concentrated to solid content of 50 w/w), maintaining the temperature, stirring, decolorizing for 0.5 hr, maintaining the temperature, filtering, and removing active carbon. And (3) raising the temperature of the filtrate to 100 ℃, fully dissolving, cooling to 28-32 ℃, filtering, compacting the filter cake, filtering without water drops, leaching the filter cake with a small amount of normal-temperature water, and drying to obtain the inositol finished product.
Example 3
A process for the preparation of inositol and phosphoric acid comprising the steps of:
(1) Taking 46L of supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anionic resin column of 4L of resin filler (gel type weakly alkaline acrylic resin LKA 98) in a countercurrent manner at a flow rate of 1.3BV/h, and returning effluent liquid to a starch factory after collecting the effluent liquid;
(2) Washing the anion resin column in the step (2) by purified water in a countercurrent way at the flow rate of 2-4BV/h until the protein content in effluent water is less than 0.05w/v%, washing the resin column by a resin volume of 1.5BV and a 5wt% hydrochloric acid solution in a positive flow way at 0.4BV/h, and collecting 6L effluent liquid for later use;
(3) Concentrating the effluent liquid collected in the step (2) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), and respectively collecting 1.6L of cut-off liquid and 4.4L of permeate (which are used for preparing hydrochloric acid solution for washing the resin column of the next batch); then, thoroughly washing the collected trapped fluid by using pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the retentate reserved in the step (3), positively flowing into a cation resin column (the filler is strong-acid cation chelating resin ZGD 851) at the flow rate of 0.65BV/h, and collecting the effluent for later use;
(5) Transferring the effluent liquid collected in the step (4) into an enamel pressure kettle, hydrolyzing for 9-11h at 175 ℃ and 0.7Mpa, filtering, and collecting filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), washing the nanofiltration membrane by using purified water (the solid content of the filtrate is measured by a refractometer to be 0 percent), returning 0.6L of the collected cut-off to the step (5) for continuous hydrolysis, and separating 2.0L of the collected permeate by using a simulated moving bed system (a filler ZGSPC106Ca resin in a chromatogram), wherein the mobile phase is deionized water, the pressure is 0.2Mpa, the separation temperature is 38 ℃, the feed flow is 36L/h, the flow of the mobile phase is 135L/h, and the valve switching time is 6 min) to obtain a phosphoric acid phase and an inositol phase; decolorizing the phosphoric acid phase (adding 5 ‰ of active carbon), filtering, and concentrating to obtain phosphoric acid product; heating and concentrating the inositol phase to solid content of 50% w/w, incubating to 95-100 deg.C, adding medical activated carbon of 2% dry weight (specifically inositol phase heating and concentrating to solid content of 50% w/w), incubating, stirring, decolorizing for 0.5 hr, incubating, filtering, and filtering off activated carbon. And (3) raising the temperature of the filtrate to 100 ℃ for full dissolution, cooling to 28-32 ℃ for filtration, compacting the filter cake, filtering without water drops, leaching the filter cake with a small amount of normal temperature water, and drying to obtain the inositol finished product.
Example 4
A process for the preparation of inositol and phosphoric acid comprising the steps of:
(1) Taking 46L of supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anionic resin column of 4L of resin filler (gel type weak base acrylic resin LKA 98) in a countercurrent manner at the flow rate of 1.4BV/h, and returning effluent liquid to a starch factory after collecting the effluent liquid;
(2) Washing the anion resin column in the step (2) by purified water in a countercurrent way at the flow rate of 2-4BV/h until the protein content in effluent water is less than 0.05w/v%, washing the resin column by a resin volume of 1.55BV and a 5wt% hydrochloric acid solution in a positive flow way at 0.5BV/h, and collecting 6L effluent liquid for later use;
(3) Concentrating the effluent collected in the step (2) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), and respectively collecting 1.6L of cut-off liquid and 4.4L of permeate (hydrochloric acid solution for preparing the next batch of washing resin columns); then, thoroughly washing the collected trapped fluid by using pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the retentate reserved in the step (3), positively flowing into a cationic resin column (the filler is strongly acidic cationic chelating resin ZGD 851) at a flow rate of 0.7BV/h, and collecting the effluent for later use;
(5) Transferring the effluent liquid collected in the step (4) into an enamel pressure kettle, hydrolyzing for 10.8h at 180 ℃ and 0.75Mpa, and filtering to collect filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), washing the nanofiltration membrane by using purified water (the solid content of the filtrate is measured by a refractometer to be 0 percent), returning 0.6L of the collected cut-off to the step (5) for continuous hydrolysis, and separating 2.0L of the collected permeate by using a simulated moving bed system (the filler in the chromatogram is ZGSPC106Ca resin), wherein the mobile phase is deionized water, the pressure is 0.25Mpa, the separation temperature is 46 ℃, the feed flow rate is 45L/h, the flow phase flow rate is 145L/h, and the valve switching time is 7 min) to obtain a phosphoric acid phase and an inositol phase; decolorizing the phosphoric acid phase (adding 5 ‰ of active carbon based on phosphoric acid phase weight), filtering, and concentrating to obtain phosphoric acid product; heating and concentrating the inositol phase to solid content of 50% w/w, incubating to 95-100 deg.C, adding medical activated carbon of 2% dry weight (specifically inositol phase heating and concentrating to solid content of 50% w/w), incubating, stirring, decolorizing for 0.5 hr, incubating, filtering, and filtering off activated carbon. And (3) raising the temperature of the filtrate to 100 ℃, fully dissolving, cooling to 28-32 ℃, filtering, compacting the filter cake, filtering without water drops, leaching the filter cake with a small amount of normal-temperature water, and drying to obtain the inositol finished product.
Example 5
A process for the preparation of inositol and phosphoric acid comprising the steps of:
(1) Taking 46L of supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anion resin column of 4L of resin filler (gel type weak base acrylic resin LKA 98) in a countercurrent manner at the flow rate of 1.5BV/h, and returning effluent liquid to a starch factory after collecting the effluent liquid;
(2) Washing the anion resin column in the step (2) by purified water in a countercurrent way at the flow rate of 4BV/h until the protein content in effluent water is less than 0.05w/v%, washing the resin column by a resin volume of 1.6BV and a 5wt% hydrochloric acid solution in a positive flow way at the flow rate of 0.6BV/h, and collecting 6L effluent liquid for later use;
(3) Concentrating the effluent collected in the step (2) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), and respectively collecting 1.6L of cut-off liquid and 4.4L of permeate (hydrochloric acid solution for preparing the next batch of washing resin columns); then, thoroughly washing the collected trapped fluid by using pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the retentate reserved in the step (3), positively flowing into a cationic resin column (the filler is strongly acidic cationic chelating resin ZGD 851) at a flow rate of 0.8BV/h, and collecting the effluent for later use;
(5) Transferring the effluent liquid collected in the step (4) into an enamel pressure kettle, hydrolyzing for 11h at 190 ℃ under 0.8Mpa, and filtering to collect filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by using a nanofiltration membrane (the molecular weight cut-off is 500 daltons), washing the nanofiltration membrane by using purified water (the solid content of the filtrate is measured by a refractometer to be 0 percent), returning 0.6L of the collected cut-off to the step (5) for continuous hydrolysis, and separating 2.0L of the collected permeate by using a simulated moving bed system (the filler in the chromatogram is ZGSPC106Ca resin), wherein the mobile phase is deionized water, the pressure is 0.35Mpa, the separation temperature is 55 ℃, the feed flow rate is 50L/h, the flow phase flow rate is 160L/h, and the valve switching time is 8 min) to obtain a phosphoric acid phase and an inositol phase; decolorizing the phosphoric acid phase (adding 5 ‰ of active carbon based on phosphoric acid phase weight), filtering, and concentrating to obtain phosphoric acid product; heating and concentrating inositol phase to solid content of 50% w/w, maintaining the temperature to 95-100 deg.C, adding medical active carbon with dry weight of 2% to the inositol phase (specifically, inositol phase heating and concentrating to solid content of 50% w/w), maintaining the temperature, stirring, decolorizing for 0.5 hr, maintaining the temperature, filtering, and removing active carbon. And (3) raising the temperature of the filtrate to 100 ℃ for full dissolution, cooling to 28-32 ℃ for filtration, compacting the filter cake, filtering without water drops, leaching the filter cake with a small amount of normal temperature water, and drying to obtain the inositol finished product.
In order to better prove that the preparation process of the invention has better technical effect, 3 comparative examples are given by taking example 4 as reference.
Comparative example 1
Compared with the example 4, the difference is that the filler in the cationic resin in the step (4) is HAD-10, and the rest operations are the same;
comparative example 2
Compared with the example 4, the difference is that the resin model in the anion resin column adopted in the step (1) is 312;
comparative example 3
Compared with the example 4, the difference is that when the simulated moving bed system is adopted for separation in the step (4), the packing in the chromatogram is 310 cation exchange resin;
as can be seen from the data in Table 1, the process of the present invention ensures the production and yield of inositol and phosphoric acid products when compared to comparative examples 1-3.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A process for the preparation of inositol and phosphoric acid, characterized in that it comprises the following steps:
(1) Taking supernatant obtained after standing and settling corn soaking water, feeding the supernatant into an anion resin column in a countercurrent manner, and collecting effluent liquid and returning the effluent liquid to a starch factory; the filler in the anion resin column is gel type weak-alkaline acrylic resin LKA98;
(2) Counter-current washing the anion resin column in the step (1) by purified water until the protein content in effluent water is less than 0.05w/v%, then forward washing the anion resin column by 5wt% hydrochloric acid solution, and collecting effluent liquid for later use;
(3) Concentrating the effluent liquid collected in the step (2) by adopting a nanofiltration membrane, and respectively collecting trapped fluid and permeate liquid; then, thoroughly washing the collected trapped fluid by using pure water until chloride ions are less than 100ppm, and collecting for later use;
(4) Taking the trapped liquid for standby in the step (3), enabling the trapped liquid to flow into a cation resin column positively, and collecting effluent liquid for standby; the filler in the cation resin column is strong acid cation chelating resin ZGD851;
(5) Hydrolyzing the effluent liquid collected in the step (4) at 160-190 ℃ under 0.6-0.8Mpa for 9-11h, and filtering to obtain a filtrate for later use;
(6) Filtering the filtrate obtained in the step (5) by adopting a nanofiltration membrane, washing the nanofiltration membrane by adopting purified water, returning the collected trapped fluid to the step (5) for continuous hydrolysis, and separating the collected permeate liquid by adopting a simulated moving bed system to obtain a phosphoric acid phase and an inositol phase; decolorizing, filtering and concentrating the phosphoric acid phase to obtain a phosphoric acid product; concentrating, crystallizing and recrystallizing the inositol phase to obtain an inositol finished product; when a simulated moving bed system is adopted for separation, the filler in the chromatogram is ZGSPC106Ca resin, the mobile phase is deionized water, the pressure is 0.1-0.35Mpa, the separation temperature is 22-55 ℃, the feeding flow is 20-50L/h, the flow of the mobile phase is 100-160L/h, and the valve switching time is 4-8min.
2. The process for preparing inositol and phosphoric acid according to claim 1, wherein the supernatant of the step (1) is introduced into the resin column at a flow rate of 1.0-1.5 BV/h.
3. The process for preparing inositol and phosphoric acid as claimed in claim 1, wherein the purified water in step (2) is introduced into the resin column at a flow rate of 2-4 BV/h; the dosage of the hydrochloric acid is 1.4-1.6BV of resin volume, and the hydrochloric acid enters the resin column at the flow rate of 0.3-0.6 BV/h.
4. The process of claim 1, wherein the flow rate of the retentate from step (4) into the cation exchange resin column is 0.5-0.8BV/h.
5. The process of claim 1, wherein the nanofiltration membrane in step (3) and the nanofiltration membrane in step (6) have a molecular weight cut-off of 500 daltons.
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| CN116119634B (en) * | 2023-04-20 | 2023-06-20 | 诸城市浩天药业有限公司 | Method for improving clarity of potassium dihydrogen phosphate product prepared from corn soaking water |
| CN116606192B (en) * | 2023-05-20 | 2025-02-28 | 诸城市浩天药业有限公司 | A method for producing inositol and by-products using corn steep liquor at low cost |
| CN116813448A (en) * | 2023-06-14 | 2023-09-29 | 诸城市浩天药业有限公司 | A method of co-producing inositol and liquid fertilizer using corn soaked water |
| CN116769857B (en) * | 2023-08-23 | 2023-11-07 | 诸城市浩天药业有限公司 | Preparation, separation and purification process of glycosylated inositol |
| CN117263776A (en) * | 2023-09-13 | 2023-12-22 | 诸城市浩天药业有限公司 | Method for preparing high-purity inositol and ammonium phosphate based on ethanol crystallization separation method |
| CN118791357A (en) * | 2024-07-24 | 2024-10-18 | 滕州聚成生物科技有限公司 | A method for co-producing inositol and phosphate by graded treatment of corn soaking water |
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| FR1399327A (en) * | 1963-06-14 | 1965-05-14 | Process for the preparation of inositehexaphosphoric acid, its salts and inositol, as well as for the buffer composition based on this acid, on its sodium salt | |
| CN1347863A (en) * | 2000-10-08 | 2002-05-08 | 中国科学院化工冶金研究所 | Inositol extracting process |
| CN112409132A (en) * | 2020-11-30 | 2021-02-26 | 诸城市浩天药业有限公司 | Method for separating inositol and by-products |
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| FR1399327A (en) * | 1963-06-14 | 1965-05-14 | Process for the preparation of inositehexaphosphoric acid, its salts and inositol, as well as for the buffer composition based on this acid, on its sodium salt | |
| CN1347863A (en) * | 2000-10-08 | 2002-05-08 | 中国科学院化工冶金研究所 | Inositol extracting process |
| CN112409132A (en) * | 2020-11-30 | 2021-02-26 | 诸城市浩天药业有限公司 | Method for separating inositol and by-products |
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