CN114604937A - Production process of potassium phytate - Google Patents
Production process of potassium phytate Download PDFInfo
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- CN114604937A CN114604937A CN202210339125.1A CN202210339125A CN114604937A CN 114604937 A CN114604937 A CN 114604937A CN 202210339125 A CN202210339125 A CN 202210339125A CN 114604937 A CN114604937 A CN 114604937A
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- resin column
- potassium
- effluent
- collected
- resin
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- 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 title claims abstract description 64
- 235000002949 phytic acid Nutrition 0.000 title claims abstract description 64
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000011591 potassium Substances 0.000 title claims abstract description 50
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 199
- 229920005989 resin Polymers 0.000 claims abstract description 199
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000005406 washing Methods 0.000 claims abstract description 82
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000001103 potassium chloride Substances 0.000 claims abstract description 59
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 59
- 239000008213 purified water Substances 0.000 claims abstract description 57
- 238000011010 flushing procedure Methods 0.000 claims abstract description 37
- 150000001450 anions Chemical class 0.000 claims abstract description 21
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 15
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 15
- 235000005822 corn Nutrition 0.000 claims abstract description 15
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 241000209149 Zea Species 0.000 claims abstract 4
- 239000007788 liquid Substances 0.000 claims description 67
- 229920002472 Starch Polymers 0.000 claims description 17
- 235000019698 starch Nutrition 0.000 claims description 17
- 239000008107 starch Substances 0.000 claims description 17
- 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 description 14
- 239000000467 phytic acid Substances 0.000 claims description 14
- 229940068041 phytic acid Drugs 0.000 claims description 14
- 239000012466 permeate Substances 0.000 claims description 10
- 238000001223 reverse osmosis Methods 0.000 claims description 10
- 239000012320 chlorinating reagent Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011575 calcium Substances 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 4
- 102000004169 proteins and genes Human genes 0.000 abstract description 4
- 108090000623 proteins and genes Proteins 0.000 abstract description 4
- 238000001728 nano-filtration Methods 0.000 abstract description 3
- 238000000108 ultra-filtration Methods 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 238000005374 membrane filtration Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 71
- 240000008042 Zea mays Species 0.000 description 11
- 239000000047 product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 235000018102 proteins Nutrition 0.000 description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- 235000004252 protein component Nutrition 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 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 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 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 description 1
- 229960000367 inositol Drugs 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 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
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to the technical field of potassium phytate production, in particular to a potassium phytate production process, which comprises the following steps: (1) taking clear corn soaking water, and feeding the clear corn soaking water into a weak alkaline anion resin column in a countercurrent manner; (2) respectively washing the anion resin column with hydrochloric acid and purified water, and collecting effluent for use and application; (3) and (3) continuously flushing the resin column in the step (2) by using a potassium chloride solution, and mechanically using the collected effluent. The production process reduces the content of calcium, magnesium ions and protein in the potassium phytate, no waste water and waste solids are discharged in the whole operation process, and the high-concentration potassium phytate solution can be obtained without ultrafiltration membrane filtration and nanofiltration membrane concentration in the whole process, so that the cost is greatly saved, and the potassium chloride is utilized to a greater extent.
Description
Technical Field
The invention relates to the technical field of potassium phytate production, in particular to a production process of potassium phytate.
Background
The existing production process for preparing potassium phytate solution comprises the steps of passing corn soaking water through a weak-base ion exchange resin column, adsorbing phytic acid in the corn soaking water, then desorbing the phytic acid by using a potassium chloride solution as a desorbent, and carrying out ultrafiltration membrane filtration and nanofiltration membrane concentration on the collected desorption solution to obtain a potassium phytate solution product with the phytic acid content of 20-25% and the chloride ion content of not more than 2000 ppm. Hydrolyzing the potassium phytate solution to obtain mixed solution of inositol and potassium dihydrogen phosphate. The process product still contains more water-soluble protein and calcium and magnesium ions, the water-soluble protein can generate pigment impurities to influence downstream products, and the calcium and magnesium ions can be chelated on phytic acid molecules to reduce the yield of the monopotassium phosphate. In addition, the ultrafiltration nanofiltration membrane equipment is used for concentration, so that the product cost is increased by the consumption of electric energy and the depreciation and loss of the membrane core. Membrane washing and regeneration will also produce a larger amount of wastewater. Therefore, how to improve the product quality, solve the three wastes and energy, and reduce the cost is a technical problem which needs to be solved urgently.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the potassium phytate production process is provided, the discharge amount of wastewater can be reduced when the potassium phytate is prepared by the production process, the cost is low, the process is simple, and a potassium phytate product with higher purity can be obtained.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a production process of potassium phytate comprises the following steps:
(1) taking clear corn soaking water, feeding the clear corn soaking water into a weakly alkaline anion resin column in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) washing the weak basic anion resin column in the step (1) by using 0.15-0.35 wt% of hydrochloric acid, and collecting effluent for later use; continuously washing the resin column with two streams of purified water, and respectively collecting the effluent liquid for reuse, wherein the specific reuse mode is that the effluent liquid of the first stream of purified water washing resin column is used as complex acid water for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as water for washing the column in the next batch;
(3) continuously flushing the resin column in the step (2) by using a potassium chloride solution, and mechanically applying the collected effluent liquid; specifically, before the resin column is flushed by the second batch of potassium chloride solution, the effluent collected by flushing the resin column with the previous batch of chlorinating agent solution is used for flushing the resin column in a countercurrent manner, and the effluent enriched by flushing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed with the resin column in a countercurrent mode, then the enriched effluent liquid is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, and the rest is done in the same way, and finally the potassium phytate solution with the phytic acid content of 20-25% w/v is obtained.
As an improved technical scheme, effluent collected after the resin column is washed by hydrochloric acid in the step (2) is filtered by a reverse osmosis membrane, collected trapped fluid is returned to a starch factory, and collected permeate is used as pure water.
As an improved technical scheme, the dosage of the hydrochloric acid in the step (2) is 1.5-2BV of resin volume; the total amount of purified water used was 2-5BV of resin volume.
As an improved technical scheme, when the resin column is washed by purified water, the first strand of purified water is 1-3BV of resin volume, and the second strand of purified water is 1-2BV of resin volume.
As a preferable technical solution, the hydrochloric acid in the step (2) is 0.3 wt% hydrochloric acid.
As an improved technical scheme, the potassium chloride solution in the step (3) is 11% w/v-13% w/v potassium chloride solution, and the dosage of the potassium chloride solution is 1.0-1.6BV of resin volume.
As a preferable technical scheme, the potassium chloride solution in the step (3) is 12% w/v potassium chloride solution, and the dosage of the potassium chloride solution is 1.5BV of resin volume.
As an improved technical scheme, the model number of the resin in the weak basic anion resin column in the step (1) is SQ-913.
After the technical scheme is adopted, the invention has the beneficial effects that:
by adopting the production process, the clarified corn soaking water flows into a weak alkaline anion resin column in a countercurrent way, the resin column is washed by 0.15-0.35 wt% of hydrochloric acid and purified water in sequence, and the respectively collected effluent is used for standby and application; wherein, when 0.15-0.35 wt% hydrochloric acid is adopted to wash the resin, protein components and trace calcium and magnesium ions on the resin can be effectively washed off, then the resin is filtered by a reverse osmosis membrane, the protein components contained in the trapped fluid are returned to a corn starch factory for utilization, and the permeate liquid is used as pure water; the method for recycling the effluent collected by flushing the resin column with the purified water is characterized in that the effluent collected by flushing the resin column with the first stream of purified water is used as the water for preparing complex acid, and then the first stream of purified water is used for preparing low-concentration dilute hydrochloric acid to flush the resin column; the effluent liquid collected by the second stream of purified water washing resin column is used as the water for washing the column of the next batch; flushing the effluent collected by the resin column by 0.15-0.35 wt% hydrochloric acid, wherein the standby use means that the effluent is filtered by a reverse osmosis membrane, the collected trapped fluid is returned to a starch factory, and the collected permeate is used as pure water; the whole operation process has no waste water and solid discharge; the method comprises the steps of washing a resin column with dilute hydrochloric acid and purified water, then washing the resin column with a potassium chloride solution, and mechanically using collected effluent liquid, specifically, washing the resin column with the effluent liquid of the previous batch in a counter-current manner before washing the resin with the next batch of potassium chloride, then continuously washing with the potassium chloride solution, and repeatedly carrying out the operations for multiple times to realize the enrichment of potassium phytate so as to obtain the potassium phytate solution with the phytic acid content of 20-25% w/v.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) washing the weak alkaline anion resin column in the step (1) by adopting the resin volume of 1.5BV and 0.15 wt% of hydrochloric acid in a countercurrent way, and reserving the collected effluent liquid for later use (filtering by adopting a reverse osmosis membrane, returning the collected trapped liquid to a starch factory, and using the collected permeate liquid as water for washing the column); continuously washing the resin column with two streams of purified water in a counter-current manner, wherein the consumption of the first stream of purified water is 1.5BV of resin volume, and the consumption of the second stream of purified water is 1.5BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first stream of purified water washing resin column is used as hydrochloric acid configuration water, the configured hydrochloric acid is used for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by adopting 1.5BV of resin volume and 11% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent is used mechanically, specifically, the effluent collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed by countercurrent, then the effluent liquid after enrichment is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, the analogy is repeated according to the above manner, and the potassium phytate solution enriched to the fourth batch is applied to obtain the potassium phytate solution with 20% w/v phytic acid content.
Example 2
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) washing the weak alkaline anion resin column in the step (1) by adopting the resin volume of 1.8BV and 0.2 wt% of hydrochloric acid in a counter-current manner, and reserving the collected effluent liquid (filtering by adopting a reverse osmosis membrane, returning the collected trapped liquid to a starch factory, and using the collected permeate liquid as water for washing the column); taking two streams of purified water, continuously washing the resin column in a counter-current manner, wherein the consumption of the first stream of purified water is 1.8BV of resin volume, and the consumption of the second stream of purified water is 1.8BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first strand of purified water washing resin column is used as hydrochloric acid preparation water, the prepared hydrochloric acid is used for washing the resin column, and the effluent liquid of the second strand of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by using 1.2BV of resin volume and 11.5% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent is used mechanically, specifically, the effluent collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed in a countercurrent mode, then the effluent liquid after enrichment is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, the process is repeated according to the above mode, and the enrichment is applied to the fourth batch to finally obtain the potassium phytate solution with the phytic acid content of 20.8% w/v.
Example 3
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) flushing the weak alkaline anion resin column in the step (1) by using 2BV of resin volume and 0.25 wt% of hydrochloric acid, and reserving the collected effluent (filtering by using a reverse osmosis membrane, returning the collected trapped fluid to a starch factory, and using the collected permeate as water for washing the column); continuously washing the resin column by taking two strands of purified water, wherein the consumption of the first strand of purified water is 2BV of resin volume, and the consumption of the second strand of purified water is 1.5BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first stream of purified water washing resin column is used as hydrochloric acid configuration water, the configured hydrochloric acid is used for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by using 1BV of resin volume and 12.5% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent liquid is used mechanically, in particular, the effluent liquid collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent liquid enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the previous two batches are sequentially and respectively flushed by countercurrent, then the effluent liquid after enrichment is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, the enrichment is performed in the same way until the fourth batch is obtained, and finally, the potassium phytate solution with the phytic acid content of 24.5% w/v is obtained.
Example 4
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) flushing the weak alkaline anion resin column in the step (1) by using 2BV of resin volume and 0.3 wt% of hydrochloric acid, and reserving the collected effluent (filtering by using a reverse osmosis membrane, returning the collected trapped fluid to a starch factory, and using the collected permeate as water for washing the column); continuously washing the resin column by taking two strands of purified water, wherein the consumption of the first strand of purified water is 2BV of resin volume, and the consumption of the second strand of purified water is 2BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first stream of purified water washing resin column is used as hydrochloric acid configuration water, the configured hydrochloric acid is used for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by using 1.5BV of resin volume and 12% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent is used mechanically, specifically, the effluent collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by using the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed in a countercurrent mode, then the effluent liquid after enrichment is respectively collected, the resin column is continuously flushed by using the third batch of potassium chloride solution, the process is repeated in the same way, the enrichment is applied to the last four batches, and finally, the potassium phytate solution with the phytic acid content of 25% w/v is obtained.
Example 5
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) flushing the weak alkaline anion resin column in the step (1) by using 2BV of resin volume and 0.25 wt% of hydrochloric acid, and reserving the collected effluent (filtering by using a reverse osmosis membrane, returning the collected trapped fluid to a starch factory, and using the collected permeate as water for washing the column); taking two streams of purified water to continuously wash the resin column, wherein the using amount of the first stream of purified water is 2.5BV of resin volume, and the using amount of the second stream of purified water is 2BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first stream of purified water washing resin column is used as hydrochloric acid configuration water, the configured hydrochloric acid is used for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by using 1.6BV of resin volume and 12.5% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent is used mechanically, specifically, the effluent collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed with the resin column in a countercurrent mode, then the enriched effluent is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, and the rest is done in the same way, and finally the 25% w/v potassium phytate solution is obtained.
Example 6
A production process of potassium phytate comprises the following steps:
(1) feeding 650L of clarified corn soaking water into a weakly alkaline anion resin column (resin type SQ-913) in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) washing the weak alkaline anion resin column in the step (1) by using 0.35 wt% hydrochloric acid with the resin volume of 2BV, and reserving the collected effluent liquid (filtering by using a reverse osmosis membrane, returning the collected trapped liquid to a starch factory, and using the collected permeate liquid as water for washing the column); taking two streams of purified water to continuously wash the resin column, wherein the consumption of the first stream of purified water is 3BV of resin volume, the consumption of the second stream of purified water is 2BV of resin volume, and respectively collecting effluent liquid for reuse; the specific application mode is that the effluent liquid of the first strand of purified water washing resin column is used as hydrochloric acid preparation water, the prepared hydrochloric acid is used for washing the resin column, and the effluent liquid of the second strand of purified water washing resin column is used as next batch of purified water for washing the resin column;
(3) flushing the resin column in the step (2) by using 1.3BV of resin volume and 13% w/v of potassium chloride solution, and mechanically using the collected effluent; the effluent is used mechanically, specifically, the effluent collected by washing the resin column with the previous batch of chlorinating agent solution is used for washing the resin column in a countercurrent manner before the second batch of potassium chloride solution is used for washing the resin column, and the effluent enriched by washing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the previous two batches are sequentially and respectively flushed by countercurrent, then the effluent liquid after enrichment is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, the enrichment is performed in the same way until the fourth batch is performed, and finally the 25% w/v potassium phytate solution is obtained.
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 embodiment 4, the difference is that 1.5 wt% hydrochloric acid is adopted to wash the resin column in the step (2), and the rest operations are the same, so as to obtain the potassium phytate solution with 23% w/v phytic acid content;
comparative example 2
Compared with the embodiment 4, the difference is that 10 wt% potassium chloride solution is adopted to wash the resin column in the step (3), and the rest operations are the same, so as to obtain potassium phytate solution with 19% w/v phytic acid content;
comparative example 3
Compared with the embodiment 4, the difference is that 2 wt% hydrochloric acid solution is adopted to wash the resin column in the step (2), and the rest operations are the same, so that potassium phytate solution with 21% w/v phytic acid content is obtained;
TABLE 1
The data in table 1 show that, by adopting the preparation process of the invention, no wastewater is discharged in the whole process, and simultaneously the contents of calcium, magnesium and protein in potassium phytate are reduced.
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 (8)
1. The production process of the potassium phytate is characterized by comprising the following steps:
(1) taking clear corn soaking water, feeding the clear corn soaking water into a weakly alkaline anion resin column in a countercurrent manner, and returning effluent to a starch factory after collecting the effluent;
(2) washing the weak basic anion resin column in the step (1) by using 0.15-0.35 wt% of hydrochloric acid, and collecting effluent for later use; continuously washing the resin column with two streams of purified water, and respectively collecting the effluent liquid for reuse, wherein the specific reuse mode is that the effluent liquid of the first stream of purified water washing resin column is used as complex acid water for washing the resin column, and the effluent liquid of the second stream of purified water washing resin column is used as the next batch of column washing water;
(3) continuously flushing the resin column in the step (2) by using a potassium chloride solution, and mechanically applying the collected effluent liquid; specifically, before the resin column is flushed by the second batch of potassium chloride solution, the effluent collected by flushing the resin column with the previous batch of chlorinating agent solution is used for flushing the resin column in a countercurrent manner, and the effluent enriched by flushing the resin column is collected; then, flushing the resin column by positive flow of a second batch of potassium chloride solution, continuously flushing the resin column by the collected effluent liquid, and collecting the enriched effluent liquid; and then, before the resin column is positively flushed by the third batch of potassium chloride solution, the eluates collected in the first two batches are sequentially and respectively flushed with the resin column in a countercurrent mode, then the enriched effluent liquid is respectively collected, the resin column is continuously flushed by the third batch of potassium chloride solution, and the rest is done in the same way, and finally the potassium phytate solution with the phytic acid content of 20-25% w/v is obtained.
2. The potassium phytate production process according to claim 1, wherein the potassium phytate production process comprises the following steps: and (3) filtering the effluent liquid collected after the resin column is washed by hydrochloric acid in the step (2) by adopting a reverse osmosis membrane, returning the collected trapped fluid to a starch factory, and using the collected permeate liquid as pure water.
3. The potassium phytate production process according to claim 1, wherein the potassium phytate production process comprises the following steps: the dosage of the hydrochloric acid in the step (2) is 1.5-2BV of resin volume; the total amount of purified water used was 2-5BV of resin volume.
4. The potassium phytate production process according to claim 1, wherein the potassium phytate production process comprises the following steps: when the resin column is washed by purified water, the amount of the first strand of purified water is 1-3BV of resin volume, and the amount of the second strand of purified water is 1-2BV of resin volume.
5. The potassium phytate production process according to claim 4, wherein the potassium phytate production process comprises the following steps: the hydrochloric acid in the step (2) is 0.3 wt% of hydrochloric acid.
6. The potassium phytate production process according to claim 1, wherein the potassium phytate production process comprises the following steps: the potassium chloride solution in the step (3) is 11% w/v-13% w/v potassium chloride solution, and the dosage of the potassium chloride solution is 1.0-1.6BV resin volume.
7. The process for producing potassium phytate according to claim 6, wherein the process comprises the following steps: in the step (3), the potassium chloride solution is 12% w/v potassium chloride solution, and the dosage of the potassium chloride solution is 1.5BV of resin volume.
8. The potassium phytate production process according to claim 1, wherein the potassium phytate production process comprises the following steps: the model of the resin in the weak basic anion resin column in the step (1) is SQ-913.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819450A (en) * | 2022-12-15 | 2023-03-21 | 河北宇威生物科技有限公司 | Processing method for extracting potassium phytate from corn soaking water |
| CN116284112A (en) * | 2023-05-26 | 2023-06-23 | 诸城市浩天药业有限公司 | Preparation method of hexapotassium phytate |
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| JPH09316089A (en) * | 1996-05-24 | 1997-12-09 | Fuji Oil Co Ltd | Purification of phytic acid |
| CN102134260A (en) * | 2010-07-13 | 2011-07-27 | 合肥富通机电自动化有限公司 | Method for preparing phytic acid |
| CN113003898A (en) * | 2021-04-24 | 2021-06-22 | 诸城市浩天药业有限公司 | Corn soaking water treatment method |
| CN113134396A (en) * | 2021-04-24 | 2021-07-20 | 诸城市浩天药业有限公司 | Process method for reducing dosage of desorbent in preparation of potassium phytate by using corn soaking water |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH09316089A (en) * | 1996-05-24 | 1997-12-09 | Fuji Oil Co Ltd | Purification of phytic acid |
| CN102134260A (en) * | 2010-07-13 | 2011-07-27 | 合肥富通机电自动化有限公司 | Method for preparing phytic acid |
| CN113003898A (en) * | 2021-04-24 | 2021-06-22 | 诸城市浩天药业有限公司 | Corn soaking water treatment method |
| CN113134396A (en) * | 2021-04-24 | 2021-07-20 | 诸城市浩天药业有限公司 | Process method for reducing dosage of desorbent in preparation of potassium phytate by using corn soaking water |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115819450A (en) * | 2022-12-15 | 2023-03-21 | 河北宇威生物科技有限公司 | Processing method for extracting potassium phytate from corn soaking water |
| CN116284112A (en) * | 2023-05-26 | 2023-06-23 | 诸城市浩天药业有限公司 | Preparation method of hexapotassium phytate |
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