CN116462168A - Production process of plant source monopotassium phosphate - Google Patents
Production process of plant source monopotassium phosphate Download PDFInfo
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- CN116462168A CN116462168A CN202310297987.7A CN202310297987A CN116462168A CN 116462168 A CN116462168 A CN 116462168A CN 202310297987 A CN202310297987 A CN 202310297987A CN 116462168 A CN116462168 A CN 116462168A
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- resin column
- inositol
- filtrate
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- 229910000402 monopotassium phosphate Inorganic materials 0.000 title claims abstract description 67
- 235000019796 monopotassium phosphate Nutrition 0.000 title claims abstract description 67
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 title claims abstract description 35
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 161
- 229920005989 resin Polymers 0.000 claims abstract description 161
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 112
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000012065 filter cake Substances 0.000 claims abstract description 90
- 239000000706 filtrate Substances 0.000 claims abstract description 87
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 claims abstract description 80
- 125000002091 cationic group Chemical group 0.000 claims abstract description 78
- 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 claims abstract description 64
- 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 claims abstract description 64
- 229960000367 inositol Drugs 0.000 claims abstract description 64
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000001103 potassium chloride Substances 0.000 claims abstract description 56
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 56
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 34
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 28
- 241000196324 Embryophyta Species 0.000 claims abstract description 25
- 125000000129 anionic group Chemical group 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 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 19
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 19
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 19
- 235000005822 corn Nutrition 0.000 claims abstract description 19
- 238000011010 flushing procedure Methods 0.000 claims abstract description 19
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 16
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 16
- 239000012047 saturated solution Substances 0.000 claims abstract description 16
- 150000001450 anions Chemical class 0.000 claims abstract description 15
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011591 potassium Substances 0.000 claims abstract description 14
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 14
- 239000012043 crude product Substances 0.000 claims abstract description 10
- 239000008213 purified water Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims description 47
- 238000001816 cooling Methods 0.000 claims description 25
- 240000008042 Zea mays Species 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 13
- 230000008025 crystallization Effects 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000002386 leaching Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 230000003301 hydrolyzing effect Effects 0.000 claims description 9
- 238000004537 pulping Methods 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 238000010979 pH adjustment Methods 0.000 claims description 7
- 238000004062 sedimentation Methods 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000001728 nano-filtration Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 241000209149 Zea Species 0.000 abstract 2
- 150000001768 cations Chemical class 0.000 description 8
- 229910001414 potassium ion Inorganic materials 0.000 description 8
- 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 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000467 phytic acid Substances 0.000 description 5
- 229940068041 phytic acid Drugs 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002699 waste material Substances 0.000 description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229920002261 Corn starch Polymers 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 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
- 238000005516 engineering process Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
-
- 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
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/12—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
- C07C2601/08—Systems containing only non-condensed rings with a five-membered ring 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention relates to the technical field of corn soaking water treatment, in particular to a production process of plant source monopotassium phosphate, which comprises the following steps: (1) Taking corn soaking water, entering a first cationic resin column, a second cationic resin column and an anionic resin column, and flushing by purified water; (2) Washing the anion resin column by adopting potassium chloride solution, and treating the collected effluent liquid to obtain a potassium dihydrogen phosphate filter cake and filtrate; (3) washing the first cationic resin column with hydrochloric acid; (4) taking filtrate containing inositol and monopotassium phosphate for treatment; (5) Taking a filter cake containing inositol and potassium chloride, and adding an inositol saturated solution for treatment; (6) Combining and post-treating the twice collected inositol crude product filter cakes to obtain an inositol product; (7) The filtrate containing phosphoric acid, methanol and trace protein is treated. The process method can obtain a high-yield potassium dihydrogen phytate product; in addition, the consumption of potassium chloride sold in the market is reduced, and the cost is saved for enterprises.
Description
Technical Field
The invention relates to the technical field of corn soaking water treatment, in particular to a production process of plant source monopotassium phosphate.
Background
In the corn starch wet milling production process, corn soaking water is used as main production wastewater, wherein the solid content is about 10-12%, and the corn soaking water mainly contains 5-6% of protein, 2-3% of lactic acid, 1% of phytic acid, 1% of sugar, 0.5% of potassium ion, 0.1% of magnesium ion, a small amount of starch residues and the like. At present, the traditional technology utilizes anion resin to adsorb phytic acid, then adopts potassium chloride to desorb, the potassium phytate obtained after desorption is hydrolyzed to obtain inositol and potassium dihydrogen phosphate, and then the inositol and the potassium dihydrogen phosphate are obtained through separation. Because the potassium ions in the corn soaking water are separately recovered with high cost, the resource waste is caused by no recovery treatment; therefore, aiming at the problems, a production process of plant source monopotassium phosphate is established.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects existing in the prior art, the production process of the plant source monopotassium phosphate is provided, and potassium ions in corn soaking water can be recovered by using the production process, so that a monopotassium phosphate product is obtained, and resource waste is avoided.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a production process of plant source monopotassium phosphate comprises the following steps:
(1) Taking supernatant fluid after corn soaking water sedimentation, sequentially and reversely flowing into a first cationic resin column, a second cationic resin column and an anionic resin column which are connected in series, and when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, reversely flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water, and when the protein content of the effluent liquid is less than 0.2wt%, stopping flushing;
(2) Adopting potassium chloride solution forward flow to flush the anion resin column in the step (1), concentrating, hydrolyzing and filtering the collected potassium phytate effluent, concentrating, crystallizing, leaching and separating the collected filtrate, and respectively collecting a potassium dihydrogen phosphate filter cake and a filtrate containing inositol and potassium dihydrogen phosphate;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking the filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding hydrochloric acid, concentrating, adding the concentrated filtrate into stirred methanol, pulping, cooling, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and a small amount of protein;
(5) Adding the filter cake containing inositol and potassium chloride in the step (4) into inositol saturated solution, stirring, centrifugally separating, and then respectively collecting filtrate and crude inositol filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filter cake is subjected to heat preservation and filtration, and the potassium chloride filter cake and the filtrate are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; wherein the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) are combined to prepare 8-25% w/v solution as the next desorbent for flushing the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating, concentrating, decoloring, filtering, heating the collected filtrate to be fully dissolved, cooling, filtering, leaching the collected filter cakes, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant source monopotassium phosphate product.
As an improved technical scheme, the total volume of the resin of the first cationic resin column and the second cationic resin column in the step (1) is 1.5-2.5 times of the volume of the resin in the anionic resin column, and the volume ratio of the resin in the first cationic resin column to the resin in the second cationic resin column is 6-8:2-4.
As an improved technical scheme, in the step (1), the resin filled in the first cationic resin column and the second cationic resin column is ZG-6, and the resin filled in the anionic resin column is LX-671.
As an improved technical scheme, the potassium phytate effluent in the step (2) is concentrated by adopting a nanofiltration membrane with the molecular weight cut-off of 500-1000 daltons, and the obtained concentrated solution is hydrolyzed for 10-12 hours at the temperature of 150-180 ℃.
As an improved technical scheme, the filtrate collected after the potassium phytate effluent liquid in the step (2) is concentrated, hydrolyzed and filtered is concentrated under the temperature of 50-100 ℃ under the pressure of-0.07 to-0.1 mpa, and is cooled to 25-30 ℃ for crystallization.
As an improved technical scheme, 30% w/w hydrochloric acid is added in the step (4), concentrated to 30-40 poise, added into methanol with the volume 1-2 times of that of the filtrate for pulping, and stirred and cooled to 20-28 ℃.
As an improved technical scheme, in the step (5), a filter cake containing inositol and potassium chloride and an inositol saturated solution are added into the inositol saturated solution according to the ratio of 1:1-2 (w/v).
As an improved technical scheme, in the step (6), after the two-time collected inositol crude product filter cakes are combined, water is added, heating and concentrating are carried out until the solid content is 45-55wt%, the temperature is kept to 95-100 ℃, a decoloring agent is added, the temperature is kept for decoloring, the filtrate collected by filtration is heated to 95-100 ℃ for complete dissolution, and then the temperature is reduced to 28-32 ℃ for filtration.
After the technical scheme is adopted, the invention has the beneficial effects that:
sequentially feeding supernatant fluid after corn soaking water sedimentation into a first cationic resin column, a second cationic resin column and an anionic resin column which are connected in series, flushing the anionic resin column by purified water, flushing the anionic resin column by newly configured potassium chloride, hydrolyzing and filtering an obtained potassium phytate effluent, concentrating and crystallizing and separating filtrate to obtain a potassium dihydrogen phosphate filter cake and filtrate containing inositol and potassium dihydrogen phosphate, adding hydrochloric acid and methanol into the inositol and potassium dihydrogen phosphate filtrate for pulping, and separating to obtain a filter cake containing inositol and potassium chloride and filtrate containing phosphoric acid, methanol and a small amount of protein; adding a filter cake containing inositol and potassium chloride into an inositol saturated solution, stirring, centrifugally separating, and then respectively collecting filtrate and a crude inositol filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filtrate is subjected to heat preservation and filtration, and the potassium chloride filter cake and the filtrate are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; combining the collected potassium chloride filter cake and the potassium chloride filter cake in the step (3) to prepare 8-25% w/v solution for flushing the anion resin column in the step (1) by the next desorbent; and (3) rectifying the filtrate containing phosphoric acid, methanol and trace protein to recover the methanol, flushing a second cationic resin column by taking the dealcoholized phosphoric acid solution as a desorbing agent to obtain a monopotassium phosphate effluent, and combining the solid phase obtained by pH adjustment, concentration, crystallization and separation with the monopotassium phosphate filter cake in the step (2) to obtain a plant monopotassium phosphate product. The process method can recycle the phytic acid and potassium ions in the corn soaking water at the same time, and obtain a high-yield potassium dihydrogen phytate product; in addition, potassium ions in the corn soaking water can be utilized to obtain desorbing agent for desorbing the phytic acid, so that the consumption of commercial potassium chloride is reduced, and the cost is saved for enterprises.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A production process of plant source monopotassium phosphate comprises the following steps:
(1) Taking 46L of supernatant fluid after corn soaking water sedimentation, countercurrent entering a first cationic resin column (ZG-6), a second cationic resin column (ZG-6) and an anionic resin column (LX-671) which are connected in series according to the flow rate of 1BV/h, countercurrent flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, and stopping flushing when the protein content of the effluent liquid is less than 0.2 wt%; wherein the total volume of the resin in the first cation resin column and the second cation resin column is 7L, and the volume ratio of the resin in the first cation resin column to the resin in the second cation resin column is 6:2; the total resin volume of the first and second cationic resin columns is 1.5 times the resin volume in the anionic resin column;
(2) Washing the anion resin column in the step (1) by 8% w/v potassium chloride solution in forward flow at a flow rate of 0.3BV/h, concentrating the collected potassium phytate effluent by adopting a nanofiltration membrane (500-1000 daltons), hydrolyzing the collected concentrated solution at 150 ℃ for 10 hours, filtering, concentrating the collected filtrate at-0.1 Mpa and 50 ℃, cooling to 25 ℃ for crystallization, leaching and separating, and collecting a potassium dihydrogen phosphate filter cake and filtrate containing inositol and potassium dihydrogen phosphate respectively;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding 150g and 30% w/w hydrochloric acid, concentrating to 40 poise, dripping into methanol (1 time of the volume of the filtrate) in a stirring state, pulping, cooling to 20 ℃, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and trace protein;
(5) Taking a filter cake containing inositol and potassium chloride in the step (4) and an inositol saturated solution according to the following ratio of 1:1 (w/v) is added into inositol saturated solution, and is stirred, centrifugally separated and then filtrate and inositol crude product filter cake are respectively collected, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filtrate is filtered at a constant temperature, and potassium chloride filter cake and filtrate are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; combining the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) to prepare 8-25% w/v solution for the next desorbent flush of the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating and dissolving (sampling and detecting that the solid content is 45 wt%), preserving heat and decoloring at 95 ℃ (adding active carbon accounting for 2% of the solid content of feed liquid), filtering, heating the collected filtrate to be fully dissolved, cooling to 28 ℃, filtering, leaching the collected filter cake, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant monopotassium phosphate product.
Example 2
A production process of plant source monopotassium phosphate comprises the following steps:
(1) Taking 46L of supernatant fluid after corn soaking water sedimentation, countercurrent entering a first cationic resin column (ZG-6), a second cationic resin column (ZG-6) and an anionic resin column (LX-671) which are connected in series according to the flow rate of 2.5BV/h, countercurrent flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, and stopping flushing when the protein content of the effluent liquid is less than 0.2 wt%; wherein the total volume of the resin in the first cationic resin column and the second cationic resin column is 9L, and the volume ratio of the resin in the first cationic resin column to the resin in the second cationic resin column is 7:3; the total resin volume of the first and second cationic resin columns is 1.8 times the resin volume in the anionic resin column;
(2) Washing the anion resin column in the step (1) by adopting 12% w/v potassium chloride solution in forward flow at the flow rate of 1.5BV/h, concentrating the collected potassium phytate effluent by adopting a nanofiltration membrane (500-1000 daltons), hydrolyzing the collected concentrated solution at 165 ℃ for 10.5 hours, filtering, concentrating the collected filtrate at-0.08 Mpa and 75 ℃, cooling to 25 ℃ for crystallization, leaching and separating, and collecting a potassium dihydrogen phosphate filter cake and filtrate containing inositol and potassium dihydrogen phosphate respectively;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding 151g and 30% w/w hydrochloric acid, concentrating to 38 poise, dripping into methanol (1.3 times of the volume of the filtrate) in a stirring state, pulping, cooling to 23 ℃, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and trace protein;
(5) Adding the filter cake containing inositol and potassium chloride in the step (4) and an inositol saturated solution into the inositol saturated solution according to the proportion of 1:1.3 (w/v), stirring, centrifugally separating, and then respectively collecting filtrate and an inositol crude filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filtrate and the potassium chloride filter cake are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; combining the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) to prepare 8-25% w/v solution for the next desorbent flush of the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating and dissolving (sampling and detecting that the solid content is 48 wt%), preserving heat and decoloring at 95 ℃ (adding active carbon accounting for 2% of the solid content of feed liquid), filtering, heating the collected filtrate to be fully dissolved, cooling to 28 ℃, filtering, leaching the collected filter cake, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant monopotassium phosphate product.
Example 3
A production process of plant source monopotassium phosphate comprises the following steps:
(1) Taking 46L of supernatant fluid after corn soaking water sedimentation, countercurrent entering a first cationic resin column (ZG-6), a second cationic resin column (ZG-6) and an anionic resin column (LX-671) which are connected in series according to the flow rate of 3BV/h, countercurrent flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, and stopping flushing when the protein content of the effluent liquid is less than 0.2 wt%; wherein the total volume of the resin in the first cation resin column and the second cation resin column is 8L, and the volume ratio of the resin in the first cation resin column to the resin in the second cation resin column is 7:3; the total resin volume of the first and second cationic resin columns is 2 times the resin volume in the anionic resin column;
(2) Washing the anion resin column in the step (1) by 15% w/v potassium chloride solution in forward flow at a flow rate of 2BV/h, concentrating the collected potassium phytate effluent by adopting a nanofiltration membrane (500-1000 daltons), hydrolyzing the collected concentrated solution at 170 ℃ for 11 hours, filtering, concentrating the collected filtrate at-0.08 Mpa and 80 ℃, cooling to 28 ℃ for crystallization, leaching and separating, and collecting a potassium dihydrogen phosphate filter cake and filtrate containing inositol and potassium dihydrogen phosphate respectively;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding 153g and 30% w/w hydrochloric acid, concentrating to 33 poise, dripping into methanol (1.5 times of the volume of the filtrate) in a stirring state, pulping, cooling to 25 ℃, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and trace protein;
(5) Adding the filter cake containing inositol and potassium chloride in the step (4) and an inositol saturated solution into the inositol saturated solution according to the proportion of 1:1.5 (w/v), stirring, centrifugally separating, and then respectively collecting filtrate and an inositol crude filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filtrate and the potassium chloride filter cake are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; combining the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) to prepare 8-25% w/v solution for the next desorbent flush of the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating and dissolving (sampling and detecting that the solid content is 52 wt%), preserving heat and decoloring at 98 ℃ (adding active carbon accounting for 2% of the solid content of feed liquid), filtering, heating the collected filtrate to be fully dissolved, cooling to 30 ℃, filtering, leaching the collected filter cake, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant monopotassium phosphate product.
Example 4
A production process of plant source monopotassium phosphate comprises the following steps:
(1) Taking 46L of supernatant fluid after corn soaking water sedimentation, countercurrent entering a first cationic resin column (ZG-6), a second cationic resin column (ZG-6) and an anionic resin column (LX-671) which are connected in series according to the flow rate of 5BV/h, countercurrent flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, and stopping flushing when the protein content of the effluent liquid is less than 0.2 wt%; wherein the total volume of the resin in the first cationic resin column and the second cationic resin column is 9L, and the volume ratio of the resin in the first cationic resin column to the resin in the second cationic resin column is 8:4; the total resin volume of the first and second cationic resin columns is 2.5 times the resin volume in the anionic resin column;
(2) Washing the anion resin column in the step (1) with 20% w/v potassium chloride solution in forward flow at a flow rate of 3BV/h, concentrating the collected potassium phytate effluent with nanofiltration membrane (500-1000 Dalton), hydrolyzing the collected concentrated solution at 180 ℃ for 12h, filtering, concentrating the collected filtrate at-0.07 Mpa and 95 ℃, cooling to 30 ℃ for crystallization, leaching and separating, and collecting potassium dihydrogen phosphate filter cake and filtrate containing inositol and potassium dihydrogen phosphate respectively;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding 153g and 30% w/w hydrochloric acid, concentrating to 30 poise, dripping into methanol (2 times of the volume of the filtrate) in a stirring state, pulping, cooling to 28 ℃, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and trace protein;
(5) Taking a filter cake containing inositol and potassium chloride in the step (4) and an inositol saturated solution according to the following ratio of 1:2 (w/v: the unit corresponding to the specific w is ton, and the unit corresponding to the v is cubic meter) adding the mixture into inositol saturated solution, stirring, centrifugally separating, and then respectively collecting filtrate and inositol crude filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filtrate is subjected to heat preservation and filtration, and the potassium chloride filter cake and the filtrate are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; combining the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) to prepare 8-25% w/v solution for the next desorbent flush of the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating and dissolving (sampling and detecting that the content of solid content is 55wt%), preserving heat and decoloring at 100 ℃ (adding active carbon accounting for 2% of the solid content of feed liquid), filtering, heating the collected filtrate to be fully dissolved, cooling to 32 ℃, filtering, leaching the collected filter cake, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant monopotassium phosphate product.
For better demonstration, the process method of the invention can better recover potassium ions in corn steep water, and 3 comparative examples are given by taking example 3 as a reference. Details are shown in Table 1.
Comparative example 1
Unlike example 3, the following is: in the step (1), the resin volume ratio of the first cationic resin column to the second cationic resin column is 5:5, and the rest operations are the same;
comparative example 2
Unlike example 3, the following is: in the step (1), the resin volume ratio of the first cationic resin column to the second cationic resin column is 2:7, and the rest operations are the same;
comparative example 3
Unlike example 3, the following is: in the step (1), the resin in the first cationic resin column and the second cationic resin column is sea-wetting HAD-10 resin, and the rest operations are the same.
TABLE 1
As can be found from the data in Table 1, the process method can recover potassium ions in the corn soaking water to obtain a high-yield potassium dihydrogen phosphate product, thereby avoiding resource waste; and compared with the comparative example, the process method of the invention also reduces the consumption of potassium chloride on the market when desorbing the phytic acid when recovering the potassium ions of the corn steep water.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (8)
1. The production process of the plant source monopotassium phosphate is characterized by comprising the following steps of:
(1) Taking supernatant fluid after corn soaking water sedimentation, sequentially and reversely flowing into a first cationic resin column, a second cationic resin column and an anionic resin column which are connected in series, and when the effluent liquid sampling pH of the second cationic resin column is more than 2.5, reversely flushing the first cationic resin column, the second cationic resin column and the anionic resin column by purified water, and when the protein content of the effluent liquid is less than 0.2wt%, stopping flushing;
(2) Adopting potassium chloride solution forward flow to flush the anion resin column in the step (1), concentrating, hydrolyzing and filtering the collected potassium phytate effluent, concentrating, crystallizing, leaching and separating the collected filtrate, and respectively collecting a potassium dihydrogen phosphate filter cake and a filtrate containing inositol and potassium dihydrogen phosphate;
(3) Adopting hydrochloric acid to reversely flush the first cationic resin column in the step (1), collecting effluent with pH less than 2.0 and then preparing the effluent as the next batch of hydrochloric acid; concentrating effluent liquid with pH of 2.0-3, crystallizing, and filtering to obtain potassium chloride filter cake for later use;
(4) Taking the filtrate containing inositol and potassium dihydrogen phosphate in the step (2), adding hydrochloric acid, concentrating, adding the concentrated filtrate into stirred methanol, pulping, cooling, and centrifugally filtering under the protection of nitrogen to obtain a filter cake containing inositol and potassium chloride and a filtrate containing phosphoric acid, methanol and a small amount of protein;
(5) Adding the filter cake containing inositol and potassium chloride in the step (4) into inositol saturated solution, stirring, centrifugally separating, and then respectively collecting filtrate and crude inositol filter cake, wherein the collected filtrate is continuously concentrated, crystals are separated out, and then the filter cake is subjected to heat preservation and filtration, and the potassium chloride filter cake and the filtrate are respectively collected; continuously cooling and crystallizing the collected filtrate, filtering, centrifugally separating, and collecting a crude inositol filter cake; wherein the collected potassium chloride filter cake and the potassium chloride filter cake in step (3) are combined to prepare 8-25% w/v solution as the next desorbent for flushing the anion resin column in step (1);
(6) Mixing the inositol crude product filter cakes collected twice in the step (5), adding water, heating, concentrating, decoloring, filtering, heating the collected filtrate to be fully dissolved, cooling, filtering, leaching the collected filter cakes, and drying to obtain an inositol product;
(7) And (3) taking the filtrate containing phosphoric acid, methanol and trace protein in the step (4), rectifying, respectively collecting methanol and phosphoric acid solution, wherein the phosphoric acid solution is used as a desorbing agent to flush the second cationic resin column, and the obtained monopotassium phosphate effluent is combined with the solid phase obtained by pH adjustment, concentration, crystallization and separation and the monopotassium phosphate filter cake in the step (2) to obtain a plant source monopotassium phosphate product.
2. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: in the step (1), the total volume of the resin in the first cationic resin column and the second cationic resin column is 1.5-2.5 times of the volume of the resin in the anionic resin column, and the volume ratio of the resin in the first cationic resin column to the resin in the second cationic resin column is 6-8:2-4.
3. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: in the step (1), the resin filled in the first cationic resin column and the second cationic resin column is ZG-6, and the resin filled in the anionic resin column is LX-671.
4. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: concentrating the potassium phytate effluent in the step (2) by adopting a nanofiltration membrane with the molecular weight cut-off of 500-1000 daltons, and hydrolyzing the obtained concentrated solution for 10-12 hours at the temperature of 150-180 ℃.
5. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: concentrating, hydrolyzing and filtering the potassium phytate effluent in the step (2), concentrating the filtrate at-0.07 to-0.1 mpa and 50-100 ℃, and cooling to 25-30 ℃ for crystallization.
6. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: in the step (4), 30% w/w hydrochloric acid is added, concentrated to 30-40 poise, added into methanol with the volume 1-2 times of that of the filtrate for pulping, stirred and cooled to 20-28 ℃.
7. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: and (5) adding the filter cake containing inositol and potassium chloride and the inositol saturated solution into the inositol saturated solution according to the ratio of 1:1-2 (w/v).
8. The process for producing plant-derived potassium dihydrogen phosphate as described in claim 1, wherein: and (3) combining the two-time collected inositol crude product filter cakes, adding water, heating and concentrating until the solid content is 45-55wt%, preserving heat to 95-100 ℃, adding a decoloring agent, preserving heat and decoloring, filtering, heating the collected filtrate to 95-100 ℃ for full dissolution, and cooling to 28-32 ℃ for filtering.
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