CN116813447A - Method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water - Google Patents
Method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water Download PDFInfo
- Publication number
- CN116813447A CN116813447A CN202310702268.9A CN202310702268A CN116813447A CN 116813447 A CN116813447 A CN 116813447A CN 202310702268 A CN202310702268 A CN 202310702268A CN 116813447 A CN116813447 A CN 116813447A
- Authority
- CN
- China
- Prior art keywords
- hydrogen phosphate
- disodium hydrogen
- inositol
- temperature
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 title claims abstract description 110
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 title claims abstract description 80
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 title claims abstract description 75
- 229960000367 inositol Drugs 0.000 title claims abstract description 75
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 26
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 26
- 235000005822 corn Nutrition 0.000 title claims abstract description 26
- 238000002791 soaking Methods 0.000 title claims abstract description 13
- 240000008042 Zea mays Species 0.000 title claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 90
- 239000000047 product Substances 0.000 claims description 85
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 claims description 68
- 229940083982 sodium phytate Drugs 0.000 claims description 68
- 238000002425 crystallisation Methods 0.000 claims description 51
- 230000008025 crystallization Effects 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 41
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 36
- 239000011347 resin Substances 0.000 claims description 36
- 229920005989 resin Polymers 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 34
- 238000004458 analytical method Methods 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 26
- 230000007062 hydrolysis Effects 0.000 claims description 23
- 238000006460 hydrolysis reaction Methods 0.000 claims description 23
- 238000004587 chromatography analysis Methods 0.000 claims description 20
- 239000012535 impurity Substances 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 19
- 239000011780 sodium chloride Substances 0.000 claims description 18
- 239000012452 mother liquor Substances 0.000 claims description 16
- 238000005119 centrifugation Methods 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 15
- 239000003957 anion exchange resin Substances 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- 239000000413 hydrolysate Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 239000012528 membrane Substances 0.000 claims description 13
- 238000001728 nano-filtration Methods 0.000 claims description 13
- 235000002949 phytic acid Nutrition 0.000 claims description 13
- 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 description 12
- 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 12
- 239000003729 cation exchange resin Substances 0.000 claims description 12
- 238000004806 packaging method and process Methods 0.000 claims description 12
- 229940068041 phytic acid Drugs 0.000 claims description 12
- 239000000467 phytic acid Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 9
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 7
- 238000004042 decolorization Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000008213 purified water Substances 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 2
- 229920002261 Corn starch Polymers 0.000 abstract description 3
- 239000008120 corn starch Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 241000209149 Zea Species 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 23
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 10
- 235000019799 monosodium phosphate Nutrition 0.000 description 10
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 150000001768 cations Chemical group 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 101100283604 Caenorhabditis elegans pigk-1 gene Proteins 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002198 insoluble material Substances 0.000 description 4
- 238000010979 pH adjustment Methods 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 238000013375 chromatographic separation Methods 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 239000002367 phosphate rock Substances 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 208000004930 Fatty Liver Diseases 0.000 description 1
- 206010019708 Hepatic steatosis Diseases 0.000 description 1
- 208000035150 Hypercholesterolemia Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229930012538 Paclitaxel Natural products 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 208000019425 cirrhosis of liver Diseases 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 208000010706 fatty liver disease Diseases 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 1
- 229960005436 inositol nicotinate Drugs 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- MFZCIDXOLLEMOO-GYSGTQPESA-N myo-inositol hexanicotinate Chemical compound O([C@H]1[C@@H]([C@H]([C@@H](OC(=O)C=2C=NC=CC=2)[C@@H](OC(=O)C=2C=NC=CC=2)[C@@H]1OC(=O)C=1C=NC=CC=1)OC(=O)C=1C=NC=CC=1)OC(=O)C=1C=NC=CC=1)C(=O)C1=CC=CN=C1 MFZCIDXOLLEMOO-GYSGTQPESA-N 0.000 description 1
- 229960001592 paclitaxel Drugs 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- -1 phytate ions Chemical class 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000012492 regenerant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- RCINICONZNJXQF-MZXODVADSA-N taxol Chemical compound O([C@@H]1[C@@]2(C[C@@H](C(C)=C(C2(C)C)[C@H](C([C@]2(C)[C@@H](O)C[C@H]3OC[C@]3([C@H]21)OC(C)=O)=O)OC(=O)C)OC(=O)[C@H](O)[C@@H](NC(=O)C=1C=CC=CC=1)C=1C=CC=CC=1)O)C(=O)C1=CC=CC=C1 RCINICONZNJXQF-MZXODVADSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—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
- 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
- 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
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application belongs to the technical field of corn starch production, and discloses a method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water. The application can effectively separate inositol from disodium hydrogen phosphate, has simple process, and the obtained product has high yield and good quality.
Description
Technical Field
The application belongs to the technical field of corn starch production, and particularly relates to a method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water.
Background
Inositol (inolitol) chemical name: cyclohexanol is an important vitamin required in higher animals. Inositol can promote fat metabolism, reduce cholesterol content in blood, and can be used as anti-fatty liver medicine for treating liver cirrhosis, hepatitis, hypercholesterolemia, hyperlipidemia and arteriosclerosis. Besides being directly used as medicines, inositol can be used as medical intermediates, such as inositol tablet, hepatic alcohol, liver soothing tablet, etc., and can be prepared into a plurality of medicines, such as inositol nicotinate, maitong, anticancer medicine taxol, etc.
Disodium hydrogen phosphate is an industrial product with wide application, and is used as a boiler water softener, a flame retardant for fabrics, wood and paper, a glaze and a welding flux; the method can also be used for producing detergents, cleaning agents of printing and dyeing plates and mordants for dyeing; in the printing and dyeing industry, disodium hydrogen phosphate is used as a stabilizer for hydrogen peroxide bleaching, and fillers for rayon (to enhance the strength and elasticity of the yarn); disodium hydrogen phosphate is also used as raw material for preparing pyrophosphoric acid and other phosphates, as culture agent for monosodium glutamate, antibiotics and biochemical sewage treatment products, and also in electroplating and tanning industries.
Corn soaking water is leftovers generated in the process of producing corn starch by a wet method, and contains rich phosphorus resources: the phytic acid contains impurities such as calcium, magnesium, protein, polysaccharide, lactic acid and the like besides the phytic acid, and the recovery of phosphorus resources from the corn soaking water can not only avoid environmental damage caused by the exploitation of phosphorite, but also relieve the situation of shortage of phosphorite resources in China. In the existing process for producing inositol and disodium hydrogen phosphate by using corn soaking water, an ideal method for removing relevant impurities is not available, so that the impurity content in the subsequent process is high, and the product quality is affected. In addition, inositol and disodium hydrogen phosphate have small molecular weight difference and small solubility difference, and traditional separation means such as membrane filtration, ion exchange resin and the like are utilized, so that the separation effect is poor and the operation cost is high.
Disclosure of Invention
The technical problems to be solved by the application are as follows: the method for co-producing the inositol and the disodium hydrogen phosphate by using the corn soaking water overcomes the defects in the prior art, can effectively separate the inositol from the disodium hydrogen phosphate, and has the advantages of simple process, stable operation, low cost, high yield of the inositol and the disodium hydrogen phosphate and good quality.
In order to solve the technical problems, the technical scheme of the application is as follows:
a method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water, which comprises the following steps:
a. adsorption of sodium phytate: the corn soaking water passes through the weak alkaline anion exchange resin at the flow rate of 1-2 BV/h;
the step aims at enabling phytic acid to be adsorbed by resin, so that organic impurities such as protein, starch and the like flow out along with corn soaking water;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 8-15% (W/V), the pH of the sodium phytate analysis solution is 5-7, and the dosage is 1.5-2.5 BV of the resin volume, thus obtaining diluted sodium phytate solution;
c. concentrating sodium phytate: adding a pH regulator into the diluted sodium phytate solution obtained in the step b to adjust the pH value to 9-11, and then filtering the diluted sodium phytate solution by a plate frame to remove insoluble matters; concentrating by using a nanofiltration membrane to obtain sodium phytate concentrated solution with the concentration of 20-40% (W/V); wherein the aperture of the plate-frame filtering cloth is 300-400 meshes, the molecular weight cut-off of the nanofiltration membrane is 500-1000D, and the chloride ion content in the sodium phytate solution is 300-600 ppm;
d. hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to the temperature of 150-180 ℃ and the pressure of 0.6-0.8 MPa, and preserving heat and pressure for 8-10 h until the hydrolysis is finished to obtain a hydrolysate;
e. separating: d, carrying out flash evaporation cooling on the hydrolysate obtained in the step d, adding activated carbon for decolorization, filtering by a plate frame, allowing filtrate to enter a crystallization tank, cooling for crystallization, and centrifuging to obtain disodium hydrogen phosphate wet product (the mole number of disodium hydrogen phosphate in the hydrolysate is 6 times that of inositol, and after concentration, crystallizing a part of disodium hydrogen phosphate to reduce the chromatographic feed quantity of a simulated moving bed); the mother liquor obtained by centrifugation contains residual disodium hydrogen phosphate and inositol, and the mother liquor is separated by simulated moving bed chromatography to separate inositol and residual disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, centrifuging by a centrifuge, and drying, crushing, packaging and the like to obtain an inositol product; the centrifugal mother liquor is mainly inositol, contains a small amount of disodium hydrogen phosphate, and can be returned to the simulated moving bed chromatography in the step e;
g. preparing a disodium hydrogen phosphate wet product: concentrating the separated disodium hydrogen phosphate solution in the step e through a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product;
h. disodium hydrogen phosphate preparation: and e, drying, crushing, packaging and other procedures on the disodium hydrogen phosphate wet product obtained in the steps e and g to obtain the disodium hydrogen phosphate product.
Preferably, the corn steep water in step a is passed through the weakly basic anion exchange resin at a flow rate of 1.5 BV/h.
Preferably, in the step b, the concentration of the NaCl solution is 11% (W/V), the pH of the sodium phytate analysis solution is 6, and the dosage is 2.0BV of the resin volume.
Preferably, in the step b, the analysis is carried out in a time-division manner, the first half is a qualified diluted sodium phytate solution, the second half has high chloride ion content and low sodium phytate content, and the next batch of analysis is carried out as a mechanically applied liquid.
Preferably, the pH regulator in the step c is Na 2 CO 3 With NaOH, or NaHCO 3 Mixing with NaOH; na (Na) 2 CO 3 With NaOH and NaHCO 3 The molar ratio of the sodium hydroxide to NaOH is 2-3:1, and the pH value is regulated to 10.
Further, the pH regulator is NaHCO with the molar ratio of 2.5:1 3 And NaOH.
Preferably, in the step c, a concentrated solution of sodium phytate with the concentration of 30% (W/V) is obtained; the aperture of the plate and frame filter cloth is 350 meshes, the molecular weight cut-off of the nanofiltration membrane is 750D, and the chloride ion content in the sodium phytate solution is 450ppm.
Preferably, in the step d, the temperature is heated to 165 ℃, and the pressure is 0.7MPa, and then the heat preservation and the pressure maintaining are carried out for 9 hours.
Preferably, in the step e, the temperature after flash evaporation is 75-95 ℃, the feeding temperature is 150-180 ℃, and the vacuum degree is-0.07 to-0.09 MPa; the aperture of the filter cloth for plate frame filtration is 300-400 meshes; the dosage of the active carbon is 1-5% (W/V) of the volume of the feed liquid, and the crystallization and centrifugation temperature is 25-35 ℃; the simulated moving bed chromatographic packing is strong acid cation exchange resin, the mobile phase is purified water, and the separation conditions are as follows: the temperature is 50-60 ℃, the pressure is 0.1-0.4 MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 5-8 m 3 And/h, the flow velocity of the mobile phase is 10-20 m 3 /h。
Further, in the step e, the temperature after flash evaporation is 85 ℃, the feeding temperature is 165 ℃, and the vacuum is-0.08 MPa; the aperture of the filter cloth for plate frame filtration is 350 meshes; the dosage of the active carbon is 3% (W/V) of the volume of the feed liquid, and the crystallization centrifugation temperature is 30 ℃; the simulated moving bed chromatographic separation conditions are as follows: the temperature is 55 ℃, the pressure is 0.25MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 6.5m 3 /h, flow rate of mobile phase 15m 3 /h。
Preferably, in the step f, the multi-effect concentrator is a plate type four-effect concentrator, the concentration vacuum is-0.07 to-0.09 MPa, the temperature is 75-85 ℃, the solid content of concentrated liquid is 35-45%, the consumption of active carbon is 3-5% (W/V) of the liquid amount, the filtering equipment is a candle filter, the crystallization centrifugation temperature is 25-35 ℃, the drying mode is fluidized bed drying, the air inlet temperature is 140-160 ℃, the air outlet temperature is 75-90 ℃, and the drying time is 6-8 min.
Further, in the step f, the concentration vacuum is-0.08 MPa, the temperature is 80 ℃, the solid content of the concentrated solution is 40%, the consumption of active carbon is 4% (W/V) of the liquid amount, the filtering equipment is a candle filter, the crystallization centrifugation temperature is 30 ℃, the drying mode is fluidized bed drying, the air inlet temperature is 150 ℃, the air outlet temperature is 85 ℃, and the drying time is 7min.
Preferably, in the step g, the multi-effect concentrator is a plate-type four-effect concentrator, the concentration vacuum is-0.07 to-0.09 MPa, the temperature is 80 to 90 ℃, and the solid content of the concentrated solution is 40 to 50 percent; the consumption of the active carbon is 2-4% (W/V) of the liquid amount, the filtering equipment is a candle filter, and the crystallization centrifugation temperature is 25-35 ℃.
Further, in the step g, the vacuum concentration is-0.08 MPa, the temperature is 85 ℃, and the solid content of the concentrated solution is 45%; the amount of active carbon is 3% (W/V) of the liquid amount, the filter equipment is a candle filter, and the crystallization centrifugation temperature is 30 ℃.
Preferably, the drying mode in the step h is fluidized bed drying, the air inlet temperature is 60-80 ℃, the air outlet temperature is 35-50 ℃, and the drying time is 3-4 min.
Further, in the step h, the air inlet temperature is 70 ℃, the air outlet temperature is 45 ℃, and the drying time is 3.5min.
Due to the adoption of the technical scheme, the application has the beneficial effects that:
1. in the application, sodium phytate solution is taken as an resolving agent for resolving and is collected in sections to obtain dilute sodium phytate solution; compared with sodium hydroxide, the sodium chloride has lower cost, and has small solubility to organic impurities such as proteins adsorbed on the resin during analysis, low content of organic impurities in analysis liquid and better quality of analysis liquid.
2. In the application, a pH regulator is added into the analysis liquid to precipitate calcium and magnesium ions, the filtrate after filtration enters a nanofiltration membrane concentration system, and sodium phytate is concentrated and residual chloride ions are removed. The pH is adjusted to ensure that the pH range of the hydrolyzed feed liquid is in the disodium hydrogen phosphate generation interval, so that the generation of sodium dihydrogen phosphate is reduced; meanwhile, as the pH value rises, calcium and magnesium ions generate precipitates, so that the impurity ion content in the feed liquid is reduced, and the purity of the crystallized product is improved. The concentration of chloride ions in the feed liquid is reduced during concentration, so that corrosion of chloride ions to equipment such as hydrolysis, concentration and the like can be reduced, the material requirement of the equipment is reduced, and the investment is saved; meanwhile, the chloride ion residue in the crystallized product can be reduced, and the product quality is improved.
3. The separation of inositol and disodium hydrogen phosphate adopts the steps that sodium phytate hydrolysate is subjected to flash evaporation, cooling, decoloration and filtration and then is subjected to primary crystallization to obtain a disodium hydrogen phosphate product; and (3) feeding the crystallized mother liquor into a chromatographic separation system to separate inositol from the rest disodium hydrogen phosphate. The traditional process adopts ion exchange resin to remove disodium hydrogen phosphate in the mother liquor, so that the resin consumption is large, the regenerant consumption is large, and the operation cost is high; the simulated moving bed chromatography utilizes the polarity difference of inositol and disodium hydrogen phosphate, uses water as a mobile phase, realizes separation of the inositol and the disodium hydrogen phosphate on a bed, and has the advantages of less resin consumption, low running cost and high separation efficiency.
In a word, the application can effectively separate inositol from disodium hydrogen phosphate, has simple process, stable operation, low cost, high yield of inositol and disodium hydrogen phosphate and good quality.
Detailed Description
The technical scheme of the application is further described below by combining examples:
example 1:
a. adsorption of sodium phytate: 70m of 3 Corn steep water is passed through the weak base anion exchange resin at a flow rate of 1 BV/h;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 8% (W/V), the pH of the sodium phytate analysis solution is 5, and the dosage is 2.5BV of the resin volume, thus obtaining diluted sodium phytate solution;
c. concentrating sodium phytate: adding the diluted sodium phytate solution obtained in the step b into a pH regulator (NaHCO with the molar ratio of 2:1 3 Mix with NaOH) to adjust pH to 9, then plate and frame filtration to remove insoluble material; concentrating with nanofiltration membrane to obtain sodium phytate concentrate with concentration of 20% (W/V) of 6.0m 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the aperture of the plate-frame filter cloth is 400 meshes, and the molecular weight cut-off of the nanofiltration membrane is 500D;
d. hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to the temperature of 150 ℃ and the pressure of 0.6MPa, and preserving heat and pressure for 10 hours until hydrolysis is finished to obtain a hydrolysate;
e. separating: d, cooling the hydrolysate obtained in the step d by flash evaporation, wherein the temperature after flash evaporation is 75 ℃ (the feeding temperature is 150 ℃ and the vacuum is-0.09 MPa); adding activated carbon with the dosage of 1% (W/V) of the volume of the feed liquid, decoloring, filtering with a plate frame with a filter cloth aperture of 300 meshes, cooling the filtrate to 25 ℃ for crystallization, and centrifuging at 1600rpm to obtain a disodium hydrogen phosphate wet product; separating mother liquor obtained by centrifugation by simulated moving bed chromatography, wherein the simulated moving bed chromatography filler is strong acid cation exchange resin, and the mobile phase is purified water; the separation conditions are as follows: the temperature is 50 ℃, the pressure is 0.1MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 5m 3 /h, flow rate of mobile phase 10m 3 /h; separating myo-inositol and the remaining disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.07 MPa, the temperature is 85 ℃, and the solid content of the obtained concentrated solution is 35%; then adding activated carbon with the dosage of 3% (W/V) of the material liquid, decolorizing, filtering with a candle filter, cooling and crystallizing in a crystallization tank, centrifuging in a centrifuge, wherein the crystallization centrifuging temperature is 25 ℃, drying the centrifuged wet product in a fluidized bed (the air inlet temperature is 140 ℃, the air outlet temperature is 75 ℃, and the drying time is 8 min), crushing, packaging and other procedures to obtain an inositol product, wherein the weight of the inositol product is 195kg; the product yield is 70.9%, and the centrifugal mother liquor returns to the simulated moving bed chromatography in the step e for separation;
g. preparing a disodium hydrogen phosphate wet product: concentrating the disodium hydrogen phosphate solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.07 MPa, the temperature is 90 ℃, and the solid content of the concentrated solution is 40%; then adding activated carbon with the dosage of 2% (W/V) of the feed liquid for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product, wherein the crystallization centrifuging temperature is 25 ℃;
h. disodium hydrogen phosphate preparation: drying the disodium hydrogen phosphate wet product obtained in the step e and the step g by a fluidized bed (the air inlet temperature is 60 ℃, the air outlet temperature is 35 ℃, and the drying time is 4 min), crushing, packaging and other procedures to obtain a disodium hydrogen phosphate product, wherein the weight of the disodium hydrogen phosphate product is 2600kg; the product yield was 79.5%.
Example 2:
a. adsorption of sodium phytate: 70m of 3 Is passed through a weak base anion exchange resin at a flow rate of 2 BV/h;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 15% (W/V), the pH value of the sodium phytate analysis solution is 7, and the dosage is 1.5BV of the resin volume, thus obtaining diluted sodium phytate solution;
c. concentrating sodium phytate: adding the diluted sodium phytate solution obtained in the step b into a pH regulator (NaHCO with the molar ratio of 3:1 3 Mix with NaOH) to adjust pH to 11, then plate and frame filtration to remove insoluble material; concentrating with nanofiltration membrane to obtain concentrated solution of sodium phytate with concentration of 40% (W/V) 2.9m 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the aperture of the plate-frame filter cloth is 300 meshes, and the molecular weight cut-off of the nanofiltration membrane is 1000D.
d. Hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to 180 ℃, maintaining the temperature and pressure for 8 hours after the pressure is 0.8MPa, and obtaining hydrolysate;
e. separating: d, cooling the hydrolysate obtained in the step d by flash evaporation, wherein the temperature after flash evaporation is 95 ℃ (the feeding temperature is 180 ℃ and the vacuum is-0.07 MPa); adding activated carbon with the dosage of 5% (W/V) of the volume of the feed liquid, decolorizing, filtering with a filter cloth with a plate frame with a pore diameter of 400 meshes, cooling the filtrate to 35 ℃ for crystallization, and centrifuging at 1200rpm to obtain disodium hydrogen phosphate wet product; separating mother liquor obtained by centrifugation by simulated moving bed chromatography, wherein the simulated moving bed chromatography filler is strong acid cation exchange resin, and the mobile phase is purified water; the separation conditions are as follows: the temperature is 60 ℃, the pressure is 0.4MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 8m 3 /h, flow rate of mobile phase 20m 3 /h; separating myo-inositol and the remaining disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.09 MPa, the temperature is 75 ℃, and the solid content of the obtained concentrated solution is 45%; then adding activated carbon with the dosage of 5% (W/V) of the feed liquid for decolorization, filtering by a candle filter, cooling and crystallizing in a crystallization tank, centrifuging by a centrifuge, wherein the crystallization centrifuging temperature is 35 ℃, drying the centrifuged wet product by a fluidized bed (the air inlet temperature is 160 ℃, the air outlet temperature is 90 ℃, and the drying time is 6 min), crushing, packaging and other working procedures to obtain inositol products, wherein the weight of the inositol products is 190kg; the product yield is 71.4%, and the centrifugal mother liquor returns to the simulated moving bed chromatography in the step e for separation;
g. preparing a disodium hydrogen phosphate wet product: concentrating the disodium hydrogen phosphate solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.09 MPa, the temperature is 80 ℃, and the solid content of the concentrated solution is 50%; then adding activated carbon with the dosage of 4% (W/V) of the material liquid for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product, wherein the crystallization centrifuging temperature is 35 ℃;
h. disodium hydrogen phosphate preparation: c, drying the disodium hydrogen phosphate wet product obtained in the step e and the step g by a fluidized bed (the air inlet temperature is 80 ℃, the air outlet temperature is 50 ℃, and the drying time is 3 min), crushing, packaging and other working procedures to obtain a disodium hydrogen phosphate product, wherein the weight of the disodium hydrogen phosphate product is 2550kg; the product yield was 80.6%.
Example 3:
a. adsorption of sodium phytate: 70m of 3 Corn steep water was passed through the weakly basic anion exchange resin at a flow rate of 1.5 BV/h;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 11% (W/V), the pH of the sodium phytate analysis solution is 6, and the dosage is 2BV of the resin volume, thus obtaining diluted sodium phytate solution;
c. concentrating sodium phytate: adding the diluted sodium phytate solution obtained in the step b into a pH regulator (NaHCO with the molar ratio of 2.5:1 3 Mix with NaOH) to adjust pH to 10, then plate and frame filtration to remove insoluble material; concentrating with nanofiltration membrane to obtain sodium phytate concentrate with concentration of 30% (W/V) 4m 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the aperture of the plate-frame filter cloth is 350 meshes, and the molecular weight cut-off of the nanofiltration membrane is 750D.
d. Hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to 165 ℃ and 0.7MPa, and preserving heat and pressure for 9 hours until hydrolysis is finished to obtain a hydrolysate;
e. separating: d, cooling the hydrolysate obtained in the step d by flash evaporation, wherein the temperature is 85 ℃ (the feeding temperature is 165 ℃ and the vacuum is-0.08 MPa) after the flash evaporation; adding activated carbon with the dosage of 3% (W/V) of the volume of the feed liquid, decoloring, filtering with a filter cloth with a plate frame with the aperture of 350 meshes, cooling the filtrate to 30 ℃ for crystallization, and centrifuging at 1400rpm to obtain a disodium hydrogen phosphate wet product; separating mother liquor obtained by centrifugation by simulated moving bed chromatography, wherein the simulated moving bed chromatography filler is strong acid cation exchange resin, and the mobile phase is purified water; the separation conditions are as follows: the temperature is 55 ℃, the pressure is 0.25MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 6.5m 3 /h, flow rate of mobile phase 15m 3 /h; separating myo-inositol and the remaining disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.08 MPa, the temperature is 80 ℃, and the solid content of the obtained concentrated solution is 40%; then adding activated carbon with the dosage of 4% (W/V) of the material liquid, decolorizing, filtering with a candle filter, cooling and crystallizing in a crystallization tank, centrifuging in a centrifuge, wherein the crystallization centrifuging temperature is 30 ℃, drying the centrifuged wet product in a fluidized bed (the air inlet temperature is 150 ℃, the air outlet temperature is 85 ℃, and the drying time is 7 min), crushing, packaging and other procedures to obtain inositol product, wherein the weight of inositol product is 200kg; the product yield is 72.7%, and the centrifugal mother liquor returns to the simulated moving bed chromatography in the step e for separation;
g. preparing a disodium hydrogen phosphate wet product: concentrating the disodium hydrogen phosphate solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.08 MPa, the temperature is 85 ℃, and the solid content of the concentrated solution is 45%; then adding activated carbon with the dosage of 3% (W/V) of the material liquid for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product, wherein the crystallization centrifuging temperature is 30 ℃;
h. disodium hydrogen phosphate preparation: drying the disodium hydrogen phosphate wet product obtained in the step e and the step g by a fluidized bed (the air inlet temperature is 70 ℃, the air outlet temperature is 45 ℃, and the drying time is 3.5 min), crushing, packaging and other working procedures to obtain the disodium hydrogen phosphate product, wherein the weight of the disodium hydrogen phosphate product is 2670kg; the product yield was 81.6%.
Example 4:
a. adsorption of sodium phytate: 70m of 3 Corn steep water was passed through the weakly basic anion exchange resin at a flow rate of 1.5 BV/h;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 11% (W/V), the pH of the sodium phytate analysis solution is 6, and the dosage is 2BV of the resin volume, thus obtaining diluted sodium phytate solution;
c. concentrating sodium phytate: adding the diluted sodium phytate solution obtained in the step b into a pH regulator (Na with the molar ratio of 2.5:1 2 CO 3 Mix with NaOH) to adjust pH to 10, then plate and frame filtration to remove insoluble material; concentrating with nanofiltration membrane to obtain sodium phytate concentrate with concentration of 30% (W/V) 4m 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the aperture of the plate-frame filter cloth is 350 meshes, and the molecular weight cut-off of the nanofiltration membrane is 750D.
d. Hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to 165 ℃ and 0.7MPa, and preserving heat and pressure for 9 hours until hydrolysis is finished to obtain a hydrolysate;
e. separating: d, cooling the hydrolysate obtained in the step d by flash evaporation, wherein the temperature is 85 ℃ (the feeding temperature is 165 ℃ and the vacuum is-0.08 MPa) after the flash evaporation; adding activated carbon with the dosage of 3% (W/V) of the volume of the feed liquid, decoloring, filtering with a filter cloth with a plate frame with the aperture of 350 meshes, cooling the filtrate to 30 ℃ for crystallization, and centrifuging at 1400rpm to obtain a disodium hydrogen phosphate wet product; separating mother liquor obtained by centrifugation by simulated moving bed chromatography, wherein the simulated moving bed chromatography filler is strong acid cation exchange resin, and the mobile phase is purified water; the separation conditions are as follows: the temperature is 55 ℃, the pressure is 0.25MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 6.5m 3 /h, flow rate of mobile phase 15m 3 /h; separating myo-inositol and the remaining disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.08 MPa, the temperature is 80 ℃, and the solid content of the obtained concentrated solution is 40%; then adding activated carbon with the dosage of 4% (W/V) of the material liquid, decolorizing, filtering with a candle filter, cooling and crystallizing in a crystallization tank, centrifuging in a centrifuge, wherein the crystallization centrifuging temperature is 30 ℃, drying the centrifuged wet product in a fluidized bed (the air inlet temperature is 150 ℃, the air outlet temperature is 85 ℃, and the drying time is 7 min), crushing, packaging and other procedures to obtain an inositol product, wherein the weight of the inositol product is 198kg; the product yield is 72.0%, and the centrifugal mother liquor returns to the simulated moving bed chromatography in the step e for separation;
g. preparing a disodium hydrogen phosphate wet product: concentrating the disodium hydrogen phosphate solution separated in the step e by a plate type four-effect concentrator, wherein the concentration vacuum is-0.08 MPa, the temperature is 85 ℃, and the solid content of the concentrated solution is 45%; then adding activated carbon with the dosage of 3% (W/V) of the material liquid for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product, wherein the crystallization centrifuging temperature is 30 ℃;
h. disodium hydrogen phosphate preparation: drying the disodium hydrogen phosphate wet product obtained in the step e and the step g by a fluidized bed (the air inlet temperature is 70 ℃, the air outlet temperature is 45 ℃, and the drying time is 3.5 min), crushing, packaging and other working procedures to obtain the disodium hydrogen phosphate product, wherein the weight of the disodium hydrogen phosphate product is 2630kg; the product yield was 80.4%.
Comparative example 1:
the NaCl in step b of example 1 was replaced by an equal amount of NaOH, the other conditions being unchanged. 185kg of inositol product weight is obtained; the product yield is 65.8%; the weight of the obtained disodium hydrogen phosphate product is 2380kg, and the product yield is 71.9%.
Comparative example 2:
the pH adjustment step of example 2, step c, was removed, with the other conditions unchanged. The weight of the obtained inositol product is 160kg; the product yield was 57.5%; the product weight of disodium hydrogen phosphate (containing more sodium dihydrogen phosphate) is 890kg, and the product yield is 45.3%.
Comparative example 3:
the pH adjustor in step c of example 3 was changed to NaOH, and the other conditions were unchanged. The weight of the obtained inositol product is 190kg; the product yield was 68.9%; the weight of the obtained disodium hydrogen phosphate product is 2415kg, and the product yield is 74.7%.
Comparative example 4:
the simulated moving bed chromatography in step e of example 4 was replaced with a cation and anion exchange resin to separate inositol from disodium hydrogen phosphate. The weight of the obtained inositol product is 175kg; the product yield was 63.4%; the weight of the obtained disodium hydrogen phosphate product is 2040kg, and the product yield is 62.1%.
Analysis of results:
the product data obtained in examples 1-3 and comparative examples 1-4 were analyzed, wherein inositol assay was performed according to the four methods of the pharmacopoeia of the people's republic of China, 2015 edition, and the results are shown in Table 1:
TABLE 1 inositol assay results obtained for examples 1-3 and comparative examples 1-4
From the results of inositol assay in examples and comparative examples, it can be seen that:
comparative example 1 after the phytic acid resolving agent of example 1 is changed from NaCl to NaOH in an equal amount, the organic impurity content in the sodium phytate resolving solution is increased due to the increase of the solubility of NaOH to organic impurities of protein, and the organic impurities interfere with inositol crystallization, so that both the yield of inositol crystallization and the purity of the product are reduced;
comparative example 2 after the pH adjustment step in step c of example 2, the hydrolysis product was mostly sodium dihydrogen phosphate, and since sodium dihydrogen phosphate has a significantly higher solubility in water than disodium hydrogen phosphate, no crystallization occurs when the hydrolysis solution is decolorized and filtered. The feed liquid enters a simulated moving bed chromatograph for separation, and as the proportion of sodium salt components to inositol components in the feed liquid is too high, the chromatographic separation effect is affected, so that the salinity in an inositol phase is obviously increased, and the crystallization yield and the product purity of the inositol are seriously affected.
Comparative example 3 removal of the pH adjustment in example 3 step cThe agent is NaHCO 3 After the mixture with NaOH is changed into NaOH, the burning residue in inositol crystallization is increased, and the yield is also reduced. This is because the carbonate ion reacts with the calcium salt to form poorly soluble calcium carbonate, and if NaOH alone is added to form slightly soluble calcium hydroxide, the removal effect of calcium ions is poor, and calcium ions which are relatively more encapsulated in crystals and entrained on the surfaces of the crystals during crystallization cause an increase in the burning residue.
Comparative example 4 after the simulated moving bed chromatography in example e was replaced with cation and anion exchange resins, the cation and anion exchange resins were based on H carried on the resin ﹢ And OH (OH) ﹣ Respectively with Na in the feed liquid ﹢ And HPO4 2﹣ Exchange occurs, and separation of inositol and sodium salt is realized. Because the resin exchange capacity is limited and penetration easily occurs in the exchange process, the cation exchange resin and the anion exchange resin are generally suitable for desalting raw materials with low salt content, and for the case of the inositol solution containing saturated disodium hydrogen phosphate, the resin consumption is much larger, the separation effect is poor, and the inositol crystallization yield and the crystallization purity are reduced.
The detection of disodium hydrogen phosphate was carried out according to GB25568-2010, and the detection results are shown in Table 2:
TABLE 2 detection results of disodium hydrogen phosphate obtained in examples 1-3 and comparative examples 1-4
| Content% (dry basis) | Water insoluble matter% | Sodium dihydrogen phosphate% | Chloride ppm | Yield% | |
| Example 1 | 98.7 | 0.04 | 0.8 | ＜50 | 79.5 |
| Example 2 | 98.9 | 0.03 | 0.5 | ＜50 | 80.6 |
| Example 3 | 99.2 | 0.03 | 0.6 | ＜50 | 81.6 |
| Example 4 | 99.3 | 0.04 | 0.6 | ＜50 | 80.4 |
| Comparative example 1 | 97.6 | 0.04 | 0.3 | ＜50 | 71.9 |
| Comparative example 2 | 21.5 | 0.15 | 76.3 | ＜50 | 45.3 |
| Comparative example 3 | 98.0 | 0.2 | 0.3 | ＜50 | 74.7 |
| Comparative example 4 | 98.8 | 0.04 | 0.5 | ＜50 | 62.1 |
From the results of the disodium hydrogen phosphate detection in the examples and the comparative examples, it can be seen that:
comparative example 1 after the phytic acid resolving agent of example 1 is changed from NaCl to NaOH with the same amount, the organic impurity content in the sodium phytate resolving solution is increased due to the increase of the solubility of the NaOH to organic impurities of protein, and the organic impurities interfere with the crystallization of disodium hydrogen phosphate, so that the crystallization yield and the product purity of the disodium hydrogen phosphate are both reduced;
comparative example 2 after the pH adjustment step in step c of example 2, the hydrolysis product was mostly sodium dihydrogen phosphate, and since sodium dihydrogen phosphate has a significantly higher solubility in water than disodium hydrogen phosphate, no crystallization occurs when the hydrolysis solution is decolorized and filtered. The feed liquid enters a simulated moving bed chromatograph to be separated, so as to obtain a sodium dihydrogen phosphate phase, and the sodium dihydrogen phosphate phase is concentrated and then subjected to cooling crystallization, wherein the crystallization yield is obviously lower than that of disodium hydrogen phosphate in the embodiment 2;
comparative example 3 removal of the pH adjustor from NaHCO in example 3 step c 3 After the mixture of the sodium hydrogen phosphate and NaOH is changed into NaOH, the insoluble substance of the obtained disodium hydrogen phosphate is increased, and the yield is reduced. The pH is regulated by promoting divalent ions of calcium and magnesium in the desorption solution to form precipitate with low solubility, such as calcium carbonate, magnesium hydroxide and the like; on the other hand, the pH range of the hydrolyzed feed liquid is ensured to be in the disodium hydrogen phosphate generation interval, and the generation of sodium dihydrogen phosphate or trisodium phosphate is reduced. In order to ensure that phosphate ions are completely combined with sodium ions after hydrolysis and improve the yield of disodium hydrogen phosphate, 6 phosphate groups exist in the phytic acid molecule, the sodium ions in the analysis solution need to be complemented, and the mole ratio of the sodium ions to the phytate ions in the analysis solution is higher than 12:1, so that the pH regulator adopts NaHCO 3 With NaOH mixture or Na 2 CO 3 The method of mixing with NaOH can lead to the pH meeting the requirement if only NaOH is used, but the mole number of sodium ions does not reach the requirement, and the yield of disodium hydrogen phosphate is also affected.
Comparative example 4 after the simulated moving bed chromatography in step e of example 4 was replaced with cation and anion exchange resins, the cation and anion exchange resins were based on H carried on the resin ﹢ And OH (OH) ﹣ Respectively with Na in the feed liquid ﹢ And HPO4 2﹣ Exchange occurs, and separation of inositol and sodium salt is realized. Resin adsorbed Na ﹢ And HPO4 2﹣ The recovery of the part of disodium hydrogen phosphate can be realized only by respectively analyzing with an analysis agent, and because of the limitation of the exchange capacity of the ion exchange resin, the concentration of the analysis solution is low, a large amount of steam is consumed for concentration, and the production cost is greatly increased. Comparative example 4 resin adsorbed Na ﹢ And HPO4 2﹣ Without recovery, the disodium hydrogen phosphate yield was significantly reduced compared to comparative example 4.
In summary, example 3 of the present application is the optimal process conditions.
It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Claims (9)
1. A method for co-producing inositol and disodium hydrogen phosphate by using corn soaking water is characterized by comprising the following steps: the method comprises the following steps:
a. adsorption of sodium phytate: the corn soaking water passes through the weak alkaline anion exchange resin at the flow rate of 1-2 BV/h;
b. analysis of sodium phytate: c, washing the resin adsorbed and saturated in the step a with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with NaCl solution; wherein the concentration of NaCl solution is 8-15% W/V, the pH of the sodium phytate analysis solution is 5-7, and the dosage is 1.5-2.5 BV of the volume of the resin, thus obtaining diluted sodium phytate solution;
d. hydrolysis of sodium phytate: c, putting the sodium phytate concentrate obtained in the step c into a hydrolysis kettle, introducing steam, heating to the temperature of 150-180 ℃ and the pressure of 0.6-0.8 MPa, and preserving heat and pressure for 8-10 h until the hydrolysis is finished to obtain a hydrolysate;
e. separating: d, carrying out flash evaporation cooling on the hydrolysate obtained in the step d, adding activated carbon for decolorization, filtering by a plate frame, allowing filtrate to enter a crystallization tank, cooling for crystallization, and centrifuging to obtain a disodium hydrogen phosphate wet product; the mother liquor obtained by centrifugation contains residual disodium hydrogen phosphate and inositol, and the mother liquor is separated by simulated moving bed chromatography to separate inositol and residual disodium hydrogen phosphate;
f. inositol preparation: concentrating the inositol solution separated in the step e by a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, centrifuging by a centrifuge, and drying, crushing, packaging and the like to obtain an inositol product; returning the mother liquor to the simulated moving bed chromatography in the step e;
g. preparing a disodium hydrogen phosphate wet product: concentrating the separated disodium hydrogen phosphate solution in the step e through a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, and centrifuging to obtain a disodium hydrogen phosphate wet product;
h. disodium hydrogen phosphate preparation: and e, drying, crushing, packaging and other procedures on the disodium hydrogen phosphate wet product obtained in the steps e and g to obtain the disodium hydrogen phosphate product.
2. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: the corn steep water was passed through the weakly basic anion exchange resin at a flow rate of 1.5 BV/h.
3. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: in the step b, the concentration of the NaCl solution is 11% W/V, the pH of the sodium phytate analysis solution is 6, and the dosage is 2.0BV of the resin volume; and collecting the solution in a separating way, wherein the first half part is qualified diluted sodium phytate solution, and the second half part is used as a mechanically applied solution for next batch analysis.
4. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: the pH regulator in the step c is Na 2 CO 3 With NaOH, or NaHCO 3 Mixing with NaOH; na (Na) 2 CO 3 With NaOH and NaHCO 3 The molar ratio of the sodium hydroxide to NaOH is 2-3:1, and the pH value is regulated to 10; obtaining sodium phytate concentrated solution with the concentration of 30 percent W/V; the aperture of the plate and frame filter cloth is 350 meshes, the molecular weight cut-off of the nanofiltration membrane is 750D, and the chloride ion content in the sodium phytate solution is 450ppm.
5. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: and d, heating to 165 ℃ and maintaining the temperature and pressure for 9 hours after the pressure is 0.7 MPa.
6. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: the temperature after flash evaporation in the step e is 75-95 ℃, the feeding temperature is 150-180 ℃, and the vacuum degree is-0.07 to-0.09 MPa; the aperture of the filter cloth for plate frame filtration is 300-400 meshes; the dosage of the active carbon is 1-5% of the volume of the feed liquid, and the crystallization and centrifugation temperature is 25-35 ℃; the simulated moving bed chromatographic packing is strong acid cation exchange resin, the mobile phase is purified water, and the separation conditions are as follows: the temperature is 50-60 ℃,the pressure is 0.1-0.4 MPa, the valve switching time is 10min, and the flow rate of the feed liquid is 5-8 m 3 And/h, the flow velocity of the mobile phase is 10-20 m 3 /h。
7. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: in the step f, the multi-effect concentrator is a plate-type four-effect concentrator, the concentration vacuum is-0.07 to-0.09 MPa, the temperature is 75-85 ℃, the solid content of concentrated solution is 35-45%, the consumption of active carbon is 3-5% of the liquid amount, the filtering equipment is a candle filter, the crystallization centrifugation temperature is 25-35 ℃, the drying mode is fluidized bed drying, the air inlet temperature is 140-160 ℃, the air outlet temperature is 75-90 ℃, and the drying time is 6-8 min.
8. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: the multi-effect concentrator in the step g is a plate type four-effect concentrator, the concentration vacuum is-0.07 to-0.09 MPa, the temperature is 80-90 ℃, and the solid content of the concentrated solution is 40-50%; the consumption of the active carbon is 2-4% of the liquid amount, the filtering equipment is a candle filter, and the crystallization centrifugation temperature is 25-35 ℃.
9. The method for co-producing inositol and disodium hydrogen phosphate by using corn steep water according to claim 1, wherein: and in the step h, the drying mode is fluidized bed drying, the air inlet temperature is 60-80 ℃, the air outlet temperature is 35-50 ℃, and the drying time is 3-4 min.
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|---|---|---|---|---|
| CN117296988A (en) * | 2023-11-29 | 2023-12-29 | 诸城市浩天药业有限公司 | Technological method for producing feed acidifier by using corn soaking water |
| CN117448390A (en) * | 2023-12-25 | 2024-01-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117296988A (en) * | 2023-11-29 | 2023-12-29 | 诸城市浩天药业有限公司 | Technological method for producing feed acidifier by using corn soaking water |
| CN117296988B (en) * | 2023-11-29 | 2024-02-13 | 诸城市浩天药业有限公司 | Technological method for producing feed acidifier by using corn soaking water |
| CN117448390A (en) * | 2023-12-25 | 2024-01-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
| CN117448390B (en) * | 2023-12-25 | 2024-03-26 | 诸城市浩天药业有限公司 | Method for producing low-molecular phosphoinositide salt by using corn soaking water |
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