CN116813448A - Method for co-producing inositol and liquid fertilizer by using corn soaking water - Google Patents
Method for co-producing inositol and liquid fertilizer by using corn soaking water Download PDFInfo
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- CN116813448A CN116813448A CN202310702272.5A CN202310702272A CN116813448A CN 116813448 A CN116813448 A CN 116813448A CN 202310702272 A CN202310702272 A CN 202310702272A CN 116813448 A CN116813448 A CN 116813448A
- Authority
- CN
- China
- Prior art keywords
- liquid fertilizer
- inositol
- resin
- potassium phytate
- solution
- Prior art date
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- 239000007788 liquid Substances 0.000 title claims abstract description 65
- 239000003337 fertilizer Substances 0.000 title claims abstract description 57
- 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 55
- 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 53
- 229960000367 inositol Drugs 0.000 title claims abstract description 53
- 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 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 42
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 42
- 235000005822 corn Nutrition 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000002791 soaking Methods 0.000 title claims abstract description 24
- 240000008042 Zea mays Species 0.000 title claims description 41
- 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 62
- 235000002949 phytic acid Nutrition 0.000 claims description 62
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 57
- 239000011591 potassium Substances 0.000 claims description 57
- 229910052700 potassium Inorganic materials 0.000 claims description 57
- 239000011347 resin Substances 0.000 claims description 39
- 229920005989 resin Polymers 0.000 claims description 39
- 230000007062 hydrolysis Effects 0.000 claims description 20
- 238000006460 hydrolysis reaction Methods 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 16
- 229910019142 PO4 Inorganic materials 0.000 claims description 15
- 239000010452 phosphate Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- 239000003957 anion exchange resin Substances 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 14
- 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 13
- 238000004458 analytical method Methods 0.000 claims description 13
- 238000001704 evaporation Methods 0.000 claims description 13
- 230000008020 evaporation Effects 0.000 claims description 13
- 125000002091 cationic group Chemical group 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 9
- 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 8
- 239000000467 phytic acid Substances 0.000 claims description 8
- 229940068041 phytic acid Drugs 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000002738 chelating agent Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 238000001728 nano-filtration Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000000413 hydrolysate Substances 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 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 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 239000013522 chelant Substances 0.000 claims description 3
- 238000013375 chromatographic separation Methods 0.000 claims description 3
- 238000004042 decolorization Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 229920002261 Corn starch Polymers 0.000 abstract description 3
- 239000008120 corn starch Substances 0.000 abstract description 3
- 241000209149 Zea Species 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 235000013399 edible fruits Nutrition 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 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
- 230000007547 defect Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000004720 fertilization Effects 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- 239000002367 phosphate rock Substances 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 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
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229930012538 Paclitaxel Natural products 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 240000003768 Solanum lycopersicum Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 238000003556 assay Methods 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
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical group [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 208000019425 cirrhosis of liver Diseases 0.000 description 1
- 238000004040 coloring Methods 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
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 208000010706 fatty liver disease Diseases 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
- 229960005436 inositol nicotinate Drugs 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 210000004185 liver Anatomy 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
- 239000012452 mother liquor 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
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229960001592 paclitaxel Drugs 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000003756 stirring Methods 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
- 235000018648 unbalanced nutrition Nutrition 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- 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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- 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)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Health & Medical 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 a liquid fertilizer by using corn soaking water. The application can produce inositol and liquid fertilizer simultaneously, and has high yield, simple process, low equipment investment, low production cost and good economic benefit.
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 liquid fertilizer 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.
The liquid fertilizer is very suitable for fertilization of automatic irrigation equipment due to the advantages of instant property, no need of stirring and dissolving and uniformity. In the countries where irrigation technology and automatic fertilization are popular, liquid fertilizers are widely used. Compared with solid fertilizer, the liquid fertilizer is easier to be absorbed by plants, and the absorption and utilization speed is high; the nutrition components are uniform, and the phenomenon of uneven quality and unbalanced nutrition elements of the solid fertilizer can not be generated; compared with the solid fertilizer production process, the liquid fertilizer production process is simpler, the equipment investment is less, and the economic benefit is better.
The corn soaking water is leftover produced in the wet process of producing corn starch and contains rich potassium, phosphorus, protein and other resource. The recovery of phosphorus resources from the corn soaking water can not only avoid environmental damage caused by phosphorite exploitation, but also relieve the situation of shortage of phosphorite resources in China, and has remarkable economic and social benefits. At present, a process for producing inositol and phosphate by using corn soaking water has been reported, wherein the phosphate is mostly solid, and the processes of decolorization, crystallization, recrystallization, centrifugation, drying and the like are needed, so that the processes are more, the equipment investment is large, and the production cost is high. Therefore, a new process method for recycling phosphorus resources needs to be developed to overcome the defects existing in the prior art.
Disclosure of Invention
The technical problems to be solved by the application are as follows: the method for co-producing the inositol and the liquid fertilizer by using the corn soaking water overcomes the defects in the prior art, and provides a novel method for simultaneously producing the inositol and the liquid fertilizer by using the phosphorus resources in the corn soaking water, which has the advantages of simple process, low equipment investment, low production cost, high yield of the inositol and the liquid fertilizer and good economic benefit.
In order to solve the technical problems, the technical scheme of the application is as follows:
a method for co-producing inositol and liquid fertilizer by using corn soaking water, which comprises the following steps:
a. pretreatment of corn soaking water: removing solid impurities by using corn soaking water, and then passing through chelating cationic resin at the flow rate of 2-3 BV/h;
this step aims at selectively removing divalent cations;
b. adsorption of potassium phytate: c, enabling the corn soaking water treated in the step a to pass through weak alkaline anion exchange resin at a flow rate of 2-3 BV/h, wherein the volume ratio of the chelating cationic resin to the anion exchange resin in the step a is 1:1-2;
the step aims at enabling phytic acid to be adsorbed by resin, and organic impurities such as protein, starch and the like flow out along with corn steep water;
c. analysis of potassium phytate: washing the resin adsorbed and saturated in the step b with water (1-2 BV clear water), washing off impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin by using KOH solution, wherein the concentration of the KOH solution is 5-10% (W/V), and the dosage is 1.5-2.5 BV of the volume of the resin to obtain potassium phytate solution;
compared with KCl, KOH is used as an analytical solution, chloride ions are not introduced, corrosion to subsequent hydrolysis, concentration, crystallization and other equipment is avoided, and equipment investment is greatly reduced; meanwhile, the quality of the liquid fertilizer prepared later cannot be influenced;
d. concentrating potassium phytate: c, the potassium phytate solution obtained in the step c is firstly passed through a ceramic membrane to remove insoluble matters; concentrating by using a nanofiltration membrane to obtain potassium phytate concentrate;
e. hydrolysis of potassium phytate: putting the potassium phytate concentrate obtained in the step d into a hydrolysis kettle, introducing steam, heating to the temperature of 150-180 ℃ and the pressure of 0.5-0.8 MPa, and preserving heat and pressure for 8-12 h until the hydrolysis is finished;
f. separating: c, carrying out flash evaporation cooling on the hydrolysate in the step e, then carrying out plate-frame filtration, and carrying out simulated moving bed chromatographic separation on filtrate to obtain inositol and phosphate phases; wherein the temperature after flash evaporation is 50-70 ℃ and the vacuum degree is-0.07 to-0.09 MPa; the filtering mode is a plate frame, and the aperture of the filter cloth is 300-400 meshes;
g. inositol preparation: concentrating the inositol solution separated in the step f through a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, reducing the temperature to 35 ℃, centrifuging by a centrifuge, drying, crushing, packaging and the like to obtain an inositol product;
h. preparing a liquid fertilizer: and d, adding 0.05 to 0.2 per mill of chelating agent into the phosphate phase separated in the step f, then, entering a multi-effect concentrator, concentrating under vacuum of-0.07 to-0.09 MPa, and concentrating to the solid content of 40 to 50 ℃ at the temperature of 80 to 90 ℃ to obtain the liquid fertilizer.
Preferably, the chelating resin in the step a is a polystyrene macroporous cation exchange resin containing carbamate groups, and the flow rate is 2.5BV/h.
Preferably, the volume ratio of the chelating cationic resin to the anion exchange resin in the step b is 1:1.5, and the corn steep water passes through the weak alkaline anion exchange resin at a flow rate of 2.5BV/h.
Preferably, in the step c, the concentration of KOH solution is 8% (W/V), and the dosage is 2.0BV of the volume of the resin.
Preferably, the analysis in the step c is carried out by collecting the potassium phytate in a time-division manner, wherein the first half section is a qualified dilute potassium phytate solution, the pH value of the second half section is increased, the potassium phytate content is low, and the potassium phytate is used as an alkaline solution for carrying out the next batch analysis.
Preferably, in the step D, the pore diameter of the ceramic membrane is 0.5 mu m, the molecular weight cut-off of the nanofiltration membrane is 1000D, and the concentration of the concentrated potassium phytate solution is 25-40% (W/V).
Further, in the step e, after the temperature is 165 ℃ and the pressure is 0.65MPa, the temperature and the pressure are maintained for 10 hours until the hydrolysis is finished.
Preferably, in the step f, the temperature after flash evaporation is 60 ℃, the filtering mode is a plate frame, and the aperture of the filter cloth is 350 meshes.
Preferably, the simulated moving bed chromatographic packing in the step f is strong acid cation exchange resin, and the mobile phase is purified water. 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。
Preferably, the amount of the activated carbon in the step g is 3-5% (W/V) of the liquid amount, and the filtering equipment is a candle filter.
Preferably, in the step h, the chelating agent is DTPMP-NaX (diethylene triamine pentamethylene sodium phosphate), sodium metasilicate or trisodium nitrilotriacetate, and the dosage is 0.05-0.2 per mill of the liquid; the multi-effect concentrator is a plate-type four-effect concentrator, and is concentrated under vacuum of-0.07 to-0.09 MPa at the temperature of 80-90 ℃ until the solid content of the concentrated solution is 40-50%.
Further, in the step h, the chelating agent is DTPMP-NaX, and the dosage is 0.1 per mill of the liquid; concentrating under vacuum-0.08 MPa at 85deg.C, and concentrating to obtain concentrate with solid content of 45%.
The main components of the obtained liquid fertilizer are dipotassium hydrogen phosphate, potassium phosphate, amino acid, magnesium, calcium and other ions.
Due to the adoption of the technical scheme, the application has the beneficial effects that:
1. divalent metal ions such as calcium, magnesium and the like in the corn soaking water are easy to remain in the phytic acid analysis solution, and are easy to generate precipitation with phosphate under alkaline conditions after hydrolysis, so that the solubility of the liquid fertilizer is affected, and therefore, the divalent metal ions are selectively removed by chelate resin before the corn soaking water is subjected to phytic acid adsorption, and turbidity and precipitation of the liquid fertilizer are avoided; meanwhile, the KOH is used as the analysis liquid, so that the influence of chloride ions on equipment and liquid fertilizer during KCl analysis is overcome;
2. the application separates inositol from other components by chromatography: flash evaporation cooling is carried out on the potassium phytate hydrolysate, and chromatographic resin separation is carried out after filtration to obtain inositol phase and phosphate phase, which are all the special technological processes of the application;
3. when the liquid fertilizer is concentrated, the phosphate is added into a specific chelating agent to carry out chelation reaction with divalent metal ions such as calcium, magnesium and the like, so that precipitation generated in the concentration process is avoided, a concentrator is blocked, and the clarity of the liquid fertilizer is influenced.
In a word, the application has simple process, stable operation, high yield of inositol and liquid fertilizer and good economic benefit; the investment of equipment is less, the operation cost is low, and the consumption caused by reprocessing of the crystallization mother liquor is avoided.
Detailed Description
The technical scheme of the application is further described below by combining examples:
example 1:
a. pretreatment of corn soaking water: 70m of 3 Removing solid impurities from the corn steep water, and then passing the corn steep water through the chelating cationic resin at a flow rate of 2 BV/h;
b. adsorption of potassium phytate: c, enabling the corn soaking water treated in the step a to pass through weak alkaline anion exchange resin at a flow rate of 2BV/h, wherein the volume ratio of the chelating cationic resin to the anion exchange resin in the step a is 1:1;
c. analysis of potassium phytate: washing the resin adsorbed and saturated in the step b with 1BV water to remove impurities on the surface of the resin, and then resolving the phytic acid adsorbed on the resin by using KOH solution, wherein the concentration of the KOH solution is 5% (W/V), the dosage is 2.5BV of the volume of the resin, so as to obtain potassium phytate solution (resolving solution) with potassium phytate content of 10.7% of 12m 3 ；
d. Concentrating potassium phytate: c, the potassium phytate solution obtained in the step c is firstly passed through a ceramic membrane with the aperture of 0.5 mu m, and insoluble matters are removed; then concentrating by using a nanofiltration membrane with the molecular weight cut-off of 1000D to obtain a potassium phytate concentrated solution with the potassium phytate content of 33.6 percent of 3.8m 3 ；
e. Hydrolysis of potassium phytate: putting the potassium phytate concentrate obtained in the step d into a hydrolysis kettle, introducing steam, heating to 150 ℃ and 0.5MPa, and preserving heat and pressure for 12 hours until the hydrolysis is finished;
f. separating: cooling the hydrolysate in the step e by flash evaporation (vacuum degree-0.07 MPa, temperature 70 ℃ after flash evaporation), filtering by a plate and frame (filter cloth aperture 300 meshes), and separating the filtrate by simulated moving bed chromatography under the conditions that 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 to obtain inositol and phosphate phases;
g. inositol preparation: concentrating the separated inositol solution in the step f through a plate type four-effect concentrator, and concentrating under vacuum to be 0.07MPa at the temperature of 75 ℃ to obtain concentrated solution with the solid content of 35%; then adding 3% (W/V) active carbon for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallizing tank, reducing the temperature to 35 ℃, centrifuging by a centrifuge, and drying, crushing, packaging and other procedures on the centrifuged wet product to obtain 190kg of inositol product with the yield of 73.6%;
h. preparing a liquid fertilizer: adding 0.05 per mill sodium metasilicate into phosphate phase separated in step f, introducing into a plate type four-effect concentrator, concentrating under vacuum-0.07 MPa at 80deg.C to solid content of 40%, and obtaining 2.6m liquid fertilizer 3 。
Example 2:
a. pretreatment of corn soaking water: 70m of 3 Removing solid impurities from the corn steep water, and passing the corn steep water through the chelating cationic resin at a flow rate of 3 BV/h;
b. adsorption of potassium phytate: c, enabling the corn soaking water treated in the step a to pass through weak alkaline anion exchange resin at a flow rate of 3BV/h, wherein the volume ratio of the chelating cationic resin to the anion exchange resin in the step a is 1:2;
c. analysis of potassium phytate: washing the resin adsorbed and saturated in the step b with 2BV water to remove impurities on the surface of the resin, and then resolving the phytic acid adsorbed on the resin by using KOH solution, wherein the concentration of the KOH solution is 10% (W/V), the dosage is 1.5BV of the volume of the resin, so as to obtain potassium phytate solution (resolving solution) with the potassium phytate content of 16.9% of 7.5m 3 ；
d. Concentrating potassium phytate: the potassium phytate solution obtained in the step c is firstly passed through a pore diameter of 0.5Removing insoluble substances by using a μm ceramic membrane; then concentrating by using a nanofiltration membrane with the molecular weight cut-off of 1000D to obtain 4.2m potassium phytate concentrate with the potassium phytate content of 29.6 percent 3 ；
e. Hydrolysis of potassium phytate: putting the potassium phytate concentrate obtained in the step d into a hydrolysis kettle, introducing steam, heating to 180 ℃ and 0.8MPa, and preserving heat and pressure for 8 hours until the hydrolysis is finished;
f. separating: cooling the hydrolysate in the step e by flash evaporation (vacuum degree-0.09 MPa, temperature after flash evaporation is 50 ℃), then filtering by a plate and frame (filter cloth aperture is 400 meshes), separating filtrate by simulated moving bed chromatography under the conditions that the temperature is 60 ℃, the pressure is 0.4MPa, the valve switching time is 10min, and the flow rate of feed liquid is 8m 3 /h, flow rate of mobile phase 20m 3 /h; separating to obtain inositol and phosphate phases;
g. inositol preparation: concentrating the separated inositol solution in the step f by a multi-effect concentrator, and concentrating under vacuum to 0.09MPa at a temperature of 85 ℃ to obtain a concentrated solution with a solid content of 45%; then adding 5% (W/V) active carbon for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallizing tank, reducing the temperature to 35 ℃, centrifuging by a centrifuge, and drying, crushing, packaging and other procedures on the centrifuged wet product to obtain 195kg of inositol product with the yield of 75.8%;
h. preparing a liquid fertilizer: adding 0.2 per mill trisodium nitrilotriacetate into phosphate phase separated in step f, feeding into a plate type four-effect concentrator, concentrating under vacuum-0.09 MPa at 90 ℃ until the solid content is 50%, and obtaining 2m liquid fertilizer 3 。
Example 3:
a. pretreatment of corn soaking water: 70m of 3 After removing solid impurities in the corn steep water, the corn steep water passes through the chelating cationic resin at a flow rate of 2.5 BV;
b. adsorption of potassium phytate: c, passing the corn steep water treated in the step a through a weak alkaline anion exchange resin at a flow rate of 2.5BV/h, wherein the volume ratio of the chelating cationic resin to the anion exchange resin in the step a is 1:1.5;
c. analysis of potassium phytate: washing the resin saturated with adsorption in step b with 1.5BV water to remove impurities on the surface of the resin, and then using KThe phytic acid adsorbed on the resin is resolved by OH solution, wherein the concentration of KOH solution is 7.5% (W/V), the dosage is 2.0BV of the resin volume, and potassium phytate solution (resolving solution) with potassium phytate content of 13.4% is obtained by 10m 3 ；
d. Concentrating potassium phytate: c, the potassium phytate solution obtained in the step c is firstly passed through a ceramic membrane with the aperture of 0.5 mu m, and insoluble matters are removed; then concentrating by using a nanofiltration membrane with the molecular weight cut-off of 1000D to obtain 4m potassium phytate concentrate with the potassium phytate content of 33.5 percent 3 ；
e. Hydrolysis of potassium phytate: putting the potassium phytate concentrate obtained in the step d into a hydrolysis kettle, introducing steam, heating to 165 ℃ and 0.65MPa, and preserving heat and pressure for 10 hours until the hydrolysis is finished;
f. separating: and d, carrying out flash evaporation cooling (vacuum degree-0.08 MPa, temperature 60 ℃ after flash evaporation) on the hydrolysate in the step e, then carrying out plate and frame filtration (filter cloth aperture of 350 meshes), carrying out simulated moving bed chromatographic separation on the filtrate, wherein the separation condition is that 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 to obtain inositol and phosphate phases;
g. inositol preparation: concentrating the separated inositol solution in the step f by a multi-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 4% (W/V) active carbon for decoloring, filtering by a candle filter, cooling and crystallizing in a crystallizing tank, reducing the temperature to 35 ℃, centrifuging by a centrifuge, and drying, crushing, packaging and other procedures on the centrifuged wet product to obtain 210kg of inositol product; the calculated yield was 77.5%;
h. preparing a liquid fertilizer: adding 0.1 per mill of DTPMP-NaX into the phosphate phase separated in the step f, then feeding into a plate type four-effect concentrator, concentrating under vacuum-0.08 MPa, and concentrating at 85 ℃ until the solid content is 45%, thus obtaining 2.3m liquid fertilizer 3 。
Comparative example 1:
step a in example 1 was removed, the other conditions being unchanged. 185kg of inositol product was obtained; the yield was calculated to be 71.7%; obtaining 2.6m liquid fertilizer 3 。
Comparative example 2:
the KOH in step c of example 2 was changed to an equivalent amount of KCl, and the other conditions were unchanged. 188kg of inositol product was obtained; the calculated yield was 73.0%; obtaining 2.2m of liquid fertilizer 3 。
Comparative example 3:
the DTPMP-NaX in step h of example 3 was removed, the other conditions being unchanged. 211kg of inositol product was obtained; the calculated yield was 77.9%; obtaining 2.3m liquid fertilizer 3 。
The results of the detection of inositol and liquid fertilizer obtained in examples 1-3 and comparative examples 1-3 are shown in tables 1 and 2.
Table 1 inositol assay data for examples and comparative examples
Note that: inositol detection the inositol detection is carried out according to the method of four parts of the 2015 edition of the pharmacopoeia of the people's republic of China
Table 2 liquid fertilizer test data for examples and comparative examples
Note that: the detection basis is GB/T15063-2020
Application example
A field test was conducted using the liquid fertilizer obtained in example 3 and a commercially available liquid fertilizer of phosphorus and potassium (manufactured by Biotechnology Co., ltd. In Fangfang Kang En). The test variety is tomato, the test site is the god of the god city, and the test time is 2022, 4 months to 8 months. The pH value of the test soil is 6.5, the organic matter is 15.5g/kg, the total nitrogen is 1.1g/kg, and the quick-acting potassium is 55mg/kg. Test samples and controls were each run in 3 replicates of 100 strains each. The test sample and the control liquid fertilizer are respectively applied after the fixed planting, the flowering phase and the first fruit picking, and the using amount is 0.1kg/m 2 . The test results are shown in Table 3.
TABLE 3 results of field trials
Analysis of results:
the following conclusions were drawn by analysis of the products of the examples and comparative examples: after the procedure of removing calcium and magnesium by the chelate resin is eliminated in comparative example 1, the burning residue in the obtained inositol product is obviously increased, and the insoluble substances and the contents of calcium and magnesium in the liquid fertilizer are increased; in comparative example 2, after KOH is replaced by equivalent KCl, the content of chloride ions in the obtained inositol product and liquid fertilizer is obviously increased, KCl is adopted for analysis, the pH value of potassium phytate solution is 4-5, the potassium dihydrogen phosphate is the most produced product after hydrolysis, and the potassium dihydrogen phosphate is easy to separate out after concentration; comparative example 3 after the chelating agent is eliminated, the insoluble matter increases obviously after the liquid fertilizer is concentrated, and the insoluble matter is calcium magnesium salt separated out in the concentration process. By combining various data, example 3 is the optimal process condition, and field experiments performed by using the liquid fertilizer obtained in example 3 and the commercially available liquid fertilizer show that: the liquid fertilizer obtained by the application can obviously improve fruit setting rate, single fruit weight, good fruit color, uniform coloring and few malformed fruits and rotten fruits.
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 liquid fertilizer by using corn soaking water is characterized by comprising the following steps: the method comprises the following steps:
a. pretreatment of corn soaking water: removing solid impurities by using corn soaking water, and then passing through chelating cationic resin at the flow rate of 2-3 BV/h;
b. adsorption of potassium phytate: c, enabling the corn soaking water treated in the step a to pass through weak alkaline anion exchange resin at a flow rate of 2-3 BV/h, wherein the volume ratio of the chelating cationic resin to the anion exchange resin in the step a is 1:1-2;
c. analysis of potassium phytate: c, washing the resin adsorbed and saturated in the step b with water to remove impurities on the surface of the resin, and then analyzing the phytic acid adsorbed on the resin with KOH solution, wherein the concentration of the KOH solution is 5-10% W/V, and the dosage is 1.5-2.5 BV of the volume of the resin to obtain potassium phytate solution;
d. concentrating potassium phytate: c, the potassium phytate solution obtained in the step c firstly passes through a ceramic membrane and then is concentrated by a nanofiltration membrane to obtain potassium phytate concentrated solution;
e. hydrolysis of potassium phytate: putting the potassium phytate concentrate obtained in the step d into a hydrolysis kettle, introducing steam, heating to the temperature of 150-180 ℃ and the pressure of 0.5-0.8 MPa, and preserving heat and pressure for 8-12 h until the hydrolysis is finished;
f. separating: c, carrying out flash evaporation cooling on the hydrolysate in the step e, then carrying out plate-frame filtration, and carrying out simulated moving bed chromatographic separation on filtrate to obtain inositol and phosphate phases; wherein the temperature after flash evaporation is 50-70 ℃, the vacuum degree is-0.07-0.09 MPa, the filtering mode is a plate frame, and the aperture of the filter cloth is 300-400 meshes;
g. inositol preparation: concentrating the inositol solution separated in the step f through a multi-effect concentrator, adding active carbon for decolorization, filtering, cooling and crystallizing in a crystallization tank, reducing the temperature to 35 ℃, centrifuging by a centrifuge, drying, crushing, packaging and the like to obtain an inositol product;
h. preparing a liquid fertilizer: and d, adding 0.05 to 0.2 per mill of chelating agent into the phosphate phase separated in the step f, then, entering a multi-effect concentrator, concentrating under vacuum of-0.07 to-0.09 MPa, and concentrating to the solid content of 40 to 50 ℃ at the temperature of 80 to 90 ℃ to obtain the liquid fertilizer.
2. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the chelate resin in the step a is polystyrene macroporous cation exchange resin containing carbamate groups, and the flow rate is 2.5BV/h.
3. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the volume ratio of the chelating cationic resin to the anion exchange resin in the step b is 1:1.5, and the corn steep water passes through the weak alkaline anion exchange resin at the flow rate of 2.5BV/h.
4. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the concentration of KOH solution in the step c is 8% W/V, and the dosage is 2.0BV of the volume of the resin.
5. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: in the step D, the pore diameter of the ceramic membrane is 0.5 mu m, the molecular weight cut-off of the nanofiltration membrane is 1000D, and the concentration of the concentrated potassium phytate solution is 25-40% W/V.
6. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: and e, heating to 165 ℃ and 0.65MPa, and then preserving heat and pressure for 10 hours until the hydrolysis is finished.
7. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the temperature after flash evaporation in the step f is 60 ℃, the filtering mode is a plate frame, and the aperture of filter cloth is 350 meshes; the separation conditions of simulated moving bed chromatography were: 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。
8. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the dosage of the activated carbon in the step g is 3-5% of the liquid amount.
9. The method for co-producing inositol and liquid fertilizer by using corn steep water according to claim 1, wherein: the chelating agent in the step h is DTPMP-NaX, sodium metasilicate or trisodium nitrilotriacetate, and the dosage is 0.05-0.2 per mill of the liquid; the multi-effect concentrator is a plate-type four-effect concentrator, and is concentrated under vacuum of-0.07 to-0.09 MPa at the temperature of 80-90 ℃ until the solid content of the concentrated solution is 40-50%.
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