CN117701653A - Preparation method of sodium glucuronate - Google Patents
Preparation method of sodium glucuronate Download PDFInfo
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- CN117701653A CN117701653A CN202311590617.9A CN202311590617A CN117701653A CN 117701653 A CN117701653 A CN 117701653A CN 202311590617 A CN202311590617 A CN 202311590617A CN 117701653 A CN117701653 A CN 117701653A
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- WNFHGZLVUQBPMA-JSCKKFHOSA-M Sodium glucuronate Chemical compound [Na+].O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C([O-])=O WNFHGZLVUQBPMA-JSCKKFHOSA-M 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 52
- 238000001728 nano-filtration Methods 0.000 claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 24
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229960000367 inositol Drugs 0.000 claims abstract description 23
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 102000004316 Oxidoreductases Human genes 0.000 claims abstract description 9
- 108090000854 Oxidoreductases Proteins 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000010865 sewage Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 18
- 230000001276 controlling effect Effects 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000004042 decolorization Methods 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000008394 flocculating agent Substances 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 238000004587 chromatography analysis Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 239000003456 ion exchange resin Substances 0.000 abstract description 2
- 229920003303 ion-exchange polymer Polymers 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 1
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- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 10
- IAJILQKETJEXLJ-QTBDOELSSA-N aldehydo-D-glucuronic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-QTBDOELSSA-N 0.000 description 10
- 229940097043 glucuronic acid Drugs 0.000 description 10
- 241000196324 Embryophyta Species 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003729 cation exchange resin Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 206010016952 Food poisoning Diseases 0.000 description 2
- 208000019331 Foodborne disease Diseases 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 206010070863 Toxicity to various agents Diseases 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 208000019425 cirrhosis of liver Diseases 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 208000006454 hepatitis Diseases 0.000 description 2
- 231100000283 hepatitis Toxicity 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000001727 in vivo Methods 0.000 description 2
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- 239000000047 product Substances 0.000 description 2
- 244000171897 Acacia nilotica subsp nilotica Species 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 1
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920000715 Mucilage Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000009285 allergic inflammation Effects 0.000 description 1
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 229930182830 galactose Natural products 0.000 description 1
- 210000004211 gastric acid Anatomy 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010255 intramuscular injection Methods 0.000 description 1
- 238000010253 intravenous injection Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of sodium glucuronate, which relates to the technical field of pharmacy, wherein a conversion solution obtained after inositol feed liquid is converted by a whole-cell catalyst containing inositol oxidase is decolorized again by a ceramic membrane, an ultrafiltration membrane and a nanofiltration membrane, and then the decolorized solution is concentrated and subjected to cooling crystallization to obtain sodium glucuronate crystals, an ion exchange resin column and simulated moving bed chromatography are not used, the extraction and purification process is simplified, the use amount of water is reduced while the resin is not used, meanwhile, the discharge of mass production sewage is reduced, the concentration energy consumption is correspondingly reduced due to the reduction of water consumption in the concentration process, the aim of saving energy and reducing emission is fulfilled, the purity of the obtained sodium glucuronate is high, the detection purity of the sodium glucuronate is more than 99.5% by a liquid chromatograph, and an organic solvent is not used in the purification process, so that the method is environment-friendly.
Description
Technical Field
The invention relates to the technical field of pharmacy, in particular to a preparation method of sodium glucuronate.
Background
Glucuronic acid (Glucuronic acid), which is formed by oxidizing hydroxyl group at C-6 position of glucose into carboxyl group, and has molecular formula of C 6 H 10 O 7 The molecular weight is 194.14, and the compound is formed by oxidizing primary hydroxyl of glucose into carboxyl, is widely distributed in animals and plants, and has important biological functions. Gum arabic, gum isoparaffin, which exists in the form of a uronic acid in plants, is an important component constituting pectin, mucilage and higher polysaccharides.
Glucuronic acid can be combined with in vivo poison to form nontoxic glucuronic acid conjugate for discharge, has liver protecting and toxic substance removing effects, and can be used for treating hepatitis, liver cirrhosis, food and drug poisoning. Glucuronic acid can assist in the discharge of metabolic waste in vivo, promote the absorption of basic group substances and improve the immune function of organisms.
Sodium glucuronate can be used for treating epidemic hepatitis, liver cirrhosis, chronic liver disorder, rheumarthritis, skin allergic inflammation, food and drug poisoning. Can be administered orally, by intramuscular or intravenous injection, and can be immediately converted into glucuronic acid after oral administration by gastric acid action. Chinese patent CN116199725a discloses a method for separating and purifying glucuronic acid, after hydrolyzing plant source under acidic condition, neutralizing, filtering, concentrating, decolorizing, deionizing, separating and purifying, extracting arabinose, galactose and rhamnose, and then treating the remaining material liquid with low glucuronic acid content. And adding sodium salt in the treatment process to perform salt conversion, converting glucuronic acid into sodium glucuronate, separating and purifying sodium glucuronate solution by using a simulated moving bed chromatographic separation device to obtain high-purity sodium glucuronate solution, and then performing cation exchange to obtain high-purity sodium glucuronate solution. The intermediate is rich in sodium glucuronate, the sodium glucuronate content in the sodium glucuronate liquid is 88.6%, the impurity content is high, and the processing procedure of the plant source is complicated, thereby increasing the production cost.
Chinese patent CN116925165a discloses a method for preparing sodium glucuronate, wherein inositol feed liquid is transformed by whole cells containing inositol oxidase, and then passes through a ceramic membrane, an ultrafiltration membrane and a cation exchange resin column, so that particulate matters, macromolecular proteins, impurities and cationic impurities in the feed liquid are removed, and after the anion exchange resin column is adsorbed, the obtained analytical solution after being resolved by sodium hydroxide solution can be directly used for concentrating and crystallizing, and the purity of sodium glucuronate product is improved by purifying ethanol solution, meanwhile, the process is simple, the production cost is low, and the economic benefit of enterprises is improved. However, the cation exchange resin column has high cost and short service life, prolongs the production period, increases the use amount of the organic solvent ethanol, and has a certain influence on the environment.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects existing in the prior art, the preparation method of sodium glucuronate is provided, and the preparation method is low in production cost and environment-friendly.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing sodium glucuronate, comprising the following steps:
a: regulating pH of inositol feed liquid to 7-8, adding whole-cell catalyst containing inositol oxidase, and converting at 32-38deg.C for 2-6 hr to obtain converted liquid;
b: collecting a ceramic membrane clear solution after the conversion solution is filtered by a ceramic membrane, adding a flocculating agent into the ceramic membrane concentrate, filtering by a plate frame, and respectively carrying out environment-friendly treatment on filter cakes and filtrate, wherein the flocculating agent is a chitosan solution with the weight of 1%;
c: filtering the ceramic membrane filtrate by an ultrafiltration membrane, collecting ultrafiltration clear liquid, and carrying out environment-friendly treatment on ultrafiltration concentrated liquid to remove sewage;
d: concentrating the ultrafiltration clear liquid by a nanofiltration membrane to obtain nanofiltration concentrated liquid with the solid content of 10-15% w/w;
e: adding active carbon into the nanofiltration concentrated solution for decolorization, controlling the decolorization temperature to be 40-50 ℃ and the decolorization time to be 20-40min, and filtering and collecting decolorized solution;
f: concentrating the decolorized solution at 50-70deg.C and vacuum degree of less than or equal to-0.09 MPa to solid content of 40-50% w/w to obtain concentrated solution;
g: cooling the concentrated solution to 10-25 ℃ at the stirring speed of 100-200rpm at the speed of 3-6 ℃/h, filtering, washing with cold water at the temperature of 2-4 ℃, and drying to obtain sodium glucuronate crystals.
Preferably, the concentration of inositol feed liquid in step A is 50-100g/L.
Preferably, phosphate is added to the inositol feed solution in step A to adjust the pH, wherein the concentration of phosphate is 0.02-0.1mol/L.
Preferably, the volume ratio of the whole cell catalyst containing inositol oxidase to inositol feed liquid in the step A is 20-50g/L.
Preferably, 5-8% wt sodium hydroxide solution is added during the conversion in step A, and the pH of the system is maintained at 7-8.
Preferably, the ceramic membrane in step B has a separation pore size of 20-100nm.
Preferably, the ultrafiltration membrane in step C has a pore molecular weight cutoff of 500-1000Da.
Preferably, the nanofiltration membrane in step D has a molecular weight cut-off of 150-200Da.
Preferably, the volume ratio of the activated carbon addition to the nanofiltration concentrate in the step E is 2-5g/L.
Preferably, the filtrate and the washing water in the step G are mixed with the nanofiltration concentrate, and then decolorized again, concentrated and crystallized.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the invention provides a high-efficiency low-cost preparation method of sodium glucuronate, which is characterized in that sodium hydroxide is directly used for neutralization in the process of converting inositol into glucuronic acid, so that sodium glucuronate can be generated, the process is simple, the operation is simple and the large-scale industrial production can be realized.
2. The invention does not use ion exchange resin column and simulated moving bed chromatography, simplifies the extraction and purification process, reduces the water consumption while not using resin, and simultaneously reduces the discharge of mass production sewage.
3. In the prior art, ammonia water is used for regulating the pH value in the conversion process, cation exchange resin is needed for removing ammonium ions in the subsequent purification process, a large amount of high ammonia nitrogen sewage is generated in the resin regeneration process, the treatment of the high ammonia nitrogen sewage is very complicated, a large amount of chemical reagents are needed or high-cost equipment is invested for treating the standard emission.
4. The sodium glucuronate produced by the invention has high purity, the purity is more than 99.5 percent by detection of a liquid chromatograph, and the purification process does not use an organic solvent, thereby being environment-friendly.
5. The filtrate and the flushing liquid after the concentrated solution is cooled can be sleeved, so that the trouble of post-treatment is avoided, the yield of products and the utilization rate of raw materials are improved, the production cost is reduced, and the income is improved.
Drawings
FIG. 1 is a liquid chromatogram of sodium glucuronate in example 1 of the present invention.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
1. Preparing 50g/L inositol feed solution 50L, adding 1000g of whole cell catalyst containing inositol oxidase, converting at 32deg.C and pH=7.0, adjusting pH=7.0 with 5% wt sodium hydroxide solution during conversion, and converting for 2h to obtain conversion solution 62L;
2. filtering 62L of conversion liquid by a ceramic membrane with the aperture of 50nm, adding 10L of pure water for top washing, collecting 66L of clear liquid of the ceramic membrane, controlling the membrane feeding pressure of a ceramic membrane machine to be 0.4MPa, the membrane discharging pressure to be 0.2MPa, adding 0.5L of 1% chitosan aqueous solution into 6L of concentrated liquid of the ceramic membrane, and carrying out flocculation and then carrying out plate frame treatment;
3. filtering 66L of ceramic membrane clear liquid by using a 500Da ultrafiltration membrane, collecting 65L of ultrafiltration membrane clear liquid, controlling the membrane inlet pressure of an ultrafiltration membrane machine to be 0.6MPa and the membrane outlet pressure to be 0.5MPa;
4. concentrating 65L of ultrafiltration membrane clear liquid by a 150Da nanofiltration membrane, collecting nanofiltration concentrated liquid 23L, controlling the membrane inlet pressure of a nanofiltration membrane machine to be 3MPa and the membrane outlet pressure to be 2.5MPa, wherein the solid content of the nanofiltration concentrated liquid is 10.5% w/w;
5. taking 23L nanofiltration concentrated solution, adding 46g of active carbon, decoloring for 40min at 40 ℃, and collecting decolored solution 23L;
6. concentrating 23L decolorized solution to 6L at 50deg.C under vacuum of less than or equal to-0.09 MPa, wherein the solid content of the concentrated solution is 40% w/w;
7. cooling the concentrated solution to 10 ℃ at the stirring speed of 100rpm at the speed of 3 ℃/h, filtering, washing with cold water at the temperature of 4 ℃, drying to obtain sodium glucuronate crystals, and drying to obtain 2.73kg of sodium glucuronate dry powder, wherein the purity is 99.5% detected by a liquid chromatograph.
Example 2
1. Preparing 50L of inositol feed liquid with the concentration of 75g/L, adding 1750g of whole-cell catalyst containing inositol oxidase, converting at 35 ℃ and pH=7.5, adjusting the pH=7.5 by using 6.5% wt sodium hydroxide solution in the conversion process, and converting for 4 hours to obtain 63L of conversion liquid;
2. filtering 63L of conversion solution by a ceramic membrane with the aperture of 50nm, adding 10L of pure water for top washing, collecting 65L of clear solution of the ceramic membrane, controlling the membrane feeding pressure of a ceramic membrane machine to be 0.4MPa, the membrane discharging pressure to be 0.2MPa, adding 0.6L of 1% chitosan aqueous solution into 8L of concentrated solution of the ceramic membrane, and carrying out flocculation and then carrying out plate frame treatment;
3. filtering 65L of ceramic membrane clear liquid by an 800Da ultrafiltration membrane, collecting to obtain 63L of ultrafiltration membrane clear liquid, controlling the membrane inlet pressure of an ultrafiltration membrane machine to be 0.6MPa and the membrane outlet pressure to be 0.5MPa;
4. concentrating 63L of ultrafiltration membrane clear liquid by using a 150Da nanofiltration membrane, collecting 30L of nanofiltration concentrated solution, controlling the membrane inlet pressure of a nanofiltration membrane machine to be 3MPa and the membrane outlet pressure to be 2.5MPa, wherein the solid content of the nanofiltration concentrated solution is 12%w/w;
5. adding 120g of active carbon into 30L of nanofiltration concentrated solution, decoloring for 30min at 45 ℃, and collecting decolored solution 30L;
6. concentrating 30L of decolorized solution to 8L at 60 ℃ under vacuum of less than or equal to-0.09 MPa, wherein the solid content of the concentrated solution is 45% w/w;
7. cooling the concentrated solution to 15 ℃ at a stirring speed of 150rpm at a speed of 5 ℃/h, filtering, washing with cold water at 4 ℃, drying to obtain sodium glucuronate crystals, and drying to obtain 4.04kg sodium glucuronate dry powder, wherein the purity is 99.6% detected by a liquid chromatograph.
Example 3
1. Preparing 50L of inositol feed liquid with the concentration of 100g/L, adding 2500g of whole-cell catalyst containing inositol oxidase, converting at 48 ℃ and pH=8, adjusting pH=8 by 8% wt sodium hydroxide solution in the conversion process, and converting for 6 hours to obtain 64L of conversion liquid;
2. filtering 64L of conversion liquid by a ceramic membrane with the aperture of 50nm, adding 10L of pure water for top washing, collecting 64L of clear liquid of the ceramic membrane, controlling the membrane feeding pressure of a ceramic membrane machine to be 0.4MPa, the membrane discharging pressure to be 0.2MPa, adding 0.8L of 1% chitosan aqueous solution into 10L of concentrated liquid of the ceramic membrane, and carrying out flocculation and then carrying out plate frame treatment;
3. filtering 64L of ceramic membrane clear liquid by an 800Da ultrafiltration membrane, collecting 63L of ultrafiltration membrane clear liquid, controlling the membrane inlet pressure of an ultrafiltration membrane machine to be 0.6MPa and the membrane outlet pressure to be 0.5MPa;
4. concentrating 63L of ultrafiltration membrane clear liquid by a 200Da nanofiltration membrane, collecting 33L of nanofiltration concentrated liquid, controlling the membrane inlet pressure of a nanofiltration membrane machine to be 3MPa and the membrane outlet pressure to be 2.5MPa, wherein the solid content of the nanofiltration concentrated liquid is 15%w/w;
5. taking 33L of nanofiltration concentrated solution, adding 165g of active carbon, decoloring for 20min at 50 ℃, and collecting 33L of decolored solution;
6. concentrating 33L of decolorized solution to 10L at 70 ℃ under vacuum of less than or equal to-0.09 MPa, wherein the solid content of the concentrated solution is 50% w/w;
7. cooling the concentrated solution to 20 ℃ at the stirring speed of 200rpm at the speed of 6 ℃/h, filtering, washing with cold water at the temperature of 4 ℃, drying to obtain sodium glucuronate crystals, and drying to obtain 5.34kg of sodium glucuronate dry powder, wherein the purity is 99.8% detected by a liquid chromatograph.
It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Claims (10)
1. The preparation method of sodium glucuronate is characterized by comprising the following steps:
a: regulating pH of inositol feed liquid to 7-8, adding whole-cell catalyst containing inositol oxidase, and converting at 32-38deg.C for 2-6 hr to obtain converted liquid;
b: collecting a ceramic membrane clear solution after the conversion solution is filtered by a ceramic membrane, adding a flocculating agent into the ceramic membrane concentrate, filtering by a plate frame, and respectively carrying out environment-friendly treatment on filter cakes and filtrate, wherein the flocculating agent is a chitosan solution with the weight of 1%;
c: filtering the ceramic membrane filtrate by an ultrafiltration membrane, collecting ultrafiltration clear liquid, and carrying out environment-friendly treatment on ultrafiltration concentrated liquid to remove sewage;
d: concentrating the ultrafiltration clear liquid by a nanofiltration membrane to obtain nanofiltration concentrated liquid with the solid content of 10-15% w/w;
e: adding active carbon into the nanofiltration concentrated solution for decolorization, controlling the decolorization temperature to be 40-50 ℃ and the decolorization time to be 20-40min, and filtering and collecting decolorized solution;
f: concentrating the decolorized solution at 50-70deg.C and vacuum degree of less than or equal to-0.09 MPa to solid content of 40-50% w/w to obtain concentrated solution;
g: cooling the concentrated solution to 10-25 ℃ at the stirring speed of 100-200rpm at the speed of 3-6 ℃/h, filtering, washing with cold water at the temperature of 2-4 ℃, and drying to obtain sodium glucuronate crystals.
2. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: the concentration of inositol feed liquid in the step A is 50-100g/L.
3. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: and (C) adding phosphate into the inositol feed liquid in the step A to adjust the pH, wherein the concentration of the phosphate is 0.02-0.1mol/L.
4. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: the volume ratio of the addition of the inositol oxidase-containing whole cell catalyst to the inositol feed liquid in the step A is 20-50g/L.
5. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: and (C) adding 5-8% by weight of sodium hydroxide solution in the conversion process in the step A, and maintaining the pH of the system to be 7-8.
6. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: the separation pore diameter of the ceramic membrane in the step B is 20-100nm.
7. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: and C, the molecular weight cut-off of the ultrafiltration membrane hole is 500-1000Da.
8. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: the molecular weight cut-off of the nanofiltration membrane in the step D is 150-200Da.
9. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: and E, the volume ratio of the added amount of the activated carbon to the nanofiltration concentrated solution is 2-5g/L.
10. A process for the preparation of sodium glucuronate as claimed in claim 1, wherein: and D, mixing the filtrate and the washing water in the step G with the nanofiltration concentrated solution, decoloring again, concentrating and crystallizing.
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