CN114436816A - Method for efficiently extracting shikimic acid by ion exchange technology - Google Patents
Method for efficiently extracting shikimic acid by ion exchange technology Download PDFInfo
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- CN114436816A CN114436816A CN202111604552.XA CN202111604552A CN114436816A CN 114436816 A CN114436816 A CN 114436816A CN 202111604552 A CN202111604552 A CN 202111604552A CN 114436816 A CN114436816 A CN 114436816A
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- JXOHGGNKMLTUBP-JKUQZMGJSA-N shikimic acid Natural products O[C@@H]1CC(C(O)=O)=C[C@H](O)[C@@H]1O JXOHGGNKMLTUBP-JKUQZMGJSA-N 0.000 title claims abstract description 49
- JXOHGGNKMLTUBP-HSUXUTPPSA-N shikimic acid Chemical compound O[C@@H]1CC(C(O)=O)=C[C@@H](O)[C@H]1O JXOHGGNKMLTUBP-HSUXUTPPSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005342 ion exchange Methods 0.000 title claims abstract description 15
- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 26
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 150000001768 cations Chemical class 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 19
- 238000000855 fermentation Methods 0.000 claims abstract description 17
- 230000004151 fermentation Effects 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000004042 decolorization Methods 0.000 claims abstract description 10
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005189 flocculation Methods 0.000 claims abstract description 7
- 230000016615 flocculation Effects 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 28
- 239000011347 resin Substances 0.000 claims description 26
- 229920005989 resin Polymers 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 13
- 230000008025 crystallization Effects 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 102000004169 proteins and genes Human genes 0.000 claims description 4
- 108090000623 proteins and genes Proteins 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 230000003311 flocculating effect Effects 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000049 pigment Substances 0.000 abstract 1
- 239000002184 metal Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- JXOHGGNKMLTUBP-UHFFFAOYSA-N 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid Chemical compound OC1CC(C(O)=O)=CC(O)C1O JXOHGGNKMLTUBP-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000218631 Coniferophyta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007232 Illicium verum Species 0.000 description 1
- 235000008227 Illicium verum Nutrition 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000218377 Magnoliaceae Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- -1 aromatic amino acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940088623 biologically active substance Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000023555 blood coagulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000011869 dried fruits Nutrition 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000007269 microbial metabolism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- 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
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for efficiently extracting shikimic acid by using an ion exchange technology, which comprises the following steps of 1) pretreating fermentation liquor; 2) adding EDTA into shikimic acid fermentation liquor for flocculation and precipitation, adjusting the pH to 2.5-2.8, and filtering by a plate frame to obtain filtrate; 3) adding activated carbon into the obtained filtrate for decolorization, and filtering after the decolorization is finished; 4) separating and purifying the filtrate by using continuous ion exchange; 5) concentrating and crystallizing; 6) centrifugally drying to obtain shikimic acid finished products. The method for extracting shikimic acid from the fermentation liquor can effectively remove mycoprotein, divalent cations, other impurities with strong binding force and pigments, has high product purity and extraction yield, reduces the production cost, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of biological fermentation, and particularly relates to a method for efficiently extracting shikimic acid by using an ion exchange technology.
Background
Shikimic acid (3, 4, 5-trihydroxy-1-cyclohexene-1-carboxylic acid, SA) is a natural organic acidMolecular formula is C7H10O5Has a relative molecular weight of 174.15Da and an ionization constant of 3.85, and is present in mature and dried fruits of conifers and Magnoliaceae fructus Anisi Stellati. Shikimic acid, a biologically active substance, is an intermediate in the synthesis of compounds such as alkaloids, aromatic amino acids and phenols in plant and microbial metabolism. Modern pharmacology indicates that shikimic acid has the functions of resisting bacteria, tumors, blood coagulation, inflammation and the like.
At present, shikimic acid is mostly extracted from star anise, the yield of the shikimic acid is greatly influenced by natural environments such as climate and the like, and the shikimic acid is severely limited due to the complex extraction process, difficult control of purity and high cost. In addition, the production of shikimic acid by microbial fermentation is increasingly being studied. However, the processes for extracting shikimic acid from fermentation broth disclosed so far all have a common disadvantage: the resin has low adsorption amount to shikimic acid, low purity of eluent, large yield and purity fluctuation among different batches and the like. This results in low production efficiency and high cost of the whole extraction process, which is not suitable for industrialization.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for efficiently extracting shikimic acid by using an ion exchange technology, which effectively removes most of impurity ions with strong binding force in a shikimic acid pretreatment solution, further remarkably improves the treatment capacity, elution yield and purity of an anion exchange resin purification step, and further improves the product purity and yield.
The present invention is realized by the following method.
A method for efficiently extracting shikimic acid by using an ion exchange technology is characterized by comprising the following steps:
step 1) fermentation liquor pretreatment: filtering shikimic acid fermentation liquor through a ceramic membrane to remove macromolecular proteins, collecting filtrate, adding NaOH to adjust the pH value to 11-12, keeping the temperature for 2h at 50 ℃, adding concentrated sulfuric acid to adjust the pH value to 2-3, and stirring for 15-20 min;
step 2) flocculation precipitation filtration: adding EDTA to complex divalent cations, flocculating for 2-3h, and filtering with a plate frame;
step 3), activated carbon decolorization: adding 0.5-2% (w/v) active carbon into the filtrate, stirring at 50-55 deg.C for decolorizing for 2-2.5h, and filtering with plate-frame filter; adding 0.5-2% (w/v) active carbon into the filtrate for secondary decolorization, stirring at 50-55 deg.C for decolorizing for 2-2.5h, filtering with plate frame, and collecting filtrate;
step 4) continuous ion exchange: the filtrate is fed forward through a cation column at the feed flow rate of 1100-1300L/h, after the feeding is finished, washing is started at the water flow rate of 1700-1900L/h, and the effluent is collected when the pH of the effluent reaches 2.5-2.8; washing the effluent liquid with water after passing through anion resin, wherein the initial flow is 1200-1500L/h, the later adjustable flow is 1500-1800L/h, and washing with water until no impurities exist in the anion resin column; eluting the anion resin column by using 3 percent NaOH, controlling the flow rate to be 1800 plus 2000L/h, starting to collect the analysis liquid when determining whether the effluent liquid of the resin column contains the analysis liquid, enabling the flow rate of the analysis liquid to be 1800 plus 2000L/h to sequentially pass through the activated cation resin column, and starting to collect the acidizing liquid when the pH value of a liquid outlet is less than or equal to 4; after the analytic solution passes through the cation column, continuing washing the cation resin column with water, stopping collecting after the pH is more than 4, and combining the washing solution and the acidizing solution to obtain a mixed solution;
step 5) concentration and crystallization: concentrating the mixed solution by 2-3 times, adding alcohol with alcohol degree of 65%, adding 2-3 times of the volume of the concentrated solution, stirring for 30min after adding materials, controlling the crystallization temperature to be less than or equal to 10 ℃, crystallizing for 24-48 h, filtering when centrifuging for 30min, fully leaching the crystal material by using 95% alcohol, then centrifugally drying, collecting shikimic acid crystals, and recovering alcohol;
step 6) centrifugal drying: stirring and centrifuging shikimic acid crystals for 40-60min to obtain shikimic acid wet product, and vacuum drying the wet product to obtain shikimic acid finished product.
Preferably, the first and second liquid crystal display panels are,
in the step 1), the aperture of the ceramic film is 100-200 nm.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), NaOH is added to adjust the pH value to 11.5.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), concentrated sulfuric acid is added to adjust the pH value to 2.5-2.8.
Preferably, the first and second electrodes are formed of a metal,
the addition amount of the EDTA is 0.1-0.2% (w/v).
Preferably, the first and second electrodes are formed of a metal,
in the step 5), the concentration conditions are as follows: 0.1-0.15MPa, concentration temperature less than or equal to 65 ℃, vacuum degree more than or equal to-0.075 MPa, and concentration for 4-5 h.
Preferably, the first and second electrodes are formed of a metal,
in the step 5), the crystallization time is 36 hours.
Preferably, the first and second liquid crystal display panels are,
in the step 6), the drying temperature is 60-70 ℃, the vacuum degree is more than or equal to-0.075 MPa, one-time stirring work is carried out at intervals of 4 hours, and the water content control requirement is less than or equal to 1.3 percent.
The beneficial effects achieved by the invention mainly comprise but are not limited to the following aspects:
1. the technical method has the advantages of high product purity and high extraction yield, realizes the continuity and automation of the production process, greatly improves the production efficiency, reduces the production cost, and is suitable for large-scale industrial production.
2. The process adopts continuous ion exchange technology, removes a large amount of impurity ions with strong binding force in the fermentation liquor, improves the product purity, can realize regeneration of resin used by the technology, avoids waste, and can greatly reduce the extraction cost of the shikimic acid.
3. The 65% alcohol is used for assisting crystallization and the 95% alcohol is used for growing crystals, the alcohol used in the process can be completely recovered, and the process can enter the shikimic acid production process again after the distillation reaches the required index, so that the repeated use of the alcohol is realized.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the following will fully describe the technical solutions in conjunction with the specific embodiments of the present application.
Example 1
A method for efficiently extracting shikimic acid by ion exchange technology comprises the following specific steps:
step 1) fermentation liquor pretreatment: filtering shikimic acid fermentation liquor through a ceramic membrane with the aperture of 200nm to remove macromolecular proteins, collecting filtrate, adding NaOH to adjust the pH value to 11.5, preserving the heat at 50 ℃ for 2h, then adding concentrated sulfuric acid to adjust the pH value to 2.5, and stirring for 15 min.
Step 2) flocculation precipitation filtration: after the shikimic acid fermentation liquor is pretreated, 0.15 percent of EDTA is added to complex divalent cations, and after flocculation is carried out for 2 hours, plate-and-frame filtration is carried out.
Step 3), activated carbon decolorization: adding 1% of active carbon into the filtrate, stirring and decolorizing at 50 deg.C for 2-2.5h, and filtering with plate-frame filter; adding 1% of active carbon into the filtrate for secondary decolorization, stirring and decolorizing at 50 ℃ for 2.5h, and filtering by a plate frame, wherein the transmittance of the filtrate is over 97%.
Step 4) continuous ion exchange: the filtrate is fed forward through a cation column at the feed flow rate of 1100-1300L/h, after the feeding is finished, washing is started at the water flow rate of 1700-1900L/h, and the effluent is collected when the pH of the effluent reaches 2.5-2.8; and washing the effluent liquid with water after passing through the anion resin, wherein the initial flow is 1200-1500L/h, the later period adjustable flow is 1500-1800L/h, and washing with water until no impurities exist in the anion resin column. Eluting the anion resin column by using 3 percent NaOH, controlling the flow rate to be 1800 plus 2000L/h, starting to collect the analysis liquid when determining whether the effluent liquid of the resin column contains the analysis liquid, enabling the flow rate of the analysis liquid to be 1800 plus 2000L/h to sequentially pass through the activated cation resin column, and starting to collect the acidizing liquid when the pH value of a liquid outlet is less than or equal to 4; and (4) after the analytic solution passes through the cation column, continuing washing the cation resin column with water, stopping collecting after the pH value is more than 4, and combining the washing solution and the acidizing solution for subsequent concentration.
Step 5) concentration and crystallization: the mixture was concentrated 2.5 times, the concentrator steam pressure: 0.1-0.15MPa, the concentration temperature is less than or equal to 65 ℃, the vacuum degree is more than or equal to-0.075 MPa, the concentration is carried out for 4h, alcohol with the alcohol degree of 65% is added, the adding amount is 2.5 times of the volume of the concentrated solution, the stirring is completed after the feeding is finished for 30min, the crystallization temperature is controlled to be less than or equal to 10 ℃, the crystallization time is 36 h, the filtration is carried out when the centrifugation is carried out for 30min, and the centrifugal drying is carried out after the crystal material is fully leached by using 95% alcohol.
Step 6) centrifugal drying: stirring and centrifuging shikimic acid crystals for 40min to obtain shikimic acid wet product, and vacuum drying the wet product to obtain shikimic acid finished product. The drying temperature is 60 ℃, the vacuum degree is more than or equal to-0.075 MPa, one-time material turning operation is carried out at intervals of 4 hours, and the water content control requirement is less than or equal to 1.3 percent. The test shows that the purity of shikimic acid product is above 99.9%, and the yield of shikimic acid is 90.4%.
Example 2
A method for efficiently extracting shikimic acid by ion exchange technology comprises the following specific steps:
step 1) fermentation liquor pretreatment: filtering shikimic acid fermentation liquor through a ceramic membrane with the aperture of 100nm to remove macromolecular proteins, collecting filtrate, adding NaOH to adjust the pH value to 11.5, preserving the heat at 50 ℃ for 2h, then adding concentrated sulfuric acid to adjust the pH value to 2.8, and stirring for 20 min.
Step 2) flocculation precipitation filtration: after the shikimic acid fermentation liquor is pretreated, 0.15 percent of EDTA is added to complex divalent cations, and after flocculation is carried out for 3 hours, plate-and-frame filtration is carried out.
Step 3), activated carbon decolorization: adding 1% of active carbon into the filtrate, stirring and decolorizing at 55 deg.C for 2-2.5h, and filtering with plate-frame filter; adding 1% of activated carbon into the filtrate for secondary decolorization, stirring and decolorizing at 55 ℃ for 2.5h, and filtering by a plate frame, wherein the transmittance of the filtrate is over 97%.
Step 4) continuous ion exchange: the filtrate is fed forward through a cation column at the feed flow rate of 1100-1300L/h, after the feeding is finished, water washing is started at the water washing flow rate of 1700-1900L/h, and the effluent is collected when the pH of the effluent reaches 2.5-2.8; and washing the effluent liquid with water after passing through the anion resin, wherein the initial flow is 1200-1500L/h, the later period adjustable flow is 1500-1800L/h, and washing with water until no impurities exist in the anion resin column. Eluting the anion resin column by using 3 percent NaOH, controlling the flow rate to be 1800 plus 2000L/h, starting to collect the analysis liquid when determining whether the effluent liquid of the resin column contains the analysis liquid, enabling the flow rate of the analysis liquid to be 1800 plus 2000L/h to sequentially pass through the activated cation resin column, and starting to collect the acidizing liquid when the pH value of a liquid outlet is less than or equal to 4; and (4) after the analytic solution passes through the cation column, continuing washing the cation resin column with water, stopping collecting after the pH value is more than 4, and combining the washing solution and the acidizing solution for subsequent concentration.
Step 5) concentration and crystallization: the mixture was concentrated 2.5 times, the concentrator steam pressure: 0.1-0.15MPa, the concentration temperature is less than or equal to 65 ℃, the vacuum degree is more than or equal to-0.075 MPa, the concentration is carried out for 4-5h, alcohol with the alcohol degree of 65% is added, the adding amount is 2.5 times of the volume of the concentrated solution, the stirring is completed after the feeding is finished for 30min, the crystallization temperature is controlled to be less than or equal to 10 ℃, the crystallization time is 36 h, the filtration is carried out when the centrifugation is carried out for 30min, and the centrifugal drying is carried out after the crystal material is fully leached by using 95% alcohol.
Step 6) centrifugal drying: stirring and centrifuging shikimic acid crystals for 60min to obtain shikimic acid wet product, and vacuum drying the wet product to obtain shikimic acid finished product. The drying temperature is 70 ℃, the vacuum degree is more than or equal to-0.075 MPa, one-time material turning operation is carried out at intervals of 4 hours, and the water content control requirement is less than or equal to 1.3 percent. The test shows that the purity of shikimic acid products reaches over 99.9 percent, and the yield of shikimic acid is 90.1 percent.
While the invention has been described with reference to specific embodiments, it will be apparent to those skilled in the art that the invention is not limited thereto, and that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (8)
1. A method for efficiently extracting shikimic acid by using an ion exchange technology is characterized by comprising the following steps:
step 1) fermentation liquor pretreatment: filtering shikimic acid fermentation liquor through a ceramic membrane to remove macromolecular proteins, collecting filtrate, adding NaOH to adjust the pH value to 11-12, keeping the temperature for 2h at 50 ℃, adding concentrated sulfuric acid to adjust the pH value to 2-3, and stirring for 15-20 min;
step 2) flocculation precipitation filtration: adding EDTA to complex divalent cations, flocculating for 2-3h, and filtering with a plate frame;
step 3), activated carbon decolorization: adding 0.5-2% (w/v) active carbon into the filtrate, stirring at 50-55 deg.C for decolorizing for 2-2.5h, and filtering with plate-frame filter; adding 0.5-2% (w/v) active carbon into the filtrate for secondary decolorization, stirring at 50-55 deg.C for decolorizing for 2-2.5h, filtering with plate frame, and collecting filtrate;
step 4) continuous ion exchange: the filtrate is fed forward through a cation column at the feed flow rate of 1100-1300L/h, after the feeding is finished, washing is started at the water flow rate of 1700-1900L/h, and the effluent is collected when the pH of the effluent reaches 2.5-2.8; washing the effluent liquid with water after passing through anion resin, wherein the initial flow is 1200-1500L/h, the later adjustable flow is 1500-1800L/h, and washing with water until no impurities exist in the anion resin column; eluting the anion resin column by using 3 percent NaOH, controlling the flow rate to be 1800 plus 2000L/h, starting to collect the analysis liquid when determining whether the effluent liquid of the resin column contains the analysis liquid, enabling the flow rate of the analysis liquid to be 1800 plus 2000L/h to sequentially pass through the activated cation resin column, and starting to collect the acidizing liquid when the pH value of a liquid outlet is less than or equal to 4; after the analytic solution passes through the cation column, continuing washing the cation resin column with water, stopping collecting after the pH is more than 4, and combining the washing solution and the acidizing solution to obtain a mixed solution;
step 5) concentration and crystallization: concentrating the mixed solution by 2-3 times, adding alcohol with alcohol degree of 65%, adding 2-3 times of the volume of the concentrated solution, stirring for 30min after adding materials, controlling the crystallization temperature to be less than or equal to 10 ℃, crystallizing for 24-48 h, filtering when centrifuging for 30min, fully leaching the crystal material by using 95% alcohol, then centrifugally drying, collecting shikimic acid crystals, and recovering alcohol;
step 6) centrifugal drying: stirring and centrifuging shikimic acid crystals for 40-60min to obtain shikimic acid wet product, and vacuum drying the wet product to obtain shikimic acid finished product.
2. The method as claimed in claim 1, wherein in step 1), the ceramic membrane has a pore size of 100-200 nm.
3. The method as claimed in claim 1, wherein in step 1), NaOH is added to adjust the pH to 11.5.
4. The method of claim 1, wherein in step 1), concentrated sulfuric acid is added to adjust the pH to 2.5-2.8.
5. The method according to claim 1, wherein the EDTA is added in an amount of 0.1-0.2% (w/v).
6. The method according to claim 1, wherein in the step 5), the concentration conditions are as follows: 0.1-0.15MPa, concentration temperature less than or equal to 65 ℃, vacuum degree more than or equal to-0.075 MPa, and concentration for 4-5 h.
7. The method according to claim 1, wherein in the step 5), the crystallization time is 36 hours.
8. The method as claimed in claim 1, wherein in the step 6), the drying temperature is 60-70 ℃, the vacuum degree is more than or equal to-0.075 MPa, the material turning operation is carried out once every 4 hours, and the water content control requirement is less than or equal to 1.3%.
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| WO2024117718A1 (en) * | 2022-11-28 | 2024-06-06 | 주식회사 엠퍼플 | Method for extracting shikimic acid by using conifers |
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| US20160176799A1 (en) * | 2014-12-19 | 2016-06-23 | Board Of Trustees Of Michigan State University | Isolation and purification of shikimic acid |
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| WO2024117718A1 (en) * | 2022-11-28 | 2024-06-06 | 주식회사 엠퍼플 | Method for extracting shikimic acid by using conifers |
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