Method for decolorizing and extracting high-purity Ecodoine based on adsorption column
By using adsorption column decolorization technology, the problems of low product yield and purity in activated carbon decolorization technology have been solved, achieving efficient extraction and purification of edodecanin, reducing costs and solid waste, and making it suitable for the cosmetics and pharmaceutical fields.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHANGHAI INST OF TECH
- Filing Date
- 2026-01-16
- Publication Date
- 2026-05-12
AI Technical Summary
In existing icotin extraction processes, activated carbon decolorization technology suffers from problems such as reduced product yield, low purity, high cost, and poor environmental performance due to non-selective adsorption.
Adsorption column decolorization technology was employed, using D101 macroporous adsorption resin and XAD-7 macroporous weakly polar adsorption resin to replace activated carbon, combined with nanofiltration, cation exchange column and crystallization process to achieve efficient extraction and purification of edodecanin.
It significantly improves the total yield and purity of ecochoride, reduces consumable costs, reduces solid waste generation, meets the needs of high-purity applications, and the decolorizing resin is recyclable and reusable, taking into account both economic efficiency and environmental protection.
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Figure CN122010849A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of chemical technology and relates to a method for extracting high-purity etordin based on adsorption column decolorization. Background Technology
[0002] Ectodextrin, also known as tetrahydropyrimidine or tetrahydromethylpyrimidine carboxylic acid, is an amino acid derivative found in microorganisms and belongs to the cyclic amino acid family. Ectodextrin is an active ingredient with comprehensive cellular protection, effectively inhibiting the cellular aging process and promoting the repair and regeneration of aging or damaged skin. Furthermore, ectodextrin exhibits significant antioxidant, anti-radiation, and moisturizing properties, effectively resisting damage caused by ultraviolet rays and achieving a noticeable whitening effect. It is commonly used in cosmetics.
[0003] The efficiency, product purity, and economic viability of the industrial extraction process for edodecanine directly determine its industrialization value. In existing edodecanine extraction processes, activated carbon decolorization is commonly used in the decolorization stage, but this technology has the following drawbacks: 1. Activated carbon adsorption is non-selective. While adsorbing impurities such as pigments in the adsorption system, it can also adsorb some of the target product due to polarity and similar molecular structure, resulting in a decrease in product yield. 2. Activated carbon is in powder form, and an additional filtration and carbon removal step is required after decolorization. This not only prolongs the process and increases the risk of human contamination, but also makes it easy for residual carbon powder to affect the purity of the product, making it difficult to meet the requirements of high-purity application scenarios. 3. Activated carbon is a disposable consumable that needs to be treated as solid waste after use. Long-term use results in high consumable costs and does not meet environmental protection requirements. 4. Activated carbon decolorization requires stirring and filtration, which is incompatible with the pre-column operation system in the icotin extraction process, requiring additional equipment.
[0004] Therefore, developing other high-purity ecodyl extraction processes has significant economic value and importance. Summary of the Invention
[0005] The purpose of this invention is to provide a method for extracting high-purity ecochorein based on adsorption column decolorization. This invention replaces activated carbon decolorization with adsorption column decolorization, avoiding the non-selective adsorption of ecochorein by activated carbon, significantly increasing the total yield, and eliminating carbon powder residue. This results in a significant increase in product purity, meeting the requirements for high-purity applications. Furthermore, the decolorizing resin is regenerable and reusable after use. Replacing disposable activated carbon with decolorizing resin reduces consumable costs and solid waste generation, achieving both economic efficiency and environmental friendliness. Moreover, adsorption column decolorization is compatible with the preceding column operation system, requiring no additional equipment investment, and has high industrial application prospects.
[0006] The objective of this invention can be achieved through the following technical solutions: A method for extracting high-purity ectoine based on adsorption column decolorization includes: centrifuging the raw material liquid containing ectoine once and taking the supernatant, heating it, centrifuging it a second time and taking the supernatant, and then sequentially passing it through nanofiltration, concentration, adsorption column treatment, cation exchange column treatment, elution, adsorption column decolorization treatment, and crystallization drying to obtain the final product.
[0007] In some specific embodiments, during the centrifugation, the centrifugation speed is 7500-8500 rpm, the centrifugation temperature is 8-12℃, and the centrifugation time is 25-35 min.
[0008] In some specific embodiments, the heating temperature is 90-100℃ and the heating time is 25-35min.
[0009] In some specific embodiments, during the secondary centrifugation, the centrifugation speed is 8000-10000 rpm, the centrifugation temperature is 20-25℃, and the centrifugation time is 15-25 min.
[0010] In some specific embodiments, the nanofiltration process involves a nanofiltration membrane with a molecular weight cutoff of 500-1000 Da, a filtration operating pressure of 0.3-0.5 MPa, and a temperature of 25-30°C; the concentration process involves a vacuum of 0.08-0.09 MPa, a temperature of 45-55°C, and concentration to a coumarin content of 100-150 g / L.
[0011] In some specific embodiments, during the adsorption column treatment, the pH of the concentrate is 1.8-2.2, the adsorption resin used is D101 macroporous adsorption resin, and the flow rate is 1-2 BV / h.
[0012] In some specific embodiments, the cation exchange column treatment uses a 732 type strong acid styrene-based cation exchange resin, with an ecodyl adsorption capacity of 75-80 g per liter of wet resin and a flow rate of 0.8-1.2 BV / h.
[0013] In some specific embodiments, the elution process uses a 0.18-0.22 mol / L NaOH solution at a flow rate of 0.5-1 BV / h, and the eluent is collected to control the elution yield of ecoxib to be ≥85%.
[0014] In some specific embodiments, the resin used in the adsorption column decolorization treatment is XAD-7 macroporous weakly polar adsorption resin, and the flow rate is 0.8-2 BV / h.
[0015] In some specific embodiments, the regeneration method of the resin used in the decolorization treatment of the adsorption column is as follows: the resin is eluted with 0.5-0.8 mol / L NaOH solution at a flow rate of 1 BV / h for 3-4 BV, and then rinsed with purified water until the pH of the effluent is 6.5-7.5, and the solution is reused 10-20 times.
[0016] In some specific embodiments, the crystallization includes mixing methanol with the clear liquid obtained from the adsorption column decolorization treatment at a volume ratio of 3-5:1, allowing it to stand at 0-5°C for 12-24 hours to crystallize, and then vacuum drying at a vacuum degree of 0.09-0.1 MPa and a temperature of 40-50°C.
[0017] Compared with the prior art, the present invention has the following beneficial effects: This invention replaces activated carbon decolorization with adsorption column decolorization, avoiding the non-selective adsorption of ecochoride by activated carbon, significantly improving the total yield, and eliminating the problem of carbon powder residue. This results in a significant increase in product purity, meeting the requirements of high-purity applications. Furthermore, the decolorizing resin is regenerable and reusable, replacing disposable activated carbon, which reduces consumable costs and solid waste generation, balancing economic efficiency and environmental protection. The adsorption column decolorization is compatible with the preceding column operation system, requiring no additional equipment investment. Attached Figure Description
[0018] Figure 1 This is a process flow diagram of a method for extracting high-purity etordine based on adsorption column decolorization in this invention; Figure 2 This is a comparison chart of the total yield of ecochuoyin obtained by the method of decolorizing and extracting high-purity ecochuoyin based on adsorption column in Examples 1-3; Figure 3 This is a comparison chart of the purity of ecochuoyin products obtained by a method for extracting high-purity ecochuoyin based on adsorption column decolorization in Examples 1-3. Figure 4 This is a comparison chart of the decolorization rate of ecochordine extraction obtained by a method based on adsorption column decolorization for extracting high-purity ecochordine in Examples 1-3; Figure 5 The images show a comparison of the residual solid impurities in ecochorein extracted using a method based on adsorption column decolorization to extract high-purity ecochorein in Examples 1-3. Detailed Implementation
[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0020] The ectoin fermentation broth used in the following examples and comparative examples was prepared from the ECT-9 glycerol bacterium disclosed in Example 4 of Chinese Invention Patent No. CN114134127A (Diaminobutyric acid acetyltransferase mutant for synthesizing ectoin).
[0021] Materials and Methods LB medium: 10 g / L tryptone, 5 g / L yeast extract, 10 g / L sodium chloride, pH 7.2. (LB solid medium with an additional 20 g / L agar powder.) Fermentation tank culture medium: Solution A: 0.1 g / L magnesium sulfate, 100 g / L glucose, autoclaved at 121℃ for 20 min; Solution B: 10 g / L ammonium sulfate, 35 g / L yeast extract, 0.01 g FeSO4 7H2O, 0.1 g / L sodium citrate, 0.25 ml / L H3PO4 (85%), and 0.5 g / L defoamer were autoclaved at 121°C for 30 min together with the fermenter. Solution C contained: 0.06 g / L calcium pantothenate, 0.018 g / L vitamin PP, and 0.05 g / L thiamin. HCl and 0.05 g / L biotin were filtered and sterilized before being added to the fermenter during inoculation.
[0022] Feeding medium: 670 g / L glucose, 10 g / L ammonium sulfate (sterilized separately), 2 ml / L antifoaming agent.
[0023] Fermentation conditions: Pick ECT9 single clones from LB plates and transfer them to LB shake flasks. Incubate at 30°C and 220 rpm for about 14 hours. Inoculate 5 v / v% into a 5 L fermenter. Fermentation temperature: 30°C. Dissolved oxygen: 30%. pH: 7.0: 25% ammonia. Fermentation is terminated after 64 hours.
[0024] Chromatographic conditions for HPLC detection of ectoine in the supernatant after centrifugation of fermentation broth: AQ-C18 column; mobile phase: 90% 5mM potassium dihydrogen phosphate, 10% acetonitrile; detection wavelength: 210nm.
[0025] Example 1: A method for extracting high-purity ecoxib based on adsorption column decolorization, such as... Figure 1 As shown, it includes the following steps: Step 1, Collection of supernatant from fermentation broth: Centrifuge the erythromycin fermentation broth and collect the supernatant. The centrifugation conditions are: centrifugation speed 8000 rpm, temperature 10℃, and centrifugation time 30 min. Step 2, heat treatment: Heat the supernatant collected in Step 1 at 95℃ for 30 minutes; Step 3, centrifugation to remove impurities: The supernatant after heating in Step 2 is centrifuged again, and the clear liquid is collected. The centrifugation conditions are: centrifugation speed 9000 rpm, temperature 22℃, and centrifugation time 20 min. Step 4, nanofiltration: The clear liquid collected in step 3 is filtered through a nanofiltration membrane, and the permeate is collected. The filtration process uses a nanofiltration membrane with a molecular weight cutoff of 1000 Da, a filtration pressure of 0.4 MPa, and a temperature of 28°C. Step 5, Concentration treatment: The nanofiltration permeate collected in Step 4 is concentrated by vacuum rotary evaporation. The concentration is carried out under vacuum of 0.08 MPa and temperature of 50°C until the ecoxib content is 125 g / L, and the concentrate is obtained. Step 6, Adsorption column treatment: Add 1.5 mol / L H2SO4 solution to the concentrate obtained in step 5, adjust the pH to 2, and then pass the adjusted concentrate through an adsorption resin column of D101 macroporous adsorption resin at a flow rate of 1.5 BV / h, and collect the effluent. Step 7, Cation Exchange Column Treatment: Pass the effluent collected in Step 6 through a cation exchange resin column packed with 2L of 732 type strong acid styrene cation exchange resin at a flow rate of 1BV / h, based on the adsorption capacity of 78g of ecodyl per liter of wet resin. Step 8, elution treatment: Pass a 0.2 mol / L NaOH solution into the cation exchange resin column from Step 7, elute at a flow rate of 0.8 BV / h, collect the eluent, and control the elution yield of ecoxib to be ≥85%; Step 9, Decolorization of the adsorption column: Pass the eluent collected in Step 8 through a decolorizing resin column of XAD-7 macroporous weakly polar adsorption resin at a flow rate of 1 BV / h, and collect the clear liquid after decolorization. The regeneration method of the decolorizing resin column is as follows: Elute the resin with 0.6 mol / L NaOH solution at a flow rate of 1 BV / h for 3 BV, then rinse with purified water until the pH of the effluent is 7, and repeat 15 times. Step 10, Crystallization and Drying: Anhydrous methanol is added to the decolorized clear liquid collected in Step 9 at a volume ratio of 4:1 to anhydrous methanol. The liquid is allowed to stand and crystallize for 20 hours at 3°C. After filtration, the crystals are collected and vacuum dried to constant weight at a vacuum degree of 0.09 MPa and a temperature of 45°C to obtain the finished product, Ecodone.
[0026] Example 2: A method for extracting high-purity ecoxib based on adsorption column decolorization includes the following steps: Step 1, Collection of supernatant from fermentation broth: Centrifuge the erythromycin fermentation broth and collect the supernatant. The centrifugation conditions are: centrifugation speed 7500 rpm, temperature 8℃, and centrifugation time 25 min. Step 2, heat treatment: Heat the supernatant collected in Step 1 at 90℃ for 25 minutes; Step 3, centrifugation to remove impurities: The supernatant after heating in Step 2 is centrifuged again, and the clear liquid is collected. The centrifugation conditions are: centrifugation speed 8000 rpm, temperature 20℃, and centrifugation time 15 min. Step 4, nanofiltration: The clear liquid collected in step 3 is filtered through a nanofiltration membrane, and the permeate is collected. The filtration process uses a nanofiltration membrane with a molecular weight cutoff of 1000 Da, the filtration pressure is 0.3 MPa, and the temperature is 25°C. Step 5, Concentration treatment: The nanofiltration permeate collected in Step 4 is concentrated by distillation using a rotary evaporator under reduced pressure. The concentration is carried out at a vacuum of 0.08 MPa and a temperature of 45°C until the ecoxib content is 100 g / L, thus obtaining the concentrate. Step 6, Adsorption column treatment: Add 1 mol / L H2SO4 solution to the concentrate obtained in step 5, adjust the pH to 1.8, and then pass the adjusted concentrate through an adsorption resin column of D101 macroporous adsorption resin at a flow rate of 1 BV / h, and collect the effluent. Step 7, Cation Exchange Column Treatment: The effluent collected in Step 6 is passed through a cation exchange resin column packed with 2L of 732 type strong acid styrene cation exchange resin at a flow rate of 0.8 BV / h. The amount of ecodyl adsorbed per liter of wet resin is 75g. Step 8, Elution: Pass a 0.18 mol / L NaOH solution into the cation exchange resin column from Step 7, elute at a flow rate of 0.5 BV / h, collect the eluent, and control the elution yield of ecoxib to be ≥85%; Step 9, Decolorization of the adsorption column: Pass the eluent collected in Step 8 through a decolorizing resin column of XAD-7 macroporous weakly polar adsorption resin at a flow rate of 1.5 BV / h. Collect the clear liquid after decolorization. The regeneration method of the decolorizing resin column is as follows: Elute the resin with 0.5 mol / L NaOH solution at a flow rate of 1 BV / h for 3.4 BV, then rinse with purified water until the pH of the effluent is 7. Repeat the process 15 times. Step 10, Crystallization and Drying: Anhydrous methanol is added to the decolorized clear liquid collected in Step 9 at a volume ratio of 3:1 to anhydrous methanol. The liquid is allowed to stand and crystallize for 12 hours at 0°C. After filtration, the crystals are collected and vacuum dried to constant weight at a vacuum degree of 0.09 MPa and a temperature of 40°C to obtain the finished product, Ecodone.
[0027] Example 3: A method for extracting high-purity ecoxib based on adsorption column decolorization includes the following steps: Step 1, Collection of supernatant from fermentation broth: Centrifuge the erythromycin fermentation broth and collect the supernatant. The centrifugation conditions are: centrifugation speed 8500 rpm, temperature 12℃, and centrifugation time 35 min. Step 2, heat treatment: Heat the supernatant collected in Step 1 at 100℃ for 35 minutes; Step 3, centrifugation to remove impurities: The supernatant after heating in Step 2 is centrifuged again, and the clear liquid is collected. The centrifugation conditions are: centrifugation speed 10000 rpm, temperature 25℃, and centrifugation time 25 min. Step 4, nanofiltration: The clear liquid collected in step 3 is filtered through a nanofiltration membrane, and the permeate is collected. The filtration process uses a nanofiltration membrane with a molecular weight cutoff of 1000 Da, a filtration pressure of 0.5 MPa, and a temperature of 30°C. Step 5, Concentration treatment: The nanofiltration permeate collected in Step 4 is concentrated by rotary evaporation under reduced pressure. The concentration is carried out at a vacuum of 0.09 MPa and a temperature of 55°C until the ecoxib content is 150 g / L, and the concentrate is obtained. Step 6, Adsorption column treatment: Add 2 mol / L H2SO4 solution to the concentrate obtained in step 5, adjust the pH to 2.2, and then pass the adjusted concentrate through an adsorption resin column of D101 macroporous adsorption resin at a flow rate of 2 BV / h, and collect the effluent. Step 7, Cation exchange column treatment: The effluent collected in Step 6 is passed through a cation exchange resin column packed with 2L of 732 type strong acid styrene cation exchange resin at a flow rate of 1.2 BV / h. The amount of ecodyl adsorbed per liter of wet resin is 80g. Step 8, elution treatment: Pass a 0.22 mol / L NaOH solution into the cation exchange resin column from Step 7, elute at a flow rate of 1.0 BV / h, collect the eluent, and control the elution yield of ecoxib to be ≥85%; Step 9, Decolorization of the adsorption column: Pass the eluent collected in Step 8 through a decolorizing resin column of XAD-7 macroporous weakly polar adsorption resin at a flow rate of 2 BV / h. Collect the clear liquid after decolorization. The regeneration method of the decolorizing resin column is as follows: Elute the resin with 0.8 mol / L NaOH solution at a flow rate of 1 BV / h for 4 BV, then rinse with purified water until the pH of the effluent is 7.5. Repeat the process 20 times. Step 10, Crystallization and Drying: Anhydrous methanol is added to the decolorized clear liquid collected in Step 9 at a volume ratio of 5:1 to anhydrous methanol. The liquid is allowed to stand and crystallize for 24 hours at 5°C. After filtration, the crystals are collected and vacuum dried to constant weight at a vacuum degree of 0.1 MPa and a temperature of 50°C to obtain the finished product, Ecodone.
[0028] Comparative Example 1: Referring to the process of Example 1, only the adsorption column decolorization treatment in step nine is replaced with activated carbon decolorization. Specifically, 1.5% (w / v, g / mL) activated carbon is added to the eluent, the mixture is stirred and decolorized for 1 hour, the carbon is removed by filtration, and the clear liquid after decolorization is collected.
[0029] Comparative Example 2: Referring to the process of Example 1, only the XAD-7 macroporous weakly polar adsorption resin used in step nine was replaced with HPD-400 macroporous strongly polar decolorizing resin.
[0030] The properties of each embodiment and comparative example are compared in Table 1: Table 1 Comparison of total yield of edodecanin extraction like Figure 2 As shown, the overall yields of Examples 1-3 of the present invention were 89.2%, 85.3%, and 90.5%, respectively, which were significantly higher than 80.1% of Comparative Example 1 (activated carbon decolorization) and 78.6% of Comparative Example 2 (strong polar resin decolorization). Among them, Example 3 achieved the highest yield of 90.5% under conditions of higher centrifugal head speed (10000 rpm), higher concentration (150 g / L), and better decolorization flow rate (2 BV / h), indicating that the process of the present invention has a significant advantage in improving product recovery rate.
[0031] Comparison of the purity of edodeoxyn products from Figure 3 As can be seen, the purities of the products in Examples 1-3 were 98.5%, 97.8%, and 99.1%, respectively, all higher than those in Comparative Example 1 (95.2%) and Comparative Example 2 (96.8%). Example 3 had the highest purity (99.1%), and its process conditions included a heating temperature of 100℃, an elution NaOH concentration of 0.22 mol / L, and low-temperature crystallization (5℃). This indicates that the optimized operating parameters are beneficial to improving product purity and meeting the requirements for high-purity applications.
[0032] Decolorization rate comparison Figure 4 The results show that the decolorization rates of Examples 1-3 were 92.0%, 89.5%, and 93.2%, respectively, which were higher than those of Comparative Example 1 (82.3%) and Comparative Example 2 (90.1%). Example 3 showed the best decolorization effect, which is related to its use of a higher regenerated alkali concentration (0.8 mol / L) and a longer number of regeneration cycles (20 times), indicating that the weakly polar resin (XAD-7) used in this invention performs excellently in terms of decolorization efficiency and stability.
[0033] Comparison of solid impurity residues Depend on Figure 5It can be seen that the solid impurity residue in Examples 1-3 is all below 0.08%, with Example 3 having the lowest (<0.03%), while Comparative Example 1 (activated carbon decolorization) has an impurity residue of 0.21%. This indicates that the resin decolorization process can effectively avoid the problem of carbon powder residue, significantly reduce the content of solid impurities, and is beneficial for the application of subsequent products in high-requirement fields such as pharmaceuticals and cosmetics.
[0034] Based on the above, the advantages of this invention are as follows: when used, it replaces activated carbon decolorization with a weakly polar adsorption column, completely avoiding the non-selective adsorption of ecochorine by activated carbon, stabilizing the total yield at 85.3%-90.5%, while avoiding the problem of carbon powder residue. The product purity reaches 97.8%-99.1%, meeting the high purity requirements of cosmetics and pharmaceuticals. The decolorizing resin can be recycled and reused, the consumable cost is lower than that of disposable activated carbon, and the amount of solid waste generated is less, taking into account both economic efficiency and environmental protection. The process is fully compatible with the column operation system of the preceding adsorption column and cation exchange column, requiring no additional equipment investment, and the operation steps are simpler than activated carbon decolorization.
[0035] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
Claims
1. A method for extracting high-purity etordine based on adsorption column decolorization, characterized in that, The method includes: centrifuging the raw material liquid containing ectoine once and taking the supernatant, heating it, centrifuging it a second time and taking the supernatant, and then sequentially passing it through nanofiltration, concentration, adsorption column treatment, cation exchange column treatment, elution, adsorption column decolorization treatment, and crystallization drying to obtain the final product.
2. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the first centrifugation, the centrifugation speed was 7500-8500 rpm, the centrifugation temperature was 8-12℃, and the centrifugation time was 25-35 min.
3. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the heat treatment, the heating temperature is 90-100℃ and the heating time is 25-35min.
4. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the secondary centrifugation, the centrifugation speed is 8000-10000 rpm, the centrifugation temperature is 20-25℃, and the centrifugation time is 15-25 min.
5. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the nanofiltration process, the nanofiltration membrane has a molecular weight cutoff of 500-1000 Da, the filtration operating pressure is 0.3-0.5 MPa, and the temperature is 25-30℃; in the concentration process, the vacuum degree is 0.08-0.09 MPa, and the temperature is 45-55℃.
6. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the adsorption column treatment, the pH of the concentrate is 1.8-2.2, the adsorption resin used is D101 macroporous adsorption resin, and the flow rate is 1-2 BV / h.
7. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the cation exchange column treatment, the cation exchange resin used is type 732 strong acid styrene-based cation exchange resin, and the flow rate is 0.8-1.2 BV / h.
8. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the elution process, the eluent used is a 0.18-0.22 mol / L NaOH solution, and the flow rate is 0.5-1 BV / h.
9. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, In the decolorization treatment of the adsorption column, the resin used is XAD-7 macroporous weakly polar adsorption resin, and the flow rate is 0.8-2 BV / h.
10. The method for extracting high-purity ecoxib based on adsorption column decolorization according to claim 1, characterized in that, The crystallization process involves mixing methanol with the clear liquid obtained from decolorization treatment by an adsorption column at a volume ratio of 3-5:1, allowing it to stand at 0-5°C for 12-24 hours to crystallize, and then vacuum drying at a vacuum degree of 0.09-0.1 MPa and a temperature of 40-50°C.
Citation Information
Patent Citations
Diaminobutyric acid acetyltransferase mutant for synthesizing Ectoine
CN114134127A